\r\n\tParaffin waxes were used in different ways according to their characteristics such as chemical stability, non-poisonous, no phase separation with only a slight volume shift during phase transformation with a negligible degree of sub-cooling and complete thermal stability.
\r\n
\r\n\tThe storage and management of thermal energy was seen as a prospective technology for efficient energy regulation and utilization. Phase change materials (PCMs), latent heat energy storage materials, can store and release significant quantities of waste heat energy during their phase transition; thus, they have enormous potential for efficient heat energy use.
\r\n
\r\n\tBecause of their low costs, high latent heat and proper thermal characteristics such as little to no supercooling, low vapor pressure, self- behaviour, paraffin has been commonly used for energy storage applications. The type of shape-stabilized or structure-stable composites must be formed by injecting paraffin into porous materials as the supporting matrix in order to preserve the shape of paraffin and avoid leakage of the melted paraffin.
\r\n
\r\n\t \r\n\tThis book focuses on thermal energy storage. In particular, the commonly used materials at high temperatures, molten salts and concrete. Also the focus is on the most promising materials with paraffin such as; carbon nanotubes/ paraffin, Nano powder/ paraffin, by-products / paraffin and clay/paraffin in for thermal energy storage.
",isbn:"978-1-83968-706-8",printIsbn:"978-1-83968-705-1",pdfIsbn:"978-1-83968-707-5",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!0,hash:"456090b63f5ba2290e24e655abd119bf",bookSignature:"Dr. Elsayed Zaki and Dr. Abdelghaffar S. Dhmees",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/10216.jpg",keywords:"Paraffin, Paraffin Wax, Phase Change, Energy Storage, Mesoporous Materials, Thermal Storage, Nanomaterials, Porous Materials, CNTs, Clay, By-Products, Applications",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"October 28th 2020",dateEndSecondStepPublish:"December 1st 2020",dateEndThirdStepPublish:"January 30th 2021",dateEndFourthStepPublish:"April 20th 2021",dateEndFifthStepPublish:"June 19th 2021",remainingDaysToSecondStep:"2 months",secondStepPassed:!0,currentStepOfPublishingProcess:3,editedByType:null,kuFlag:!1,biosketch:"Currently, Dr. Elsayed Zaki is a visiting researcher at the Department of Chemical and Biomolecular Engineering, Iacocca Hall, Lehigh University, USA., he has been a researcher of applied chemistry in the Petroleum Applications Department, Egyptian Petroleum Research Institute from 1 March 2015 to the present, he is serving as an editorial member of several reputed journals and is a member of a number of international organizations among which Royal Society of Chemistry.",coeditorOneBiosketch:"Dr. AbdelGhaffar S. Dhmees is a Senior of Dynamic light Scattering Lab., Nanotechnology center, Egyptian Petroleum Research Institute.",coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"220156",title:"Dr.",name:"Elsayed",middleName:null,surname:"Zaki",slug:"elsayed-zaki",fullName:"Elsayed Zaki",profilePictureURL:"https://mts.intechopen.com/storage/users/220156/images/system/220156.jpg",biography:"Dr Elsayed Zaki received his PhD in physical chemistry from the Department of Chemistry, Faculty of Science,– Mansoura University, Egypt. Currently, he is a visiting researcher at the Department of Chemical and Biomolecular Engineering, Iacocca\nHall, Lehigh University, USA. He has been a researcher of applied\nchemistry in the Petroleum Applications Department, Egyptian\nPetroleum Research Institute from 1 March 2015 to present.\nHe is currently serving as an editorial member of several reputed journals such as: Industrial & Engineering Chemistry Research, American Chemical Society, International Journal of Hydrogen Energy, Archives in Cancer Research, Herald Journal of Agriculture and Food Science Research, on the scientific and technical committee and editorial review board on Chemical and Molecular Engineering (WASET), Open Journal of Applied Sciences, Advances in Chemical Engineering and Science, Journal of the Chemical Society of Pakistan, International Conference on Chemical, Metallurgy and Environmental Engineering, Universal Researchers in Environmental & Biological Engineering, Asia-Pacific Chemical, Biological & Environmental Engineering Society, International Journal of Chemical and Biomolecular Science\nin Public Science Framework, Biomedical and Pharmacology Journal, International Academy of Chemical, Civil & Environment Engineering, International Journal of Ambient Energy, he was appointed to editorial board for the International Journal of Materials Science and Applications, he was appointed to editorial board for Advances in Materials, he was appointed to editorial board for International Journal of Science, Technology and