Emulsion type and its droplet size [4].
\r\n\t● Can varying levels of privacy assurance be built into DP models, to accommodate varying willingness to share personal information than others, especially if this results in more utility for them.
\r\n\r\n\t
\r\n\t● How is differential privacy able to address evolving statistical distributions of model features in streaming data use-cases?
\r\n\t
\r\n\t● How shall we statistically account for excess randomness introduced by privacy-preserving methods?
\r\n\tThis book aims to provide an account of the current state-of-the-art in DP and developments in this strategically important area.
",isbn:null,printIsbn:"979-953-307-X-X",pdfIsbn:null,doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"bf30fcb3624ab9bbb9aee57efd21aff5",bookSignature:"Dr. Douglas McNair",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/10177.jpg",keywords:"Differential privacy, anonymization, reidentification risk, data-sharing, complexity theory, big-O analysis, machine learning, privacy assurance, open science, utility preservation, VLDB engineering, distributed noise generation, probabilistic inference, multiple imputation, cryptography, distributed computing, adversary attacks, nonrandom linkage disequilibrium, regulatory compliance",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"November 27th 2019",dateEndSecondStepPublish:"March 31st 2020",dateEndThirdStepPublish:"May 31st 2020",dateEndFourthStepPublish:"August 1st 2020",dateEndFifthStepPublish:"October 31st 2020",remainingDaysToSecondStep:"a year",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!0,biosketch:null,coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"219757",title:"Dr.",name:"Douglas",middleName:null,surname:"McNair",slug:"douglas-mcnair",fullName:"Douglas McNair",profilePictureURL:"https://mts.intechopen.com/storage/users/219757/images/system/219757.jpg",biography:"Doug McNair serves as a Senior Advisor in Quantitative Sciences – Analytics Innovation in Global Health at the Bill & Melinda Gates Foundation. He assists the foundation’s R&D in drug and vaccine development for infectious diseases, childhood diseases, and neglected tropical diseases. Current projects include product development programs in Discovery & Translational Sciences involving Bayesian Networks. His activity also includes machine-learning and modeling of health economics collaborating with BMGF\\'s Global Development division. Previously, Doug was President of Cerner Math Inc., responsible for Artificial Intelligence components of Cerner’s EHR solutions, discovering AI predictive models from real-world de-identified EHR-derived Big Data. 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From chapter submission and review, to approval and revision, copy-editing and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. 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Venkateswarlu",coverURL:"https://cdn.intechopen.com/books/images_new/371.jpg",editedByType:"Edited by",editors:[{id:"58592",title:"Dr.",name:"Arun",surname:"Shanker",slug:"arun-shanker",fullName:"Arun Shanker"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"878",title:"Phytochemicals",subtitle:"A Global Perspective of Their Role in Nutrition and Health",isOpenForSubmission:!1,hash:"ec77671f63975ef2d16192897deb6835",slug:"phytochemicals-a-global-perspective-of-their-role-in-nutrition-and-health",bookSignature:"Venketeshwer Rao",coverURL:"https://cdn.intechopen.com/books/images_new/878.jpg",editedByType:"Edited by",editors:[{id:"82663",title:"Dr.",name:"Venketeshwer",surname:"Rao",slug:"venketeshwer-rao",fullName:"Venketeshwer Rao"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"4816",title:"Face Recognition",subtitle:null,isOpenForSubmission:!1,hash:"146063b5359146b7718ea86bad47c8eb",slug:"face_recognition",bookSignature:"Kresimir Delac and Mislav Grgic",coverURL:"https://cdn.intechopen.com/books/images_new/4816.jpg",editedByType:"Edited by",editors:[{id:"528",title:"Dr.",name:"Kresimir",surname:"Delac",slug:"kresimir-delac",fullName:"Kresimir Delac"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"16796",title:"Initial Growth Process of Carbon Nanotubes in Surface Decomposition of SiC",doi:"10.5772/17253",slug:"initial-growth-process-of-carbon-nanotubes-in-surface-decomposition-of-sic",body:'Carbon nanotubes (CNTs) are cylinders of graphene which is a single planar sheet of sp2-bonded carbon atoms. From their unique structures, they exhibit several novel properties, such as high strength, high performance in electrical and thermal conductors, etc. Therefore, since the discovery by Iijima in 1991 (Iijima, 1991), CNTs have been one of the hottest topics in both physics and material science. Mainly, their structures are specified with four parameters; the number of walls, diameter, length and chirality. Dependent of the number of walls, CNTs are categorized as single-walled nantoubes (SWNTs) and multi-walled nanotubes (MWNTs) and SWNT structure can be specified uniquely with a chiral vector Ch = na1 + ma2 (n, m are integers, 0 ≤ │m│ ≤ n) defined relative to the two-dimensional graphene sheet (Saito et al., 1998). Figure 1 shows the graphene honeycomb lattice. The unit cell is spanned by the two vectors a1 and a2 and contains two carbon atoms, where the basis vectors of length a0\n\t\t\t\t\t= 0.246 nm form an angle of 60º. The chiral vector Ch can be expressed by these two vectors a1 and a2, and it corresponds to a section of the SWNT perpendicular to the nanotube axis. In Fig. 1, the chiral vector Ch\n\t\t\t\t\t= 6a1\n\t\t\t\t\t+ 3a2 of an (6, 3) tube is shown. The translation vector, T, which is parallel to the nanotube axis and is normal to the chiral vector Ch in the unrolled honeycomb lattice is also shown and it can be expressed in terms of the basis vectors a1 and a2 as, T = 4a1\n\t\t\t\t\t– 5a2. The electronic structure of a SWNT is determined by these two indices (n, m) and the SWNTs could be semiconductors and metals, depending on them. For example, metallic CNTs show the relation, n – m = 3q, with q being an integer. The diameter of a SWNT, d, is also specified with these chiral indices as,
The band gap of semiconducting SWNTs is inversely proportional to the diameter. Therefore, it is important to control and obtain SWNTs with unique chirality at will, for realization of CNT devices.
Graphene honeycomb lattice with the lattice vectors a1 and a2. The chiral vector Ch\n\t\t\t\t\t\t= 6a1\n\t\t\t\t\t\t+ 3a2 of the (6, 3) tube and the translation vector T = 4a1\n\t\t\t\t\t\t– 5a2 are shown.
There have been three main methods to produce CNTs; arc discharge, laser ablation and chemical vapour deposition (CVD). Arc discharge and laser ablation utilize the evaporation of a graphite target to create gas-phase carbon fragments which recombine to form CNTs. Although both produce CNTs with high crystallinity due to the high growth temperature, it is difficult to control the structure of CNTs. Recently, CVD has been widely used for CNT growth because it is suitable for organizing CNTs over a large surface. CVD utilize metal catalyst particles in the gas phase or on surfaces, decomposing a carbon containing feedstock gas, such as acetylene or ethanol. These procedures can be applied to control the structure of CNTs through the size and shape of catalyst. So far, the diameters of CNTs could be controlled to some extent through the control of catalyst particle size (Jeong et al., 2007). However, there still remains some distribution in the CNT diameter, and also the control of chirality has never been achieved.
Schematic illustration of CNT growth by surface decomposition of SiC.
As distinct from these conventional growth techniques, surface decomposition of SiC has been reported as a novel CNT growth technique during recent years. It was first discovered by M. Kusunoki et al. in 1997, who found that CNTs grew on SiC(-1-1-1) surface after heating a 3C-SiC single crystal at 1700ºC using YAG laser during a transmission electron microscope (TEM) observation (Kusunoki et al., 1997). They observed that CNTs were mostly oriented along the [111] direction. Later, they reported that CNTs could be easily produced on 6H-SiC(000-1) surface only after heating in a vacuum electric furnace (Kusunoki et al., 2000). The schematic picture of the growth process of CNTs by surface decomposition of SiC is shown in Fig. 2. As heating temperature rises, Si atoms are desorbed and CNTs grew into the SiC substrate the axes of which are kept perpendicular to the substrate surface. This growth method has an exclusive characteristics because it needs no catalyst, and self-aligned CNTs were grown with desorption of Si atoms.
Also, they pointed out that CNT growth was strongly dependent on the polar faces of SiC. Figures 3(a) and (b) shows schematic cross-sectional and top view of 6H-SiC, respectively, and SiC (000-1) and (0001) faces are shown at the top layer and bottom in Fig. 3(a). On the (000-1) face (carbon–face), there are dangling bonds from carbon atoms which are perpendicular to the substrate surface, while dangling bonds from Si atoms are seen on the (0001) face (Si-face). Kusunoki et al. pointed out that CNT growth was observed only on carbon-faces of SiC single crystals, such as (000-1) face of 6H-SiC and (-1-1-1) face of 3C-SiC, while graphite sheets were formed on the surface after heating Si-faces (Kusunoki et al., 2000).
