180° Peel adhesion (N/cm) from float glass for curved OLED display OCAs after varying dwell times.
\\n\\n
IntechOpen was founded by scientists, for scientists, in order to make book publishing accessible around the globe. Over the last two decades, this has driven Open Access (OA) book publishing whilst levelling the playing field for global academics. Through our innovative publishing model and the support of the research community, we have now published over 5,700 Open Access books and are visited online by over three million academics every month. These researchers are increasingly working in broad technology-based subjects, driving multidisciplinary academic endeavours into human health, environment, and technology.
\\n\\nBy listening to our community, and in order to serve these rapidly growing areas which lie at the core of IntechOpen's expertise, we are launching a portfolio of Open Science journals:
\\n\\nAll three journals will publish under an Open Access model and embrace Open Science policies to help support the changing needs of academics in these fast-moving research areas. There will be direct links to preprint servers and data repositories, allowing full reproducibility and rapid dissemination of published papers to help accelerate the pace of research. Each journal has renowned Editors in Chief who will work alongside a global Editorial Board, delivering robust single-blind peer review. Supported by our internal editorial teams, this will ensure our authors will receive a quick, user-friendly, and personalised publishing experience.
\\n\\n"By launching our journals portfolio we are introducing new, dedicated homes for interdisciplinary technology-focused researchers to publish their work, whilst embracing Open Science and creating a unique global home for academics to disseminate their work. We are taking a leap toward Open Science continuing and expanding our fundamental commitment to openly sharing scientific research across the world, making it available for the benefit of all." Dr. Sara Uhac, IntechOpen CEO
\\n\\n"Our aim is to promote and create better science for a better world by increasing access to information and the latest scientific developments to all scientists, innovators, entrepreneurs and students and give them the opportunity to learn, observe and contribute to knowledge creation. Open Science promotes a swifter path from research to innovation to produce new products and services." Alex Lazinica, IntechOpen founder
\\n\\nIn conclusion, Natalia Reinic Babic, Head of Journal Publishing and Open Science at IntechOpen adds:
\\n\\n“On behalf of the journal team I’d like to thank all our Editors in Chief, Editorial Boards, internal supporting teams, and our scientific community for their continuous support in making this portfolio a reality - we couldn’t have done it without you! With your support in place, we are confident these journals will become as impactful and successful as our book publishing program and bring us closer to a more open (science) future.”
\\n\\nWe invite you to visit the journals homepage and learn more about the journal’s Editorial Boards, scope and vision as all three journals are now open for submissions.
\\n\\nFeel free to share this news on social media and help us mark this memorable moment!
\\n\\n\\n"}]',published:!0,mainMedia:{caption:"",originalUrl:"/media/original/237"}},components:[{type:"htmlEditorComponent",content:'
After years of being acknowledged as the world's leading publisher of Open Access books, today, we are proud to announce we’ve successfully launched a portfolio of Open Science journals covering rapidly expanding areas of interdisciplinary research.
\n\n\n\nIntechOpen was founded by scientists, for scientists, in order to make book publishing accessible around the globe. Over the last two decades, this has driven Open Access (OA) book publishing whilst levelling the playing field for global academics. Through our innovative publishing model and the support of the research community, we have now published over 5,700 Open Access books and are visited online by over three million academics every month. These researchers are increasingly working in broad technology-based subjects, driving multidisciplinary academic endeavours into human health, environment, and technology.
\n\nBy listening to our community, and in order to serve these rapidly growing areas which lie at the core of IntechOpen's expertise, we are launching a portfolio of Open Science journals:
\n\nAll three journals will publish under an Open Access model and embrace Open Science policies to help support the changing needs of academics in these fast-moving research areas. There will be direct links to preprint servers and data repositories, allowing full reproducibility and rapid dissemination of published papers to help accelerate the pace of research. Each journal has renowned Editors in Chief who will work alongside a global Editorial Board, delivering robust single-blind peer review. Supported by our internal editorial teams, this will ensure our authors will receive a quick, user-friendly, and personalised publishing experience.
\n\n"By launching our journals portfolio we are introducing new, dedicated homes for interdisciplinary technology-focused researchers to publish their work, whilst embracing Open Science and creating a unique global home for academics to disseminate their work. We are taking a leap toward Open Science continuing and expanding our fundamental commitment to openly sharing scientific research across the world, making it available for the benefit of all." Dr. Sara Uhac, IntechOpen CEO
\n\n"Our aim is to promote and create better science for a better world by increasing access to information and the latest scientific developments to all scientists, innovators, entrepreneurs and students and give them the opportunity to learn, observe and contribute to knowledge creation. Open Science promotes a swifter path from research to innovation to produce new products and services." Alex Lazinica, IntechOpen founder
\n\nIn conclusion, Natalia Reinic Babic, Head of Journal Publishing and Open Science at IntechOpen adds:
\n\n“On behalf of the journal team I’d like to thank all our Editors in Chief, Editorial Boards, internal supporting teams, and our scientific community for their continuous support in making this portfolio a reality - we couldn’t have done it without you! With your support in place, we are confident these journals will become as impactful and successful as our book publishing program and bring us closer to a more open (science) future.”
\n\nWe invite you to visit the journals homepage and learn more about the journal’s Editorial Boards, scope and vision as all three journals are now open for submissions.
\n\nFeel free to share this news on social media and help us mark this memorable moment!
\n\n\n'}],latestNews:[{slug:"intechopen-supports-asapbio-s-new-initiative-publish-your-reviews-20220729",title:"IntechOpen Supports ASAPbio’s New Initiative Publish Your Reviews"},{slug:"webinar-introduction-to-open-science-wednesday-18-may-1-pm-cest-20220518",title:"Webinar: Introduction to Open Science | Wednesday 18 May, 1 PM CEST"},{slug:"step-in-the-right-direction-intechopen-launches-a-portfolio-of-open-science-journals-20220414",title:"Step in the Right Direction: IntechOpen Launches a Portfolio of Open Science Journals"},{slug:"let-s-meet-at-london-book-fair-5-7-april-2022-olympia-london-20220321",title:"Let’s meet at London Book Fair, 5-7 April 2022, Olympia London"},{slug:"50-books-published-as-part-of-intechopen-and-knowledge-unlatched-ku-collaboration-20220316",title:"50 Books published as part of IntechOpen and Knowledge Unlatched (KU) Collaboration"},{slug:"intechopen-joins-the-united-nations-sustainable-development-goals-publishers-compact-20221702",title:"IntechOpen joins the United Nations Sustainable Development Goals Publishers Compact"},{slug:"intechopen-signs-exclusive-representation-agreement-with-lsr-libros-servicios-y-representaciones-s-a-de-c-v-20211123",title:"IntechOpen Signs Exclusive Representation Agreement with LSR Libros Servicios y Representaciones S.A. de C.V"},{slug:"intechopen-expands-partnership-with-research4life-20211110",title:"IntechOpen Expands Partnership with Research4Life"}]},book:{item:{type:"book",id:"3370",leadTitle:null,fullTitle:"Radio Frequency Identification from System to Applications",title:"Radio Frequency Identification",subtitle:"from System to Applications",reviewType:"peer-reviewed",abstract:"RFID based application creates tremendous new business opportunities such as the support of independent living of elderly and disabled persons, efficient supply chains, efficient anti-counterfeiting and better environmental monitoring. RFID data management, scalable information systems, business process reengineering, and evaluating investments are emerging as significant technical challenges to applications underpinned by new developments in RFID technology. This book presents the contributions from world leading experts on the latest developments and state-of-the-art results in the RFID field to address these challenges. The book offers a comprehensive and systematic description of technologies, architectures, and methodologies of various efficient, secure, scalable, and reliable RFID and RFID based applications.",isbn:null,printIsbn:"978-953-51-1143-6",pdfIsbn:"978-953-51-6347-3",doi:"10.5772/46210",price:139,priceEur:155,priceUsd:179,slug:"radio-frequency-identification-from-system-to-applications",numberOfPages:460,isOpenForSubmission:!1,isInWos:null,isInBkci:!1,hash:"2d7aeb6d453d7f56ee45fd7fe20e8ebc",bookSignature:"Mamun Bin Ibne Reaz",publishedDate:"June 5th 2013",coverURL:"https://cdn.intechopen.com/books/images_new/3370.jpg",numberOfDownloads:61696,numberOfWosCitations:54,numberOfCrossrefCitations:42,numberOfCrossrefCitationsByBook:3,numberOfDimensionsCitations:67,numberOfDimensionsCitationsByBook:5,hasAltmetrics:1,numberOfTotalCitations:163,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"April 26th 2012",dateEndSecondStepPublish:"May 17th 2012",dateEndThirdStepPublish:"August 21st 2012",dateEndFourthStepPublish:"November 19th 2012",dateEndFifthStepPublish:"December 19th 2012",currentStepOfPublishingProcess:5,indexedIn:"1,2,3,4,5,6,7",editedByType:"Edited by",kuFlag:!1,featuredMarkup:null,editors:[{id:"129681",title:"Dr.",name:"Mamun Bin Ibne",middleName:null,surname:"Reaz",slug:"mamun-bin-ibne-reaz",fullName:"Mamun Bin Ibne Reaz",profilePictureURL:"https://mts.intechopen.com/storage/users/129681/images/system/129681.jfif",biography:"Mamun Bin Ibne Reaz was born in Bangladesh, in December 1963. He received his B.Sc. and M.Sc. degree in Applied Physics and Electronics, both from University of Rajshahi, Bangladesh, in 1985 and 1986, respectively. He received his D.Eng. degree in 2007 from Ibaraki University, Japan. He is currently a Professor in the Department of Electrical, Electronic and Systems Engineering, Universiti Kebangsaan Malaysia, Malaysia involved in teaching, research and industrial consultation. He is a Senior Associate of the Abdus Salam International Centre for Theoretical Physics (ICTP), Italy since 2008. He is also a Senior Member of IEEE. He has published extensively in the area of IC Design, Biomedical application IC and Smart Home. He is author and coauthor of more than 300 research articles in design automation, IC design for biomedical applications and Smart Home. He is also the recipient of more than 50 research grants (national and international).",institutionString:"National University of Malaysia",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"3",totalChapterViews:"0",totalEditedBooks:"2",institution:{name:"National University of Malaysia",institutionURL:null,country:{name:"Malaysia"}}}],equalEditorOne:null,equalEditorTwo:null,equalEditorThree:null,coeditorOne:null,coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"762",title:"Wireless Communication System",slug:"electrical-and-electronic-engineering-wireless-communication-system"}],chapters:[{id:"44959",title:"RFID Applications and Challenges",doi:"10.5772/53368",slug:"rfid-applications-and-challenges",totalDownloads:3989,totalCrossrefCites:1,totalDimensionsCites:4,hasAltmetrics:0,abstract:null,signatures:"Ming-Shen Jian and Jain-Shing Wu",downloadPdfUrl:"/chapter/pdf-download/44959",previewPdfUrl:"/chapter/pdf-preview/44959",authors:[{id:"5797",title:"Dr.",name:"Ming-Shen",surname:"Jian",slug:"ming-shen-jian",fullName:"Ming-Shen Jian"},{id:"157925",title:"Dr.",name:"Jain-Shing",surname:"Wu",slug:"jain-shing-wu",fullName:"Jain-Shing Wu"}],corrections:null},{id:"44994",title:"Choosing the Right RFID-Based Architectural Pattern",doi:"10.5772/54069",slug:"choosing-the-right-rfid-based-architectural-pattern",totalDownloads:2395,totalCrossrefCites:0,totalDimensionsCites:0,hasAltmetrics:1,abstract:null,signatures:"Michel Simatic",downloadPdfUrl:"/chapter/pdf-download/44994",previewPdfUrl:"/chapter/pdf-preview/44994",authors:[{id:"30022",title:"Prof.",name:"Michel",surname:"Simatic",slug:"michel-simatic",fullName:"Michel Simatic"}],corrections:null},{id:"44997",title:"An RFID Anti-Collision Algorithm Assisted by Multi-Packet Reception and Retransmission Diversity",doi:"10.5772/53906",slug:"an-rfid-anti-collision-algorithm-assisted-by-multi-packet-reception-and-retransmission-diversity",totalDownloads:2305,totalCrossrefCites:0,totalDimensionsCites:0,hasAltmetrics:0,abstract:null,signatures:"Ramiro Sámano-Robles, Neeli Prasad and Atílio Gameiro",downloadPdfUrl:"/chapter/pdf-download/44997",previewPdfUrl:"/chapter/pdf-preview/44997",authors:[{id:"34207",title:"Dr.",name:"Ramiro",surname:"Robles",slug:"ramiro-robles",fullName:"Ramiro Robles"}],corrections:null},{id:"44973",title:"Implementation of a Countermeasure to Relay Attacks for Contactless HF Systems",doi:"10.5772/53393",slug:"implementation-of-a-countermeasure-to-relay-attacks-for-contactless-hf-systems",totalDownloads:2622,totalCrossrefCites:5,totalDimensionsCites:5,hasAltmetrics:0,abstract:null,signatures:"Pierre-Henri Thevenon and Olivier Savry",downloadPdfUrl:"/chapter/pdf-download/44973",previewPdfUrl:"/chapter/pdf-preview/44973",authors:[{id:"39836",title:"Dr.",name:"Olivier",surname:"Savry",slug:"olivier-savry",fullName:"Olivier Savry"},{id:"159662",title:"Dr.",name:"Pierre-Henri",surname:"Thévenon",slug:"pierre-henri-thevenon",fullName:"Pierre-Henri Thévenon"}],corrections:null},{id:"45041",title:"Localizing with Passive UHF RFID Tags Using Wideband Signals",doi:"10.5772/53769",slug:"localizing-with-passive-uhf-rfid-tags-using-wideband-signals",totalDownloads:4700,totalCrossrefCites:1,totalDimensionsCites:3,hasAltmetrics:1,abstract:null,signatures:"Andreas Loeffler and Heinz Gerhaeuser",downloadPdfUrl:"/chapter/pdf-download/45041",previewPdfUrl:"/chapter/pdf-preview/45041",authors:[{id:"26430",title:"Mr.",name:"Andreas",surname:"Loeffler",slug:"andreas-loeffler",fullName:"Andreas Loeffler"},{id:"167121",title:"Prof.",name:"Heinz",surname:"Gerhaeuser",slug:"heinz-gerhaeuser",fullName:"Heinz Gerhaeuser"}],corrections:null},{id:"44982",title:"Integrating RFID with IP Host Identities",doi:"10.5772/53525",slug:"integrating-rfid-with-ip-host-identities",totalDownloads:3126,totalCrossrefCites:2,totalDimensionsCites:5,hasAltmetrics:1,abstract:null,signatures:"Steffen Elmstrøm Holst Jensen and Rune Hylsberg Jacobsen",downloadPdfUrl:"/chapter/pdf-download/44982",previewPdfUrl:"/chapter/pdf-preview/44982",authors:[{id:"95664",title:"Associate Prof.",name:"Rune",surname:"Jacobsen",slug:"rune-jacobsen",fullName:"Rune Jacobsen"},{id:"166212",title:"BSc.",name:"Steffen Elmstrøm Holst",surname:"Jensen",slug:"steffen-elmstrom-holst-jensen",fullName:"Steffen Elmstrøm Holst Jensen"}],corrections:null},{id:"44987",title:"Design of a Zeroth Order Resonator UHF RFID Passive Tag Antenna with Capacitive Loaded Coplanar Waveguide Structures",doi:"10.5772/53284",slug:"design-of-a-zeroth-order-resonator-uhf-rfid-passive-tag-antenna-with-capacitive-loaded-coplanar-wave",totalDownloads:3205,totalCrossrefCites:1,totalDimensionsCites:1,hasAltmetrics:0,abstract:null,signatures:"Muhammad Mubeen Masud and Benjamin D. 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\r\n\tSchiff base (imine -N=CH-) is one of a popular group of organic compounds prepared from primary amines and aldehyde. Not only as organic compounds but also as ligands for metal complexes, a number of studies have been carried out so far. In this context, this book aims to record a wider range of interdisciplinary content on Schiff base compounds, with an emphasis on the latest advances. This book will aim to compile research results, commentary, reviews, etc., that have dealt with preparation, spectroscopy, crystallography, (asymmetric) synthetic roles, physical properties (magnets, optics, and so on), computational chemistry, and/or theoretical chemistry and their discussions. The book will also intend to focus on Schiff base and its strong connection from organic chemistry to biochemistry or polymer materials chemistry.