Society, Organic & Medicinal Chemistry International Journal (OMCIJ), Universal Journal of Pharmaceutical Research, International Journal of Nano and Material Sciences, he is an advisory board member of World Journal of Pharmacy and Pharmaceutical Sciences, Cogent OA, Taylor & Francis\nGroup, SciFed Journal of Polymerscience. \nHe is a member of the Royal Society of Chemistry (MRSC), Chemicals Development Services Center (CDSC), Egyptian\nCorrosion Society (ECS), The Arab Society of Material Science, Petroleum and Mineral Resources Society, Egyptian Petroleum Association, The Egyptian Society of Polymer Science and Technology, Egyptian Syndicate of Scientific Professions, Asia-Pacific Chemical, Biological & Environmental Engineering Society (APCBEES), Society of Petroleum Engineers (SPE), World Academy of Science, Engineering and Technology (WASET), The International Association of Engineers (IAENG), Egyptian Association for Science and Engineering (EASE), Sesame User\nOffice (SUO) Synchrotron- Light for Experimental Science and Applications in the Middle East, Sesame Users’ Committee (SUC) Synchrotron-Light for Experimental Science and Applications in the Middle East, International Association of Advanced Materials (IAAM), The Society of Digital Information and Wireless \n Communications (SDIWC), The International Society for Environmental Information Sciences (ISEIS ), The Organization for Women in Science for the Developing World (OWSD), and the International Union of Pure and Applied Chemistry.",institutionString:"Egyptian Petroleum Research 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1. Introduction
Nowadays the most common way to obtain bioactive peptides is by enzymatic hydrolysis of protein solutions. The most studied substrates used to produce bioactive peptides are milk proteins in the form of co-products from dairy industries: caseins, cheese whey, buttermilk, whey protein concentrates and isolates or even pure single proteins that can be obtained at a reasonable price on an industrial scale (e.g. β-lactoglobulin, β-Lg).
Different specific and non-specific enzymes are used to obtain hydrolysates (trypsin, pepsin, pancreatin and alcalase). The catalytic activity of some of them is quite specific and the composition of the hydrolysate is predictable when substrates are quite pure [1]. In other cases, the activity of the enzyme is non-specific and produces a complex mixture of peptides and amino acids in which individual effect of each molecule in the subsequent fractionation process is difficult to demonstrate and quantify. The design of an efficient fractionation methodology is then of paramount importance for peptides separation and even more, when the process must applied on an industrial scale. Separation technologies, which discriminate small differences in charge, size and hydrophobicity, can be employed to fractionate protein hydrolysates and obtain peptide fractions with higher functionality or higher nutritional value in a more purified form. Membrane separation techniques seem to be well suited for this purpose. These processes are based upon selective permeability of one or more of the liquid constituents through the membrane according to the driving forces.
2. Overview of techniques used for peptide fractionation
Due to the demonstration of their impact on human health, the market for functional food and nutraceuticals containing bioactive peptides is increasing very rapidly and, consequently, the food and bio-pharmaceutic industries are looking for processes allowing the production of this kind of products from natural sources. Considering that most functional peptides are present in complex mixtures containing a large number of hydrolysed protein fractions, their separation and purification are required.
The methodologies commonly used for peptide fractionation and enrichment include: selective precipitation, membrane filtration, ion exchange, gel filtration technologies and liquid chromatography [1]. However, significant differences concerning the number and type of extracted peptides occur among extraction procedures. Additionally, undesired peptides, such as allergenic or bitter-tasting peptides, could be enriched in the process when using some of those techniques [2].
Fractionation methods involving precipitation steps are carried out by means of the addition of organic solvents like ethanol, methanol or acetone; adding acids like trichloroacetic acid (TCA), sulphosalicylic acid or phosphotungstic acid (PPTA); by means of the addition of salts (ammonium sulphate) or just by adjusting the pH to the isoelectric point. Precipitation often results in a selective fractionation of peptides depending on their solubility in the precipitating agent [3]; however the addition of chemical compounds causes in some cases peptide degradation and changes in the biological and physical properties.
