Advantage of bioethanol.
\r\n\tIC offer services both at the macro-scale (country) and at the micro-scale (cities). The stability and the protection of these networks on both scales are a significant task, entrusted to the Operators who operate CI in a concession mandate. Due to the high level of interdependency of CI, which exchange services to each other for their functioning, their management and protection cannot be carried out by a "linearized" strategy (each infrastructure managed and protected independently on the others) due to the presence of tight links which connect each other. CI protection through provision of "smart" properties such as resilience, has become a complex task which must be tackled not only by deploying advanced technological means but also by triggering new management strategies, enabling holistic and global management policies.
\r\n\r\n\tThe book aims at providing an overview of the understanding of complex phenomena taking place on interdependent networks and of the advanced technical solutions related to management, risk analysis and resilience enhancement of networks, either from a theoretical and operational (i.e. with solution related to real or realistic cases) points of view. A large emphasis is provided to the capability opened by the use of field and remote sensing tools for monitoring and assessing risks on CI. The use of comprehensive data set, the access to big data is going to open the way to the realization of new tools for supporting the decision making process needed for both daily and emergency management.
",isbn:"978-1-83962-621-0",printIsbn:"978-1-83962-620-3",pdfIsbn:"978-1-83962-628-9",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"7cfcd62bae8c99be207e18bb73e2a7b1",bookSignature:"Dr. Vittorio Rosato and Dr. Antonio Di Pietro",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/10256.jpg",keywords:"Complex systems, Interdependence, Resilience, Cascading effects, Event prediction, Emergency management, Decision support, AI, Field sensors, Remote sensing, IoT, GIS",numberOfDownloads:525,numberOfWosCitations:0,numberOfCrossrefCitations:0,numberOfDimensionsCitations:0,numberOfTotalCitations:0,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"June 15th 2020",dateEndSecondStepPublish:"July 6th 2020",dateEndThirdStepPublish:"September 4th 2020",dateEndFourthStepPublish:"November 23rd 2020",dateEndFifthStepPublish:"January 22nd 2021",remainingDaysToSecondStep:"8 months",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:"Supervisor and Project Evaluator for EU, for the Italian Ministry of University and Research, and that of Economic Development; Consultant for several Italian Regions and the Italian Ministry of Defense; Coordinator of several National Projects; Co-founder of two SMEs active in software engineering and biotechnology; Author of more than 140 scientific papers in peer reviewed journals and conference proceedings.",coeditorOneBiosketch:"A full researcher at ENEA (Italian Energy, New Technology and Environment Agency) since 2007 and a joined member to the Laboratory for the Analysis and Protection of Critical Infrastructures (APIC) from 2015. Dr. Di Pietro took part in several European and Italian national research projects and acted as an advisor for certain Evaluation Studies commissioned by the EU.",coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"27002",title:"Dr.",name:"Vittorio",middleName:null,surname:"Rosato",slug:"vittorio-rosato",fullName:"Vittorio Rosato",profilePictureURL:"https://mts.intechopen.com/storage/users/27002/images/system/27002.jpg",biography:"Vittorio Rosato received the Laurea degree (M.Sc.) in Physics from the University of Pisa (Italy) and a Ph.D. in Condensed Matter Physics from the University of Nancy (France). He has extensively been working in Computational Physics, particularly in Condensed Matter and Material Science in his positions as Research Assistant at the University College of Wales in Aberystwyth (UK) and at the Centre d'Etudes Nucleaires in Saclay (France). Staff Scientist at ENEA (Italian National Agency for New Technologies, Energy and Sustainable Economic Development) since 1990, he is currently Head of the Laboratory of Analysis and Protection of Critical Infrastructures and Manager of the Italian Node of the European Infrastructure Simulation and Analysis Centre (EISAC.it).\nHis current research activities span from risk analysis to the design of Decision Support Systems for the management of complex technological networks. He acts as Supervisor and Project Evaluator for EU, for the Italian Ministry of University and Research, and that of Economic Development; he is also consultant for several Italian Regions and the Italian Ministry of Defense. He is and has been Coordinator of several National Projects. He is co-founder of two SMEs active in software engineering and biotechnology. He is author of more than 140 scientific papers in peer reviewed journals and conference proceedings.",institutionString:"ENEA (Italian National Agency for New Technologies, Energy and Sustainable Economic Development)",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"2",totalChapterViews:"0",totalEditedBooks:"0",institution:null}],coeditorOne:{id:"284589",title:"Dr.",name:"Antonio",middleName:null,surname:"Di Pietro",slug:"antonio-di-pietro",fullName:"Antonio Di Pietro",profilePictureURL:"https://s3.us-east-1.amazonaws.com/intech-files/0030O00002bReF6QAK/Profile_Picture_1581328351906",biography:"Antonio Di Pietro received the Laurea degree (M.Sc.) in Informatics Engineering from Sapienza University of Rome (Italy) and a Ph.D. in Methodologies for Emergency Management in Critical Infrastructures from Roma Tre University (Rome).\nHe has been working as a full researcher at ENEA (Italian Energy, New Technology and Environment Agency) since 2007 and in 2015 he joined the Laboratory for the Analysis and Protection of Critical Infrastructures (APIC) in the same institution.\nHis research interests include modelling and simulation of critical infrastructures and the development of Decision Support Systems integrating seismic and meteorological natural threat modeling. He is also an Unmanned Aerial Vehicles (UAV) ENAC-certifed pilot to perform critical operations involving aerial photogrammetry tasks for biological and Infrastructure monitoring applications. He took part in several European and Italian national research projects and acted as an advisor in some Evaluation Studies commissioned by the EU. He has also been advisor of several M.Sc. students and also a teacher in several professional courses on Software Engineering and Databases.",institutionString:"ENEA (Italian National Agency for New Technologies, Energy and Sustainable Economic Development)",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"1",totalChapterViews:"0",totalEditedBooks:"0",institution:null},coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"11",title:"Engineering",slug:"engineering"}],chapters:[{id:"74122",title:"Risk Analysis in Early Phase of Complex Infrastructure Projects",slug:"risk-analysis-in-early-phase-of-complex-infrastructure-projects",totalDownloads:87,totalCrossrefCites:0,authors:[null]},{id:"74493",title:"Flood Risk Analysis for Critical Infrastructure Protection: Issues and Opportunities in Less Developed Societies",slug:"flood-risk-analysis-for-critical-infrastructure-protection-issues-and-opportunities-in-less-develope",totalDownloads:50,totalCrossrefCites:0,authors:[null]},{id:"74123",title:"Resilience in Critical Infrastructures: The Role of Modelling and Simulation",slug:"resilience-in-critical-infrastructures-the-role-of-modelling-and-simulation",totalDownloads:78,totalCrossrefCites:0,authors:[null]},{id:"73984",title:"Validation Strategy as a Part of the European Gas Network Protection",slug:"validation-strategy-as-a-part-of-the-european-gas-network-protection",totalDownloads:35,totalCrossrefCites:0,authors:[null]},{id:"74174",title:"Defects Assessment in Subsea Pipelines by Risk Criteria",slug:"defects-assessment-in-subsea-pipelines-by-risk-criteria",totalDownloads:44,totalCrossrefCites:0,authors:[null]},{id:"74240",title:"Analyzing the Cyber Risk in Critical Infrastructures",slug:"analyzing-the-cyber-risk-in-critical-infrastructures",totalDownloads:85,totalCrossrefCites:0,authors:[null]},{id:"74141",title:"Italian Crisis Management in 2020",slug:"italian-crisis-management-in-2020",totalDownloads:49,totalCrossrefCites:0,authors:[null]},{id:"74668",title:"A Strategy to Improve Infrastructure Survivability via Prioritizing Critical Nodes Protection",slug:"a-strategy-to-improve-infrastructure-survivability-via-prioritizing-critical-nodes-protection",totalDownloads:34,totalCrossrefCites:0,authors:[null]},{id:"74143",title:"Resilience of