Schematic representations of (a) cross-sectional view and (b) top view of 6H-SiC, and (c) zigzag-type of a SWNT. The top side and bottom side of (a) correspond to (000-1) and (0001) faces, respectively.
So far, through high-resolution TEM (HRTEM) images, they revealed several characteristics of CNTs grown by this method: (a) most CNTs are two to five layered 2-5 nm in diameter, (b) The CNTs are grown perpendicular to the SiC surface, (c) The density of CNTs is above 1012 cm-2, which is higher than those grown by other methods, (d) The CNTs are atomically bonded with the SiC crystal at the interface and (e) most of the CNTs have unique chirality, that is, zigzag-type (Fig. 3(c)) (Kusunoki et al., 2002). Although there are still several problems to be resolved for device fabrication, such as purity of the CNT film and homogeneity in the number of walls and diameter, CNTs grown by surface decomposition of SiC have several advantages to realize CNT devices. Among these useful properties, the unique chirality of grown CNTs is the most important and mysterious, because the growth of CNTs with unique chirality has never been attained by other growth techniques. Therefore, surface decomposition method might play an important role in fabrication of CNT devices. Also, elucidation of the mechanism of selectively chirality alignment will be invaluable and useful to control and align chirality of CNTs grown with other methods.
The formation process in the initial stage of CNT growth by surface decomposition of SiC has been reported by several groups. TEM studies by Kusunoki’s group showed that arced sheets of carbon with an outer diameter of 5 nm and height of 1-2 nm appeared on the SiC(000-1) face after heating at 1250ºC for 30 min (Kusunoki et al., 2000). After heating at 1300ºC, two-, to three-layered carbon nanocaps 3-5 nm in diameter and 3-5 nm in height were generated in a dense formation on the surface. After heating at higher temperature, CNTs grew below these carbon nanocaps with desorption of Si atoms indicating that these carbon nanocaps correspond to the top of CNTs. This means that the structure of CNTs is closely related to the carbon nanocaps, and elucidation of the formation mechanism of the carbon nanocaps is a key point to clarify unique chirality of CNTs grown by this method.
Schematic illustration of the initial growth process of carbon nanocaps and CNTs proposed by Watanabe’s group.
Except for pioneering and essential investigation by Kusunoki’s group, few studies have been reported about the formation mechanism of carbon nanocaps. Watanabe et al. carried out TEM and scanning tunnelling microscope (STM) observation for CNT growth on 3C-SiC(-1-1-1) and proposed a model for carbon nanocap formation. The schematic figure of their model is shown in Fig. 4 (Watanabe et al., 2001). In their model, at first, amorphous carbon was formed on the SiC surface with the evaporation of Si atoms. Then, they were crystallized and graphene flakes were formed and aligned parallel to the SiC surface with the temperature rise. Finally, lifting of part of the graphene, carbon nanocaps were formed. This model is significant as first attempt to explain this unique phenomenon. However, intuitively, their model seems to have some discrepancy against the observed experimental results; in their model, the diameter of a CNT would be enlarged, however, TEM observation showed that the diameter was maintained during the growth. Also, it seems to be difficult to explain the reason why enormously high-density CNTs are grown. To clarify the real growth process, analysis at the atomic level is essential, including the alignment and direction of C-C bonding during the crystallization
In this study, we investigated the details of formation process of carbon nanocaps using various experimental techniques; STM, X-ray photoemission (XPS) and near edge X-ray absorption fine structure (NEXAFS) spectroscopies. Based on these experimental results, we attempted to propose a formation mechanism of carbon nanocaps.
To clarify the details of formation process of carbon nanocaps, it is essential to clarify the surface structure and composition. However, few studies have been reported with combing XPS measurement and STM observation for formation process of carbon nanocaps. Here, we carried out both XPS measurements and STM observations for carbon nanocaps formed on 6H-SiC(000-1) (Maruyama et al., 2006, 2007). Figure 5(a) and (b) show XPS spectra of 6H-SiC(000-1) surface before and after heating at 1100ºC in UHV, respectively, where the spectrum of Fig. 5(a) is that from the sample after etching with 10% HF for 15 min. To grow carbon nanocaps, the temperature was slowly increased, keeping the heating rate below 2ºC/min in the temperature region above 400ºC. Both spectra were measured at room temperature with a laboratory photon source (Mg\n\t\t\t\t\tKα : 1253.6 eV) at the take-off angle of 20º from the surface plane, to enhance the surface sensitivity. As expected, no elementary carbon was observed before heating. It should be noted that some oxides such as SixCyOz are main components on the surface and the SiC component is weak. Taking into account that the escape depth of photoelectron was about only one nanometer in the measurement condition, most of SiC(000-1) surface was covered with these oxides even after HF etching. After heating at 1100ºC, a component of elementary carbon derived from sp2 bonding became dominant, corresponding to both desorption of Si. The component from the SiC substrate is still observed, which suggests that the carbon layer accumulated on the SiC surface was very thin and about a few nanometers. Relative intensity of each component in XPS spectra was estimated as the sum should be one, and its temperature dependence is shown in Fig. 5(c). After heating above 1000ºC, the component of elementary carbon (sp2) appeared and it gradually increased, as the heating temperature rose. On the other hand, those related from SiC and SixCyOz gradually decreased with the temperature, although a small amount of oxides still remained at 1200ºC. The increase of the component of carbon sp2 bonding correspond to the progress in the desorption of Si atoms and the accumulation of carbon atoms on the SiC surface, which leads to carbon nanocap formation.
Surface structure change with the heating temperature is shown in Fig. 6. These STM images were observed at room temperature after heating at each temperature in UHV. After heating at 800ºC, step-like structures appeared on some portion of the surface (a). The area of each terrace was small and several tens of nanometers. After heating at 1100ºC, densely packed grains, around 1-2 nm in size, were observed over the entire surface (b). These nanoparticles formed clusters at 1150ºC, keeping the sizes of individual particles unchanged (c). The cluster size ranged from around 3 to 5 nm. Taking into account the result of XPS measurements, the nanoparticles were elemental carbon which were accumulated after desorption of Si. After heating at 1200ºC, the SiC surface was covered by a large number of grains ranging in size from around 3 to 5 nm, as shown in STM images of Fig. 6(d). The blowup in Fig. 6(d) shows that their surfaces were covered with cobweb-like patterns, indicating that the carbon nanocaps were formed at this temperature.
XPS spectra of SiC(000-1) surface of (a) before heating (after HF etching), and (b) after heating at 1100ºC in UHV. Both spectra were measured at the take-off angle of 20ºfrom the surface plane. (c) Temperature dependence of relative intensities of each component in XPS spectra.
STM images of 6H-SiC(000-1) substrate obtained in subsequent stages of the annealing process under UHV: (a) after annealing at 800ºC, (b) 1100ºC, (c) 1150ºC, and (d) and (e) 1200ºC. (e) is a blowup of (d).
Figure 7 shows another STM images for carbon nanocaps formed on SiC(000-1) which were annealed at 1250ºC in a vacuum electric furnace (Bang et al., 2006). Carbon nanocaps formed on the entire surface were clearly shown in (a). Figure 7(b) shows an atomic-resolution STM images of the blowup of a cap structure produced on a 6H-SiC(000-1) substrate. They showed convex structures, 3-5 nm in diameter and 1-2 nm in height, exhibiting cobweb-like patterns, as shown in Fig. 6(e).
a) and (b) STM image of the cap structures produced on 6H-SiC(000-1) substrates after heating at 1250ºC in a vacuum electric furnace. (c) Height profile of cap structures in the direction marked by an arrow in (b).
Figure 8(a) shows one portion of the surface of a carbon nanocap formed on 6H-SiC(000-1) after annealing in a vacuum electric furnace and (b) and (c) show magnified feature of STM images of (a). Figure (b) and (c) are the same except for the markers shown by open circles and a square. (Bang et al., 2006). Figure 8(b) clearly reveals the cobweb-like pattern, which corresponds to carbon networks, on the surface of carbon nanocaps. In Fig. 8(c), one large circle, one large square, and nine small circles can be seen. There are six small open circles around the right large open circle, which confirms that this pattern is a carbon network composed of hexagons. In contrast, the left large square is surrounded by only five small circles, which indicates that the portion of network represented by the left large open square is a pentagon on the nanocap surface. It is well known that a convex carbon network contains several pentagons, as observed on the surface of fullerenes. Given the convex shape of the nanocap, it is reasonable to observe a pentagon on the surface. These STM observations support the assumption that the carbon nanocap had been already crystallized when it was formed on the SiC surface.