Chromatographic methods for peptide separation are currently used at lab-scale: high performance liquid chromatography (HPLC), fast protein liquid chromatography (FPLC), isoelectric focusing (IEF) and ion exchange chromatography (IEC) are some of them. In most cases, one or two cycles of successive HPLC separation had been adequate to isolate peptides one by one. In the same way, IEC has been used for the enrichment of casein phosphopeptides from casein hydrolysates or for the isolation of cationic antibacterial peptides from lactoferrin. However, although chromatographic processes can provide good separation selectivity, the low productivity and high production costs involved in these processes make impossible its use at industrial scale.
Size exclusion chromatography (SEC) and more frequently Ultrafiltration-Nanofiltration (UF-NF) are the main techniques used to isolate peptides according to their molecular size [4-10]. In addition it is possible to obtain more purified hydrolysate samples by removing salts and other interfering components by means of UF membranes [11]. In fact, investigations into these methodologies under optimized conditions to reduce time and cost are ongoing [12].
Pressure-driven membrane-based processes, such as UF and NF, are used to fractionate peptide mixtures and amino acids [13]. These types of membrane have been widely used to fractionate milk protein hydrolysates with the aim of enhancing their biological or functional properties [14-15]. It has been shown that variations in operating conditions may favor the permeation of bioactive peptides [16-17].
Membrane technology has become an important separation technology in recent decades probably because their main advantages (it works without the addition of chemicals, with a relatively low use of energy, it has low processing costs, the scale-up is an easy subject and the process lines are well arranged) make it the ideal technology for use on an industrial scale. In addition, membrane processes are especially suitable for the food industry, because of the mild working conditions, relatively easy scale up and low processing costs in comparison to chromatographic techniques.
The separation of peptides by UF mainly depends on the molecular weight (MW) cut-off (MWCO) of the membrane. However, when the MW of the peptides involved in the process is quite similar, their isolation is a hard subject; in these cases, NF is the best membrane separation technique [18]. The fact that NF membranes are usually charged offers the possibility of separating solutes through a combination of size and charge mechanisms.
3. Membrane technology applied to peptide fractionation
Membrane processes are now viewed as efficient tools for the development of new value-added products by separating minor compounds such as bioactive peptides [19]. These separation processes are based upon selective permeability of one or more of the liquid constituents through the membrane according to the pressure difference. Amongst the pressure-driven membrane techniques, which main features are summarized in Figure 1, UF and NF have been tested for the fractionation of protein hydrolysates due to the fact that the molecular weight of most bioactive peptides is within the normal pore size range of these membranes.
Figure 1.
Pressure-driven membrane processes
UF is commonly applied to prepare enriched bioactive solutions from protein hydrolysates and improve the bioactivity of peptides. This process is also used to separate peptides with a size lower than 7 kDa [20]. The fractions are collected by subsequently filtration in two or three streams to obtain peptides with different size [21]. For example, amino acids and small peptides can be separated at pH 4.6 into four ranges of molecular mass (I<30 kDa, II>30 kDa (protein fraction), III>10 kDa (protein fraction), IV>0.3 kDa) [22]. Recent results on fractionation peptides by UF-membranes show that crude yoghurt fractions obtained after ion exchange can be separated into four fractions by successive UF using membranes with molecular cut off sizes of 30, 10 and 3 kDa [23]; whereas UF membranes < 1 kDa are efficient for peptides fractionation from milk hydrolysates if the last permeate contains free amino acids [21].
The combination of membrane processes (UF and NF) is also often used to separation of peptides. The first step of these processes consists in the UF of the hydrolysate in order to obtain complete rejection of intact proteins and intermediate peptides. The resulting permeate fractions is then subjected to a fractionation by NF and a peptide fraction having a molar mass < 1 kDa is isolated of the mixture by means of these membranes.
In this case, permeates obtained after UF could be adjusted at two pH values (9.5 and 3.0) that corresponded to the different charged states of the membrane and of the peptides to improve of separation of polypeptides of molar mass < 1 kDa [23-24].
Recently a method that couple UF and HPLC has also been applied on milk hydrolysate samples for enhance the peptides separation. A current study showed that an UF-membrane was enough to concentrate peptides and subsequently, both permeate and retentate were fractioned by SE-HPLC to obtain small peptides with biological activity [25].