Critical Infrastructures: A Risk Assessment Methodology for Energy Corridors",slug:"resilience-of-critical-infrastructures-a-risk-assessment-methodology-for-energy-corridors",totalDownloads:66,totalCrossrefCites:0,authors:[null]}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"205697",firstName:"Kristina",lastName:"Kardum Cvitan",middleName:null,title:"Ms.",imageUrl:"https://mts.intechopen.com/storage/users/205697/images/5186_n.jpg",email:"kristina.k@intechopen.com",biography:"As an Author Service Manager my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review, to approval and revision, copyediting 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"}},{type:"book",id:"3621",title:"Silver Nanoparticles",subtitle:null,isOpenForSubmission:!1,hash:null,slug:"silver-nanoparticles",bookSignature:"David Pozo Perez",coverURL:"https://cdn.intechopen.com/books/images_new/3621.jpg",editedByType:"Edited by",editors:[{id:"6667",title:"Dr.",name:"David",surname:"Pozo",slug:"david-pozo",fullName:"David Pozo"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"52832",title:"Laser Ablation of Polymethylmethacrylate (PMMA) by Phase- Controlled Femtosecond Two-Color Synthesized Waveforms",doi:"10.5772/65637",slug:"laser-ablation-of-polymethylmethacrylate-pmma-by-phase-controlled-femtosecond-two-color-synthesized-",body:'\nFemtosecond (fs) laser micromachining has been studied intensively for the past two decades. One of the advantages of using ultrashort laser pulses rather than longer pulses for laser material processing pertains to the nonthermal ablation mechanism. By considerably reducing the area of heat-affected zones, precise laser micro- and nanomachining have become feasible for fs machining. To date, fs laser micromachining has been performed on a variety of wide-band-gap materials, such as polymers [1, 2], fused silica [3–6], and silicon [7–10]. However, almost all of these studies employed one-color laser pulses. More recently, coherent waveform-synthesized two-color laser pulses have been successfully used for increasing plasma generation [11], generating high harmonics [12], and producing broadband terahertz radiation [13]. By studying femtosecond laser ablation of polymethylmethacrylate (PMMA), our group demonstrated that the ablated hole areas exhibited clear modulation with a contrast of 22% by varying the relative phase between the ω and 2ω beams [14]. It was assumed that different peak intensity for the synthesized waveform was responsible for the observed phenomena. The physical mechanism was not clear.
\nIn general, ultrafast laser ablation of dielectrics, such as PMMA, has been explained by the photochemical, photothermal, and photophysical models [15]. In the photochemical model, direct bond breaking in PMMA is achieved by exposing it to an ultrashort laser pulse for producing several reaction products, such as CO, CO2, CH4, CH3OH, and HCOOCH3. In the photothermal model, electronic excitation by picosecond laser pulses results in thermal bond breaking, leading to the formation of PMMA monomers. Among these models, the most interesting one is the photophysical one, in which both thermal and nonthermal bond breaking occur simultaneously. In thermal bond breaking, electronic excitation by ultrashort laser pulses results in ultrashort-laser-induced ionization in the picosecond (ps) and fs ranges. The three main processes of photophysical laser-induced breakdown are (i) excitation of conduction band electrons through ionization, (ii) heating of conduction band electrons through irradiation of the dielectric, and (iii) plasma energy transfer to the lattice, which causes bond breaking [16–19].
\nThe Keldysh formalism, describing electron tunneling through a barrier created by the electric field of a laser, is often employed for modeling laser breakdown of materials by photoionization, including both multiphoton and tunneling cases. The Keldysh parameter can be expressed as the square root of the ratio between the ionization potential and twice the value of the ponderomotive potential of the laser pulse. Alternatively, it can be expressed as the ratio of tunneling frequency to the laser frequency. The tunneling time or the inverse of the tunneling frequency is given by the mean free time of an electron passing through a barrier width, ltunneling = Ip/eE(t, ϕ), where Ip is the ionization potential, e is the electron charge, and E(t, ϕ) is the optical field.
\nDepending on the laser intensity used for above-threshold ionization [20–22], two regions of photoionization exist: the tunneling ionization region [20, 23, 24] and multiphoton ionization region [25–28]. In tunneling ionization, the electric field is extremely strong. The Coulomb well can be suppressed to cause the bound electron to tunnel through the barrier and be ionized. At lower laser intensities, the electron can absorb several photons simultaneously. The electron makes the transition from the valence band to the conduction band if the total energy of the absorbed photons is greater than or equal to the band gap of the material.
\nThe boundary between tunneling ionization and multiphoton ionization is unclear. Schumacher et al. showed that there should be a so-called intermediate region that exhibit both tunneling and multiphoton characteristics. Mazur et al., following the Keldysh formalism, estimated that the intermediate region corresponded to a Keldysh parameter γ ≈ 1.5 [29].
\nThe tunneling ionization rate is a function of the electric field. It is well known that the multiphoton ionization rate can be expressed as ϖmpi ∝ σkIk, where I is the laser intensity and σk is the multiphoton absorption coefficient for k photons [30]. When the ionization occurs in the intermediate region, an electron can absorb several photons and be ionized by the tunneling effect. In this regime, the ionization rate can also vary with phase of the exciting electric field. The laser intensity required, however, is considerably lower than that in the pure tunneling ionization case.
\nIn this chapter, we present the current progress on laser ablation of polymethylmethacrylate (PMMA) by phase-controlled femtosecond two-color synthesized waveforms. Significantly, laser breakdown (ablation) of transparent materials through photoionization in the intermediate regime (Keldysh parameter γ ≈ 1.5) was demonstrated for the first time. The modulation of ablated hole area as well as the dependence of the ablation threshold on the relative phase between the ω and 2ω beams were observed. The data correlated closely with the theoretically predicted phase dependence of the photoionization rate using the Keldysh formalism.
\nIn this section, some key concepts of ultrafast laser ablation will be summarized. This includes light-matter interaction mechanisms such as photochemical, photothermal and photophysical. Dielectric breakdown due to ionization by tunneling, multiphoton and avalanche processes are described. Most relevant for this work, the so-called intermediate regime of photoionization, will be formulated by using the Keldysh equation, defining the Keldysh parameter used throughout this chapter.
\nLaser ablation is one of the manifestations of light-matter interactions. As expected, the ablation processes depend on characteristics of the irradiating laser, such as its intensity, wavelength, and polarization. When ultrafast laser are used, ablation mechanism become more complicated. For polymeric materials, not only photoionization but also the direct bond breaking will lead the ablation process. The main mechanisms are photochemical, photothermal, and photophysical. These three effects are located in different regions of laser pulse.
\nFor ultrafast laser ablation of PMMA, there are two dominant mechanisms, i.e., photochemical and photothermal. In photochemical events, absorption of photons by the material being processed lead directly to covalent bond breaking [15]. The polymeric materials, such as PMMA, are generally made of a wide variety of chromophores, which may dissociate into reactive fragments by absorption of energetic UV photons. Absorption of less energetic photons, e.g., those in the visible or near infrared band, can also lead to the above photochemical processes [15]. Photothermal effect is another basic mechanism of laser ablation. Irradiated by ultrashort laser pulses, the irradiated material absorbs photons and transfer energy to electrons such that photoionization of the material can occur. In this case, excited electrons can heat up the lattice and induce bond breaking [15]. Depending on fluence of the irradiating laser, ablation could be originated through either tunneling ionization or above-threshold ionization (ATI). Multiphoton and avalanche ionization are two main mechanisms of ATI.