Crystallization during the formation of carbon nanocaps was directly confirmed by in situ NEXAFS measurements. The left part of Fig. 9 shows carbon K edge NEXAFS spectra of SiC(000-1) surfaces at 1190 and 1250C obtained using a synchrotron light source. All spectra were measured in Auger electron yield detection mode, with the sample maintained at the heating temperature to carry out in situ measurements. The arrangement of the sample and the synchrotron radiation source is shown schematically in the right part of Fig. 9, where the angle between the incident X-rays and the electron energy analyzer was fixed at 60, and the incident angle, θ, is defined as the angle between the light source direction and the sample surface. In Fig. 9, NEXAFS spectra obtained with different θ values are shown for each temperature and are normalized to the highest peaks. The light from the synchrotron source was linearly polarized, so that when θ = 90, the electric field vector, E, is parallel to the sample surface, whereas when θ = 30, E contains components both parallel and perpendicular to the surface.
a) STM image of another region of the sample shown in Fig. 7. (b) and (c) Magnified feature of STM images of the cap structures in (a). (b) and (c) are exactly the same image, except for the open circle and square markers in (c). The large circle on the right is surrounded by six small circles, while the large square on the left is surrounded by five small circles.
As seen in Fig. 9, for both incident angles, and irrespective of the temperature, sharp C-C π* resonance peaks were observed at approximately 285 eV in all spectra. In addition, at 1250C, broad σ* resonances were observed in the region from 290 to 315 eV, accompanied by a sharp σ* bound exciton at ~291.5 eV ((a) and (b)). These two peaks are characteristic of carbon materials composed of well-ordered graphene sheets. Therefore, the spectra in Figs. 9(a) and (b) are expected to be associated with carbon nanocaps. At 1190C, slight differences were observed between the spectra for the two incident angles. At θ=30º, the spectrum was quite similar to that at 1250ºC. On the other hand, at θ=90º, the relative intensity of the σ* to the π* resonance increased, and the σ* bound exciton peak became blurred. It has been reported that for amorphous carbon, the NEXAFS spectrum exhibits a structureless σ* resonance and the relative intensity of the σ* to the π* resonance is higher than that for graphite (Comeli et al., 1988). Therefore, the spectra at 1190C were considered to be derived from a mixture of ordered graphene layers and amorphous carbon. Taking the STM results into account, the spectra at 1190C are associated with crystallization during the production of carbon nanocaps. It is well known that the π* resonance peak is strongly enhanced when the electric field vector of the incident X-rays is parallel to the π* orbitals (Banerjee et al., 2005). Therefore, the increased relative intensity of the π* resonance at θ=30º indicates that the majority of π* orbitals were nearly perpendicular to the surface, that is, most C-C bonds were directed nearly parallel the surface at the beginning of carbon nanocap formation. On the other hand, the carbon nanocaps are dome-like and they consist of graphene sheets with almost the same amount parallel and perpendicular to the SiC surface (Kusunoki et al., 2000, Bang et al., 2006). That is why there was no remarkable difference in the spectra at 1250C for the two incident angles.
Left part: NEXAFS spectra of 6H-SiC(000-1) during heating at 1250ºC (a) and (b), and 1190ºC(c) and (d). The spectra of (a) and (c) were measured at an incident angle of light source was 30º, while those of (b) and (d) were at 90º. Right part: Scheme of registration of angular dependence of NEXAFS, where E and θ is electric field vector and incidence angle of X-ray beam. The incidence angle, θ, is measured as an angle between the direction of X-ray and the sample surface and the angle between the incident X-ray and the electron energy analyzer was fixed at 60º.
One of the most significant and important characteristics of CNT films grown by surface decomposition of SiC is their unique chirality. As stated above, Kusunoki et al. pointed out that the CNTs mostly exhibit zigzag-type chirality (Kusunoki et al., 2002). Taking into account that the carbon nanocaps were the tips of CNTs and that CNTs grow from below the carbon nanocaps, this suggests that they have chemical bonds perpendicular to the SiC(000-1) surfaces at its periphery, connected with zigzag-type CNTs (Fig. 3(c)). On the other hand, considering that aligned CNTs were apt to form on the carbon-face of SiC, Irle et al. pointed out that dangling bonds of carbon-face play a key role to form cap structures, based on quantum chemical molecular dynamics simulations (Irle et al., 2006).
Our XPS and STM results show that amorphous carbon nanoparticles are accumulated on SiC surface before the carbon nanocap formation (Maruyama et al., 2006). These nanoparticles assemble and coalesce as the temperature rises and finally are crystallized to carbon nanocaps. From the NEXAFS results, majority of C-C bonds are directed toward perpendicular to the surface at the beginning of crystallization. Therefore, utilizing dangling bonds on SiC surface, crystallization occurred, which serves to form carbon nanocaps. Considering that the final structure is a dome-like, the bond alignment perpendicular to the surface should occur circumferentially.
On the basis of the various experimental results, we propose a model for carbon nanocap formation by surface decomposition of SiC. Schematic images are shown in Fig. 10. (1) At first, carbon nanoparticles are accumulated as Si atoms are desorbed from SiC surface. (~1100ºC) (2) Upon heating, carbon particles start migration on the SiC surface as a result of the thermal energy, forming clusters of several tens of carbon nanoparticles to reduce the surface energy further (~1150ºC) (Fig. 10(b)). Then, the redistribution of carbon atoms begins within each nanoparticle cluster, and the nanoparticles begin to coalesce (Fig. 10(c)). At around 1200ºC, coalescence proceeds within the clusters, and crystallization occurs, forming CNT nanocaps. In the crystallization, the size of clusters is presumably almost the same as that of the formed nanocaps. Thus, we believe that the size of clusters determines the nanocap size. (5) Above 1200ºC, CNT growth into SiC proceeds by the sublimation of Si atoms from the SiC(000-1) surface. The NEXAFS spectra which suggest that the C-C bonds are directed nearly parallel to the surface at the beginning of crystallization, indicates that the direction of C-C bonds were changed during the crystallization. (Some difference might be seen in the measurement temperature between STM and NEXAFS because of the detection limitation of a pyrometer.) Taking into account the final structure of carbon nanocaps, we speculate that crystallization occurs at the periphery of amorphous carbon dome, and formation of C-C bonding utilize the dangling bonds from carbon atoms on the SiC(000-1) surface (Fig. 10). From the standpoint of crystal growth, this means that nucleation starts to occur at the edge in the carbon nanocaps.
Schematic model of the carbon nanocap formation process during surface decomposition of SiC. (a) formation of carbon nanoparticles by surface decomposition of SiC, (b) aggregation of carbon nanoparticles, (c) coalescence, (d) start of crystallization utilizing the dangling bonds, (e) progress of crystallization, and (f) complete formation of carbon nanocap. (The portion consisting of elementary carbon is shown as grey area.)
Recently, graphene growth from SiC(000-1) carbon-face by surface decomposition has been reported and a lot of researchers have been focusing on it because of its superiority in electronic property (Jernigan et al., 2009, Tedesco et al., 2009). From the point of view of growth technique, the method of graphene growth on SiC(000-1) is remarkably similar to that of CNT growth by surface decomposition, but one significant difference is the heating rate. In the growth of graphene, in general, the temperature of SiC is quickly increased to the growth temperature, typically, about several minutes to ~1400ºC (Gamara et al., 2008). On the other hand, in the CNT growth by surface decomposition, the heating rate is typically 1-15ºC/min (Kusunoki et al. 1999, 2002) and much slower than that in the graphene growth. This low heating rate might be necessary to enhance the migration of carbon atoms, assembling and leading to formation of carbon nanocaps.
In early studies, Kusunoki et al. proposed a chemical reaction process for CNT growth by surface decomposition of SiC as follows (Kusunoki et al. 1999):
In their CNT growth, heating of SiC was carried out using a vacuum electric furnace whose pressure was about 10-2 Pa. In this circumstance, residual gases, such as O2, H2O, CO etc., should exist in the furnace during the growth. They considered that these residual gases reacted with Si atoms on SiC surface, leading to the desorption.