There are also other important UF-processes to separate specific compounds of whey as caseinomacropeptide (CMP). A first method was designed to obtain CMP fractions trough UF membranes with MWCO 20-50 kDa by two diafiltration steps [26]. The method is based on the ability of CMP to form non-covalent linked polymers with a molecular weight up to 50 kDa at neutral pH, which dissociate at acid conditions. The dissociated form of CMP permeates through the UF-membrane at pH 3.5, whereas the majority of whey proteins such as β-Lg, α-lactalbumin (α-La), immunoglobulins (IGs) and bovine serum albumin (BSA) are held back. At pH 7.0, permeate containing CMP can be concentrated by means of the same membrane; however a low permeation rate is obtained with this technique. A second method for separation of CMP can be seen in [27]. Thermal stability of CMP is used in comparison to that of the rest of whey proteins. Complete denaturation and aggregation of proteins is obtained by treating whey at 90°C for 1h; with this method, the denatured proteins can be removed by centrifugation at 5200 g and 4°C for 15 min and the supernatant containing CMP can be concentrated by UF with MWCO 10 kDa after pH adjustment to 7.0; however whey proteins lose part of their functionality due to the denaturation.
Another method for separation of CMP consists in the pretreatment of whey protein concentrate with the enzyme transglutaminase (Tgase) followed by microfiltration [28]. The amino acid sequence of CMP includes two glutamine and three lysine residues, whereby this peptide can be cross-linked by tranglutaminase. The covalent linked CMP aggregates can be removed be means of microfiltration or diafiltration to obtain CMP-free whey protein.
3.1. Enzymatic membrane reactor equipped with membranes: first step to peptide fractionation
Enzymatic membrane reactor (EMR) consists on a coupling of a membrane separation process with an enzymatic reaction. EMR allows the continuous production and separation of specific peptide sequences by means a selective membrane, which is used to separate the biocatalyst from the reaction products and the peptides fractionation [29]. At present, EMR is used when working on an industrial scale. This technology for peptides separation is gaining interest, because it is a specific mode for running batch or continuous processes in which enzymes are separated from end products with the help of a selective membrane. By that way, it is possible to obtain complete retention of the enzyme without deactivation problems typical of enzyme immobilization. Furthermore, EMR have been shown to improve the efficiency of enzyme-catalyzed bioconversion and to increase product yields [13, 30-31].
EMR technology has been investigated for the production and separation of peptides since the 90´s. Antithrombotic peptides derived from hydrolysed CMP can be recovered by UF membranes [32-33] and Lactorphin have been successfully produced through continuous hydrolysis of whey in an UF-reactor [34-35]. Multicompartment EMR has also been designed for the continuous hydrolysis of milk proteins. Nowadays, this technique is operated under an electric field for continuous harvesting of some biologically active peptides, such as phosphopeptides and precursors of casomorphins from the tryptic digest of β-casein [36]. Special attention had also had the study of the hydrolysis of whey protein isolates (WPI) using a tangential flow filter membrane (TFF) of 10 kDa in EMR [37]. The factors influencing on the operation of the EMR (substrate concentration, ionic strength, and transmembrane pressure) have been studied and discussed in other research works [30, 38]. In recent years, the use of EMR has emerged as an exciting area of research due to their low production cost, product safety and easy scaled up [39]. Table 1 summarizes some examples of processes for the separation or concentration of bioactive peptides by means of UF membranes. UF offers possibilities for a large-scale production of bioactive peptides but seems limited because of fouling and poor selectivity. Another drawback of UF membranes is their pore size, because the large pores are not selective enough to fractionate small peptides MW of bioactive peptides is usually smaller than 1 kDa). To sum up, with the use of an EMR equipped with UF membranes, the first peptide fractionation is achieved but if a more purified permeate is required; NF membranes should be used as an additional step instead of UF membranes.
3.4. NF membranes and peptide fractionation
NF is a pressure-driven membrane technique in which the pore size of the membrane is in the nanometers range. As can be observed in Figure 1, this technique is an intermediate step between reverse osmosis (RO) and UF and it is useful to separate/fractionate solutes with MW lower than 5 kDa. Transmembrane pressure in NF is lower than in RO and the permeate flux is usually higher, which represents an important energetic advantage in industrial applications. NF membranes of cut-off < 1 kDa are particularly useful for the filtration of the smaller peptides from hydrolysates solutions.