\nIn a large band gap material, it is difficult to ionize the constituent atoms by absorbing only one photon from commonly available lasers. Theoretically, an atom might absorb two or more photons simultaneously, giving electrons sufficient energy to cross the band gap from the valence band to the conduction band. This is illustrated schematically in Figure 1. For multiphoton ionization to occur, the laser intensity needs to be in the range of 1012 –1016 W/cm2. In contrast, the avalanche ionization mechanism, for which the laser intensity required is in the range of 109 –1012 W/cm2, depicts the process whereas a small number of initial electrons of the materials are accelerated to a high value of kinetic energy. Afterwards, high-energy electrons will collide with another electron of lower energy, which is shown schematically in Figure 1. Afterwards, the two electrons are accelerated by the laser field collide with other electrons in an avalanche-like process, leading to large amount of electrons with high energies to form a plasma.
\nSchematic diagrams illustrating the processes of (a) multiphoton ionization and (b) avalanche ionization of materials.
Finally, in the photophysical mechanism, nonthermal, photochemical, thermal, and photothermal processes all play their respective roles. Two independent mechanisms of bond breaking could be present. Further, bond breaking energies for the ground state and the excited state chromophores are, in general, different. The photophysical mechanism of ablation usually applies for irradiating lasers with short laser pulses, of which the pulse duration is in the ps and fs range.
\nIn a class paper, Keldysh showed that the total photoionization rate of a material upon irradiation by a laser can be written as [31, 32]:
\nwhere γ = ω(mIp)1/2/eF is the so-called Keldysh parameter, ω is laser frequency, m is the electronic mass, e is the electronic charge, ℏ is plank constant, and
The symbol
where K and E are first and second kind of the complete elliptic integrals and Φ is the Dawson integral.
\nIn the presence of high-intensity or strong electric field of the laser, we are in the region of tunneling ionization or γ << 1. The rate of tunneling ionization is given by
\nOn the other hand, if γ >> 1, the ionization is in the regime of multiphoton absorption. The probability of multiphoton absorption is given by
\nThe photonionization rate and Keldysh parameter are plotted as a function of laser intensity (λ = 800 nm) in PMMA.
Photonionization rates are plotted as a function of the Keldysh parameter for NIR (λ = 800 nm) ultrafast laser ablation of PMMA.
Below, we have plotted the effective ionization potential
Photonionization rates and Keldysh parameter are plotted as a function of laser intensity for NUV (λ = 400 nm) laser ablation of PMMA.
Photonionization rates are plotted as a function of the Keldysh parameter for NUV (λ =400 nm) ultrafast laser ablation of PMMA.
The solid blue lines in Figures 2–5 correspond to the photoionization rate of PMMA calculated using Eq. (1). The full expression of Keldysh formula (Eq. 1) take into account both tunneling and multiphoton ionization processes. The dashed black line and dotted red line represent the tunneling ionization and multiphoton ionization rates determined from Eqs. (4) and (5), respectively. When the Keldysh parameter, γ ≈1.5, tunneling and multiphoton ionization rates overlap each other for PMMA irradiated with either NIR (800 nm) or NUV (400 nm) beams. We defined this overlapping region as an intermediate regime. To predict the ionization rate in the intermediate regime, we assume the process resembles that of tunneling ionization. The ionization rate depends on the instantaneous field amplitude, FL(t), which is given by [22]:
\nIn order to understand the phase dependence of observed dual-color laser ablation phenomena, we proceed as follows: assume that the irradiating laser consists of beams at two commensurate laser frequencies, i.e., the fundamental (ω) laser beam and its second harmonic (2ω). The dual-color laser field F(t) can then be written as
\nwhere Fω and F2ω are the envelope function of the fundamental and second-harmonic laser fields, respectively; ϕ is the relative phase of the second-harmonic (2ω) beam with respect to that of the fundamental (ω) beam.
\nThe Keldysh model above can be used to describe the photoionization phenomenon due to either the multiphoton or tunneling route. Typically, the Keldysh parameter is defined by the square root of the ratio of ionization potential and twice the ponderomotive potential of the laser pulse. Some researchers also define it as the ratio of tunneling frequency to the laser frequency [33]. In the original derivation, the Keldysh parameter was used to describe the phenomenon of an electron tunneling through a barrier created by the optical field. The tunneling time or the inverse of the tunneling frequency is determined by the mean free time of the electron passing through a barrier width l.
\nwhere Ip is the ionization potential, e is the electron charge and FL(t,ϕ) is the electric field of the incident laser. The average velocity of an electron can be written as,
\nwhere me is the mass of an electron. By combining Eqs. (8) and (9), the tunneling time is given by
\nTunneling can occur if the mean tunneling time, which is given by Eq. (10), is less than half the period of the laser. Taking this into account, we modify the Keldysh parameter,γ as appropriate for this study as
\nwhere tlaser is the period of laser, llaser is the mean distance that an electron moves during half of period tlaser at a mean velocity of <v>, and vlaser is the laser frequency. When the Keldysh parameter γ has relative phase dependence at dual-color synthesized waveform condition, the ionization rate can be calculated after we determine the effective frequency of the dual-color laser pulse.
\nFor the purpose of defining the envelope equation for single-cycle pulse of the synthesized waveform, we express the complex electric field as [34]
\nwhere ω0 is the effective carrier frequency denoted as
\nIn Eqs. (12) and (13), E(ω) is the Fourier transform of E(t) and ψ is the imaginary part of the complex envelope. Substituting the effective carrier frequency into Eq. (1), we can plot the photoionization rate as a function of laser intensity and the relative phase between the fundamental (ω) and second-harmonic (2ω) beams in our experiment, which is shown in Figure 6.
\nAccording to Figure 6, the ionization rate is predicted to be dependent on the relative phase of the fundamental (800 nm) and second-harmonic (400 nm) beams. Further, the modulation of ionization rate is more pronounced at higher laser intensities.
\nThe total ionization rate versus laser intensity and relative phase of fundamental (ω) and second-harmonic (2ω) laser beams.
Recall that ablation by a laser with low and high intensities would fall into the regimes governed by multiphoton and tunneling ionization mechanisms, respectively. Conventionally, tunneling ionization corresponds to a regime in which the Keldysh parameter γ << 1. In this limit, the strength of the field is more than the value necessary to overcome the barrier. For a weaker field such that the Keldysh parameter γ >> 1, the main mechanism for ionization is due to the multiphoton ionization. In this regime, the electric filed strength is below the value that required for overcoming the barrier. In order to calculate the Keldysh parameter for the dual-color case, we need to define the period of the laser tlaser. It can be easily shown that the period of dual-color synthesized waveform by NIR (800 nm) and NUV (400 nm) beams is essentially that of the period of fundamental (ω) beam. Therefore, Eqs. (1) and (11) can be combined to determine the ionization rate as shown in Figure 6.
\nIn the intermediate ionization regime, which is defined by γ ≈1.5, the ionization rate has a strong phase dependence. Likewise, the electron tunnel time now depends on the phase difference between the two colors. Note that the electric field is actually lower than the value required for electrons to overcome the barrier.
\nAblation threshold is an important parameter for laser material processing. It is a function of the laser pulse duration, wavelength, and intensity. According to the simplified Fokker-Planck equation [35]:
\nwhere n is the free electron number, β is the avalanche ionization factor, assuming that the photogenerated electron distribution grows in magnitude without changing its shape. P(I) is the multiphoton ionization rate. It can be approximated by the tunneling ionization rate by using Keldysh equation.