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OCA usage increased significantly as consumer electronics devices saw the transition from resistive to capacitive touch with its first implementation in the LG Prada phone in 2006 [1]. The advantage of using an OCA shows improvements in mechanical, optical and electrical performance of the display module and device. The initial application in OCAs in rigid OLED-based devices was similar to LCD devices, but as plastic OLED (pOLED) devices were introduced to the market, OCAs enabled new form factors, such as curved OLEDs in the Galaxy Round and Galaxy Gear S [2] as well as the Galaxy Note Edge [3].
There are two important mechanical considerations for optically clear adhesives – does it stick (adhesive strength) and how strong is it (cohesive strength). Adhesive strength can be defined by the work of adhesion, which is the amount of work required to separate the adhesion from the adherend. Adhesion can be achieved through van der Waals interactions, hydrogen bonding, acid–base, ionic, covalent and mechanical interlocking [4, 5, 6]. Film based OCAs are pressure sensitive adhesives, while LOCAs are liquids that are dispensed and cured. Pressure sensitive adhesives exhibit tack when the modulus is below 3 × 105 Pa or the so-called Dahlquist criterion [7] at the application temperature.
Once the adhesive sticks, the cohesive strength of the material determines the mechanical properties of the bond. Conventional adhesives are functional to the point of bond failure. For optically clear adhesives, they are functional to the point of cavitation that can occur at a significantly lower strength than bond failure [8]. The cohesive strength of an OCA can be designed to resist cavitation and bubble formation when it is warranted.
OCAs are often tested for reliability and durability at elevated temperatures and humidity (e.g. 65°C/90% RH). It is important to have sufficient adhesive strength to maintain performance through these conditions. Potential failure modes include moisture ingress at the interface and bulk plasticization of the adhesive. The adhesive should be selected to have sufficient strength based on the design of the module/device and the necessary durability for the adhesive.
Optically clear adhesives are typically based on acrylate chemistry, having a refractive index of 1.47–1.48 that is comparable to glass and other important materials (e.g. PET, polarizer, etc.) in a display device. By matching the index and using an adhesive to replace an air gap, this significantly reduces the amount of light reflected at an interface (∼4% [9]). By using an OCA, both contrast and brightness can be improved in a device.
Reliability and durability of OCAs in elevated temperatures and humidity can have an impact on optical properties. The adhesive can absorb moisture under these conditions, becoming supersaturated at elevated temperatures. When the adhesive returns to ambient conditions, the excess moisture phase separates in the material becoming apparent as haze in the bulk of the material. This can be avoided by designing the adhesive to be anti-whitening [10]. Durability under UV exposure is a requirement in automotive and high performing consumer electronics applications. A common failure mode under these conditions is yellowing. Careful materials selection and formulation by the materials supplier can prevent yellowing by UV. Circular polarizers in OLED devices can reduce UV transmission to the OLED panel [11]. As POL-less devices [12] become a reality, the OCA will need to take on UV blocking functionality to protect the OLED device.
The electrical functionality of OCAs includes protecting sensitive touch sensors as well as enabling superior touch functionality. Industrial pressure sensitive adhesives often contain acrylic acid [13] to achieve good adhesion. Acidic species corrode touch sensors, such as ITO. Therefore, adhesives selected for bonding in optical applications must be acid-free. The potential module stack configurations for touch will be described in the next section. OCAs can be designed with an optimal dielectric constant at the touch sensing frequency (100 kHz) [14] from low (Dk < 3) to high (Dk > 9) to maximize the signal-to-noise ratio and minimize current and power to drive the touch circuit.
The first OLED displays bonded in consumer electronics were rigid (Figure 1a) and sealed in glass barriers. While they cannot provide the promise of flexible form factors, the OLED patterning process can still make non-rectangular form factors such as rounded corners or notches, although LCDs can now also create these shapes of viewing areas. Rigid OLEDs also can provide higher contrast and wider color gamut compared to liquid crystal displays (LCDs), but the requirements for the adhesive are not dissimilar to those for rigid LCD optical bonding.
OLED displays may be categorized according to the type of encapsulation and touch sensor used. (TFT = thin film transistor) (a) Rigid OLED, so named because the OLED is protected by an inflexible glass barrier with frits sealing the edges. Such designs may use a transparent conductor deposited on the glass as a touch sensor or use a separate film layer, as in (b) and (d). Architectures b-d use thin, flexible encapsulation (TFE), enabling these OLED to flex and bend. (b) GF1 means one glass cover and one film touch sensor layer. (c) On-cell touch, also called touch on encapsulation (TOE), is similar to (a) but with the sensor deposited on the flexible encapsulation layer. Therefore, the sensor substrate can be thinner than in GF1. (d) Another popular design emphasizing touch performance is GF2, which uses a single film layer with touch sensing layers patterned on both sides. (Graphic by Erik Iverson, 3M Display Materials & Systems Division).
When OLEDs are manufactured on thin, plastic substrates like polyimide, they can enable new form factors that are bent or formed into curved shapes (Figure 1b–d). Now many different manufacturers are introducing dynamically flexible devices that can fold repeatedly, such as the Royole FlexPai [15], Samsung Galaxy Fold [16], and Huawei Mate X [17]. Besides these single-axis folding devices, the LG Signature OLED TV R9, announced in 2019 [18], demonstrates that even very large OLED modules can be constructed to roll open and closed from a cylindrical shape less than 30 cm in diameter. Although TVs are not often touch-enabled, this type of flexible device should still use optical bonding to add protective layers to the OLED.
Whatever the form factor, OLED display modules all require additional layers for durability, user interface, and optical functionality. At least one layer each of cover window (CW), touch sensor (TS), and circular polarizer (CP) is generally included, and these must be laminated together with OCA or LOCA for best contrast, brightness, and mechanical durability. The cover window is generally made of glass, although in a few cases manufacturers have used plastics like polycarbonate (PC), polyethylene terephthalate (PET), or clear polyimide (CPI). Plastic cover windows will not shatter and can more easily flex to meet the needs of dynamically foldable or flexible displays. Commonly an ink border or bezel, 10–60 μm thick, is printed around the perimeter of the CW to hide non-transparent supply circuitry in the TS and display layers.
The touch sensor itself may include a thin passivation layer over the functional layer (usually made of ITO, but sometimes metal mesh or silver nanowires) to protect the sensor from environmental aggressors. The CP may be positioned above the touch sensor (Figure 1b) to decrease the visibility of circuit patterns in the touch sensor. While Figure 1 shows at most one separate TS layer, closely related to GF2 (Figure 1d) is GFF (not pictured), in which two films comprise the touch sensor, each with one sensing layer, adhered with a thin OCA between them. Without separate sensor layers to resolve horizontal and vertical position, the touch sensitivity and precision of a GF1 design may be less than a GF2 design.
As of 2018, OLEDs were used almost exclusively in smartphones and smartwatches, so special requirements for bonding larger displays (
Besides the general requirements for optical adhesives described in Section 1, OCA1 requires a balance between adhesive strength and capability to cover the step height of the ink bezel. Certainly strength, usually in terms of a high shear modulus, is critical to help the whole display resist impacts, a major source of user frustration every day when screens break. OCA1 is closest to an impact event on the cover window surface, but all adhesives bonded together in the display system will contribute to its resilience to impacts when the device is dropped.
On the other hand, the OCA must move sufficiently under the shear forces of lamination but then hold its position and shape afterwards, even through temperature cycles of regular use. As bezels are often now less than 1 mm wide, the OCA must bond over an ink step that may be less than 10 times longer than it is high – a challenging aspect ratio to cover without trapping an air bubble at the base of the ink step. Furthermore, the OCA must be strong enough to resist temperature cycling and moisture exposure that could pull it away from the ink step, creating edge bubbles. Bending the display around a curved edge only increases the stress on the adhesive and magnifies the challenges.
The inherent viscoelasticity of OCAs as pressure-sensitive adhesives enables good step coverage of ink or flexible printed circuit (FPC) bond lines. However, as design trends push displays to be thinner and thinner, the solution for great step coverage often comes with UV post-curable OCAs, when narrow bezels make LOCA impractical. Such OCAs are applied in a more viscous, yet still solid, film form with some initial tack. They can flow with the pressure of lamination to cover steps ink steps that are 30–50% the thickness of the OCA. A heated autoclave process step may further improve step coverage capability. Then the laminate is irradiated with light, generally in the UVA spectrum, to increase the bonding within the adhesive, effectively “locking” it in place to improve its durability to the level of a high-modulus adhesive.
In most designs, especially those with the touch sensor on the encapsulation (Figure 1a,c), OCA1 benefits from a higher Dk, as much as 9, to increase capacitive coupling between the finger and the sensor. However, designs with a separate touch sensor (Figure 1b,d) often require a
These properties benefit reliability, durability, and esthetics – all values to the end user of the device. On the other hand, manufacturers and the display supply chain have other requirements. To improve overall process yield and efficiency, these players desire re-workability: targeted or triggered failure of the adhesive cleanly and without residue from one interface. Then components may be separated; expensive parts, especially the OLED and the cover glass, may be recovered. The challenge is that the re-work condition – be it heat, cold, light exposure, or some other factor – must be outside the realm of normal operating conditions so that the display does not de-bond prematurely after it leaves the factory line.
Dimensional stability is another property more visible to the manufacturers than to the end user. OCAs may be delivered as master rolls, and LOCAs will be dispensed or printed as a liquid, but for aggressive tolerances and more complex shapes like rounded corners, manufacturers often opt for individual pre-cut adhesive parts. In that case, the cut OCA must maintain its shape and dimension through environmental conditions of shipping and duration of expected shelf life. The flow, creep, or oozing of the adhesive at elevated temperatures must be limited; consider that the inside of an uncontrolled shipping container can easily exceed 50°C. Similarly, the shipment and packaging format interplays with the formulation; the sustained pressure of a stack of cut parts should also cause only minimal oozing. These properties for cut-part stability are often at odds to the viscosity needed for an uncured PSA to cover steps, as described earlier.
Most OCAs for display bonding are designed to resist whitening, as described in the previous section. Some degree of water resistance has been valuable in OCAs, but the next frontier may be resistance to a broader range of chemical ingress, especially for designs in which the bezels are very narrow or non-existent. Wearable displays also encounter more splashes compared to phones, which may often be partly protected inside a pocket or bag. Normally, a rim tape or lens bonding adhesive may adhere the cover window to the device housing underneath the bezel, and materials chemists may use a wider range of polymers to block chemical ingress, since the material does not need to be optically transparent. The challenge is heightened since everyday chemicals that might contact screens include oils/fats (cooking oil, sweat), alcohols, acids (soda, vinegar), and bases (ammonia, cleaning products) – both hydrophobic and hydrophilic substances.
While manufacturers generally select OCAs for OLED separately from the layers they bond, the CP OCA is widely sold with the CP itself, a different supply chain. Thus, low cost for the integrated product is key, in addition to technical requirements of good adhesion to the CP at a thickness of ≤25 μm. Since the polarizer absorbs a large fraction of UV light, this OCA cannot practically be UV post-curable. As future CPs continue to decrease in thickness [19, 20, 21], with thinner protective layers around the optically active layers, the CP OCA may need to serve a greater role in protecting the polarizer from harmful environmental factors.
The performance requirements of an OCA to bond layers in a flexible OLED display are quite different from a rigid, flat device. The neutral plane must be balanced to minimize strain in critical layers of the device. Thin film transistors (TFTs), thin flexible encapsulation (TFE), and touch sensors are predicted to be most vulnerable, although newer silver nanowire and metal mesh sensors are more flexible than ITO [22, 23]. Although manufacturers continue to improve the durability of OLED displays, publicly available literature indicates that critical components are still quite sensitive to strain. The SiO2 layer of the TFT on polyimide may break at 0.2% tensile strain [24] and the TFE at around 0.3% in bending [25].
When the form of the device requires the OLED to bend only once (during manufacturing), the cover window can be made of glass, which offers the best resistance to scratches and protects the display from impacts to the screen. However, the modulus (
Examples of OCAs that have the strength needed for durable curved bonding are 3M™ Contrast Enhancement Films (CEF) 30xx and 31xx, where xx denotes the thickness in mils. Table 1 describes one important property, peel adhesion, for these adhesives. Their primary difference is that CEF30xx is UV post-curable for step coverage, as described above, and its samples in the table were cured with 1 J/cm2 UVA prior to peel testing.
180° Peel adhesion (N/cm) from float glass for curved OLED display OCAs after varying dwell times.
ASTM D3330 modified test method, 1-cm-wide strips, 305 mm/min peel rate, 2.0 mil polyester backing. All dwells at 23°C/50% relative humidity.
To minimize strain on a flexible OLED display, an adhesive should either perfectly mechanically decouple the layers from each other in bending (
The elasticity requirement contrasts with the common viscoelasticity of OCAs in static applications, and a soft (low modulus) adhesive would typically also sacrifice adhesion. Practically speaking, the foldable OCA should still maintain peel adhesion of 1 N/cm at a minimum. The surface energy and cleanliness of the interfaces with the adhesive also affect adhesion, however, so this property may be improved with plasma treatment or primer layers to increase surface energy.
When a flexible display is expected to bend thousands of times, a foldable OCA should retain these mechanical properties with minimal shift or hysteresis through repeated stress/strain cycling. Besides testing in application, the adhesive properties may be characterized through tensile, compressive, and shear loading, for example, using mechanical load frames, rheometers, or texture analyzers [28]. Some mechanical testing to support the simulation of flexible adhesives is described later in Section 4.
Even a folding radius of 5 mm can require shear strain of >300% in the adhesives during folding (depending on the thickness of the various display layers). Foldable adhesives must certainly shear to this extent without breaking or permanently deforming but are also expected to release strain quickly when stress is removed upon unfolding. However, recovery time of the flexible display also greatly depends on the properties of the other film layers, which have much higher moduli, so it is difficult to distill the recovery requirement for the system into a generic recommendation for the adhesives.