Fig. 11. shows C 1s XPS spectra for 6H-SiC at 1270ºC under various oxygen pressures. The main peak at around 284.3 eV and the shoulder peak at around 282.7 eV are derived from carbon sp2 and SiC components, respectively, and these spectra are normalized with the main peaks. It is clearly shown that the ratio of the peak intensity of the SiC component to that of the carbon sp2 component decreased as the oxygen partial pressure increased, confirming that oxygen enhances the decomposition of the SiC surface and promoting the carbon nanocap formation. Thus, surface reaction represented with eq. (2) seems to be reasonable. In the case of CNT growth in a vacuum electric furnace, the main reaction may be replaced by the reactions as follows, since residual gases are mainly composed of CO and H2O.
or
As for the reaction of oxygen with SiC surface, thermal oxidation of SiC surface has been an interesting theme from a fundamental surface science perspective, since it is chemically much more complex than that of Si. So far, three distinct regions have been observed in the phase diagram describing the SiC+O2 interaction; “passive oxidation”, “active oxidation” and “surface segregation of carbon” (Song & Smith, 2002). In the passive oxidation, which occurs under high oxygen pressure and low temperature, SiO2 layer grows on the surface, and, in the active oxidation, which occurs under low oxygen pressure and high temperature, SiC surface is etched by the reaction with oxygen. In addition, under the lower oxygen pressure and the higher temperature, surface segregation of carbon has been observed. The CNT growth by surface decomposition of SiC should occur under the third mode where segregation of carbon atoms proceeds on the surface. However, it has not been well investigated between the reaction with oxygen gas and the CNT growth in surface decomposition of SiC. To clarify these, it is necessary to minutely control oxygen pressure and investigate the relation among the pressure, temperature and surface decomposition of SiC during the CNT growth.
Fig. 12 shows a phase diagram for the interaction of O2 with the SiC surface, where formation of carbon nanocaps and SiO2 are separately shown (Maruyama et al., 2007). All data were obtained by heating the 6H-SiC(000-1) in a vacuum electronic furnace and in a UHV chamber where the oxygen gas was introduced by controlling the pressure, and the heating rates were kept below 1ºC/min which were low enough to form carbon nanocaps. In the figure, the surface covered with carbon nanocaps, elemental carbon (not formed nanocaps), SiO2, and tiny amount of SiO2 (weak SiO2 peak was observed in XPS spectra) are shown as open circles, open squares, solid squares and solid triangles, respectively. In addition, the boundary between passive oxidation (P. O.) and active oxidation (A. O.) and that between active oxidation (A. O.) and “surface segregation of carbon (S. C) ” which were obtained by extrapolating the experimental results for thermal oxidation of 6H-SiC(000-1) reported by Song and Smith (Song & Smith 2002) to wider ranges in both oxygen pressure and temperature. In their data, the critical oxygen pressure at which the active-transition occurred was estimated to be,
C 1s XPS spectra for 6H-SiC(000-1) after heating at 1270ºC for 30 min under UHV and various oxygen partial pressures (10-4 and 10-3 Pa).
Phase diagram for the interaction of O2 with the 6H-SiC(000-1) face. Our experimental results are indicated: the open circles, open squares, solid squares and solid triangles correspond to the surfaces covered with carbon nanocaps, elemental carbon (not formed nanocaps), SiO2, and tiny amount of SiO2. The active-passive oxidation (A. O. –P. O.) and active oxidation (A. O.) - “surface segregation of carbon” (S. C.) boundaries reported by Ref. (Song and Smith, 2002) are also shown as thick solid line and dashed line, respectively.
where P0=2.7×1015\n\t\t\t\tPa and ΔE = 4.8 eV. It should be noted that carbon nanocaps were formed in the “surface segregation of carbon” region, and formation of carbon nanocap was observed above 1200ºC, irrespective of the ambient pressure. This indicates that the heating above 1200ºC is necessary to coalesce and crystallize amorphous carbon layer to form nanocaps.
Previous studies reported that graphitization of amorphous carbon occurs just above 1000ºC (Botti, 2005; Chadderton & Chen, 1999). In the case of CNT growth by surface decomposition of SiC, both accumulation of sufficient carbon atoms and carbon migration are important to form carbon nanocap. This might lead to necessity of the higher temperature. On the other hand, SiO2 layers were formed on the SiC surface in the passive oxidation region, except for the UHV region, where slight elementary carbon was seen because of insufficient oxygen gas. Although, in our experimental result, data were not obtained in the just active oxidation region, shown between the dashed line and solid line, it was clearly shown that carbon nanocaps were formed above 1200ºC in the “surface segregation of carbon” region.
Effect of hydrogen gas on carbon nanocap and CNT formation is another interesting theme, since reduction of residual oxides on SiC surfaces has been reported after annealing SiC in ambient hydrogen gases (Seyller, 2004) and this may affect the formation of carbon nanocaps. Figure 13 shows survey XPS spectra for SiC(000-1) surfaces after annealing at 1250ºC for 30 min in a hydrogen atmosphere at various pressures (Ueda et al., 2010). The O 1s peak was not observed for the samples annealed at 10-3 and 10-2 Pa, whereas the O 1s peak was clearly observed for that annealed at 10-4 Pa. Figures 14(a) and (b) shows Si 2p and C 1s spectra for 6H-SiC(000-1) after annealing at 1250ºC in a hydrogen atmosphere of 10-2 Pa.
XPS survey spectra for 6H-SiC(000-1) substrates after annealing at 1250ºC in a hydrogen atmosphere of: (a) 10-2, (b) 10-3 and (c) 10-4 Pa.
For comparison, Si 2p spectrum of the sample after annealing at 1250ºC in a UHV is also shown in (c). In the Si 2p spectrum for the sample after annealing in a hydrogen atmosphere, only SiC component was observed and the component of SixCyOz related oxides were negligible, while there still remain some oxides after annealing in a UHV. These results confirm removal of residual SixCyOz oxides by annealing a hydrogen atmosphere of sufficient high pressure, as reported by Seyller. Figure 14(b) shows a C 1s XPS spectrum of the same sample. Except for a peak derived from adsorbed CO molecules, the spectrum consists of only a SiC-component at 282.7 eV and carbon sp2 hybridization bonding at 284.3 eV, and no SixCyOz related oxides components were observed, consistent with the Si 2p spectrum in (a).
a) Si 2p and (b) C 1s XPS spectra for 6H-SiC(000-1) substrates after annealing at 1250ºC in a hydrogen atmosphere of 10-2 Pa. (c) Si 2p XPS spectrum for 6H-SiC(000-1) substrates after annealing in a UHV. All spectra were deconvoluted into a set of Gaussian peaks after implementing background subtraction that accounted for previous XPS spectra of SiC (Hornetz et al., 1995).
STM images of 6H-SiC(000-1) for 30 min after annealing at 1200ºC in (a) a UHV and (b) a hydrogen atmosphere of 10-2 Pa.
STM images of SiC(000-1) substrates after annealing at 1200ºC for 30 min in the UHV and a hydrogen atmosphere of 10-2 Pa are shown in Fig. 15 (Ueda et al., 2010). The images reveal that convexities corresponding to carbon nanocaps were presented over the entire surface, independent of the annealing conditions. On the sample surface annealed in a UHV, the resulting carbon nanocaps were mainly in the diameter range of 1-3 nm, but nanocaps of more than 4 nm were observed. There were also some areas where no carbon nanocaps were formed. On the other hand, carbon nanocaps whose diameters were mainly distributed between 3 and 4 nm were formed on the SiC surface annealed in a hydrogen atmosphere, as shown in Fig. 15(b). The change in the diameter distribution is summarized in Fig. 16, which shows histograms of carbon nanocap diameter after annealing in a hydrogen atmosphere of 10-2 Pa. They indicates that the distribution of carbon nanocap diameter after annealing in the hydrogen atmosphere was narrower than that found in the UHV, demonstrating that the homogeneity of carbon nanocaps can be improved by reducing the native oxide from the SiC(000-1) surface.
Histograms, (a) and (b), of carbon nanocap diameter correspond to the samples shown in Fig. 15(a) and (b), respectively.