\nFirst of all, we need to calculate the number of free electrons generated by the laser pulse, assumed to be Gaussian in shape, I(t) = I0exp(−4ln2t2/τ2), where τ is the pulse duration. By solving the equation above, the free electron number can be obtained as
\nwhere α is the absorption coefficient of the material and n0 is the total number of free electrons which is generated through multiphoton or tunneling ionization mechanism,
\nThe ablation threshold, Fth, can then be written as
\nwhere the density of free electrons, ncr correspond to the threshold fluence, Fth. For ablation with ultrafast laser pulses, contribution by the avalanche ionization mechanism is not significant. Dielectric breakdown or ablation is through the processes of photoionization by tunneling and multiphoton ionization mechanisms. When the free electron number increases, the ablation threshold decreases.
\nThe experimental setup for laser ablation by dual-color femtosecond synthesized waveform [14] is shown schematically in Figure 7. The laser source was an amplified Ti: Sapphire laser system (Spitfire, Spectra Physics), which generates 70 fs laser pulses at a central wavelength of 800 nm (λ1) with an energy up to 1.5 mJ at 1 kHz.
\nAs shown in Figure 7, we adopt an inline arrangement for phase control of the fundamental and second harmonic of the laser output. The 800-nm fs pulses were focused onto the sample surface by a single convex lens with a focal length of 300 mm. Meanwhile, the fundamental beam frequency was doubled in a 100-μm-thick type-I Beta Barium Borate (β-BBO) crystal in the same beam path to generate 2ω pulses at 400 nm (λ2). Both beams were reflected from the silicon wafer at some incident angle, taking advantage of the fact that reflectivity of silicon varies with wavelengths and polarizations of the fundamental and second-harmonic beams (see the inset in Figure 7). We can control the intensity ratio P2ω/Pω of the two (collinear) beams by adjusting the incident angle. A pair of wedge prisms with controllable optical path difference was used to precisely adjust the relative time delay between the ω and 2ω pulses. We also employed a 5-mm-thick β-BBO to compensate the group velocity mismatch (GVM) of the two colors in the beam path. Besides, the ω and 2ω fields with original polarizations perpendicular to each other, were passed through a dual-color zero-order wave plate serving as a half-wave plate for 800 nm to make polarizations of the two colors parallel. Finally, the ω and 2ω pulses, overlapped in time with the same linear polarizations were focused on the sample. The spatial and temporal overlap and adjustment of the phase difference between the ω and 2ω fields were conducted using a procedure described previously [14].
\nExperimental setup for laser ablation of PMMA by femtosecond dual-colour synthesized waveforms. The polarizations of fundamental and second harmonic pulses were controlled by the half-wave plate. ND: neutral density filter; BBO: Barium borate; GVD: group velocity dispersion. The inset shows the reflectivity of the silicon wafer as a function of the incident angle for both polarizations.
Ultrafast laser-induced ablation or breakdown of wide band gap materials, such as polymers [1, 2, 36–41], fused silica [6], and silicon [7, 42] have already been intensively studied. Among them, various kinds of polymers, such as polymethylmethacrylate (PMMA) [2, 36, 38–41], polyimide (PI) [1], polyethylene (PE) [37], polypropylene (PP), and polycarbonate (PC) [2], have drawn a lot of attention due to their potential industrial applications. Compared to ns-laser ablation, the energy ablation threshold fluence of fs-laser at approximately the same incident wavelength is known to be reduced [43]. This can be attributed to the fact that the breakdown intensities in the fs regime approach that of the threshold of multiphoton ionization of which the electron densities is high enough to cause damage [35]. On the other hand, because the induced energy absorbed by electrons is much faster than that transferred to a lattice [35]; therefore, the nonthermal ablation nature of such behavior achieved by applying fs-lasers could lead to a significant reduction of heat-affected zones. Also of interest is the possibility of decreasing the threshold for ablation. For example, Stuart et al. observed a continuously decreasing threshold with a gradual transition from the thermal regime where the longer pulses (>100 ps) dominated the ablation compared with the shorter pulses (<10 ps), which is caused by multiphoton ionization and plasma formation [17].
\nTo date, studies of single-color femtosecond laser ablation of PMMA were overwhelmingly conducted using the Ti: sapphire laser system of which the central wavelength is around 800 nm [44–46]. On the other hand, photoablation of materials with ultraviolet (UV) lasers has also gained in popularity [36, 47–49]. The mechanism for ablation of materials by UV light is mainly through the photochemical process by one-photon absorption. Most of the dielectrics, such as glass and polymer, have relatively high absorption coefficient in the UV region. This is in contrast to the commonly accepted mechanism for ablation of PMMA using 800 nm laser pulses, such as photothermal, photophysical, or multiphoton ionization and tunneling ionization, as mentioned previously. Therefore, it is of interest to conduct a comparative study of single-color femtosecond laser ablation of PMMA using the Ti: sapphire laser and its second harmonic.
\nImages of single-color (800 nm) and single-shot ablated holes. The input laser fluence are equal to (a) 2.63 J/cm2 and (b) 5.90 J/cm2 , respectively.
In Figure 8, we show images of single-shot ablated holes in PMMA irradiated with femtosecond pulses at the wavelength of 800 nm. By changing the input laser fluence from 2.63 to 5.90 J/cm2, areas of the holes are found to be equal to 155.25 and 1359.50 μm2, respectively.
\nThe photon energy for 800 nm is equal to 1.55 eV and the material band gap of PMMA is 4.58 eV. Therefore, more than three incident photons are needed for photoabsorption, leading to ablation. For such studies, one of the key parameter for studying the mechanism of ablation is its threshold. The method we used to define the ablation threshold value is measuring the ablated hole areas by using an optical microscope. In Figure 9, we have plotted hole-area of the ablated holes as a function of the irradiating laser fluence.
\nHole-areas of the single-shot, single-color (800 nm) femtosecond laser ablated holes are plotted as a function of the irradiating laser fluence. Error bars are indicated.
Assuming the irradiating beam has a Gaussian spatial profile, the generally accepted scaling law for ablated holes for incident laser fluence is given by
\nwhere D is the diameter of the ablated region, w is effective laser beam width, F is the incident laser fluence and Fth denotes the ablation threshold (unit here is J/cm2). Following Eq. (18), the ablation threshold Fth can be determined by fitting the experimental data to be 2.63 J/cm2.
\nTo compare, we conducted similar ablation studies with exciting wavelength at 400 nm. Recall that the material band gap of PMMA is 4.58 eV, which means the dominated mechanism for photoablation on PMMA at 400 nm is also multiphoton absorption. The photon energy for 400 nm is equal to 3.1 eV. Therefore, more than two incident photons are needed for photoabsorption, leading to ablation. In Figure 10, we show images of single-shot ablated holes in PMMA irradiated with femtosecond pulses at the wavelength of 400 nm. By changing the input laser fluence from 1.78 to 3.92 J/cm2, the hole areas are found to increase from 155.25 to 1359.50 μm2, respectively.
\nImages of single-color (400 nm) and single-shot ablated holes. The input laser fluence are equal to (a) 1.78 J/cm2 and (b) 3.92 J/cm2, respectively.
Figure 11 shows determination of the ablation threshold in the case of exciting wavelength at 400 nm. It can be seen that the same scaling behavior is observed in the case of ablation by the near IR beam. Our data show that the ablation threshold for PMMA irradiated by the near UV light of 400 nm is about 1.38 J/cm2.
\nSingle-colour ablation results for PMMA irradiated by femtosecond laser pulses with a central wavelength 400 nm. The fitted ablation threshold Fth is equal to 1. 38 J/cm2.