Many trends in OLED design focus on enabling greater flexibility, and new adhesives will be needed to support this as well. Through the next decade, manufacturers will push for narrower folding/rolling radii, multiple folding axes in displays, and longer device lifetimes, especially in terms of cycles of flexing. As folding radius decreases below 3 mm, the required shear strain will likely increase from 300% to roughly 500 to 700% or more. Additional folding axes will also increase the total magnitude of shear displacement, as each axis adds its own displacement to the system. A rollable display can be considered as the limit of many axes of folding across the length of the device. Rolling devices will initially launch with radii of several centimeters, which is larger than today’s one-axis folding displays, but the shear will add with each bend such that the “creep” with applied stress will be a more critical property. With larger creep, even a flexible adhesive could shear out several mm at the edge when the display is rolled, resulting in unsightly uneven edges or, worse, display layers pressing into the bezel/frame bonding and generating further stress.
Thinner display modules will assist flexibility, so trends in integrating functional components are likely to continue. These may include coated circular polarizers [19, 20, 21] or color filters integrated with the OLED encapsulation [12]. With thin flexible cover windows, expect adhesives on either side of the OLED display to play a greater role in protecting the module from impact damage. This will be especially true for plastic CWs compared to glass, since they have lower elastic moduli.
Plastic cover windows may see further growth in automotive displays, but for different reasons. Some manufacturers and safety authorities have been concerned about the possibility of display cover glass shattering in an impact or crash and thus have preferred plastic CW for safety reasons. High-performance plastic CWs are often made of PC or PMMA (poly[methylmethacrylate]), so durable bonding to these low surface energy plastics, with their tendency to release gases under heating, will be important to future automotive OCAs. The reliability and accelerated aging tests for transportation applications are generally more severe than those for consumer electronics. The displays must withstand extremes of heat (often −40 to +110°C), humidity, and light (especially UV) irradiation, but also conditions like sand for desert environments and salt spray on the coasts. Finally, the interiors of many concept cars already feature large displays on the complex curves that designers favor for esthetics and ergonomics. Expect curved displays to grow in size and in popularity in production models in the coming years.
Although it takes time to decrease costs and prove reliability, gradually OLEDs will expand into outdoor applications as well, as consumers begin to expect a certain level of display quality from their everyday interactions with personal and mobile devices. These outdoor bonding applications will demand reliability from the OCA, like the automotive market. Transparent OLED displays are still in their infancy and will likely require lower levels of optical absorptivity, haze, reflectivity, and color for all layers, including optical adhesives.
A different design trend in OLED displays that has already begun in today’s devices is the integration or hiding of the many cameras and sensors that now support the devices’ interactions with their users and environments. The goal is always to expand the active area to occupy an ever-greater fraction of the viewable front of the device. Additionally, a camera behind the display provides a more natural interaction in video calling; the camera may track a user’s gaze at the same location where the user views the other person’s face, giving the impression of eye contact. The implication for bonding with OCAs is stricter dimensional control and tolerance requirements, extending to non-rectangular shapes. Already many sensors and cameras can fit in a droplet or notch shape cut of out of the display and adhesives at one edge of the screen. When the camera(s) are behind the display, some adhesive layers must precisely maintain a small hole in the middle of the part, as an aperture for the camera.
3M has been investigating fatigue and shear performance of polymer film substrates and multi-layer stacks consisting of OCAs (Optically Clear Adhesives) and polymer films in response to dynamic bending. This work was prompted, in-part, to support materials and systems development in the realm of foldable OLED (Organic Light Emitting Diode) market technologies and applications. One device that is used to study the dynamic bending performance of these films and film stacks is an internally-designed and built bend tester. Samples can be mounted to the bend tester and folded to a specific bend radius and number of bend cycles at a defined cycle rate (bend cycles per minute). From a materials perspective, failure in the form or yielding, breakage and buckling can occur during testing. In actual flexible device constructions, the light emitting and barrier layers can be compromised over certain stress and strain thresholds. These failures are influenced largely by the stress or strain amplitude as the samples are placed in the folded conformation of interest. In this section, we will discuss the methodology behind development of a controlled and repeatable folding test that minimizes bending stress on foldable test specimens, types of defects observed in single and multi-layer polymeric stacks consisting of OCA, and additional methods of concept differentiation by incorporating ITO (Indium Tin Oxide) coated PET (polyethylene terephthalate) into the multi-layer test specimens.
One of the first design parameters considered during initial folding test method development is the hinge design (or pivot locations) of the test apparatus. It is important to have at least some understanding of the impact of hinge design selection. Some types of hinge design can impart added strain (or stretching) on samples during the process of folding. With single hinge folding design, or folding with only one pivot point, there will be one or more critical angles in which the test specimen is stretched beyond its original length. This type of tester design is undesirable because the design of the tester can damage the samples, and will introduce added variables, such as test specimen attachment location and attachment adhesive properties, that will dictate how much overall strain is imparted to the sample during the action of folding and unfolding. Slight changes in attachment location and attachment adhesive properties will have an impact on variability and reproducibility of the test results. Note, this logic can be applied to certain mandrel bend folding designs as well, if the strain on test specimens is not actuated to prevent sample lengthening or stretching during folding. For this reason, we have defined a dual pivot testing apparatus (Figure 2), which can prevent added strain or stretching of the samples during folding.
(a, b) Specimen geometry during folding for a single vs. dual pivot test apparatus. Tester mounting plates are depicted in blue, attachment adhesive is depicted in yellow, test specimen is depicted in orange, pivot locations are depicted by ‘+’ signs. (a) shows a single pivot hinge design, in which samples can be stretched at a critical closing angle during testing. (b) shows a dual pivot hinge design, which can eliminate added stretching of the test specimen during folding. (Figures by Tom Corrigan, Ph.D. 3M Corporate Research Systems Laboratory).
In many cases, test specimens will consist of alternating layers of polymer film and adhesive. The primary roles of the adhesive in such constructions will be to adhere the layers together and to prevent added strain on sensitive layers, such as the display or fragile coatings. The mechanical benefit of the adhesive is maximized when specimen layers can freely move and shear across one another during folding and unfolding, thus minimizing stress on fragile layers. For this reason, attaching specimens to the test apparatus using adhesive (instead of clamping) is recommended, especially if it is representative of actual folding device construction. If specimens are attached to the folding test apparatus with clamps, there will be new test variables to consider, such as clamping pressure and location.
When attaching specimens to the folding apparatus using adhesive or tape, the next decision becomes where to attach the test specimen. Samples attached too close to the apex of the fold can add strain on the samples, due to lateral pulling of the samples to the mounting plates during folding. This can also add undesired variability to the test response, in addition to added strain on test specimens. Test specimen shape in the folded configuration can be measured or modeled. For our folding test method, we have defined an attachment location (denoted as Lfree in Figure 3b, below) not closer than 3*g/2, where g is the distance between confining test plates and attachment adhesive.
(a, b) Specimen geometry denoting location of attachment location with bond all the way to edge of substrate backing in (a), while (b) depicts a region without adhesive contact near the fold region.
Misalignment of the test specimen can be caused by off-centered attachment of the test specimen, misalignment of the pivot points (non-parallel or collinear; Figure 4), or curved/warped mounting plates. Such forms of misalignment can result in different patterns and variability in the test response (from left to right sides of the test apparatus, for example; Figure 5).
Shown above are modeling results, which depict changes in strain on test specimens depending on their alignment on the test apparatus. (Courtesy of Samad Javid, 3M Corporate Research Process Lab).
(a, b) Results from testing of 4mil low melt PEN (polyethylene naphthalate) at a nominal gap size of 4 mm. Sample position is measured in inches from left to right side of test apparatus. Samples were checked every 10,000 fold cycles. (a) shows the difference in test response observed when test plates are very flat (2 test cycle replicates are depicted on this plot by red and blue), vs. curved with variation of folding gap by only 0.05 mm as measured with a feeler gauge (data depicted as a general smile pattern in green). (b) shows a sinusoidal test response (plotted in red and green) as a result of loose bearings design, which control the motion profile of the test plates. Tighter bearings design, in this case, yield a flatter more controlled test response profile (plotted in blue).
Both temperature and humidity can affect the test response, particularly for multi-layer test specimens that include adhesive in some layers, since some adhesives may be quite sensitive to moisture uptake. Dependent on the substrates used, this water uptake could apply to films, as well. Specimens should be conditioned at well-defined environmental parameters prior to testing. Testing should also take place in a controlled temperature and humidity environment. Doing so can help improve the repeatability and reliability of the test.
Lamination conditions, sample edge quality and surface treatments that impact adhesion can also influence the test response. Differing amounts of stored stress introduced during manufacturing, and tension applied during the lamination and sample preparation process can change the starting stress states of a test specimen, which can then influence the stress profiles during folding and unfolding.
Depicted below are several types of failure modes observed during bend testing of single and multi-layer test specimens. Crazing (Figure 6a) is caused by slippage of crystal structures and void formations in polymeric films. Local buckling (Figure 6c) is caused by adhesion failure between layers. Global buckling (Figure 6d) is caused by severe instability, which can result in inverted folding of the test specimen.
Depiction of typical failure modes in foldable testing, including substrate crazing (whitening) (a), breakage (b), local buckling (c) and global buckling (d).
There is widely available literature to explain the effects of decoupling and isolating multiple neutral planes in a multi-layer construction [14, 29]. In the ideal case, the neutral planes of each layer in the composite construction are preserved by frictionless slip (or perfect decoupling of each layer). In reality, the lay-up construction (modulus and thickness of each layer), in addition to assembly (such as tension during the lamination process) of the test specimen or display stack will influence stress profiles. 3M Foldable OCA has a lower modulus over a wide range of operating temperatures, as compared to standard commercial OCAs. This offers greater ability to decouple the stiff layers in a flexible display module and reduce the overall bending strain [29, 30].
A simple experiment was performed to assert the performance of 3M™ OCA CEF35, a 3M Foldable OCA. A thin layer of ITO was coated onto 2mil PET. The ITO coated PET was used to create 3-layer test specimens, comprising either a standard OCA 8146–2 or CEF35 at the same thickness of 2 mils (Figure 7a). The test specimens were folded, with ITO on the out-folded/tension side, using a dual pivot bend tester. The folding rate for this test was 30 cycles per minute, with nominal folded gap size of 4 mm. Samples were conditioned for 24 h and tested at 23C, 50%RH. Electrical resistance of the ITO coating was measured at the end locations of each test specimen (using an Ohm meter) after 0, 1, 10, 100, 1000 and 10,000 fold cycles. Results (Figure 7b) showed significantly less resistance increase for stacks constructed with CEF35 than for those containing OCA 8146–2, proving experimentally that CEF35 more effectively decouples the polymer film layers, due to a lower shear modulus (G’) and higher yield under minimal load, thus, causing less damage to the conductive layer.
(a) shows descriptions of test specimens comprising a single layer of 2mil PET, and 3-layer samples comprising of 2mil 3MÔ OCA 8146–2 (a standard 3M OCA) and 2mil 3MÔ CEF35 (a 3M foldable OCA). (b) Results show that less resistance increase is observed for the test specimens comprising of 3MÔ foldable OCA, CEF35, than for specimens containing standard 3MÔ OCA 8146-2. These results suggest that the strain amplitude on the tensioned ITO coated side of the test specimen is reduced when using 3MÔ foldable OCA, thus reducing damage to the fragile coating.
In conclusion, there are several factors to consider when designing a reliable and repeatable folding test method. Factors such as hinge or pivot design, attachment location, sample and fold axis alignment, as well as sample preparation and conditioning, and surface treatments can all have an impact on the reliability and repeatability of the test. Once these factors are controlled, the folding test can be an effective tool for use in differentiating multi-layered constructions representative of foldable displays. IEC standard 62715-6-1 [31] can be referenced and calls out several different methods of bending deformation that can be used to evaluate Flexible Display Devices. Common failure modes include crazing, breakage, local and global buckling. Most, if not all, of these failure modes can be influenced by the properties of the adhesive used to construct the test specimen. 3M Foldable OCA can help to decouple the polymeric film layers of a multi-layer test specimen, and therefor reduce strain on fragile coatings and components, due to its low modulus as compared to standard OCAs, such as 3M OCA 8146.
For foldable AMOLED (OLED) display panels, the repeated folding and unfolding create new mechanical requirements and challenges beyond those of fixed displays. In most applications, the multiple functional layers of a foldable display are bonded by optically clear adhesives (OCA) to form a multilayered thin panel or film stack that is flexible to allow folding of the panel.
The folding of a multilayered panel will introduce bending stress and shear stress not only within the individual layers but also between the bonded layers. Depending on the panel layup design, these bending stresses can reach very high levels causing various failures including fracture of individual layers or sensitive components within a layer, delamination, and buckling. Understanding the nature of these stresses will help in producing robust designs that ensure reliable folding performance.
Because the folding of a display by nature is a problem of large deflection of a multilayer film stack, the classical beam bending theory such as the Euler–Bernoulli approach will be limited in its ability to describe accurately the bending stress and interlaminar stress. The thin nature of the OLED display also makes it difficult to experimentally measure the stresses or visualize the deformation of the layers within the panel. Modeling then becomes an effective tool to provide insights into the mechanical folding behavior. Numerical analysis methods, such as finite element analysis (FEA), offer detailed information of stress and related deformation in each layer of the film stack, and allow virtual testing to evaluate different design scenarios [14, 32, 33, 34, 35].
In this chapter, we will provide an introduction of the folding simulation of OLED display panels. The aim is to demonstrate the basic process of modeling the folding and the potential failure modes of foldable displays to help design engineers to become familiar with:
The interactions between layers of the display film stack with its bonding layers, the OCA layer, and the role of OCA on the folding performance of the film stack.
Some basic modeling methods to simulate the folding of the film stack and the OCA.
As general guidance, we will use modeling examples of a simplified but representative display film stack to describe and discuss the models and the results.
We will also focus on the roles of the soft bonding layer, the OCAs, in the discussions of the modeling results. We will examine the overall performance of the film stack to provide basic understanding of the effectiveness of a soft bonding layer in reducing bending stress and mitigating related potential failure modes. This understanding can be valuable because the material properties and thickness of the functional layers in a display, such as the OLED, circular polarizer film, and the touch sensor film are designed to achieve their specific optical or electronic functions, and the options to vary the thickness and material properties of these functional layers may be limited. Managing a film stack’s neutral plane by employing thicker or stiffer supplementary layers may be undesirable if the display panel is to be flexible. On the other hand, when the display panels become thinner, this imposes its own set of challenges in durability and usability. Optimization of the display film stack through the design of the bonding layer becomes an attractive and often a necessary option.
The typical functional layers of an OLED film stack may include: cover film, the touch sensor layer, circular polarizer, thin film encapsulation (TFE) layer, the AMOLED (OLED) display unit, the back sheet, substrate, and others. The OLED display unit itself also consists of multiple components including a flexible substrate, encapsulation/barrier, thin film transducer (TFT), and transparent electrode. In more recent developments, display manufacturers are also pursuing integration of some of these components for thin form factors with fewer layers. The OCAs are placed between layers to bond them into an integrated display film stack that is flexible to allow folding as shown in Figure 1. The common industry practice for specifying the extent of the folding is by the radius of curvature of the folded region.