XPS result suggests that native SixCyOz oxide on 6H-SiC still remain even after carbon nanocap formation without pre-annealing in H2 ambient (Fig. 5(b)). Therefore, carbon nanocap formation should be disturbed among the areas covered with the oxides, because those areas should be suppressed sublimation of Si atoms. Such a localized suppression will induce an inhomogeneous distribution of an amorphous carbon layer, which, in turn, will have a deleterious effect on the size uniformity of the resulting carbon nanocaps. On the other hand, if there is no native oxide on the surface, simultaneous desorption of Si atoms would occur and homogeneous distribution of amorphous carbon layer would be formed. This process would produce carbon nanocaps with a uniform size.
CNT growth by surface decomposition of SiC is not only an interesting method as peculiar crystal growth but also has various characteristics useful for device applications. Development of this growth technique should directly lead to realization of CNT devices in future, replaced by conventional semiconductor devices. There still remain several problems to be solved for fabrication of CNT devices. To understand its growth mechanism is essential to control structural parameters of CNTs, which is absolutely necessary for realization of CNT devices. To clarify the formation process of carbon nanocaps, which are precursors of CNTs, determining the structures of CNTs, is the first step to reach this objective.
The authors are grateful to Prof. Amemiya for his help during NEXAFS measurements and also thank Dr. Ito, Mr. Kawamura, Ms. Fujita and Mr. Tanioku for assisting with our study on STM observation. A part of this work was supported by the Japan Society for the Promotion of Science (JSPS), a Grant-in-Aid for Scientific Research (C) 17560015 and 21510119, and by the Ministry of Education, Culture, Sports, Science and Technology (MEXT) through the 21st century COE program “Nano Factory”. We are grateful to Professor T. Yokoyama and Dr. T. Nakagawa of the Institute for Molecular Science (IMS), Okazaki, for providing the XPS facility through the Nanotechnology Support Project in Central Japan, financially supported by the Nanotechnology Network. The NEXAFS measurements were performed under the approval of Photon Factory Program Advisory Committee (Proposal No. 2009G530). We would also like to to thank the Academic Research Institute of Meijo University for their financial support.
In this chapter we will be briefing about the emulsion and its types. We will also be discussing in detail about nanoemulsions, its types, fabrication, application and its properties.
\nAn emulsion system generally consists of two or more liquids that are immiscible. They are a type of colloids, which are two-phase systems of matter. In emulsion systems, the two phases are dispersed and continuous. One liquid is dispersed (the disperse phase) in the other (the continuous). The different types of emulsion systems can include: oil-in-water (o/w), water-in-oil (w/o), and oil-in-oil (o/o) [1]. The oil-in-oil phase can be polar oil dispersed in non-polar oil, or vice versa. An emulsifier is usually used to disperse immiscible liquids. The emulsifier also plays an important role in the formation and long-term stability of the emulsions. Emulsions can also be classified on the type of emulsifier or the structure of the system. Emulsions being liquids do not have any static internal structure. The droplets are assumed to be statistically distributed in the liquid matrix. According to IUPAC, in emulsions the droplets can be amorphous, liquid-crystalline, or any mixture. The droplet diameters in the dispersed phase range between 10 nm and 100 μm (which may exceed the size limits for colloidal particles) [2]. Some common example of emulsion systems are homogenized milk, some cutting fluids for metal working, egg yolk is an emulsion with the emulsifying agent lecithin, butter is an emulsion of water in fat, and an emulsion of silver halide in gelatin is used as a coating in the photosensitive side of a photographic film [3].
\nEmulsion system can be classified based on their droplet size as macroemulsion, nanoemulsion, and miniemulsion (Table 1).
\nEmulsion type | \nDroplet size (μm) | \n
---|---|
Macroemulsion | \n1–100 | \n
Microemulsion | \n10–100 | \n
Nanoemulsion | \n20–500 | \n
Emulsion type and its droplet size [4].
Emulsion systems find a wide range of applications in the field of food, cosmetics, agriculture, pharmaceuticals (preparation of drugs and drug delivery).
\nAs the name suggests, the size of the droplets in this type of emulsion is in nanometer ranges. They not only differ in size but also in the many properties and method of preparation. The main difference between nanoemulsion and conventional emulsion (macroemulsion) is the size and shape of the droplets in the continuous phase. In macroemulsion, the shape is usually spherical but in nanoemulsions a variety of shapes can be seen like swollen micelles and bicontinuous structures. Though micro and nanoemulsions are similar in their sizes the method of preparation differs between them. Both of them require energy inputs, but nanoemulsions mostly use mechanical shear while micro emulsions make use of spontaneous emulsification methods. Microemulsions also need a high surfactant concentration compared to nanoemulsions. The application of nanoemulsion in pharmaceutical, food, cosmetic, and chemical industry is comparatively more than microemulsion since moderate surfactant concentration is sufficient for their making [5].
\nNanoemulsions are said to be kinetically stable and thermodynamically unstable. Their stability can be altered by their preparation methods like adding specific co-surfactants. They usually use high energy methods for their preparation but low energy based methods can also be used with the help of some special conditions using certain chemical potential of the component [6]. Nanoemulsions are said to be transparent, biodegradable, and biocompatible. Normal emulsions usually undergo sedimentation by gravity, which is overcome by nanoemulsions. Nanoemulsions exhibit Ostwald ripening phenomenon. Due to this, small molecules collide and form large globules. To overcome this, co-surfactants are added or second oil is added to the dispersion phase. Proper manufacturing procedure also helps overcome Ostwald ripening [7]. Nanoemulsions provide a wide surface area and so allow active components to penetrate easily and faster. Another important characteristic of nanoemulsion is their transparent optical property. This is mainly due to their size, which is one fourth of the wavelength of visible light [8]. Nanoemulsions have the ability to solubilize both hydrophobic and hydrophilic substances, and hence enhance their permeability and bioavailability [9]. This makes them very useful as drug delivery systems for both the type of drugs.
\nNanoemulsions are also said to have tunable rheological properties. They are tuned by controlling the dispersed phase volume, droplet size or the addition of salt and depletion agents [4]. Hence nanoemulsions can be tuned from being a free flowing fluid to a gel like substance [10]. Addition of polymers also tunes the rheological properties. The polymers associate either with themselves or with the nanoemulsions. A thermo reversible gel was made, where a polymer gelator (with two hydrophobic end groups) was added. At temperatures greater than the gelling temperature, the polymer’s two hydrophobic ends bridges with the nanoemulsion droplets making them a gel. At lower temperature, they detach and hence return to a transparent fluid like structure.
\nThere are three types of nanoemulsion based on the composition:
Oil in water: oil droplets are dispersed in continuous aqueous phase.
Water in oil: water droplets are dispersed in continuous oil phase.
Bi-continuous (double): micro domains of oil and water are interdispersed within the system [11].
As already mentioned, nanoemulsions are being used in a wide range of fields. There is a lot of research and development work done in the field of nanoemulsions. Many bioactive substances are present in natural available substances, emulsification of these bioactive components is a trending research topic. In September 2018, water compatible form of coconut oil through nano-emulsification was developed [12]. The nanoemulsion was made successfully using PHC as a surfactant at a concentration of 5% {w/w}. Nanoemulsions have also found an important space in field of pharmaceuticals. Many of the oral drugs synthesized do not have aqueous stability almost insoluble) and have low bioavailability. A low energy method to make composite hydrogel beads encapsulated with single and multiple hydrophobic drugs was developed [13]. This makes nanoemulsions a promising carrier of hydrophobic drugs. It was shown that nanoemulsions were used to enhance the antileishmanial activity of Copaifera spp. oleoresins against both Leishmania amazonensis and Leishmania infantum strains [14].
\nRecently a new technique for making Pickering nanoemulsions using Silica nanoparticles was developed which is highly scalable and energy efficient. Nanoemulsions are usually stabilized using surfactants. The use of surfactants has some disadvantages which include surfactant desorption and Ostwald ripening. Hence a new interest of making nanoparticle stabilized nanoemulsion (Pickering nanoemulsions) has evolved. Nanoparticles have higher desorption energy barrier. However, the limitation of nanoparticles as stabilizing agent was obtaining the size in nano-range. In the traditional method to make Pickering emulsions (high energy and low energy methods, described in the next section) many steps were involved, a single step method was developed using vapor condensation. Moreover the traditional methods used in the preparation of Pickering nanoemulsions had some disadvantages. High energy methods reduced the adsorption of the particles on the droplets while, low energy methods were unable to produce Pickering nanoemulsions and clogging of nanoparticles was seen. The concentration of nanoparticles required in the new methods was also less compared to that required in traditional methods. In this process, oil was taken and cooled below the dew point, during which the water condenses on the oil. If the oil has the right properties and sufficient concentration of nanoparticles, then water drops self-disperse within the oil. The nanoparticles then will self-assemble around them to form nanoemulsions [15]. Nanoemulsions are studied in great detail due to their potential applications. Improvements in their preparation methods and the fields in which they can be used are the ongoing trends in nanoemulsions.