As we noted earlier, laser ablation studies were conducted almost exclusively with single-color laser beams [6, 7, 37, 42]. There are a few studies that employed two-color lasers. These studies can be organized into two categories: incoherent combination and coherent superposition of the two-color laser beams. An example of ablation by incoherently combined two-color beams is the work of Théberge et al., in which the authors observed an increase in volume of the ejected material by applying the superposition of fs and ns pulses. This was attributed to the free electrons and defect sites induced by the fs pulses, which could be exploited by the ns pulses [6]. Besides, Okoshi et al. reported that dual-color fs pulses with a fluence ratio of (2ω:ω = 2:78 mJ/cm2) could etch PE deeper and faster. It was proposed that an isolated carbon, in addition to C=O and C=C–H bonds, was formed on the ablated surface after treating PMMA with 2ω or dual-color pulses. The higher photon energy of 2ω pulses then cuts the chemical bonds of PE to form the modified layer on the ablated surface [37]. In related studies of fused silica, because of the creation of defect states or free electron plasma by dual-color fs pulses at zero delay, the enhancement of absorption/reflection was observed [6]. For silicon, upon using ns and picosecond (ps)-laser pulses, it was also shown that a weak 2ω beam can be beneficial in exciting electrons into conduction band to launch the ablation process of silicon [42]. In contrast, for fs pulses, where a sufficient population on the conduction band can be created by multiphoton absorption, this effect became insignificant [42].
\nAll the above studies employ relatively long-time delays between the two colors, on the scale of the carrier lifetime (≈ picoseconds). If the relative delay is of the order of an oscillation period between dual-color fs pulses, interesting phenomena could unfold. In other fields, a dual-color coherently superposed beams achieved by relative-phase control of each color were applied to study the physical mechanism of intense-field photoionization, especially in the gas phase [11, 24]. Schumacher et al., for example, studied the electric-field phase-dependent photoelectrons created in a regime including the multiphoton and tunneling signatures simultaneously by changing the dual-color relative phase [24]. Later, Gao et al. claimed this phase-difference effect resembled the phenomenon of quantum interference (QI) between the different channels characterized by the number of photons. In other words, phase-dependent photoemission is not a classical-wave effect, but rather a quantum-mechanical one. Recently, in comparison with monochromatic excitation, the threshold of plasma formation has been demonstrated to be significantly improved with the superposition of an ns infrared laser pulses and its second-harmonic field [11]. The authors explained their measurements by the effect of a field-dependent ionization cross section [11]. In the following, we report results of our studies of the ablation of PMMA using dual-color waveform synthesis of ω and 2ω beams of an fs Ti: sapphire laser.
\nIn Figure 12, we show images of single-shot ablated holes in PMMA irradiated with dual-color (ω and 2ω) femtosecond pulses. In this experiment, the average powers of ω and 2ω beams are 200 and 40 mW, respectively. The corresponding laser fluence for the fundamental (NIR) beam is equal to 7.55 J/cm2. Phase dependence of ablated holes was observed. Figure 12(a), for which the relative phase ϕ = π, the ablated hole area is equal to 844.95 μm2. When the relative phase ϕ = 0, area of the ablated hole is 982.31 μm2 (see Figure 12b).
\nImages of single-shot ablated holes in PMMA irradiated by dual-colour (ω and 2ω) femtosecond lasers. The laser fluence for the fundamental beam is equal to 7.55 J/cm2 and ratio of second-harmonic to the fundamental beams was 1:5. The hole areas of (a) 844.95 μm2 (b) 982.31 μm2 were observed when the relative phase ϕ were set to π and 0, respectively. The length of the red double-arrows in Fig. 12 (a) and (b) are both equal to 10 μm.
The ablated hole area versus relative prisms’ thickness with sinusoidal fitting in the case of single shot. The period for the ablated hole areas’ change is equal to 19.5 μm.
By varying the prism thickness traversed by the laser beams (see Figure 7), we observed that hole areas oscillated, as shown in Figure 13. Theoretically, we expect a sinusoidal variation with a period (relative phase change of 2π) of 20 μm. This is in good agreement with experimentally determined period of 19.5 μm in Figure 7.
\nAccording to our model, the two-color ionization rate would depend on the relative phase. In Figure 14, we have plotted the ionization rate according to Eq. (6) for synthesized dual-color instantaneous field from Eq. (7) as a function of the relative phase. The corresponding ablated hole areas are also plotted for comparison. The difference in period between the fitting curve in Figure 13 and the simulation curve in Figure 14 is only 1.3%.
\nThe ablated hole area and simulated dual-color ionization rate versus relative phase in the case of single shot. The observed modulation contrast in ablated area is ≈28% (peak to peak).
The ablation threshold measurement. The single-shot ablated hole areas in PMMA irradiated by femtosecond dual-color synthesized waveforms are plotted as a function of laser fluence. Four sets of data for different values of relative phases are shown.
In order to study how the relative phase affects the ablation threshold, we conducted a series of experiments in which the wedge prism’s thickness was fixed at some value and the laser fluence varied. The family of experimentally measured ablated hole areas for three values of relative phase as a function or irradiating laser fluence are plotted in Figure 15. The same scaling law for the single-color case was used to fit the experimental data. In this manner, we were able to determine the ablation threshold for a given value of relative phase. The ablation thresholds are 2.49, 2.58, 2.89 and 2.80 J/cm2, respectively, for the relative phase to be equal to 0, −π/2, π and 3π/2.
\nInterestingly, the fitted ablation thresholds also exhibit apparent dependence on the relative phase between ω to 2ω beams for our dual-color pulses. This is shown in Figure 16. The period of the sinusoidal oscillation is ≈ 2.4π.
\nThe ablation threshold in PMMA irradiated by femtosecond dual-color synthesized waveforms is plotted as a function of relative phase changes. The period for the ablation thresholds’ change is ≈2.4π.
Because the ablation threshold is dependent upon the number of free electrons created in the material [35, 50], we believe the observed periodicity in ablation threshold in Figure 16 demonstrates how electric field of the synthesized waveform affects the variation of ablation threshold. In the above experiments, the beam waists for every condition deliberately kept to be approximately the same. These are equal to 49.42, 54.58, 46.46, 46.69 and 47.51 μm in the cases of relative phase set at −π/2, 0, π/2, π and 3π/2. That is, variation in the beam spot size is small, ±3.90%.
\nIn this work, we have investigated single-shot laser ablation of polymethylmethacrylate (PMMA) using dual-color waveform synthesis of the fundamental (ω) and its second harmonic (2ω) of a femtosecond Ti: Sapphire laser. For comparison, single-color studies were also conducted. The threshold fluence for single-color ablation of PMMA irradiated by fundamental (ω) (NIR) and its second-harmonic (2ω) (NUV) beams were found to be respectively, 2.63 and 1.38 J/cm2. Changing the relative phase of the fundamental (ω) and second-harmonic (2ω) outputs of the exciting laser resulted in clear modulation of the ablated area. The modulation as well as the ablation threshold depends on the relative phase between the ω and 2ω beams. The ablation thresholds for ablation of PMMA irradiated by two-color femtosecond frequency-synthesized waves are 2.49, 2.58, 2.89 and 2.80 J/cm2, respectively, for the relative phase to be equal to 0, −π/2, π and 3π/2. The results correlated well with the theoretical model of laser breakdown (ablation) of transparent materials through photoionization in the intermediate regime (Keldysh parameter γ ≈ 1.5). Our study clearly illustrates the potential applications of using phase-controlled synthesized waveform for laser processing of materials.
\nThis work was funded by the grant of the National Science Council 102-2622-E-007-021-CC2, 101-2221-E-007-103-MY3, and 101-2112-M-007-019-MY3. The authors would like to thank Dr. Wei-Jen Chen for many useful discussions. They would also like to thank Prof. Ru-Pin Pan for the use of the microscope.
\nThe globe needs urgently to resort another option of sources of energy as a result of the rapid world energy supply exhaustion [1]. As a result of the depletion in oil, the world global warming and the effects of greenhouse making the earth on the condition of alarming [2]. Despite seeing the world are completely dependent on the limited sources of fossil-based petroleum that can later not withstand to meet future demands.