The folding of a multilayered panel will introduce bending stresses, both in-plane tensile or compressive stresses and shear stresses between the layers. While each individual layer is flexible to withstand being folded into a small radius of curvature, the bonded multilayer panel will exhibit a much higher stiffness due to the larger thickness of the whole panel, and potentially generate very high bending stresses. The high bending stresses may cause failure in various forms. Of the various components and layers in an OLED display panel, the permeation barrier layer, the indium tin oxide (ITO) layer, and the oxide dielectric layers of thin film transistors (TFT) are sensitive to tensile stress and strain, and they can fracture at a relatively low tensile strain [24, 36].
While there are many other design requirements for a display unit, in terms of folding mechanical performance, flexibility, integrity, and durability without damage are required, and fracture, delamination, or buckling under repeated bending must be prevented.
Other design requirements, including impact resistance to drop impact of display device or ball/foreign object impact, and scratch resistance are also critical for foldable displays. They are interrelated with the foldability performance, and often have competing design requirements. A more systematic and holistic design approach is necessary to incorporate all the aspects of design to achieve balanced optimal performance with some trade-offs, if necessary, among the various competing design requirements. Various modeling work has been performed in these areas at 3M, however, this belongs to a more expansive scope beyond that of the current chapter. For a more focused discussion, this modeling section will be limited to the topic of integrity for foldability.
In the following sections, the general practice of finite element analysis for simulating the folding of a film stack will be discussed first, followed by a modeling example to illustrate the potential failure modes of the film stack that need to be addressed in the design of foldable displays and the effects of OCA in mitigating these failure modes.
The thin film nature of the film stack makes it suitable for using a 2D model to represent the stack without losing much fidelity, especially when edge effects are not significant. To model the interactions among the different functional layers, each layer should be modeled as an individual part of the film stack. In particular, this simulates the deformation behavior that is critical in understanding the effects of OCA on the folding performance of film stack. The finite element mesh size should be sufficiently fine to resolve the stress gradient of the critical layers both in their thickness direction and in the in-plane direction, especially in the bend region where stresses vary through the thickness direction.
The bonding of the OCA to film can be simulated by various interaction definitions such as nodal constraint or node coupling of the mesh of the OCA layer to the mesh of the substrate film layer. This approach will typically not allow the simulation of the separation or debonding of the OCA from the substrates, however, it can offer most of the needed information to evaluate the bond performance without the added complexity of simulating the debonding process. To simulate the debonding process, cohesive elements may be used to represent the OCA bond. If cohesive elements are used, care should be taken to incorporate the cohesive law that describes the debonding force-displacement of the OCA bond attached to the specific films of the actual application because the bond strength depends on the specific substrate films. Also, separate cohesive laws for tension (normal to bond interface) and shear should be used to accurately represent the OCA bond behavior which will require calibrations of the cohesive laws from test data such as those from butt joint or T-joint tests and lap shear tests. In general, the correct application of cohesive elements or cohesive contact for OCAs is more involved. Proper training on the technique will help to avoid misrepresentation of OCA bonds. It is recommended that users consult with 3M technical support for test methods or test data related to bond strength simulation.
Being a type of pressure sensitive adhesive, OCA needs to be soft enough to flow under application of pressure to wet the substrate in close proximity. This intimate contact between OCA and the substrate allows molecular interactions such as van der Waals forces to form the basis of the adhesion that underwrites the overall bond strength. This flow-like behavior of OCA can be described by a combination of nonlinear elastic and viscoelastic/viscoplastic material models.
For OCA’s viscoelastic behavior, its relaxation function can be defined in terms of a series of exponentials known as the Prony series. For the nonlinear elastic or hyperelastic constitutive models, the models such as the polynomial hyperelastic models are most commonly used. They include the neo-Hookean model, Mooney-Rivlin model, and Yeoh model. All are effective in describing OCAs’ ability to be stretched to very large strain. Other forms of hyperelastic models including Arruda-Boyce and Ogden models may also be used. The commercial finite element analysis packages, such as ABAQUS, ANSYS, and COMSOL offer the finite strain computational methods and material model libraries that allow advanced simulation of OCAs. Users can apply the material model calibration tools provided by the finite element analysis software packages to evaluate the material parameters for these constitutive models from OCA material characterization test data. It is also recommended that they contact 3M technical support for information on OCA material data for their specific applications.
Several material characterization tests are needed to generate data for the calibration of the constitutive models mentioned above. For calibrating the elastic or hyperelastic material models, one or more of the tests listed below needs to be performed on the OCA:
Uniaxial tensile
Simple shear
Biaxial tensile
Compression and/or bulk compression
For viscoelastic model calibration, the dynamic mechanical analysis (DMA) test can be performed to produce master curves of the storage modulus and loss modulus of OCA to calibrate the Prony series. Otherwise, relaxation or creep test data at various strain rates and temperatures of interest may be used for the Prony series calibration.
For calibration of OCA bond strength models, such as the cohesive zone model, the proper measurements of the bond strength using T-joint specimens and lap shear specimens should be emphasized. These tests should be performed on the actual substrate materials of the film stack, especially if the potential failure mode may be adhesion failure. 3M Technical Support can be a source for information related to the test methods for adhesive characterization.
The following is an example of finite element analysis of dynamic folding simulation of a display film stack, followed by discussions of the analysis results to assess the folding performance.
In the finite element analysis (FEA) presented here, a simplified 7-layer film stack was used to represent a foldable OLED display (Table 2). The film stack was assumed to be attached to two rigid back plates joined by hinges. The center portion of the film stack was not attached to the rigid back plate to allow for folding of the stack. The folding action simulated here is the so-called ‘out-folding’ such that the film stack is folded towards its back layer. In the fully folded configuration, the space between the straight sections of the outer layer is 10 mm resulting in the bend section of the film stack forming an approximate semi-circle of radius 5 mm as shown in Figure 8. In the simulation, the film stack was folded in 3 s, then held in the folded configuration for 24 h before it was unfolded in 3 s. The material properties and the thickness of each layer used in this work are listed in Table 2. The total thickness of the film stack simulated here was 0.475 mm (layup 1) and 0.275 mm (layup 2). The simulation was repeated for the two film stack layups bonded by 3M™ Foldable OCA CEF35 and 3M™ OCA 8211. 3M™ CEF35 has a lower storage modulus than that of 3M™ OCA 8211, and exhibits a more elastic behavior as indicated by its lower Tan delta value (Table 2) than that of 3M™ OCA 8211.
Layers | Thickness (μm) | Material | Modulus of elasticity, E, (GPa) | Storage Modulus, G\', (GPa) at frequency of 1 rad/s | Tan Delta |
---|---|---|---|---|---|
Cover film | 150 (50) | PET | 3.5 | NA* | NA |
OCA | 25 | 3MTM CEF35 (OCA 1) 3MTM OCA 8211 (OCA 2) | / | 0.03E-3 0.07E-3 | 0.33 0.70 |
Circular polarizer | 75 (125) | Triacetate | 3.2 | NA | NA |
OCA | 25 | 3MTM CEF35 (OCA 1) 3M OCA 8211 (OCA 2) | / | 0.03E-3 0.07E-3 | 0.33 0.70 |
AMOLED | 75 | Polyimide substrate | 3.5 | NA | NA |
OCA | 25 | 3MTM CEF35 (OCA 1) 3M OCA 8211 (OCA 2) | / | 0.03E-3 0.07E-3 | 0.33 0.70 |
Back plate | 100 (150) | PET | 2.7 | NA | NA |
The simplified 7-layer display film stack layup and the properties used in the simulation.
*NA = Not Applicable
The thickness shown in brackets in the table are the values used for stack layup 2.
Simulation results showing the 4 stages of folding. The film stack is folded towards its back layer in the form of the so-called “out-folding”.
The simulation was performed using the ABAQUS finite element analysis package. Due to the large ratio of film stack panel width to thickness, a 2-dimentional plane strain model meshed with the plane strain solid element, CPE4, was used. Six elements were used through the thickness for the OCA layer, and four elements through the thickness for each of the other functional layers.
The following potential failure modes typical for foldable displays were predicted for various film stack layups by the simulation and are also observed in experiments:
Failure due to tensile strain from bending exceeding the critical values for specific components/layers in the display film stack
Buckling
Debonding between layers of the film stack
Figure 9 shows the finite element analysis results of these failure modes. In the following sections, each will be discussed with emphasis on the effects of OCA’s soft properties on the bending performance.
The predicted potential failure modes of foldable display film stack.
For film stacks bonded by 3M™ CEF35 and 3M™ OCA 8211, the results show that the lower modulus of 3M™ CEF35 allows large shear slippage between layers leading to reduced bending stress in the film stack. The in-plane strain in the OLED layer is shown in Figure 10 for the two film stacks bonded by 3M™ CEF35 and 3M™ OCA8211. The maximum tensile strain occurs in the bend section at the bending symmetry plane after the film stack is completely folded. The maximum tensile strain ranged from 0.2% to 0.6% in the stacks bonded by 3M™ CEF35, and from 0.4% to 0.9% for stacks bonded by 3M™ OCA 8211. Depending on the critical strains of the OLED, ITO, or TFE, a less stiff OCA may make the difference between failure and no-failure of the display panel.
Contour plots of in-plane bending strain in the OLED layer when the film stack is fully folded for the film stacks bonded by 3M OCAs (only the OLED layer is shown in this figure).
When the OCA’s shear deformation between layers is sufficiently high to allow adjacent layers to slip over each other, each layer can bend without much constraint from the adjacent layers. This shear decoupling effect can result in much reduced bending stresses in some of the layers leading to a neutral plane in each of the layers, especially for the layers closer to the center of the film stack. In Figure 11, the bending stress (the stress in the direction parallel to the neutral plane of the film stack) of the film stack bonded by 3M™ CEF35 is shown. The plot shows the bending stress distribution at the cross-section of A-B, which is the location where the maximum bending stress will occur within the bend region of the film stack. For this 7-layer film stack of a total thickness of 0.475 mm (Table 2), the bending stress on each of the three OCA layers is negligible due to its low stiffness. The low stiffness of OCA, on the other hand, facilitates relatively high shear strain, in the range of 300–400% (Figure 12). This large shear strain between the layers allows each of the CWF, OLED, and back plate films to bend relatively independently from others resulting in a neutral plane in each of these functional layers, as indicated by the zero-bending stress location within each layer.
Bending stress distribution at the cross-section A-B which is the plane of symmetry of the folded film stack.
Contour plots of shear stress in the transition region for the film stack (layup 1) showing the large shear deformation of the OCA layers.
The ability of soft OCA to shear easily provides an effective design option to achieve multiple neutral planes in a film stack. This can be of great value since it can enable more freedom of choice regarding material properties and thicknesses of other functional layers without compromising their specific optical or electronic performance in a display.
Under bending, a thin display film stack that is partially attached to a stiffer back plate is susceptible to buckling failure that leads to optical distortion and possible debonding, either within the film stack layers or from the back plates on which the film stack is attached. Buckling of the film stack can be further categorized into global buckling and local buckling types.
Global buckling typically gives the film stack a wavy appearance. It happens during unfolding after the film stack is held in the folded configuration for a period of time. In the folded configuration, shear creep in the OCA may occur which can be observed at the end of the film stack where each layer slips over the adjacent layer (Figure 13). This creep induced shear slip cannot be immediately recovered upon unfolding. During unfolding, the top layers of the film stack shown in Figure 11 will then be under compression while the bottom layers will be in tension. Depending on the amount of the shear creep and the overall stiffness and thickness of the film stack, this may lead to instability and global buckling as shown in Figure 14. The more elastic behavior of 3M™ CEF35 limits the shear creep deformation and, in turn, leads to reduced buckling during unfolding.
Simulation results showing the shear deformation between layers (a), and the predicted maximum shear strain in OCA layer and the comparison with the bond strength of the OCA (b).
Displacement contour plots comparison of buckling of the film stack bonded by 3M™ CEF35 and 3M™ OCA 8211 immediately after unfolding showing the improved buckling resistance of 3M foldable OCA. The displacement, U2, is in the direction perpendicular to the film surface (unit: mm).
Local buckling often appears as a fine and thin wrinkle or wrinkles on the surface on the compressive side of the folded film stack [36]. It occurs during folding but may still be visible after unfolding if the buckling is allowed to set in over a period of time or if the buckling causes debonding in the region.
During folding, high compressive stress can develop in the bend region. Local buckling occurs only in the layers on or close to the surface of the film stack on the compressive side of the neutral plane. If the compressive stresses in these layers are not reduced through OCA’s shear deformation, they may cause these layers to buckle or bulge out especially if any geometric off-axis imperfection is present in these layers. As shown in Figure 15, the buckling deformation will stretch the OCA that bonds the buckled layers to the remaining un-buckled layers resulting in tensile stress in OCA in the direction perpendicular to the bonding interface. Depending on the OCA bond strength, this tensile stress can cause delamination in this region.
Predicted local buckling on a film stack bonded with an OCA with a stiffness of 10% of that of 3M™ CEF35. The inserts are the photos of a local buckling on the actual film stack.
Local buckling was not predicted in the film stacks bonded by 3M™ CEF35 or 3M™ OCA 8211 (the layup specified in Table 2). However, if the OCA modulus is reduced to 10% of that of 3M™ CEF35, the simulation predicted that local buckling could occur which is shown in Figure 15 for a particular film stack. On the other hand, reducing the thickness of OCA to increase the constraint to buckling deformation can effectively improve the local buckling resistance as shown in Figure 16. Our studies have shown that reducing OCA thickness and increasing OCA stiffness can improve film stack’s buckling resistance, while reducing OCA stiffness to facilitate shear slip is also critical in reducing the compressive stress that is the root cause of buckling. All these demonstrate that the design for buckling resistance is a balancing act and represents one of the most challenging aspects in film stack optimization. The competing requirements of stiffness to resist buckling and flexibility for folding, as well as, for minimizing the cause of buckling further highlights the importance of leveraging OCA’s broader range of properties to achieve the optimal film stack performance.
Simulation results showing the effect of OCA thickness on local buckling. The film stacks shown here were bonded with 3M OCA of different thickness. The ratios of the surface layer thickness to the underlying OCA layer thickness is 2.0 for the layup on the left, and 1.0 for the layup on the right.
Another failure mode often observed in the foldable display is delamination or debonding, which is characterized by separation of layers either near the ends of the display panel, or within the bend region.
Typically, the debonding at the end of the film stack is due to shear strain in the OCA exceeding the OCA bond shear strength, while the delamination within the bend region is the result of high interlayer tensile stresses on OCA due to local buckling as described above.