\nThe fabrication of nanoemulsion involves the preparation of macroemulsions and then it’s conversion to nanoemulsion by various methods, all of which can be categorized into either Low energy or High energy methods [5, 16]. Techniques which involve modification of factors responsible for the hydrophilic–lipophilic balance come under Low energy methods and those that use mechanical devices to break down the particles to small sizes are referred to as high energy methods. As much as composition is responsible for the properties of the nanoemulsion so is the technique used for its preparation. In this section a brief insight is given on a few widely used methodologies.
\nIn contrast to the low energy methods for nanoemulsion formation, high energy methods require the use of many devices which uses mechanical or chemical energy as input to form small droplets because they are non-equilibrium systems which cannot be formed spontaneously [17]. These devices often entail a huge initial cost as well as expenses to maintain throughout use. The purpose of these devices in high energy methods is to provide intense mechanical energy that helps to break up macroscopic phases or turn larger droplets into smaller droplets [18]. These devices provide forces so strong that it disrupt water and oil phases to form nanoemulsions. In high energy methods, input energy density is about 108–1000 W/kg. The required energy supplied is in very shortest duration of time to the system in order to obtain homogeneous small sized particles. In addition to this, the high energy methods for 55 nanoemulsion formation are not limited by the types of oil and emulsifiers that can be used like the low energy methods are. At present high energy methods are more frequently utilized in the food industry than low energy methods with high pressure valve homogenization, microfluidization, and sonication being the most common [19]. All this high energy methods are impacted by emulsion component characteristics (i.e. oil, type, surfactant type, surfactant concentration, viscosity, etc.) and equipment characteristics (i.e. size of the equipment, pressure used, number of passes/time in equipment, design, etc.). The input energy density is about 108–1010 W/kg [20]. These parameters should be optimized for each and every system and high energy method.
\nHPVH is the most popular method used for the production of nanoemulsions. The most common use is in applications from ketchup processing to milk homogenization and to manufacture nanoemulsions that particle sizes are up to 1 nm [18]. When using a HPVH, a coarse emulsion is initially made using a high-speed mixer, fed into the input valve of the HPVH, and then flowed between the valve seat and valve at a high velocity. The macroemulsion is forced to pass through a small orifice at an operating pressure between 500 and 5000 Psi [18]. Since several forces like hydraulic shear, intense turbulence and cavitation act together extremely small droplet sized nanoemulsions are achieved. The process is repeated till the final product reaches our desired droplet size and polydispersity index (PDI). Lower the PDI means higher uniformity of droplet size in nanoemulsions. Mono-disperse samples have PDI lesser than 0.08, narrow size distribution range is 0.08–0.3 and PDI greater than 0.3 indicates broad size distribution [18].
\nWith an increase in velocity, the pressure decreases causing an instantaneous pressure drop and encouraging the coarse emulsion to impinge on the impact ring [21]. Sometimes HPVH passes through two valves and thus emulsion production will break up into two stages: in the first stage the droplets are broken up and in the second stage a lower pressure is utilized to disrupt any ‘flocs’ formed by the initial valve [22]. Obtaining submicron levels requires large amount of energy and high temperature which can deteriorate the components. Thermolabile compounds like proteins, enzymes and nucleic acids may be damaged easily [18] (Figure 1).
\nSchematic representation of high pressure valve homogenizer [18].
Emulsions produced by sonication use ultrasonic homogenizers (UH) to provide high intensity of ultrasonic waves to the sample. The frequency of the waves (29 kHz or larger) is higher than the maximum audible frequency of human ear (16–18 kHz) [17]. These waves provide around 56 disruptive forces to breakup oil and water phases thus forming small droplets on the principle of cavitation. Input energy comes from a sonicator probe which can be directly placed in the sample. There are two mechanisms which take part in sonication [17]. Firstly, acoustic field creates interfacial waves which makes oil phase to disperse in the continuous phase as droplets. Secondly, ultrasound provokes acoustic cavitation which provides formation and collapse of microbubbles respectively since there is a pressure fluctuation of a single sound wave [23]. By this enormous levels of highly localized turbulence is generated and it causes micro implosions which disrupt large droplets into sub-micron size. Since most of the ultrasonic systems emits sound field which are inhomogeneous, so in order to have droplets to experience highest shear rate, recirculation of the emulsion through the region of high power must be provided and on repeating recirculation we obtain uniform droplet size at dilute concentration [18].
\nPresently sonication has been well established for the laboratory scale but it may be difficult to implement on a production scale because of issues like low throughput. Optimization of parameters (like emulsifier type, amount emulsifier and viscosity of phases) is necessary to prepare nanoemulsions having fine droplets [18]. Even, the high local intensity provided by sonication could lead to detrimental quality effects by way of protein denaturation, polysaccharide polymerization or lipid oxidation of the emulsion components [23] (Figure 2).
\nSchematic representation of ultrasonic jet homogenizer [23].
Microfluidization is the most widely employed and novel technique in the pharmaceutical and cosmetic industry in order to acquire fine emulsions [18]. High pressure is provided by device called Microfluidizers (MF). Initially a coarse emulsion is made using a high speed mixer which is then fed into the hood and accelerated at high velocities within the channels using a pumping device and the macroemulsion to go through the interaction chamber by the high pressure forces and thus nanoemulsions with submicron ranged particles are produced [17]. The channels are made to collide into each other within the interaction chamber [21]. Uniform nanoemulsion can be produced by repeating the process many times and vary the operating pressure to get desired particle size [18].
\nThe main parts of a MF include a fluid inlet (where the coarse emulsion is fed), a pumping device (to help move the emulsion through), and the interaction chamber or nozzle (where the particle collision occurs) [22]. A collision between crude emulsion jets from two opposite channels in the nozzle of microfluidizers is observed. The mobility of crude emulsion is supplied by a pneumatically powered pump that has capability of compressing air up to pressures between 150 and 650 MPa [18]. This high pressure forces the crude emulsion stream to go through microchannels and after the collision of two opposite channels enormous level of shearing force is produced. Hence, by the help of this force fine emulsions are produced [23] (Figure 3).
\nSchematic representation of microfluidizer [23].
Requiring no expensive equipment, easier implementation and better efficiency in terms of energy are the reasons for the growing interest in low energy methods [16, 17, 24, 25]. Moreover, encapsulation of drugs and macromolecules can be carried out due to mild operating temperatures. The necessity for higher amounts of surfactants may be a downside [17]. The whole concept of low energy synthesis has its roots in modification of factors responsible for the hydrophilic–lipophilic balance of the surfactant-oil–water mixture [26]. These include environmental factors like temperature, composition and the chemical potential of the components. Spontaneous Emulsification (SE) and Phase Inversion are two commonly implemented synthesis [17, 24].
\nAn emulsion can be fabricated by diluting a biphasic system leading to diffusion of one phase to another. This is usually done by adding the organic phase into the aqueous phase and then a surfactant which is water miscible. The migration of the surfactant causes disorder at the interface of the two phases leading to an increase in the surface area along with the formation of oil droplets in the aqueous phase [16].
\nTo obtain nanoemulsions, the same dilution process is performed on microemulsions. The properties of the nanoemulsion depend on the oil viscosity, surfactant hydrophilic–lipophilic balance and solvent miscibility with water. With the help of an appropriate dilution procedure and composition, both W/O and O/W microemulsions can be used to obtain nanoemulsion. While obtaining it from O/W microemulsion the composition of microemulsion and the procedure of dilution does not matter, whereas while starting with W/O microemulsion the dilution procedure and /or the composition of microemulsion matters. O/W and W/O nanoemulsions can be formed even without a surfactant, this is called the Ouzo effect also known as Solvent displacement method [24, 27, 28]. This phenomenon has mainly been used for fabricating polymeric nanoparticles or nanocapsules using nanoemulsion as a template in drug delivery [25].
\nAs addressed earlier, there are different types of Nanoemulsions, either oil in water (O/W) or water in oil (W/O). Phase inversion, as the name suggests, is a fabrication method that involves conversion of O/W to W/O emulsion or vice versa. It utilizes the energy released during this conversion for the formation of droplets. This physical process can be brought about by varying the temperature or phase volume ratio, giving rise to phase inversion temperature (PIT) method and phase inversion composition (PIC) method [29].