The world depletion fossil fuel happened, resulting in the continual price rising and the pressure for independence of oil and environments concerns lead to strong markets for biofuel [3]. The utilization of natural resources fuel leads to the vast side problem. The rapid increased of CO2 level in the environment resulted in the global warming resulting to the negative results of the burning of fuel from petroleum-based [4]. The worlds are concern about the climatic change and the consequent need to decreasing of greenhouse emissions gasses leading to the encouragement of the usage of bioethanol as an alternative or replacement [5]. Another challenge is as a result of the arise waste dumping in an open place resulting in malignant to the natural habitat at surrounding environments of the dumpsite. The concept of producing energy in the form of a solution by utilization of the waste is affordable, cheap and efficient. Recently, an enormous number of renewable sources of energy is rapidly growing technologies of renewable energy including solid biomass, liquid fuels and biogases [6]. A biofuel is a generated fuel through biomass rather than the one produced from the formation of the geological process of oil and fossils fuel. As a result of biomass can be technically utilized directly as fuel. The term biofuel and biomass are interchangeably used. Biomass with complex or free sugar that can later form soluble sugar is used for the production of bioethanol. The feedstock is divided mostly into three major groups; starchy crops, (sugar crops and by-products of sugar refineries) and lignocellulosic biomass (LCB), they differ respectively from the sugar solutions in them [7]. Production of bioethanol from the conventional feedstock like starch-rich feedstocks (corn, potato) and sugarcane has been previously reported as the first-generation process. Nevertheless, they have economic and social barriers [8]. Bioethanol second-generation process is gaining momentum. Lignocellulosic biomass (corn stover, sugarcane bagasse, straws, stalks and switchgrass) are used for the second-generation process. One of the significant alternative processes of bioethanol production with easy adaptability of this biofuel to prevailing engines with better octane rating [9, 10]. Any plant material with significant amounts of sugar is utilized as a source of raw materials in bioethanol production. Sugarcane, pineapple and potato are one of the major plants that resulted in a high yield of bioethanol as byproducts due to the presence of a high amount of sugarcane in it [11] (Figure 1).
The amount of bioethanol production depends on the substrate used as shown in the figure above. Adapted from Khandaker et al. [11].
Yeast is described as basidiomycetous or ascomycetous fungi responsible for reproducing through fission or budding and formed spores which are not enclosed in the fruiting body [13]. S. cerevisiae is the most popular yeast in the production of ethanol due to its wide tolerance of PH making it less susceptible to infection. The ability of yeasts in catabolize six-carbon molecules is the bedrock to the production of bioethanol without proceeding to the final products of oxidation which is CO2. Diauxic shift and fermentative metabolism are the process of the production of bioethanol dependent Alcohol dehydrogenase (EC 1.1.1.1) enzymes which is encoded on the ADH1locus. During the fermentation of glucose, ADH1 catalyzes led to the production of ethanol and reduction of acetaldehyde, similarly, the reverse reaction can be catalyzed: is the process of conversion of ethanol to acetaldehyde, albeit with lower catalytic efficiency [14].
Fresh citrus fruits are consumed or the citrus juice is mostly preserved which it’s in ready form of consumption or concentrated form. After the extraction of citrus fruit juice, the remaining parts of the fruits serve as a rich source of lignocellulosic material and also utilized as a raw material for the fermentation of bioethanol. Simultaneous saccharification and fermentation from plantain, banana and pineapple peel through the cultured of S. cerevisiae and A. niger [15]. Different temperature (20–50°C) was used to be examined the simultaneous saccharification and fermentation of banana peels to obtain bioethanol using co-cultures of S. cerevisiae and A. niger at different pH of 4 to 7 for seven days.
The present study observed that the maximum temperature and pH for the banana peels fermentation was 30°C and 6. With these maximum conditions of temperature and pH, different concentrations 3 and 12% of yeast were utilized for performing fermentation. The study found the period for the whole fermentation to complete reduced drastically [16]. The high glucose content in pineapple and orange resulted in the excellent yield of bioethanol [11] (Figure 2).
Percentage of sugar composition in various fruits and vegetables [12].
Rotten, peels, shells and a scraped portion of vegetables is one kind of biodegradable vegetable waste that generated in large amounts, usually dumped on ground for rotten near the household area. This act not emits an obscene odor but also creates a big irritation by attracting pigs, rats and bird as well as vectors of various human diseases. Vegetable waste mainly generates during the processing and packaging of vegetables, after preparation of cooking and post-harvest losses due to lack of storage facilities. Bioethanol can be produced through fermentation under controlled conditions. Microbial decomposition of vegetable waste generates bioethanol with high humus content. Many researchers have stated that vegetable waste is carbohydrate-rich biomass one of the potent substrates of renewable energy generations.
Research on the usage of fruit and vegetable wastes for the manufacture of biofuel is fetching attractive in different countries. Sulaiman et al. [17] abstracted a halal biorefinery for the production of bioethanol and biodiesel and value-added products in Malaysia. Vegetable wastes arise throughout the supply chain from the producer to consumer and vary widely depending on its harvesting, processing and marketing [18]. Vegetable waste can be raw, cooked, inedible and edible; parts are generated during production, harvesting, precooling, grading, storage, marketing and consumption at the consumer place. All the cut-down vegetable waste goes to landfill. Landfills spread offensive smells, produce methane which is a common greenhouse gas, and also produced a large amount of harmful leachate that can contaminate water and soil. Nevertheless, microbial digestion of vegetable waste can be used to produce bioethanol, renewable bioenergy. Vegetable waste has chemical potentials due to the high amount of saccharide in the form of lignocellulose. Promon [19] reported that vegetable waste as a high source of lignocellulose could be hydrolyzed into D-xylose and glucose.
Vegetable waste is a renowned nonedible source of lipids, amino acids, carbohydrates, and phosphates [20, 21]. All of these nonedible lignocellulose biomasses can also use for the production of bioethanol. Lignocellulose contains of 30–50% of cellulose, 20–40% of hemicellulose and lignin around 10–15% [22]. Cellulose is the main assembly of lignocellulosic built biomass which is a glucose homologous polymer associated by b-1,4 glycosidic bond [23]. After, glucose and other simple sugars production from all the sugar sources, the bioconversion endures till bioethanol is produced. Vegetable waste is widely used raw material for the production of bioethanol because it contains hemicellulose and cellulose, which can be changed into sugar by the hydrolysis method in presence of microorganisms [24]. The sugar content in vegetable waste extracts around 5% [25]. Yeast, fungi and bacteria can be used for the fermentation process [26].
Pretreatment: The pretreatment is the most costly and complicated step in the conversion of LCB into ethanol. The LCB in cellulose is usually sheathed or coated by hemicelluloses resulting in hemicellulose complex cellulose that works as a chemical barrier and attacked and prevent the chances of complex enzymes under its natural condition [27]. The complexes cellulose-hemicellulose are further subjected encapsulated with signs leading to the production of physical, physical barrier to the biomass of hydrolysis to produce fermentable sugars [28].
Chemical pretreatment: Primarily acids and alkali working on the biomass of the delignification, the degree of decreasing of crystallinity of cellulose and polymerization. HNO3, H3PO4, HCl and H2SO4 are utilized during acid pretreatment of biomass in the process the major alkali used is NaOH. Pretreatment of acid is applied in the stabilization of the fraction of hemicellulosic in the biomass, thereby making cellulose enzymes more accessible [29]. Physical pretreatments: This process convert the biomass through the increased surface accessibility area and pore volume, decreased in the degree of the polymerization of cellulose, hydrolysis of hemicellulose, partial depolymerization of lignin and its crystallinity. Physicochemical pretreatment: The exploitation of the usage of conditions and chemical compounds that affect the chemical and physical properties of the biostimulants including a large number of technologies example fiber explosion ammonia, steam exploitation, CO2 explosion, ammonia recycling percolation wet oxidation, soaking aqueous ammonia etc. Similarly, other pretreatments methods like technologies from physicochemical also increased the accessibility area surface of the enzyme biomass, cellulose crystallinity decreased and removal of lignin and hemicellulose during pretreatment.