In Figure 12, the shear stress of the film stack is shown for the transition region where the bent section meets the straight section. The corresponding shear strain values are indicated on the plots. Figure 13 shows the shear stress at the end of the film stack. For both the film stacks bonded by 3M™ CEF35 and 3M™ OCA 8211, along the length of the film stack, the maximum shear strain occurs in the transition region. The higher the shear strain in the OCA, the more shear slip is allowed between layers, which reduces the bending stress in the layers. For the layers on the compressive side of the neutral plane, this means reduced compressive stress and the reduced possibility of local buckling of these layers. For the layups simulated in this work, the shear strain can be as high as 600% as shown in Figure 12. The softer 3M™ CEF35 allows not only large shear strain upon folding leading to improved local buckling resistance, it also can effectively resist debonding due to its high bond strength (Figure 13).
The simulation examples of folding OLED display film stacks discussed here demonstrate OCAs’ abilities to reduce bending stresses and to create multiple neutral planes in a film stack. The simulation examples also demonstrate three potential failure modes for film stacks under dynamic folding and unfolding.
Fracture due to high tensile bending stress
Buckling
Local buckling of a few layers in the film stack and global buckling of the panel where the entire film stack buckles and assumes a wavy form
Delamination or debonding
As shown in these simulation examples, these failures can be addressed through design and selection of appropriate OCAs. It is also evident that the folding performance of a display is a system-level response, where performance is governed by the properties of each layer in the stack layup as well as the display attachment methods and folding hinge design. The softest layers in the film stack, the OCAs, play a critical role in optimizing the film stack’s folding performance when the options to alter the mechanical properties or thickness of other functional layers to improve overall stack flexibility are restricted by their designed functionalities. Design of display film stacks that utilize OCAs’ unique characteristics can lead to increased robustness of integrated system solutions for foldable displays.
The authors declare no conflicts of interest.
“Breakthrough innovations” is a hot topic aimed at stimulating industry research towards realisation of bioeconomy, sustainability, and high returns on investments. Eco-friendly inequities exist due to rapid population explosion, continuous resource exhaustion, industry biomaterial supply concerns and linear model of produce-consume-dispose [1]. Ultimately, innovative research solutions have been sought to ensure sustainability along the entire food system [2] to address the above challenges. The research solutions have been mainly in biobased industries, notably renewable resources, a component of sustainable biobased industries. However, bio-industries are subjected to considerable technological innovations and sustainable alternative challenges. Thus, the trend is geared towards developing integrated biorefineries with the goal of achieving availability and flexibility of multiple feedstocks’ low inputs and maximum outputs [3]. There are several waste resources that can be valorised to produce unmatched feedstocks for the sustainable biorefinery developments. Examples of current integrated biorefinery feedstocks and products include vegetable oils, high value-added bio-lubricants, cosmetics and bioplastics obtained from low input and under-utilised oil crops, which are not in competition with food and feed supply [4]. Others include green, clean, post-use biodegradable, compostable and efficient alternative supplies.
Cassava resources are versatile biomass supply chains that are bio-transformed into industrial feedstocks to replace fossil oil product streams [5]. Their biopolymers’ processing and products’ development using traditional techniques is accompanied by significant wastes with negative environmental impacts [6]. Cassava is a higher producer of significant wastes (peel pulp, wastewater, and leaves) during postharvest processing. Nonetheless, a comprehensive impression of cassava biomaterials, covering a wide spectrum of novel processing technologies, and underutilised and low-cost biomass, is evident.
This chapter presents a thorough discussion of bitter cassava biomaterial innovations and novel processes for bio-transforming this low-cost underexploited crop. Use of an integrated sustainable process to indirectly reduce waste streams is demonstrated. A special focus is dedicated to production of biodegradable products from intact bitter cassava waste streams of nascent sector as promising feedstocks for application in food, supplement, and packaging systems. Ultimately, concretising the concept of innovative application of cassava biomaterials can be a useful resource for academia, industry, bioeconomy, and policy.
Bitter cassava is an equivalent of sweet cassava. While sweet cassava is edible and safe for instant use in fresh and processed forms, bitter cassava is only safe for usage after intricate processing and is regarded as a staple food [6]. Bitter cassava roots contain high toxic hydrogen cyanide (HCN) levels above 100 mg/kg on fresh basis, even going beyond 900 mg/kg in tropical regions: with the minimum reference limit of 0.02 mg/kg on dry weight [7]. Increasing region-specific sweet cassava profiles as biomaterials for foods, feeds, pharmaceuticals, and confectionery industries have greatly augmented unparalleled investment into non-traditional underutilised crops [4, 8]. In East and Central Africa, bitter cassava varieties (such as Karangwa/Tongolo) have existed for decades. Anecdotal evidence points to the advantages of bitter cassava as a food and industrial crop with superior product (e.g., Flour and crude alcohol) qualities. Bitter cassava is highly preferred due to: i) its potential to be grown organically than sweet varieties because of their more toxicity levels deterring foraging rodents and pests from feasting on the crop; ii) imposing the need to process roots directly after they are harvested deters thieving from the field; and iii) as the processing adds value in terms of time invested, the social obligation of sharing cassava with neighbours is reduced [9].
Due to high potential cyanide content in bitter cassava, the code of practice allows adequate postharvest processing [10]. The appropriate postharvest processing, in particular fermentation, is effective in reducing HCN to minimum concentrations. Conversely, inadequate, notably using rudimentary techniques, leads to high HCN residuals in the final products. The peel (cortex) contains more HCN than edible portion (parenchyma) (Figure 1). As such the peels are frequently detached from the edible portion and discarded. This underutilised waste, estimated at 30% represents a great loss of feedstock and energy resources as well as potential source of eco-system contamination [4, 11, 12]. In major bitter cassava growing regions, it is transformed into primary, intermediary, and tertiary products using rudimentary fermentation processes. Traditionally, different detoxification processes, such as solid-state fermentation and retting in river ponds are used minimise HCN in bitter cassava [13]. This uncontrolled large-scale upstream and downstream process-fermentation into food and beverages contributes significantly to unsustainability, thus requiring valorisation [11, 14]. As the peel is disposed-off and its utilisation limited due to high HCN content, high fibre, and low protein; this presents exceptional opportunities to biotransformation into innovative biomaterials such as biodegradable plastics for diverse applications [4, 11, 15].
Intact root showing different components.
Cassava biomaterials are not restricted to only those produced with sweet cassava (such as food, pharmaceutical, beverage, coatings, civil works, textile industry), but emphasise biomaterials that are developed innovatively from bitter cassava wastes. Investments in bitter cassava biomaterial innovations are based on: i) the need to solve the increased environmental waste, which is caused by a linear and irreversible behavioural pattern that follows a produce-consume-dispose model; ii) innovations in biomaterial development, spurred by bitter cassava superior end-product qualities, that force nascent communities and processors to invest in the staple crop sustainably; iii) the need to reduce waste in environment and develop industrial products, in tandem, for a more competitive resource economy; and iv) solving issues of finite natural material sources and competition for food supply. Precisely, bitter cassava is a renewable resource with no competition for food supply, its valorisation minimises waste and environmental impact and is a cost-effective option.
To this end, a circular utilisation model is explored in tackling cassava biomaterial innovations. This strategy ensures that bitter cassava waste is transformed into value-added resources that later biodegrades into environment post-use, in a process of eco-designing of biomaterials for food and non-food applications.
Converting bitter cassava wastes into high premium resources demands an unusual approach, entailing departure from traditional cassava processing methods to robust processing methodologies. As such, a new systematic improved downstream processing methodology, known as “Simultaneous release recovery cyanogenesis (SRRC)” has been developed and piloted with success to ease downstream production of bitter cassava biomaterial as a template for diverse use [4]. The SRRC constitutes two main stages and unique procedures to produce a biopolymer derivatives biomaterial (Figure 2). The term “biopolymer derivatives” refers to the product recoveries from the intact root of bitter cassava, and these mainly consist of different proportions of starch, cellulose, hemicellulose, holocellulose and lignin [11, 16]. Waste derivatives are the product derivatives of waste solids and wastewaters.
Schematic flow of SRRC methodology for production of biomaterials.
Smart sourcing and preparation of starting materials is an indispensable step in the production of good quality, safe and adequate volumes of biomaterials. Bitter cassava is best sourced at maturity of 12–18 months after planting and should be designated as right harvesting time of adequate biopolymers. Using intact root (IR) is an indirect and logic approach of preventing wastes finding their way into the environment. The IR is a whole root of cassava that is composed of residues (peel, cambium, phloem, central xylem fibre) and edible parenchyma. The derivative wastes consist of the peel, internal root centre fibre (xylem bundles), unwanted trimmed solids and wastewaters. Using the SRRC methodology, intact roots are subjected to mechanical tissue rupture, biopolymer release and cyanide toxin loss. The processes typically involve feeding intact roots into automated grating machine and the resulting pulp mass obtained after mechanical tissue rupture and cell disruption (MTRCD). The MTRCD serves the twin role of actuating total cyanogens hydrolysis into release of volatile hydrogen cyanide and bringing together different biopolymer components for possible modification. In effect, the process involves crushing the intact root into finest pulp using high shear rate pulpers, which is also intended to improve the pulp texture and decrease the extraction time in the subsequent processes of release and recovery [16]. The biopolymer derivatives release is often achieved through homogenisation under the influence of extraction buffers (food grade NaCl and NaHSO3), followed by filtration, centrifugation and washing in distilled water [4]. The derivatives recovery is realised by filtration, centrifugation, washing in distilled water, wastewater recycling and drying in a convectional laminar flow dryer. Resulting biomaterial powder is cooled and stored in airtight bags to prevent post-processing absorption of moisture as the derivatives powder is highly hygroscopic. Processing intact root using SRRC produces fibre-rich derivatives, which has been confirmed to offer better mechanical and barrier properties in the biomaterials [4]. Whether to use intact root or derived wastes depends on the envisioned final product; with edible bio-products, intact root is preferred while non-edible products (e.g., goods carrier bag, derived root residues) are the choice. During SRRC, an efficient mechanical pulping is crucial to achieve good quality (finer fibrous, 30–50 μm) and non-toxic (HCN threshold levels, near 0 ppm) biomaterials. Thus, a pulping efficiency (PE) of ≥90% was found to be sufficient when applied in pulping process using a time-dependent model (Eq. (1)) [16]. The PE of this magnitude is required because of the recalcitrant nature of most cellulosic fibre mass, which succumbs at higher shear rates. The achieved finer biomaterial powder (30–50 μm) is usually a result of softer cellulosic mass when compared to other woody plants.
S, pulping time; V, pulper velocity; Ɛ, pulping efficiency.
The SRRC concept restricts between 16 and 30% wastes disposed directly into the environment. This is achieved by processing fresh bitter cassava roots, and thus avoiding underlying costs, energy, time, intended and unintended disposal efforts, of additional alternative processes for waste management. The most economic SRRC design for sustainable valorisation of bitter cassava waste into value added biomaterials avoids the need to dispose indirectly wastes into environment leading to sustainability. The SRRC processing is a unique methodology concentrated at the early stage of the design (pulping, reaction, and release) to enhance biomaterial modifications, and therefore it can be applied in processes of sweet cassava waste and most crops’ residues. The SRRC reduces the extraction time and improves biomaterial texture with nominal size of 30–50 μm (finer matrices) with potential for extensive application. The ≥90% PE confers total cells breakdown and disruption, ensuring that enzyme linamarase hydrolyses linamarin (precursor of cyanide related compounds) into HCN. Cyanogenesis process is proportional to PE, only achieved in SRRC and not common with traditional methods, ensuring the safety of biomaterials (HCN near zero) [11]. The total HCN loss can be attributed to the functionalised ionic buffers and bisulphite in solution (pH 5.0–5.5) during the reaction and release stage. The affinity of bisulphites for the ketones makes them unavailable. This creates the desired gradient leading to fast HCN loss and might explain the significant detoxification of biomaterials. Ketones are released together with HCN during linamarin hydrolysis. Concurrently, residual sulphur of the bisulphite forms complexes with HCN to form a non-toxic thiocyanate compound. This is a significant outcome of SRRC; in the absence of this process in traditional processing, there is partial detoxification with production of unsafe biomaterials that cannot be applied in industry. Strikingly, SRRC ensures better productivity of the biomaterials as illustrated by the optimised model [11]. The high yield (45.8% w/w) of biopolymer derivatives is attributed to ionic buffers converting nearly all root biomass into biomaterials.
Biopolymer derivatives, a main biomaterial of SRRC and bitter cassava outcomes, can be used as a main ingredient in food, bioplastic, and packaging industries due to its compatible, biodegradable, polysaccharide-rich (starch, cellulosic fibrous, lignin), safety (0.4–2.5 ppm HCN), colourless (white) and particle size uniformity (30–50 μm and free-flowing) properties [4, 11, 15, 16, 17]. The biopolymer derivative is made available in powder form (Figure 3). The biomaterial colour is an impurity and often removed using rudimentary means in traditional processes. Nonetheless, the colourless characteristic of the biomaterial is achieved by reaction additives (sodium salts of bisulphites and ionic buffers) (Eqs. (2) and (3)), acting as bleaching agents. As indicated previously, compatibility was realised by combination and modification of different polysaccharides in the root during pulping and reaction processes. Biodegradable, polysaccharide-rich, toxin-free, and particle size uniformity are accomplished by using intact root and SRRC downstream processing. The amylose content of the biomaterial ranges between 18 and 24%, and higher corresponding amylopectin is attributed to inclusion of the peel waste and impact of SRRC on the peel structure [4].
Biomaterial route showing (a) intact bitter cassava root; (b) periderm-free intact root; (c & d) colourless biopolymer derivatives.
The biomaterial powder is highly stable at moisture content of ≤5% but instability is often encountered when the powder is stored and handled under moisture content ≤10% because the powder is highly hygroscopic.
The biomaterial has homogeneous particle sizes with round and polygonal shapes, and with slightly bigger round granule size [11].
Filmogenic solutions are prepared by using different proportions of the bitter cassava biomaterial powder, glycerol solution and distilled water (Figure 4). The resulting mixture is heated while agitated continuously until a gel is formed and turns clear. It is important that the gel is free from bubbles as they change the microstructure of the film sheet. Immediately, a known volume of the gel is cast onto glass plates and held shortly at ambient conditions to allow them to stabilise, concurrently bubble bleeding occurs. The stabilised gel casts are heated and maintained at known temperatures. The films are peeled off the plates and stabilised under environmental conditions of temperature and relative humidity.
Schematic flow of film fabrication process.
The physico-chemical characteristics of films (Table 1) perform a critical part in diverse end use systems, and knowledge of their properties is important in assessing package perform along the distribution chain. Intact bitter cassava-based films (BCFs) are transparent, with values as low as 3.6% than those obtained from starch of all botanical origin which posts 11.9% [4]. They are comparable to most commercial NatureFlex (4.6%) and Polylactide (3.9%), and much lower than polypropylene (13.6%). The low values tending to zero and higher values leaning to 100%, determined by spectrophotometric transmission and chroma lightness index respectively, indicate more transparency (Figure 5a). It can be confirmed that intrinsic modification of the intact bitter cassava root by SRRC produces more transparent films. Transparent films are important in many applications, particularly in packaging where products in the distribution chain are required to be viewed by buyers.