The selectivity of NF membranes is based on both size and charge characteristics of the solutes and on the interaction between charged solutes and membrane surface. Hydrodynamic parameters (mainly transmembrane pressure and linear velocities) and membrane material exert influence on membrane selectivity too. NF membranes have a slightly charged surface; because the dimensions of the pores are less than one order of magnitude larger than the size of ions [54].
Protein Hydrolysate Source
Biological Activity
References
Bovine caseinomacropeptide
Antithrombotic
[32-33]
Calcium bioavailability improvement
[40]
Bone and teeth mineralization
Bovine whey β-lactoglobulin
ACE inhibitor
[41]
Opioid
[42]
Anti microbial
[43]
Muscular contraction
[44]
Bovine whey α-lactalbumin
ACE inhibitor
[4]
Fish protein
ACE inhibitor
[45]
Alfalta white protein
ACE inhibitor
[46]
Alfalta leaf protein
Antioxidant
[47]
Wheat gluten
ACE inhibitor
[48]
Soybean protein
ACE inhibitor
[49]
Soybean β-conglycinin
ACE inhibitor
[50]
Sea cucumber gelatin
ACE inhibitor
[51]
Potato
Antimicrobial
[52]
Potato
Antimicrobial
[53]
Table 1.
Bioactive peptides obtained by means of UF membranes
3.4.1. NF transport mechanism
The mechanism behind the selectivity of membrane processes is generally the size of the component. This mainly applies in the case of UF membranes and in the case of NF membranes with uncharged solutes. Charge effects are minimized in this case and the transmission of the solutes depends largely on the size exclusion effects of the membrane. This sieving effect is usually modeled and corrected [55] using continues hydrodynamic models such as originally proposed by Ferry. In this model, the membrane is assumed to be a network of perfectly cylindrical and parallel pores in which solvent velocity follows Poiseuille’s law with a parabolic profile and solutes are assimilated to hard spheres. The transmission coefficient (Tr) of a given solute can be calculated according to equation (1) However, the selectivity of NF membranes is based on both size and charge characteristics of the solutes and on the interaction between charged solutes and membrane surface [56].
Tr = (1-( λ(λ-2))2 exp (-0.7146 λ2)
Where λ is the relation between the radius of the solute and the radius of the pore.
The selectivity of the separation when using NF membranes is based on the following factors: a) Solute (peptide) size, shape and charge. b) Membrane pore size and surface charge (sign and surface charge density). c) Hydrodynamic conditions of the fractionation process (transmembrane pressure, lineal velocities and solute concentration). d) Membrane characteristics (manufacture process, surface roughness, porosity, film layer material and hydrophilic/hydrophobic surface). All these aspects must be considered in order to estimate the viability of a peptide fractionation process.
Especially in NF membranes involving peptide fractionation from mixtures, charge exclusion mechanisms are predominant in the separation. The charge effects affect membrane-peptide and peptide-peptide interactions in the mixture or at the membrane surface. The transport mechanism through the pores is governed by convective and diffusive fluxes as well as by electromigrative flux. These phenomena make the prediction of the separation selectivity a difficult objective.
The current state of science the knowledge of the NF process is not sufficient to make a model fulfilling the requirements. The difficulties in modeling permeate flow rates and solute rejection come from the scale at which the different phenomena takes place at the membrane surface and through the membrane pores, where most of the hydrodynamic and macroscopic interactions begin to break down. However, simplified approaches could be used to explain qualitatively the experimental results obtained, as can be seen below.
The solute transfer through the membrane follow two main steps: distribution of ionic species at the selective interface according to their charge (both solutes and membrane) and transfer by a complex combination among diffusion, convection and electrophoretic mobility through the membrane, at least at low feed concentrations [13]. According to Donnan theory, the passage of charged solutes through a charged NF membrane is likely to be different whether they are considered to be co-ions, i.e. with the same charge of the membrane, or counter-ions, i.e. with a charge of opposite sign. In fact, due to electrostatic repulsive/attractive forces between the membrane and the solutes the concentration of co-ions will be lower in the membrane than in the solutions. On the contrary, the counter-ions have a higher concentration in the membrane than in the solution. This concentration difference of the ions generates a potential difference at the interface between the membrane and the solution, which is called Donnan potential. Under equilibrium conditions, electro-neutrality and equality of electrochemical potentials are maintained through the system. The Donnan equilibrium depends on the ion concentration, the fixed charge concentration in the membrane and the valences of the co-ions and counter-ions. Figure 2 shows an adapted schematic representation [57] of the influence of the electrostatic interactions in the transmission of charged peptides through a charged NF membrane.