Biological pretreatment: Microorganisms are used are utilized particularly fungi as brown rot, white rot and soft fungi rot, the most efficient among them are white fungi rot. The above treatment became effective through the alteration of the cellulose and lignin structure and separates them from the lignocellulosic matrix. While white, soft rot and brown rot fungi attack cellulose and lignin [30].
Detoxification: Pretreatment is an important aspect of converting LCB into ethanol.
It has a significant effect on the complete process leading to the generation of lignocellulose-derived by-products under the conditions of pretreatment such as acetic acid, sugar acids, levulinic acid, formic acid, furfural and hydroxymethyl furfural acts as enzymes inhibitors for the microorganisms fermentation for the subsequent stage if the accumulation is sufficiently high [31].
Inhibitors can be checked out by:
Chemical approach: by addition of alkali such as NaOH, reducing agents such as (sulfite, dithionite and dithiothreitol) Ca(OH)2, NH4OH, Reducing
Treatment using enzyme: peroxidase, laccase
Vaporization and heating: heat treatment, evaporation
Extraction using liquid–liquid: Supercritical fluid extraction such as (Trialkylamine, supercritical CO2), Ethyl acetate,
Extraction using liquid–solid: Lignin, Ion exchange and Activated carbon,
Treatments using microbes: thermospheric, Coniochaeta ligularia, reibacillus and Trichoderma reesei [7].
Hydrolysis: Hydrolysis is described as an industrial process where hemicellulose and cellulose present in the feedstock are converted to fermentable sugars. The fermentable sugars are maltotriose, maltose, sucrose, glucose, fructose they are generally accounting to 60–70% of the total solid dissolved. Enzymatic hydrolysis, alkaline or either acid is utilized in the conversion of cellulose and hemicellulose into their monomers sugar.
Acid hydrolysis is the oldest technology for cellulose biomass conversion to ethanol [32]. The acid hydrolysis is basically classified into two: concentrated acid hydrolysis and dilute acid. The diluted acid procedure is conducted through high pressure and temperature with a reaction time scale of one minute, reactivating continues process. The procedure of the concentrated acid utilized relatively low pressure and temperature with a much longer reaction time [33] (Figure 3).
Dilute acid hydrolysis flow chart of recovery bioethanol [37].
Dilute acid hydrolysis the following method it is used for hydrolysis of hemicellulose and as a cellulose pretreatment to make it most accessible for the enzymes. However, both the polymers of carbohydrate are hydrolysed using acid dilution under two stages, hydrolysis process: the following stage is carrying out at a minimum temperature to utilized the hemicellulose conversion as the fraction of hemicellulose biomass for the depolymerization at a low temperature than the portion of cellulose due to the difference in the structure between these two polymers of carbohydrate [34]. The dilution of acid involved a process of a solution of sulfuric acid 1% concentration in a reactor with continues flow at a temperature of 215°C [35]. Most of the process of the acid dilution to a sugar recovery is limited to efficiency of about 50%. The most paramount challenge in the hydrolysis of acid dilution is the raising of glucose yields greater than 70% in a viable economical industrial process with a maintaining high rate of cellulose hydrolysis with minimization of decomposition of glucose. Shrinking bed reactor countercurrent technologies have been 100% success in the yielding of glucose from cellulose [36].
Concentrated Acid Hydrolysis the method provide rapid and complete cellulose of hydrolysis to glucose and sugars of hemicelluloses to 5-carbon with a little bit of degradation. The concentration of the acid process utilized mild temperature relatively, the pressure created from the pumping pressure from vessel to vessel is utilized. Dilution acid process is shorter than the reaction time [35]. Depolymerization of the cellulosic fraction is the next step. Soaking and dewatered of solid residue from the first stage was carried out in 30–40% sulfuric acid for 50 minutes. For furthering of cellulose hydrolysis is carried out at 373 k [37]. Recovery of higher sugar efficiency was the primary advantage of the concentrated acid process [38]. The process of concentrated acid offers significant cost reduction than the process of dilute sulfuric acid [39].
Alkaline hydrolysis the major significant from pretreatment of alkali is the removal of lignin, which greatly improved the reactivity of the remaining aspects of polysaccharides [40]. In the biomass, the aligning structure is altered by glycosidic and ester degrading side chains of the biomass through the alkaline solvents, resulting in swelling as well as cellulose decrystallization [41]. Hydrolysis of alkaline is a very slow process that requires neutralization and the recovery of the added alkali is needed. Hydrolysis of alkaline is very suitable for agricultural residue and herbaceous and woody biomass is not suitable due to its high contents of lignin [42]. Previous experiments results confirmed that hydrolysis of alkaline has the highest reaction rate, followed by hydrolysis of acid and finally degradation of hydrothermal from the glycosidic bond cleavage insoluble water carbohydrate concerned. In other to the obtained significant yield of sugar by hydrolysis of alkaline, it is very challenging as a result of dimeric and mono carbohydrates such as fructose, maltose, cellobiose or glucose are attacked severely by the temperature of alkali at 100°C [42].
Enzymatic hydrolysis for enzymatic hydrolysis to take place it required the feeds to be hydrolysed by the enzyme to become fermentable sugars. Breaking down of cellulose take place using three types of enzymes β-glucosidases, cellobiohydrolases and endo-β-1,4-glucanases. The most effective and promising among them is the enzymatic process due to the specificity of the enzyme on the substrate relatively working on the minimum temperature and generating lower inhibitors. LCB enzymatic done usually by using either microorganisms producing an enzyme that secrets directly on the enzymes during their developments in the media or enzymes system that are commercially available where the latter is widely utilized and more feasible. The commercial-scale of cost-effective ethanol its major challenge is the enzymes costs [43]. The type of biomass and the conditions of hydrolysis is the major factors dependable for the conversion of lignocellulosic biomass to fermentable sugars. Many factors are solely responsible for the yield of sugar during hydrolysis of the enzyme. The factors are generally divided into two groups. (1) factors related substrate, and interlinked with one other (2) enzymatic and factors related process. Enzymes hydrolysis is the saccharification preferred method as a result of its; high yield, high selectivity, minimum energy cost and operating milder condition than other processes [14].
Fermentation process: Bioethanol production largely depends on three processes which are simultaneous saccharification and fermentation, (SSF) and simultaneous saccharification and co-fermentation (SSCF) and separate hydrolysis and fermentation (SHF). Ethanol fermentation is completely separated lignolistic hydrolysis in SHF fermentation. Hydrolysis enzymatic separation and fermentations enabled the operation of the enzymes at a higher temperature and excellent performance. The organisms in the fermentation process operate at a lower temperature for sugar utilization optimization. SSCF and SSF fermentation and hydrolysis process occur concurrently to keep the glucose concentration low, the whole process occurs in a short process. While the SSF fermentation pentose is separated from glucose while SSCF pentose and glucose are in the same reactor [44]. Both SSCF and SSF are more efficient and preferred over the SHF as a result the operation of the later cannot be performed on the same reactor [37].