Property | Bitter cassava film | Commercial PLA film |
---|---|---|
Moisture (%) | 0.19–0.45 | 0.10–0.20 |
Optical (%) | 3.43–5.29 | 1.45–1.50 |
Solubility (%) | 15.52–30.54 | 0.00 |
Water vapour permeability (gmm/(M2.24h,kPa) | 3.19–4.50 | 180.0–190.0 |
Glass transitional temperature (°C) | 44.05–56.23 | 55.0–60.0 |
Melting temperature (°C) | 193.57–213.63 | 130.0–180.0 |
Tensile strength (MPa) | 3.71–48.44 | 40.1–49.5 |
Heat of fusion (J/g) | 64.0–70.5 | 21.5–25.4 |
Degradation temperature (°C) | 370.0–380.0 | 350.0–400.0 |
Glass transition temperature (°C) | 50.0–60.0 | 60.0–65.0 |
Melting temperature (°C) | 200.0–220.0 | 170.0–230.0 |
Crystallinity (%) | 50.5–59.5 | 10.0–15.0 |
Elongation at break (%) | 17.3–18.7 | 33.4–35.0 |
Elastic modulus (MPa) | 0.11–15.95 | 2000–2300 |
Transparency (%) | 3.0–5.0 | 3.0–5.0 |
Seal strength [N/25 mm] | 305.0–325.5 | 25.5–30.5 |
Contact angle (0) | 70–105 0 | 60.0–95.0 |
Biodegradability (days) | 20–100 | 40–50 |
Characteristics of bitter cassava films in kin to commercial PLA bio-film.
Bitter cassava film depicting a) transparent nature; b) carrier bag; and c) scanning electron microscope revealed mesh structure.
BCFs are fairly water resistant after 30 days, which is explained by the relatively stable network components in the film structure imparted by the root waste and SRRC [4, 15, 17]. Intact bitter cassava biopolymer derivatives is able to produce both water soluble and resistant films which can find application in packaging fresh foods and acting as a goods carrier bag used in an environment whereby high water resistance is high (Figure 5b).
BCFs possess homogeneous surfaces, which can be attributed to complete solubilisation of biopolymer derivatives in the polymer matrix, near zero solvent migration at the interface and strong and uniform adhesion of ingredients culminating into homogeneous mesh network structures in the film matrix (Figure 5c) [4].
BCFs are either hydrophilic or hydrophobic; those characterised with contact angles (CA) 700 ≤ CA < 900 contain polar functional groups that render them hydrophilic. The CA is the measure of wettability of solids and gives an indication of the extent liquids spread over solid surface [18]. The surface energy is essential in assurance of printability, adhesion, and transparency of flexible films. The BCFs have contact angles <900 (hydrophilic) and > 900 with printability features and can be used as goods carrier bags (Figure 5b) respectively. Nonetheless, BCFs are observed to swell differently at diverse RH; lower and higher swelling is clear at higher and lower RH respectively due to differences in plasticisation.
The fluid barrier properties of biomaterials are essential for prediction of the product-package shelf-life. The BCFs accurate performance veracity is a function of their flexibility in extremely demanding distribution situations, a role of their ability to respond timely and achieve fluid barrier appropriately. The BCFs have suitable permeability to water vapour (WVP) like commercial films polylactic acid (PLA) and Natureflex (NVS) currently applied in packaging fresh foods. This is fundamentally due to their widespread pore size distributions that contribute to fluid pathways, which are tortuous and exceedingly variable [19]. Depending on the nature of the films and their intended use, their equilibrium moisture contents (EMC) increase correspondingly with relative humidity (RH) at constant temperatures. This is caused by advanced amounts of moisture resulting into augmented mobility and dissociating. By contrast, the films EMC reduces when exposed to higher temperatures at constant RH due to film adsorption behaviour [19]. At high EMC, films moisture attraction is high with enhanced capacity adsorption and faster mobility of water causing a reduction in intermolecular attractive forces. The exponential increase of films WVP at higher temperatures is linked to higher activation energy for moisture permeation but also it is due to molecular initiation triggering film section crusade with creation of hollows that ease solvents motion through permeable films.
The permeability to oxygen (OP) of BCFs is higher than those of commercial NVS films. By contrast, permeability to carbon dioxide (CDP) by films is lower than the commercial ones. This is a good indication that the BCFs are adequate to be used in packaging fresh foods that are not highly respiring. When placed in distribution chain, BCFs under highly variable temperature and RH, the OP and CDP experience slight decreases due to antagonistic nature of RH on diffusion [19]. The interference of OP at higher RH and temperature is caused by increased molecular kinetics resulting into water molecules interfering with film voids but also on chain mobility. At higher RH and temperature, crystalline films are transformed into amorphous films (due to raised glass transition temperature and crystallinity) causing decreases in OP. The ability of these films to regulate barrier properties to gas and water, implies that they can be applied as breathable films, and is important for the choice of using them in commercial applications.
BCFs are permeable to organic and inorganic solvents differently [19] Toluene and paraffin, which are common organic solvents in the distribution chain, behave differently towards films. The higher interaction of paraffin is due to forming complexes with the film but also clinging to film surfaces. The information about the behaviour of solvents in contact with films is vital for their safe handling in the distribution chain. For example, toluene permeation makes film brittle and more crystalline with reduced molecular relaxation [19].
BCFs produce strong films that can have wide-ranging applications. Experiments have shown that BCFs tensile strength (TS) compares with commercial PLA and lies in the range of NVS and orientated polypropylene (OPP). BCFs flexibility is comparable to commercial PLA [4]. Similarly, it has also been shown that BCFs can be produced as weak films when the end use is targeted.
The seal integrity plays a vital role in packages and laminations in commercial setting. The BCFs have stand-alone self-sealing abilities compared to most commercial films that require an extra coating to enhance their sealing capacity. BCFs demonstrate comparable sealing strength with NVS, PLA and OPP that have supported sealing abilities [4]. BCFs exhibit last sealing strength for 12 h under environmental conditions (15–20°C and 50–60%RH), implying that films adhered firmly naturally [4].
BCFs are thermally stable under the influence of high temperatures. Their glass transition and melting temperatures, heat of fusion and crystallinity fall within the range of commercial PLA and LLDPE [4]. They are thermally stable than commercial films with the onset of total degradation occurring at 373°C, which is higher than most polymer networks degrading at 340–360°C [19].
BCFs are highly biodegradable in varying environmental conditions, decomposing in composite pits (within 21 days), open environment during wet conditions (maximum 45 days) and open environment during dry conditions (maximum 90 days). In all disposal environments, the bio-decomposition process uses naturally occurring bacterial/fungi to biodegrade the film into carbon dioxide, water, and compost. This is important for clean environment and sustainability, in contrast with fossil-based films that take more than 1000 years to decompose. When these biofilms are kept at room temperature and away from direct sunlight and humidity, they can biodegrade beyond 365 days. This is important when they are used as goods carrier bags and reused again.
A key part of sustainability is the minimisation of wastes during the biomaterial recovery from bitter cassava environmental waste. A sustainable system is an integrated and key strategy to realise green environment and value-added biodegradable products, and thus contributing to universal sustainability perception. The approach focuses on exploring individual process and model synergies and facilitating SRRC downstream process transition to advance cassava waste feedstocks for biodegradable product innovations. The approach emphasises developing and optimising an integrated process design based on optimising the structure of SRRC with efficient production of packaging materials and sustainable utilisation of cassava waste biomass feedstocks (waste solids and waste waters), meanwhile unlocking indirect and sustainable valorisation of cassava wastes. Apart from integrating individual processes, the strategy is intended to bring them, exclusively, into better efficient levels, through modelling and optimisations, and offer increased productivity of biodegradable packaging materials, thus creating a sustainable utilisation pull to reinforce the exploitation and competitiveness of bitter cassava crop. Standardisation, though process optimisation, of producing biomaterials eases the choice and cost of processes, by defining the design space, process parameters and biomaterial functional properties. In effect, robust production processes provide standard/optimal approaches for leveraging desired biomaterials with marginal costs and maximum functionality [20]. Besides, the effort is to bring the processing technology of small to medium enterprises (SMPs) to maturity through innovations in indirect waste disposal routes; and upgrading the development of simple, convenience and attractive substitute process designs that address cassava wastes accruing using SMPs rudimentary processing technologies.
Bitter cassava wastes that are generated by independent processes are being traditionally minimised in the environment by valorisation of bagasse into organic acids, ethanol, aroma and biocomposites [20, 21]. Although the above processes are popular approaches, they have disadvantages of their fundamental high production costs, energy, and time. Optimal design models of individual processes are used as a solution, which gives best interface leverages in a sustainable cassava minimisation approach. In designing an integrated process, process modelling is used to ensure a holistic design for efficient utilisation of cassava wastes without compromising competition for food supply. Thus, to ensure efficient production of biomaterials, an integrated process design is used [16]. In this design, processes are well-defined and conceptualised before they are used in the integrated downstream processing model. In effect, only processes which add value in minimising waste at low cost, are energy efficient and time saving are selected and analysed in the integration design. Primarily, to increase the efficiency and functionality, the design is partitioned into unit operations whereby optimisations are focused. The source includes but not limited to recovering biomaterials from: i) the whole root of bitter cassava; ii) detached residue portions (peel, fibre, trimmings); and iii) wastewater streams.
The innovations to process design integration fall into three optimised and pooled processes to maximise recovery of safe biomaterials, i.e., efficient mechanical pulping; reaction and release; and recovery.
Efficiency of mechanical pulping is well explained in subsections 3.11–3.12. Precisely, the yield of biomaterials and loss of total cyanide certainly need to be augmented in optimising efficiency.
Reaction and release process is a key stage due to the need to free fully the biomaterials at minimum costs, taking into consideration protection of the environment due to released hydrogen cyanide. There are several variables to aid release, the processing conditions, and the desired biomaterial properties but their levels are highly variable. Resultantly, key buffers and bisulphates are preferred in order to infer release of biomaterials. Based on this approach, the research is done for purposes of not only releasing the biomaterials but also consider their yield, safety and customised for multiple functions.
Regarding reaction and release step, desirability function approach is used to optimise multiple response processes, which exploits optimal processing conditions and parameters and obtain the most desired yield, safety, and functionality of biomaterials. According to [16, 22], joint Pareto front and multi-objective desirability (MOD) approaches is used in the standardisation of the reaction and release process. In Pareto front/solutions, distribution to parameter choices is made in such a way that trade-offs ensure unequal distribution in which some factors are constrained in place of alternatives in order to find feasible choices that lie on the Pareto font [22]. In this case, choices are efficient and not dominated by any other choice. On the other hand, the MOD approach is used in target desirability optimisation due to its capacity predict desirables within anticipated ranges [16].
In the recovery step important processes take place, and they include: removing cyanogens and bisulphite residuals remaining in the wet biomaterials released; dehydrating released biomaterials in a safe and economic way through serial washing and recycling and optimal drying (Figure 6). In traditional washing and clarification, a lot of purified water is deployed in serial washing with implications of energy costs in purification and biomaterials carried in wastewaters. In the current innovative designs, waste solvent is recycled thus reducing greatly on the costs of purification while ensuring zero contaminated biomaterials free from unwanted solvent and other clarifying-induced defects.
Illustration of biomaterial drying process: (a) cross-sectional design of recirculating laminar flow chamber for studying optimisation and (b) mass and energy transfer.
Conventional drying involves a lot of energy spent in the process, usually involving several hours (25°C, 12–16 h) of laminar flow drying without causing defects to the biomaterials in contrast to dying in ovens [16]. During the optimal recovery stage, energy is significantly minimised by optimised conditions in the designed recirculating laminar flow chamber (Figure 6). The purpose is to minimise the resident time of the biomaterial in the chamber while attaining the required residual solvent and drying process efficiency (productivity). As such operating conditions (air temperature, heat transfer coefficient, air flow rate, solvent partial pressure and velocity distributions) of the recirculating chamber are modelled and optimised to minimise significantly the polymer-solvent concentration and biomaterial resident time. Optimal conditions for drying polymer-solvent biomaterials is an outcome of a trade-off between minimising residual solvent dose producing gradients for fast dying without changing biomaterial quality. Thus, an adequate chamber with recirculating laminar flow is designed and deployed (Figure 6) for trial studies using computational fluid dynamics and mass and energy transport modelling [23]. In trying to attain optimal drying, interactions between biomaterial properties, dying conditions, biomaterial (polymer) solvent transport and mass/energy transport are managed. The fans enable to obtain uniform air flowing through the biomaterial. For a known uniform thickness (30 microns), temperature, time and polymer solvent amount profiles evolve as air (20–30°C, 30–40%RH) circulates through chamber containing biomaterials.
Biomaterials from optimised recirculating laminar flow chamber processes are recovered and dried efficiently (high recovery, very low moisture, near zero contamination, low energy usage). The mechanism of drying biomaterial involves heat transfer from the convective air provided by external heat source and mass transfer in the biomaterial involving adsorption, diffusion, and desorption. At all stages of the drying process, drying rate is a function of solvent transport from the inside and surface of the biomaterial to the gas phase. Desorption (i.e., solvent transport from biomaterial surface) is characterised by mass transfer coefficients, gas temperature, velocity, and partial pressure, while diffusion (i.e., solvent transport within biomaterial) depends on temperature and solvent concentration [23]. Important scenarios above are modelled, optimised and outcomes presented (Table 2). The optimised drying rate in recirculating laminar flow ensures short resident time compared to laminar flow (Table 2, Figure 7), implying reduced energy in drying.
Parameters | Laminar flow | Recirculating airflow |
---|---|---|
Wet Biomaterial thickness, μm | 30 | 30 |
Dry biomaterial thickness, μm | 24 | 20 |
Initial air temperature, 0C | 25 | 25 |
Final air temperature, 0C | 30 | 30 |
Residence time, min. | 360 | 240 |
Chamber partial pressure, kPa | 102 | 102 |
Air Velocity, m/s | 1.5 | 2.1 |
Initial solvent (moisture) content, mg | 60 | 60 |
Final solvent content, mg at 240 min | 32 | 5 |
Maximum weight loss, % | 47 | 92 |
Heat transfer coefficient, cals−1 cm−2 °C−1 | 0.0033 | 0.0024 |
Parameters at optimal drying of biomaterials in Laminar flow and recirculating laminar flow.
Drying rates of biomaterials in recirculating laminar and laminar flows.
The biomaterials’ optimisation in recirculation laminar flow (RLF) chamber ensure that they are minimally degraded by heat and are more permeable to water vapour. Conversely, the RLF-based dying does not influence the structural and physico-chemical changes; this is also true for drying in laminar flow (LF) chamber [16]. By contrast, biomaterial thermal degradation increases in LF drying.
SRRC-produced biomaterials have benefits of a relatively low cost; particularly those from bitter cassava possess secondary metabolites with unrivalled properties and varied uses, and thus have an edge over commercially available starch [4]. As a multifunctional, safe and dynamic matrix, bitter cassava biomaterials have potential application in pharmaceuticals, nutraceuticals and food supplements [15, 24]. SRRC-produced bitter cassava biomaterial is used as suitable matrix in the development of novel oral tablet excipient in iron and zinc supplements [11].