\nIn these emulsification methods it is very important to know the behavior of the surfactant as it plays a significant role in minimizing both droplet size and polydispersity of the nanoemulsion formed. Its properties also depend on the kinetics of the emulsification process, especially if they have high viscosity [27].
\nThe Phase inversion temperature (PIT) method is used when the surfactants are sensitive to changes in temperature. The principle of this method is based on the changes in surfactant spontaneous curvature (molecular geometry) with temperature. For example, in poly(oxyethylene)-type non-ionic surfactant, increase in temperature causes dehydration of the poly(oxyethylene) chains whereas at low temperature these chains are hydrated and hence are hydrophilic in nature. At one temperature the surfactant exhibits both hydrophilic and lipophilic properties, this temperature is known as HLB temperature (Hydrophilic–Lipophilic Balance) [17, 27]. So, at this temperature the surfactant is equally soluble in the oil and aqueous phase [16, 17].
\nUsing PIT very small sizes of droplets can be obtained. At the HLB temperature due to the low interfacial tension the surfactant forms a layer but as soon as the temperature is changed by quick cooling or heating, the surfactant molecules move from one phase into another resulting in the formation of small oil droplets. The movement of the surfactant molecules depends on its hydrophilicity or lipophilicity of its chain which in turn depends on temperature [16, 17] (Figure 4).
\nShows the curvature of surfactant and the favorable emulsion formed by heating and cooling [16].
Phase inversion composition is performed when the surfactant properties changes due to dilution of one of the phases. It involves dilution of oil phase with water or vice versa which causes an increase or decrease in hydration degree of surfactant. In phase inversion composition, phase transition takes place at constant temperature. At one point in the dilution process the affinity of the surfactant becomes equal for both the phases that is it exhibits both hydrophilic and lipophilic properties. This point is known as the emulsion inversion point [4]. At this stage a layer of microemulsions is formed. A slight change in the proportion of oil and water causes instability of the microemulsion layer which disintegrates to form nanoemulsion that are kinetically stable. It was found out that with further dilution the droplet size does not change [28]. The properties of the nanoemulsion obtained depends on conditions such as shear rate and the addition rate [30]. Heat sensitive compounds can be encapsulated by using this fabrication method for nanoemulsions.
\nTo obtain an O/W nanoemulsion, initially a W/O microemulsion (consisting of surfactant) is required to which aqueous phase is added in a controlled manner. The resulting system is stirred for breakdown of the residues and for homogeneity [24]. This process is depicted in Figure 5.
\nShows the process of phase inversion by dilution with aqueous phase [4].
A great attention is given towards the use of nanoemulsions in research, dosage form design and pharmacotherapy owing to their optical clarity, ease of preparation, thermodynamic stability and increased surface area. Some of the problems associated with conventional drug delivery systems such as low bioavailability and noncompliance which can be overcome by nanoemulsions are discussed here (Figure 6).
\nApplications of nanoemulsions in drug delivery [31].
It is the most effective form of drug delivery system usually adopted for active ingredients with low bioavailability and narrow therapeutic index. Here the therapeutic peptides or drugs prepared in the form of solutions or suspensions, are given as injections. Intravenous, intramuscular and subcutaneous drug delivery systems are the most commonly used parenteral routes.
\nDissolution of enormous amounts of hydrophobic compounds coupled with mutual compatibility and ability to safeguard drugs from hydrolysis and enzymatic degradation make nanoemulsions ideal vehicles for parenteral transport [32]. Nanoemulsions help in sustained and controlled drug delivery through parenteral routes. Since nano emulsions are cleared more slowly (more residence time) than the coarse particles, they are advantageous over macroemulsion systems when delivered parenterally [33].
\nNanoemulsions loaded with thalidomide have been synthesized. A dose as low as 25 mg leads to plasma concentrations which can be therapeutic when delivered through this system [34].
\nOwing to patient compliance, convenience, ease of formulation and higher absorption in the intestine, oral drug delivery is the most widely distributed and preferred form of drug administration.
\nWhen compared to conventional oral formulations, nano emulsion formulations provide several benefits in oral drug administration. Some of these benefits include increased absorption, improved clinical potency and decreased drug toxicity [33]. Hence, drugs such as steroids, hormones, diuretics and antibiotics can be ideally delivered using nano emulsions.
\nTopical drug delivery also has several advantages over other modes of drug administration such as the avoidance of hepatic first pass metabolism, reduction of toxicity and targeted drug delivery to the affected portion of the skin. Here self-administration is also possible. The transparent nature and fluidity of nanoemulsions not only gives a pleasant skin feel but also helps in eliminating the drug input by just removing the transdermal patch without any irritation [32].
\nOwing to the large surface area of the droplets, nanoemulsions enable rapid penetration of active ingredients through the skin. This is one of the most valuable properties of nanoemulsions due to which the use of special penetration enhancers which cause incompatibility of the formulation can be minimized [33].
\nFor the treatment of eye diseases, drugs are delivered topically in ocular dosage forms such as solutions, suspensions and ointments. Due to physiologically protective mechanisms such as tear dilution, lacrimal drainage, protein binding and enzymatic degradation which are activated as soon as the ophthalmic solutions of the drug are applied, typically less than 3% of these topically applied drugs permeate the corneal epithelium, reach the aqueous humor and finally enter the systemic circulation. O/W Nanoemulsions (Oil in Water nano emulsions) have been researched for ocular administration to dissolve poorly soluble drugs, to increase absorption and also to attain prolong release profile [33].
\nCationic submicron emulsions are promising carriers for DNA vaccines to the lung since they are able to transfect pulmonary epithelial cells thereby inducing cross priming of antigen-presenting cells and directly activate dendritic cells, resulting in stimulation of antigen-specific T-cells [35].
\nThere might be adverse side effects of oils and surfactants on the alveoli of lungs. Hence extensive studies are required for the development of successful inhalable submicron emulsions for pulmonary delivery [32].
\nNanoemulsions serve as a waterproof medium for bio-catalytic or enzymatic reactions to occur. The enzymes in low water content exhibit greater solubility in non-polar reactants and higher thermal stability. As a result, the thermodynamic equilibrium also shifts towards condensation [36].
\nReactions such as synthesis of esters, peptides and sugar acetals transesterification, hydrolysis and steroid transformation are catalyzed by enzymes in nano-emulsions. Lipases are the most widely used class of enzymes in microemulsion-based reactions [33].
\nThe non-toxic disinfectant cleaner developed by Enviro Systems Inc. has wide applications in commercial markets such as healthcare, hospitality, travel, food processing, and military. This product which kills a wide spectrum of bacteria, virus and fungi in 5–10 minutes without any hazards needs no warning labels. This can be absorbed through the skin, inhaled or swallowed without causing any irritation to the eyes and does not cause any harmful effects [33]. One such NE is Parachlorometaxylenol (PCMX) marketed as EcoTru [36].
\nLipophilic compounds such as flavors, omega3fatty acids, vitamins, nutraceuticals and preservatives can be encapsulated, stabilized and delivered using nanoemulsions. This is one of the emerging fields in the food industry [37]. Research is mainly focused on nanoemulsion technology that is suited for functional foods.
\nEncapsulation is a useful technique to deliver bioactive molecules within living cells. Here, the bioactive ingredient is entrapped in a core or filled within a carrier (coating, matrix, membrane, capsule, or shell) [38].
\nThis technology is used in food industry to:
Mask the unpleasant taste or odor of some bioactive materials.
Increase the bioavailability of some components.
Improve stability of food ingredients.
Decrease air-induced food degradation.
Reduce Evaporation of food aroma.
Another important application of this technique that is worth mentioning is in probiotics [38]. (Probiotics are the microorganisms that provide health benefits when consumed in adequate amounts) (Figure 7).
\nApplications of nano-emulsion based delivery systems in food industry [38].
Biologically active lipids such as omega-3 fatty acids can be encapsulated by nano-emulsions from food grade ingredients. Omega-3 fatty acid supplementation has a protective effect against cancer, cardiac death, sudden death, cognitive aging, asthma, inflammation and myocardial infarction [38]. α-Linolenic acid (ALA), an Omega-3 fatty acid, is one of two essential fatty acids together with linoleic acid. ALA is necessary for health and cannot be synthesized within the human body [38].
\nWhat are cosmetics?‘Personal Care Products’ or ‘Beauty Products’ such as skin creams, lotions, perfumes, lipsticks, fingernail polishes, eye and face make-up products, hair dyes and deodorants which are used by people to cleanse or change the look of the face or body are cosmetics. They do not alter the body’s structure and function. Cosmetics are superficial and can also be therapeutic.