Batch, fed-batch, repeated batch or continuous mode are important technology of bioethanol fermentation. Hadiyanto et al. [45] stated that the substrate is provided at the early stages of the process without removal or addition of the medium in a batch process. The process is known as the simple system of a bioreactor with a flexible, multi-vessel and Cassy control system. In a closed-loop system with high inhibitors and sugar concentration at the beginning and ends of the fermentation is maintained and the process carried out with high product concentration [46]. Complete sterilization, require fewer labour skills, can control easily, very easy to manage feedstocks, and flexible to various product specifications are benefits of the batch system [47]. However, the productivity of the system is very low and need intensive and high labour costs. Both inhibitions of growth of the cells and production of ethanol may come from the presence of significant amount/ high concentration of sugar in the fermentation chamber [48]. However, Fed-batch fermentation overcomes the inhibition and enhanced production of ethanol. In Fed-batch fermentation, combine a form of batch and continuous modes are operated which involves increasing substrate to the fermenter devoided removing it from the medium. The size of culture in fed-batch varies significantly, but the substrate must be fed with the right component properly at a certain rate. When the low substrate concentration is maintained, higher ethanol yield in feb-batch is observed. This is because low substrate concentration permits the smooth conversion of a reasonable amount of fermentable to ethanol [47]. The benefits of this feb-batch include; higher ethanol yield, greater dissolved oxygen in the fermentation chamber, Low fermentation time and medium component exhibit a low toxic effect [48]. Fed-batch is successfully operated in non-uniform SSF system by repeatedly adding pretreated feedstock to achieve comparatively high sugar and ethanol yield [14].
Continuous operation is achieved by unceasing addition of culture medium, substrate and nutrients to bioreactor embodied active microorganisms. In continuous operation mode, the culture size is kept constant and the end products of fermentation are siphoned from the media continuously. Discrete product types such as ethanol, cells and residual sugar could be accessed from the top of bioreactor [14]. The advantages of continuous system over batch and fed-batch; small size bioreactor, higher ethanol yield and cost-effective. However, shortcomings of this technique are; the greater tendency of contamination than other types [37]. The capability of Saccharomyces cerevisiae to ferment and produce ethanol is drastically decreasing with longer cultivation time.
Bioethanol fuel has the following intrinsic quality: high-octane number; this measure the engine performance (Table 1). The more the octane number the higher compression that the fuel can endure before ignition. Higher octane number qualifies fuel to be used in high-performance gasoline engines that need compression ratios to be high. Hence, the use of gasoline with a low octane number causes the engine knocking [49]. It drastically decreases the emission of substances that are a threat to human health eg. CO (Table 2). The utilization of ethanol does not employ engine modification, it does not emit CO2, the cost of production is low, and it is eco-friendly, hence flipside of the solution to global environmental contamination [50, 51].
Bioethanol fuel property | Advantages | References |
---|---|---|
High oxygen content (35% w/w) | i. Increased combustion efficiency ii. Reduced hydrocarbon and carbon monoxide emissions | [52, 53] |
High octane number (107) and high latent heat of vaporization (0.91 MJ/kg) | i. Prevents premature ignition and cylinder knocking ii. Spontaneous ignition in internal combustion engines when bioethanol petrol blends are used | [54, 55] |
Low energy content (21.2 MJ/dm3) | i. Increased compression ratio ii. Decreased burn time iii. Increased power | [56, 57] |
Advantage of bioethanol.
Bioethanol | Fossil ethanol |
---|---|
Renewable | Non-renewable |
Waste plant material used as feedstock | Fossils source |
Cost-effective | expensive |
Least pollutants are released | Many pollutants are released |
Difference between bioethanol and fossil ethanol.
Temperature: the roles of temperature for S. cerevisiae to ferment sugar and the production of ethanol were studied. Results from previous studies show S. cerevisiae cells increased exponentially as the incubation begins and then get into stationary phase after prolong incubation for all operating temperatures. Experiments prove that as the temperature is progressively increasing, the time required for fermentation decreases. Nevertheless, at much high-temperature S. cerevisiae cells growth is inhibited and decline in ethanol production is drastic [58] (Figure 4). This may be due to that temperature affects the transport system or the level soluble substances and solvent in the S. cerevisiae cells are saturated which in turn causes the build-up of toxins ethanol inclusive inside cells [58, 59, 60].
Effect of temperature on bioethanol yield [61].
Whereas low temperature slows the growth rate of cells which may be due to their low tolerance to ethanol at lower temperatures [62, 63].
Effect of Feedstock Concentration: feedstock encloses nutrients for microorganism’s growth during the fermentation process. At high feedstock concentration, the rate hydrolysis is speed up because more compound is bound to enzymes’ active site. With fixed number of enzymes and low amount of substrate cause decrease in production of ethanol because bound to enzymes’ active site. A small amount of ethanol will be obtained because of low substrates bound to the enzyme’s active site. Hence, the increase in feedstock concentration favors the production of ethanol [64] (Figure 5). However, according to Lin et al. [58] prolong exposure to a higher concentration of feedstock lead to diminishing the production of bioethanol.
Effect of feedstock on bioethanol production [65].
Effect of pH: Fermentation process is pH sensitive. In an acidic medium with moderate pH, high ethanol production was observed (Figure 6). Moderately acidic pH, cell permeability to some essential nutrients is influence by the concentration of H+ in the fermentation broth [28]. It has been experimentally observed that both growth and survival rate of S. cerevisiae is persuaded by pH in the 2.75–4.25 range. However, during fermentation for ethanol production, 4.0–4.25 is the optimum range of pH. When pH is ≤4.0, incubation period longer than necessary is required even though it does not cause a significant decrease in ethanol production. A substantial reduction of ethanol production was observed at pH above 5.0 [66, 67] (Figure 6).
Effect of pH on bioethanol production [57].
Time of Fermentation: the rate at which growth of microorganisms occurs is affected by fermentation time (Figure 7). The shorter the fermentation times the more inefficient fermentation due to inadequate microorganisms growth. Equally, longer fermentation time cause affects S. cerevisiae growth due to high concentration of ethanol in the broth. However, using a low temperature and long fermentation result in lowest ethanol yield [28].
The production of ethanol by S. cerevisiae in the industrial medium in (a) aerobic conditions and (b) aerobic–anaerobic conditions [68].
Agitation rate this controls to regulate the entry of nutrients from the fermentation broth to inside cells and eviction of ethanol from the cells to the fermentation broth. Higher rate of agitation leads to higher production of ethanol. It plays a role in triggering sugar takes up and the inhibition of ethanol to the cell is reduced. The frequently used agitation rate for fermentation by yeast cells is 150–200 rpm. It is inadvisable to use excess agitation rate as it reduces metabolic activities of the cell and hence, unsuitable for smooth production of ethanol [28].
Inoculum concentration does not have any significant effect on the production of ethanol but the ethanol consumption rate and sugar yield [69]. When the is an increase in the number of cells from 1 × 104 to 1 × 107 cells per ml, increased ethanol production is also observed. It has been reported that when Inoculum concentration exceeds 107 and 108 cells per ml, no significant effect on the ethanol production observed [28]. At the elevated concentration of inoculum, reduction of fermentation time is observed as there is rapid cell growth.
The total results revealed the vegetables and fruits waste could be utilized for the production of bioethanol from recycled agricultural waste and management process. The discussions showed that bioethanol optimum yield is produced at pH 4, the temperature at 32°C and using 3 g/L yeast. The engine cars utilized efficiently bioethanol produced from waste rotten pineapple because it does not have high content and any dangerous elements. The principle or idea of using vegetables and fruits waste to produce bioethanol will aid in keeping the environment clean from the waste of agriculture. The process helped in overcoming to the challenges of depletion of fossil fuel with the creation of bioresearch energy. Bioethanol produced from the agricultural waste of vegetables and fruits is of good qualities with making the engine to produce less emission. Vegetables and fruits waste are good economical choice for the production of bioethanol because of its low cost and availability.
The authors wish to acknowledge the support of Center for Research Excellence and Incubation Management (CREIM), Universiti Sultan Zainal Abidin (UniSZA), Malaysia, Gong Badak, 21300 Kuala Nerus, Terengganu Darul Iman, Malaysia and KPT Grant (Project code: FRGS/1/2019/WAB01/UNISZA/02/2).
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