In the production of iron and zinc tablets, the goal is to have a sustainable delivery system through chasing a carrier and delivery process that is inexpensive, green, and user-friendly. The manufacture follows a two-step process. Firstly, is to identify key bitter cassava biomaterial properties suitable for the development of self-sustaining excipient with important functionalities [11]. Next, based on the results from the first step, optimise the functionalities using granulation, formulate iron and zinc tablets and conduct dissolution tests.
In the preparation of biomaterial for excipient manufacture and dissolution tests, intact bitter cassava root biomass and SRRC methodology are explored [4]. In the conventional methods of producing biomaterials, peeled roots are the choice starting materials. For current innovation, tablets formation is done by exploring the capacity of biomaterial powder to produce strong tablets and is done by using both intact and peeled roots-derived biomaterials (Figure 8). Detailed procedure for tablets fabrication and dissolution tests can be found in the works of [11]. Iron and zinc are included prior to tablet formation and after granulation process. The quantities of iron and zinc included in the tablets are based on the dietary requirements of men (11 mg/day) and women (8 mg/day) while correcting for experimental loss [11, 25]. A suitable design is important if the minerals are to be distributed evenly in the tablets and an effective dissolution is needed. The design is defined based on three tablet sizes (100, 250, 500 mg), which corresponds with common pharmaceutical tablets in the market (Table 2) and the in vitro dissolution is accomplished using the US Pharmacopoeia (USP) method [11, 26]. For better elucidation of the dissolution mechanisms (behaviour, release type, application angle of tablets), mathematical models are applied [11].
Procedural investigation of excipient tablet production.
The physico-chemical properties of biomaterials play a vital role in tablet manufacture where flowability and compaction are the key properties. The biomaterials have uniform particle size and shape distribution of <3 mm, low bulk, and true densities, high tapped density and increased interparticle voids [11]. The uniform particle size is crucial in effective compaction/compression and regulated delivery matrices [11]. High tapped density is due to higher contract surface area, which is a benefit to tablet filling, higher solubility and dispersibility. Biomaterial flow properties and compressibility and solid excipient durability (desired strength, porosity and dissolution) are a function of bulk, tapped and true densities. The bulk and tapped density of the biomaterial are close to each other, which implies that it has better flow properties [11]. The biomaterial inter-particulate and intra-particulate interaction is low because of the low Carr’s index (CI) and Hausner ratio (HR). The CI indicates compressibility or flowability of a powder, while HR is the number that relates to the flowability of a powder or granular materials. It has a low angle of repose and low porosity, an indication of particle uniformity and excellent flowability, which implies that the biomaterial powder cannot cake. The angle of repose of a powder or granular material is the sharpest angle of descent or dip relative to the horizontal plane to which a material can be heaped without dropping and is between 0 and 900. The biomaterials have low water retention capacity (WRC), water holding capacity (WHC) and swelling capacity (SC) although their WRC increases and WHC and SC decreases with time. The biomaterials have higher hydration capacity due to higher surface energy. The implication is the physical structural changes and hydration properties of the biomaterials fibres and their hydrophilic nature allows maximum moisture uptake offering a hint of better disintegrating of excipients [11].
The novel Iron-Zinc excipient tablet (Figure 9) can be used extensively in developing food supplements, and as a pharmaceutical tablet with other active compounds due to its compatible, biodegradable, safe and fast dissolution properties [11]. Tablets have uniform weights (av. weight 484 ± 0.68 mg (Table 3), which is far lower than the recommended limit of 0.05. Uniformity and thickness of tablets are indication of good packing of tablets. The tablets exhibit reduced thickness corresponding to increases in compression force [11]. Tablets display adequate mechanical properties (hardness and tensile strength). The bitter cassava tablets are weak binders and strong disintegrants; these properties are crucial to the developments of fast release excipients where iron and zinc deliveries are fast demanded and in adequate amounts [24]. Tablet friability is compared to the USP standards implying that they can resist mechanical stress in the distribution chain. Tablet matrix porosity decreases as compression force is increased. Porosity is a function of particle size and shape; regular shaped particles become less and can fill up void spaces between large particles. In the low porosity tablets, small particle sizes allow flexibility for the tablets to pack more efficiently. However, the medium to high porosity biomaterials of bitter cassava does not permit flexibility in tablet packing suggesting a fast dissolution rate. Tablets exhibit higher disintegration time (DT) due to relatively medium to higher porosity, which facilitates rapid water penetration into the tablet resulting into bond rupture and disintegration [11]. The DT is the measure of time required for the tablet to disintegrate into particles under a given set of conditions.
The tablet prototypes containing biomaterial with: (a) no mineral; (b) iron; and (c) zinc.
Parameter | Biomaterial type | |||
---|---|---|---|---|
Bulk density (g/cm3) | 0.38 | |||
Tapped density (g/cm3) | 0.4 | |||
True density (g/cm3) | 1.49 | |||
Carr’s Index (%) | 9.38 | |||
Hausner’s ratio | 1.13 | |||
Flow rate (g/s2) | 20.91 | |||
Angle of repose (0) | 28.52 | |||
Porosity (%) | 68.87 | |||
Hardness (KG) | 4.32 | 4.42 | 4.64 | |
Diameter (mm) | 13.09 | 13.08 | 13.07 | |
Thickness (mm) | 3.16 | 3.14 | 3.11 | |
Weight (mg) | 546.36 | 551.48 | 542.62 | |
Tensile strength (MPa) | 0.35 | 0.37 | 0.41 | |
Disintegration time (s) | 903 | 895 | 878 | |
Friability | 0.67 | 0.56 | 0.51 |
Physical properties of bitter cassava biomaterial and excipient*.
Tablet size of 500 mg analysed at compaction pressures of 200, 500 and 700 MPa.
CP, compression pressure.
The tablet matrix morphology and microstructure are considerably homogeneous, non-aggregated and uniformly blended with iron and zinc [11]. These patterns provide hope for tablets as inert excipients for oral dosage solid forms. Nutrient analysis has shown that zinc is released faster than iron in the tablet matrix, which seems to indicate that the matrix has minor resistance to zinc release than do for iron [11]. Tablet excipients release iron and zinc better in acidic conditions than alkaline conditions within 45 minutes; this has implications for these tablets in the gastrointestinal movements and safe delivery in human body. This confirms that the nutrients have faster absorption in the stomach that in intestines. Furthermore, within 45 minutes of tablet disintegration suggests that they have one of the fastest release rates of iron and zinc nutrients and is attributed to easy tablet matrix erosion. Besides, high erosion rates of the tablet matrices are explained by high gelling, swelling and release of nutrients as fast as possible [11]. Noticeably, the low weight tablets release nutrient from the matrix faster because nutrients diffuse quicker from matrix surfaces.
Food industry packaging challenges created by the failure to maintain quality and safety of fresh and minimally processed foods in distribution have been mitigated mainly by modified atmosphere packaging (MAP). The MAP is a widely established system for the preservation of quality and managing shelf-life of fresh foods driven by the need and legislation to replace chemical preservatives. In the MAP system, the in-package environment is modified to match the requirements for storing fresh foods. While MAP is a popular packaging system, it has outstanding flaws such as design errors, which are corrected by active (gas flushing) and passive (equilibrium MAP) techniques [27]. Noticeably, Equilibrium MAP (EMAP) is universally used system for fresh respiring foods [15]. Notably, an EMAP is established inside the package when gas transmission rate matches product gas consumption rate [15]. Other current extenuation actions to the design errors include use low-cost biodegradable biomaterials for EMAP of fresh fruits and vegetables and cherry tomatoes [15, 28, 29] and joint plasma treatment and EMAP for cherry tomatoes [30]. A more robust package design was achieved using an ultimate EMAP across package distribution conditions [15]. This has an advantage of using the biomaterial film with heat sealing, heat resistance, relatively water resistance, good barrier, transparent and good mechanical properties in addition to their cost-effective, less competition with food supply biodegradability in all environments, ability to make pouches and bags, printing capacity, and non-perforation needs [4, 15, 16, 20].
When planning to design an EMAP for fresh foods, the fresh product respiration and transpiration behaviour and mass transfer of the package are important considerations and must be fully explored and understood [15]. The design trial includes defining the design requirements of bitter cassava biomaterial film EMAP that is stable in distribution chain characterised by low conditions (10°C, 75% RH). This is affected by knowing the impact of packaging parameters (perforation, RH, temperature) on gas (oxygen, carbon dioxide) composition, the optimal design parameters and gas composition and validated optimal EMAP [15]. The EMAP design follows the conceptual flow depicted in Figure 10. To design an integrated package, an active coated product is factored in the EMAP evaluation.
Practical study of an EMAP design.
The dynamics of an In-package headspace gas plays an important role in attainment of EMAP for food products. When cherry tomatoes are used in the EMAP trials and stored using BCFs, the headspace oxygen reached equilibrium (2–3%) after 180 h at 10°C for 75% RH (Figure 11). The recommended headspace oxygen is 3–5% for safe storage of tomatoes [30].
Progress of headspace oxygen (%) of stored cherry tomatoes in EMAP.
Since the shelf-life of the products is associated mainly with microbiological quality, modifying the in-package atmosphere through EMAP is often intended to limit microbial contamination.
Cherry tomatoes stored in the EMAP show visible mould around 360 h at 10°C and 75% RH and demonstrated reduced weight loss. The loss in normal EMAP is attributed to the combined effect transpiration rate of cherry tomatoes and permeability of bitter cassava films [15].
Colour is a key indicator of market value of the product. An EMAP did not have significant effect on the colour of cherry tomatoes during the 21 days of storage; however insignificant changes are apparent due to the nature of biological materials. A colour index of 1.1 was observed with cherry tomatoes storage with EMAP.
Reduced total soluble solids (TSS) is often encountered when tomatoes are stored for a long time. Like any other storage medium, EMAP decreases cherry tomato TSS (Figure 12). In this case, there is a possibility of packaging contributing to the reduced hydrolysis of insoluble polysaccharides into simple sugar [31].
Status of cherry tomato quality at different storage times: (a) weight loss; (b) TSS; (c) colour difference.
According to [32], the global cassava processing market reached a volume of 298.8 Million Tons in 2020, implying that industrial application has grown correspondingly in food, ethanol, paper and cardboard, textiles, pharmaceutical, glues and adhesives. It is reported that food industry accounts for around a half of the total global cassava consumption followed by feed industry [32]. The use of cassava in most industrial applications such as food, pharmaceuticals, beverages, civil works and textile industries is mainly done with sweet cassava starch and flour.
Food application of cassava. By improving properties of cassava flour using enzymatic and thermal modification, has been found to be acceptable in using modified flour as a key ingredient in the production of gluten-free baked products such as pasta and bread [33, 34].
Textile application of cassava. Because of starch qualities such as flexibility, resistance to abrasion and the ability to form a bond with the fibre, it is used in sizing, finishing, and printing in textile industry [35]. Of the total cassava starch used in textile, an estimated 80 percent go into sizing unit operation, which involves shaping and forming yarn fibres into warp. In this case, starch is used to coat the surfaces of the twisted warp that is then subjected to thermal treatment into a beam of warp ready for weaving. When the yarn is moisturised with cassava starch, the threads become smooth, greasy, slippery and hairless. In this case, starch behaves as a lubricant.
Pharmaceutical application of cassava. Tapioca starch, obtained from the roots of cassava by physical and chemical modifications (oxidisation, esterification, etherification, and treatment with enzyme) is applied in medicine and pharmaceuticals. Native and modified tapioca starch are used as diluents, binders and disintegrants in tablet and capsule formulations [36]. The excellent flowability and swelling power of native tapioca starch renders it useful as diluent for capsule and tablet formulations. Native tapioca starch produces tablets with higher tensile strength, less friability, least tendency to brittle fracture, longer disintegration time and slower drug dissolution rate, thus is preferred in paracetamol tablets when compared with cereal starches. Similarly, modified tapioca starch such carboxymethyl starch is generally used in medicine, pharmaceuticals, cosmetics and food due to their improved hydrophilicity, increased water absorption, reduced tendency of retrogradation, lowered gelatinization temperature, increased solubility in cold water with clear gel and higher storage stability [36, 37]. Acid-modified tapioca starch is an important filler or binder in direct compression with higher tensile strength, lower friability, faster dissolution than the native tapioca starch [38].
Application of cassava in civil works. Research has demonstrated that waste cassava is an ingredient in building materials [39]. It is demonstrated that when waste cassava, cement, charcoal and sand mixed in 2.5 kg composite and made into bricks, a denser texture of the bricks is obtained with perfect binding and compaction [39]. The relative strength is reported to be 711.5 kg/cm2 in addition to the brick being more environmentally responsive. Elsewhere, experimental trials of cassava starch modified concrete confirmed improved compressive, split tensile, flexural and elastic modulus of concrete at an optimum of 0.8% as well increased setting time and durability, with potential application in retarding admixtures [40, 41].
Application of cassava in beverages. Research trials confirm application of cassava into spirits and beers [42]. Using enzymes, cassava is liquefied and saccharified serially into, fermentable broth (circa 184 g/l of fermentable sugars), alcohol (circa10% ethanol) and spirits (40% ethanol by volume) with consumer acceptance [42].
Of recent, cassava coating is used in active packaging using both sweet and bitter varieties. Cassava-based edible coatings is used universally in preservation of foods. Trials have shown that edible cassava starch coating extended the shelf-life of Andean blackberries by 100% after 10 days in storage [43] and prevent decay and extend shelf life of black mulberries under refrigerated conditions [44].
Green environment, sustainability, resource renewability and efficiency, industry biomaterial supply, and circular produce-consume-dispose model could be spurred by exploiting innovative research solutions into cassava waste biomass. This chapter demonstrates that cassava varietal-specific waste can be transformed fully into sustainable and efficient feedstocks for bioplastics, packaging, and food supplement industries. Using innovative SRRC improved downstream processes and integrated sustainable process, up to 30% waste from bitter cassava can provide stand-alone feedstock requirements for food, medical, packaging industries. Valorisation of wastes reveals application in Iron-Zinc supplements and extending shelf life of tomatoes, which has advantage of improving nutrition status of vulnerable communities but also avoiding use of pesticides in fruit marketing. Either way, health is improved for the communities. Innovative SRRC improved processing methodology can be an alternative solution that eliminates the burden of drudgery and rudimentary process of small and medium enterprises (SMEs) to increase their market participation. As a supplementary bonus, valorisation of bitter cassava wastes into bioplastics would likely avert consequences of littering and burning of plastics (mainly carrier bags) that impact negatively on the environment and public health. Ultimately, committed used of SRRC in bitter cassava processing would help SMEs to have a sustainable non-food feedstock resource, contribute national environment programmes and improve community incomes.
Authors acknowledge the support provided by National Agricultural Research Organisation (NARO), Uganda, and School of Engineering, University College Cork, Ireland for resource provision during the doctoral studies.
Author declare no conflict of interest for this work.