\nNanoemulsions are potential vehicles for optimum dispersion of active ingredients and their controlled delivery in particular skin layers. Their lipophilic interior makes them more suitable for the transport of lipophilic substances when compared to liposomes. Small sized droplets and high surface area of nano-emulsions contribute greatly in inhibiting inherent creaming, flocculation, sedimentation and coalescence which are frequently observed in macroemulsions [33]. They have gained popularity in cosmetics due to ease of permeability and penetration into the skin owing to their small size and high surface area, solubility, transparency and color.
\nAdvantages of using Nanoemulsions in cosmetics
As mentioned earlier, nano-emulsions help to overcome problems such as inherent creaming, flocculation, coalescence, and sedimentation.
Relatively less surfactants (5–10%) [39] are used for nano-emulsion formulation (approved for human use) making them non-toxic and non-irritant. Hence, they can be easily applied onto the skin and mucous membranes [40].
Healthy human and animal cells are not damaged by nano-emulsions. As a result, they are best suited for human and veterinary therapeutic purposes [40].
Nano-emulsions can also be easily formulated in the form of foams, cream, liquids, sprays.
Significant improvement in dry hair aspect (after several shampoos) is obtained with a prolonged effect after a cationic nanoemulsion use [39].
Oil in water nanoemulsions, due to their lipophilic interior have numerous applications in cosmetics such as formulation of lotions, sunscreens and skin creams, hair care products and make up removal substances. Other extremely important and fast growing applications include Emulsion based wet wipes and PEG (Polyethylene glycol) free nanoemulsions [40].
\nThe recent trends are shifting towards highly effective safer and natural cosmetic products. Cosmetic manufacturers are developing new methods to prepare nano versions of formulations for better permeability, effectiveness and increased customer satisfaction. This new technology is based on manufacturing low viscosity oil in water nanoemulsions which are free of synthetic chemicals like PEG. The phase inversion method of fabricating nanoemulsions leads to an important application in the cosmetic industry -formulating lotions to be impregnated in wet wipes. These are primarily used for make-up removal and wet wipes [11].
\nIndustries are working on developing low energy methods coupled with low input homogenizers and absence of PEG, energy input for heating/cooling steps to formulate natural products [11]. The main constituents of this formulation are PEG free emulsifiers, cosmetic oils in high amounts and co-surfactants. When water is added to such a liquid and clear oil phase, a temporary micro-emulsion is formed which is then converted to stable, low-viscosity nanoemulsion. This low viscous phase is beneficial as it helps in converting the emulsion from water in oil to oil in water nanoemulsion. This step being dependent on water concentration is termed as phase inversion concentration which occurs by elimination of the co-surfactant into water. Some of these products developed are TEGO Wipe DE and TEGO Wipe DE PF which are based on nanoemulsions impregnated in wet-wipes and also used for lotions and sprays [41, 42].
\nThe human body is protected from external harm such as chemical and micro-organism intrusion, UV exposure, dryness and mechanical damage by a natural barrier, the skin.
\nHence the multi-layered skin serves as the first line of body defense. The external and internal layers of the skin mainly include the stratum corneum (composed of dead keratinized cells) and below the stratum corneum are the epidermis, dermis and the subcutaneous tissue. The excellent barrier properties of the skin are due to the presence of lipid matrix (containing ceramides, fatty acids, cholesterol and cholesteryl esters) among the keratinized cells which has cement like property [28].
\nWhen a drug or an active ingredient is topically applied on the skin surface, there theoretically three different ways through which the drug/active ingredient can penetrate through the skin. These are known as ‘The Penetration Pathways’. The penetration pathways are:
The intercellular pathway
The hair follicle pathway
The transcellular pathway
The intercellular pathway: This is the most widely known pathway. In this pathway, diffusion of the active ingredient occurs through the stratum corneum via the lipid layers surrounding the corneocytes.
\nThe hair follicle pathway: The hair follicles are surrounded by a dense network of blood capillaries which support efficient penetration. These serve as reservoir for the topically applied active compound.
\nThe transcellular pathway: This is the less understood pathway. Here the drugs are directly transported through the lipid layers and corneocytes to the living cells (Figure 8).
\nPenetration pathways of the active ingredient through the skin. (1) Represents the intercellular pathway, (2) represents the hair follicle pathway and (3) represents the transcellular pathway [28].
While nanoemulsions are an efficient vehicle for transferring and administering topical drugs into the body, they have some limitations. These are low viscosity, spreadability constraints due to skin as a barrier and rheological properties.
\nTo overcome these problems associated with nanoemulsions, a hydrophilic gelling system was integrated with nanoemulsions to increase the efficiency of transdermal drug delivery. These integrated systems are termed as nano emulgels [43].
\nNanoemulgel are usually three-dimensional, spherical gels composed of a cross-linked network of polymeric (natural or synthetic substances) [44]. They are highly preferred over other nanomaterials for drug delivery due to their unique and advantageous features. The most important ones being biocompatibility, stimuli–response behavior softness, their ability to swell up to achieve a controlled, triggered response at the target site. They also protect the guest molecules i.e., the molecules they are carrying from degradation and elimination.
\nThe versatility of their architecture allows for incorporation of a plethora of guest molecules ranging from inorganic nanoparticles to biomacromolecules like proteins and DNA with suitable modifications of the materials used for their construction without compromising their gel behavior. This multi-functionality and stability is hard to find in other types of nanoparticulate systems [43, 45, 46].
\nNanogel properties can be used in various fields to achieve biomedical applications.
\nStimuli response behavior: This involves the response of the nanogels to the external environment in the body such as pH, temperature, redox reactions, enzyme concentration etc. It employs the unique ability of the gel network to swell and unwell for this purpose. The nanogels can be composed of different materials depending on the type of response to be initiated. The deswelling and swelling occurs in the presence of changes in pH and concentration of the surrounding environment. For example, a gel network made of polysaccharide functionalized with PBA (aminophenyl boronic acid) is used to detect the fluctuations in glucose concentration, pH, concentration of the cationic and anionic groups bound to the gel and the PBA grafted to the gel which induces the release insulin by deswelling [44].
\nAnother very important feature is protecting the cargo molecules from degradation and elimination and early clearance carrying small molecules for drug delivery by retaining them within the gel via hydrogen-bonding and hydrophobic interactions. Cationic gel polymers are also useful in carrying molecules of opposite charges such as oligonucleotides, proteins, RNA molecules or a combination of them to achieve multi-target drug delivery. This has been proven to be useful for cancer treatment in animals.
\nThese hydrogels show immense amount of versatility, biocompatibility and fluid like transport properties which make them ideal carriers for imaging probes and scanning techniques such as optical imaging and multi-modal scanning [46]. It is also useful for anti-aging, skin care and moisturizing creams [31].
\nNanoemulsions are a relatively new class of dispersions which have gained popularity due to their high efficiency in delivery. There have been a lot of efforts and research to develop the preparation methods of nanoemulsions. This emerging component of nanotechnology has become an irreplaceable part and parcel of the cosmetic and pharmaceutical industries. Further research and development in this field can prove to be very crucial for these industries. Nanoemulsions have a huge potential to change the approaches to many fields as discussed in this chapter and it can also play much more important roles in the future due to its uniqueness and increasing research in its field.
\nThe market for nanoemulsions is expected to grow at the rate of 8.8% between the years 2018 and 2023 [47].The growth is expected to be driven by the increasing demand for the treatment of chronic diseases and vaccine development. Nanoemulsions have huge potential to improve the efficacy of cancer immunotherapy by multiple folds. The major hindrance to the growth is the expensive manufacturing methods and scaling up with cost effectiveness. The technological innovation and scaling opportunities is expected to decrease the cost of production. Due to its unique properties, nanoemulsions can also become an active component in the chemical, agricultural and engineering fields. Nanoemulsions can also find an application as drug delivery platforms to noval phytopharmaceuticals given the new interest in herbal drug formulations in the world [32].
\nThe authors listed in this paper wish to express their appreciation to the RSST trust Bangalore for their continuation support and encouragement. As a corresponding author, I also express my sincere thanks to all other authors whose valuable contribution and important comments make this manuscript in this form.
\nThe authors listed in this paper have no conflict of interest known best from our side. There was also no problem related to funding. All authors have contributed equally with their valuable comments which made the manuscript to this form.
There was no funding provided for the above research and preparation of the manuscript.
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