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His research interests include epidemiological patterns and molecular analysis of antimicrobial resistance and modulation and vaccine development against animal pathogens of public health concern.",institutionString:"Cholistan University of Veterinary and Animal Sciences",institution:{name:"University of Agriculture Faisalabad",country:{name:"Pakistan"}}},{id:"333753",title:"Dr.",name:"Rais",middleName:null,surname:"Ahmed",slug:"rais-ahmed",fullName:"Rais Ahmed",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/333753/images/20168_n.jpg",biography:null,institutionString:null,institution:{name:"University of Agriculture Faisalabad",country:{name:"Pakistan"}}},{id:"62900",title:"Prof.",name:"Fethi",middleName:null,surname:"Derbel",slug:"fethi-derbel",fullName:"Fethi Derbel",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/62900/images/system/62900.jpeg",biography:"Professor Fethi Derbel was born in 1960 in Tunisia. He received his medical degree from the Sousse Faculty of Medicine at Sousse, University of Sousse, Tunisia. He completed his surgical residency in General Surgery at the University Hospital Farhat Hached of Sousse and was a member of the Unit of Liver Transplantation in the University of Rennes, France. He then worked in the Department of Surgery at the Sahloul University Hospital in Sousse. Professor Derbel is presently working at the Clinique les Oliviers, Sousse, Tunisia. His hospital activities are mostly concerned with laparoscopic, colorectal, pancreatic, hepatobiliary, and gastric surgery. He is also very interested in hernia surgery and performs ventral hernia repairs and inguinal hernia repairs. He has been a member of the GREPA and Tunisian Hernia Society (THS). During his residency, he managed patients suffering from diabetic foot, and he was very interested in this pathology. For this reason, he decided to coordinate a book project dealing with the diabetic foot. Professor Derbel has published many articles in journals and collaborates intensively with IntechOpen Access Publisher as an editor.",institutionString:"Clinique les Oliviers",institution:null},{id:"300144",title:"Dr.",name:"Meriem",middleName:null,surname:"Braiki",slug:"meriem-braiki",fullName:"Meriem Braiki",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/300144/images/system/300144.jpg",biography:"Dr. Meriem Braiki is a specialist in pediatric surgeon from Tunisia. She was born in 1985. She received her medical degree from the University of Medicine at Sousse, Tunisia. She achieved her surgical residency training periods in Pediatric Surgery departments at University Hospitals in Monastir, Tunis and France.\r\nShe is currently working at the Pediatric surgery department, Sidi Bouzid Hospital, Tunisia. Her hospital activities are mostly concerned with laparoscopic, parietal, urological and digestive surgery. She has published several articles in diffrent journals.",institutionString:"Sidi Bouzid Regional Hospital",institution:null},{id:"229481",title:"Dr.",name:"Erika M.",middleName:"Martins",surname:"de Carvalho",slug:"erika-m.-de-carvalho",fullName:"Erika M. de Carvalho",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/229481/images/6397_n.jpg",biography:null,institutionString:null,institution:{name:"Oswaldo Cruz Foundation",country:{name:"Brazil"}}},{id:"186537",title:"Prof.",name:"Tonay",middleName:null,surname:"Inceboz",slug:"tonay-inceboz",fullName:"Tonay Inceboz",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/186537/images/system/186537.jfif",biography:"I was graduated from Ege University of Medical Faculty (Turkey) in 1988 and completed his Med. PhD degree in Medical Parasitology at the same university. I became an Associate Professor in 2008 and Professor in 2014. I am currently working as a Professor at the Department of Medical Parasitology at Dokuz Eylul University, Izmir, Turkey.\n\nI have given many lectures, presentations in different academic meetings. I have more than 60 articles in peer-reviewed journals, 18 book chapters, 1 book editorship.\n\nMy research interests are Echinococcus granulosus, Echinococcus multilocularis (diagnosis, life cycle, in vitro and in vivo cultivation), and Trichomonas vaginalis (diagnosis, PCR, and in vitro cultivation).",institutionString:"Dokuz Eylül University",institution:{name:"Dokuz Eylül University",country:{name:"Turkey"}}},{id:"71812",title:"Prof.",name:"Hanem Fathy",middleName:"Fathy",surname:"Khater",slug:"hanem-fathy-khater",fullName:"Hanem Fathy Khater",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/71812/images/1167_n.jpg",biography:"Prof. Khater is a Professor of Parasitology at Benha University, Egypt. She studied for her doctoral degree, at the Department of Entomology, College of Agriculture, Food and Natural Resources, University of Missouri, Columbia, USA. She has completed her Ph.D. degrees in Parasitology in Egypt, from where she got the award for “the best scientific Ph.D. dissertation”. She worked at the School of Biological Sciences, Bristol, England, the UK in controlling insects of medical and veterinary importance as a grant from Newton Mosharafa, the British Council. Her research is focused on searching of pesticides against mosquitoes, house flies, lice, green bottle fly, camel nasal botfly, soft and hard ticks, mites, and the diamondback moth as well as control of several parasites using safe and natural materials to avoid drug resistances and environmental contamination.",institutionString:null,institution:{name:"Banha University",country:{name:"Egypt"}}},{id:"99780",title:"Prof.",name:"Omolade",middleName:"Olayinka",surname:"Okwa",slug:"omolade-okwa",fullName:"Omolade Okwa",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/99780/images/system/99780.jpg",biography:"Omolade Olayinka Okwa is presently a Professor of Parasitology at Lagos State University, Nigeria. She has a PhD in Parasitology (1997), an MSc in Cellular Parasitology (1992), and a BSc (Hons) Zoology (1990) all from the University of Ibadan, Nigeria. She teaches parasitology at the undergraduate and postgraduate levels. She was a recipient of a Commonwealth fellowship supported by British Council tenable at the Centre for Entomology and Parasitology (CAEP), Keele University, United Kingdom between 2004 and 2005. She was awarded an Honorary Visiting Research Fellow at the same university from 2005 to 2007. \nShe has been an external examiner to the Department of Veterinary Microbiology and Parasitology, University of Ibadan, MSc programme between 2010 and 2012. She is a member of the Nigerian Society of Experimental Biology (NISEB), Parasitology and Public Health Society of Nigeria (PPSN), Science Association of Nigeria (SAN), Zoological Society of Nigeria (ZSN), and is Vice Chairperson of the Organisation of Women in Science (OWSG), LASU chapter. She served as Head of Department of Zoology and Environmental Biology, Lagos State University from 2007 to 2010 and 2014 to 2016. She is a reviewer for several local and international journals such as Unilag Journal of Science, Libyan Journal of Medicine, Journal of Medicine and Medical Sciences, and Annual Research and Review in Science. \nShe has authored 45 scientific research publications in local and international journals, 8 scientific reviews, 4 books, and 3 book chapters, which includes the books “Malaria Parasites” and “Malaria” which are IntechOpen access publications.",institutionString:"Lagos State University",institution:{name:"Lagos State University",country:{name:"Nigeria"}}},{id:"273100",title:"Dr.",name:"Vijay",middleName:null,surname:"Gayam",slug:"vijay-gayam",fullName:"Vijay Gayam",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/273100/images/system/273100.jpeg",biography:"Dr. Vijay Bhaskar Reddy Gayam is currently practicing as an internist at Interfaith Medical Center in Brooklyn, New York, USA. He is also a Clinical Assistant Professor at the SUNY Downstate University Hospital and Adjunct Professor of Medicine at the American University of Antigua. He is a holder of an M.B.B.S. degree bestowed to him by Osmania Medical College and received his M.D. at Interfaith Medical Center. His career goals thus far have heavily focused on direct patient care, medical education, and clinical research. He currently serves in two leadership capacities; Assistant Program Director of Medicine at Interfaith Medical Center and as a Councilor for the American\r\nFederation for Medical Research. As a true academician and researcher, he has more than 50 papers indexed in international peer-reviewed journals. He has also presented numerous papers in multiple national and international scientific conferences. His areas of research interest include general internal medicine, gastroenterology and hepatology. He serves as an editor, editorial board member and reviewer for multiple international journals. His research on Hepatitis C has been very successful and has led to multiple research awards, including the 'Equity in Prevention and Treatment Award” from the New York Department of Health Viral Hepatitis Symposium (2018) and the 'Presidential Poster Award” awarded to him by the American College of Gastroenterology (2018). He was also awarded 'Outstanding Clinician in General Medicine” by Venus International Foundation for his extensive research expertise and services, perform over and above the standard expected in the advancement of healthcare, patient safety and quality of care.",institutionString:"Interfaith Medical Center",institution:{name:"Interfaith Medical Center",country:{name:"United States of America"}}},{id:"93517",title:"Dr.",name:"Clement",middleName:"Adebajo",surname:"Meseko",slug:"clement-meseko",fullName:"Clement Meseko",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/93517/images/system/93517.jpg",biography:"Dr. Clement Meseko obtained DVM and PhD degree in Veterinary Medicine and Virology respectively. He has worked for over 20 years in both private and public sectors including the academia, contributing to knowledge and control of infectious disease. Through the application of epidemiological skill, classical and molecular virological skills, he investigates viruses of economic and public health importance for the mitigation of the negative impact on people, animal and the environment in the context of Onehealth. \r\nDr. Meseko’s field experience on animal and zoonotic diseases and pathogen dynamics at the human-animal interface over the years shaped his carrier in research and scientific inquiries. He has been part of the investigation of Highly Pathogenic Avian Influenza incursions in sub Saharan Africa and monitors swine Influenza (Pandemic influenza Virus) agro-ecology and potential for interspecies transmission. He has authored and reviewed a number of journal articles and book chapters.",institutionString:"National Veterinary Research Institute",institution:{name:"National Veterinary Research Institute",country:{name:"Nigeria"}}},{id:"158026",title:"Prof.",name:"Shailendra K.",middleName:null,surname:"Saxena",slug:"shailendra-k.-saxena",fullName:"Shailendra K. Saxena",position:null,profilePictureURL:"https://s3.us-east-1.amazonaws.com/intech-files/0030O00002bRET3QAO/Profile_Picture_2022-05-10T10:10:26.jpeg",biography:"Professor Dr. Shailendra K. Saxena is a vice dean and professor at King George's Medical University, Lucknow, India. His research interests involve understanding the molecular mechanisms of host defense during human viral infections and developing new predictive, preventive, and therapeutic strategies for them using Japanese encephalitis virus (JEV), HIV, and emerging viruses as a model via stem cell and cell culture technologies. His research work has been published in various high-impact factor journals (Science, PNAS, Nature Medicine) with a high number of citations. He has received many awards and honors in India and abroad including various Young Scientist Awards, BBSRC India Partnering Award, and Dr. JC Bose National Award of Department of Biotechnology, Min. of Science and Technology, Govt. of India. Dr. Saxena is a fellow of various international societies/academies including the Royal College of Pathologists, United Kingdom; Royal Society of Medicine, London; Royal Society of Biology, United Kingdom; Royal Society of Chemistry, London; and Academy of Translational Medicine Professionals, Austria. He was named a Global Leader in Science by The Scientist. He is also an international opinion leader/expert in vaccination for Japanese encephalitis by IPIC (UK).",institutionString:"King George's Medical University",institution:{name:"King George's Medical University",country:{name:"India"}}},{id:"94928",title:"Dr.",name:"Takuo",middleName:null,surname:"Mizukami",slug:"takuo-mizukami",fullName:"Takuo Mizukami",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/94928/images/6402_n.jpg",biography:null,institutionString:null,institution:{name:"National Institute of Infectious Diseases",country:{name:"Japan"}}},{id:"233433",title:"Dr.",name:"Yulia",middleName:null,surname:"Desheva",slug:"yulia-desheva",fullName:"Yulia Desheva",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/233433/images/system/233433.png",biography:"Dr. Yulia Desheva is a leading researcher at the Institute of Experimental Medicine, St. Petersburg, Russia. She is a professor in the Stomatology Faculty, St. Petersburg State University. She has expertise in the development and evaluation of a wide range of live mucosal vaccines against influenza and bacterial complications. Her research interests include immunity against influenza and COVID-19 and the development of immunization schemes for high-risk individuals.",institutionString:'Federal State Budgetary Scientific Institution "Institute of Experimental Medicine"',institution:null},{id:"238958",title:"Mr.",name:"Atamjit",middleName:null,surname:"Singh",slug:"atamjit-singh",fullName:"Atamjit Singh",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/238958/images/6575_n.jpg",biography:null,institutionString:null,institution:null},{id:"252058",title:"M.Sc.",name:"Juan",middleName:null,surname:"Sulca",slug:"juan-sulca",fullName:"Juan Sulca",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/252058/images/12834_n.jpg",biography:null,institutionString:null,institution:null},{id:"191392",title:"Dr.",name:"Marimuthu",middleName:null,surname:"Govindarajan",slug:"marimuthu-govindarajan",fullName:"Marimuthu Govindarajan",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/191392/images/5828_n.jpg",biography:"Dr. M. Govindarajan completed his BSc degree in Zoology at Government Arts College (Autonomous), Kumbakonam, and MSc, MPhil, and PhD degrees at Annamalai University, Annamalai Nagar, Tamil Nadu, India. He is serving as an assistant professor at the Department of Zoology, Annamalai University. His research interests include isolation, identification, and characterization of biologically active molecules from plants and microbes. He has identified more than 20 pure compounds with high mosquitocidal activity and also conducted high-quality research on photochemistry and nanosynthesis. He has published more than 150 studies in journals with impact factor and 2 books in Lambert Academic Publishing, Germany. He serves as an editorial board member in various national and international scientific journals.",institutionString:null,institution:null},{id:"274660",title:"Dr.",name:"Damodar",middleName:null,surname:"Paudel",slug:"damodar-paudel",fullName:"Damodar Paudel",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/274660/images/8176_n.jpg",biography:"I am DrDamodar Paudel,currently working as consultant Physician in Nepal police Hospital.",institutionString:null,institution:null},{id:"241562",title:"Dr.",name:"Melvin",middleName:null,surname:"Sanicas",slug:"melvin-sanicas",fullName:"Melvin Sanicas",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/241562/images/6699_n.jpg",biography:null,institutionString:null,institution:null},{id:"117248",title:"Dr.",name:"Andrew",middleName:null,surname:"Macnab",slug:"andrew-macnab",fullName:"Andrew Macnab",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"University of British Columbia",country:{name:"Canada"}}},{id:"322007",title:"Dr.",name:"Maria Elizbeth",middleName:null,surname:"Alvarez-Sánchez",slug:"maria-elizbeth-alvarez-sanchez",fullName:"Maria Elizbeth Alvarez-Sánchez",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"Universidad Autónoma de la Ciudad de México",country:{name:"Mexico"}}},{id:"337443",title:"Dr.",name:"Juan",middleName:null,surname:"A. Gonzalez-Sanchez",slug:"juan-a.-gonzalez-sanchez",fullName:"Juan A. Gonzalez-Sanchez",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"University of Puerto Rico System",country:{name:"United States of America"}}},{id:"337446",title:"Dr.",name:"Maria",middleName:null,surname:"Zavala-Colon",slug:"maria-zavala-colon",fullName:"Maria Zavala-Colon",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"University of Puerto Rico, Medical Sciences Campus",country:{name:"United States of America"}}}]}},subseries:{item:{id:"3",type:"subseries",title:"Bacterial Infectious Diseases",keywords:"Antibiotics, Biofilm, Antibiotic Resistance, Host-microbiota Relationship, Treatment, Diagnostic Tools",scope:"