Because of the electro-neutrality principle, and on the assumption that the charge density of the membrane is quite higher than the net charge of the co-ions, is possible to calculate the distribution of the co-ion resulting from a binary electrolyte AB→AzA+BzBbetween the membrane surface and the solution as a function of the charge density of the membrane.
K=CBmCB=(zB.CB)zB/ZA(ZB.CBm+Zx.Cxm)E1
\n\t\t\t\t\t
Figure 2.
Schematic representation of solute flows across a negatively charged NF membranes. Je: electromigrative flow as a consequence of the transitory electric field. Tr: transmission of the solute. Attractive (>> <<) and repulsive (<< >>) electrostatic interactions between charged solutes and the membrane are also represented.
CBm and CB represent the concentration of co-ions B in the membrane and in the solution respectively. The coefficient of distribution, K, can be used to predict the rejection value of a binary electrolyte if the ionic transport is mainly due to convection and size exclusion effects are negligible. Under these conditions, K will mainly depend on: the co-ion valence (zB), the counter-ion valence (zA), the membrane charge (Cxm), its valence (zx) and the concentration of the co-ion in the solution (CB).
According to equation 2, Donnan equilibrium predicts that an increase in the concentration of co-ions in the global solution and/or a decrease in the membrane charge density lead to a decrease in the exclusion of co-ions from the membrane surface (K is increased) and to a decrease in the retention of the binary salt (co-ion and cointer-ion) in order to maintain electroneutrality in both sides of the membrane [58-59]. The concentration of co-ions in the membrane will change according to the valence of the co-ion and counter-ions present in the solution. Thus, if the valence of the co-ion (zB) has a lower value and the valence of the counter-ion (zA) is increased, the concentration of co-ions in the membrane will be favored. For example, the retention of some common salts by descending order (Na2SO4 > NaCl > CaCl2) through a negatively charged NF membrane can be predicted according to these principles [60-63].
Donnan theory is generally used to describe the permeability and selectivity of NF membranes using solutions containing only one amino acid. For example, for an amino acid co-ion and its associated counter-ion, in accordance with the Donnan equilibrium, the amino acid is electrically rejected by the charged active layer of the membrane. Simultaneously, the counter-ion is retained to ensure the balance of charges as the consequence of the electromigrative flow that opposes the convective one. However unfortunately, the extrapolation of Donnan theory to predict the behavior of individual solutes in mixed solutions containing several negative, neutral and positive solutes is very limited, mainly because of coupling and competitive effects. For this reason, NF process of complex mixtures of amino acids and peptides is a difficult object for mathematical modeling [64].
3.4.2. NF Applied to amino acid and peptide fractionation: Review
To clarify the mechanisms involved in the separation of biomolecules by NF membranes several fundamental researches have been published. Table 2 shows relevant NF studies involving amino acids and peptides. The data obtained are relative at different factors affecting the separation of single amino acid (AA) solutions, peptides mixtures and protein hydrolysates. For example, the influence of pH in the retention of amino acids through NF membranes was studied to analyse the separation of small peptides (only two amino acids). In this case, different isoelectric points (pI) by adjusting the pH of the mixture were considered in peptides rejection [65]. Another report showed the separation of a mixture of nine amino acids on the basis of electrostatic interactions of solutes-membrane [66]. According to results, pH has the greater influence on membrane selectivity. In addition the content of inorganic ions compared to the content of ionized amino acids affects also the separation. Therefore these variables are crucial for optimization of membrane selectivity.
Reference
Solution
Experiments
Membrane
[65]
Single AA solutions Mixtures of dipeptides
pH variation experiments Separation experiments of mixed dipeptides
Flat-sheet membranes Materials: Phosphatidic Acid (PA), Thin Film Composite (TFC), Sulfonated Polyethersulfone SPES) and Sulfonated Polystyrene (SPE) MWCO: 0.2-3 kDa Charge at pH 7: negative (SPES, SPE and TFC) or amphoteric (PA)
[66]
Mixtures of AA
Separation of a mixture of 9 AAs on the basis of differential electrostatic interactions with the membrane Membrane selectivity as a function of pH, AA concentration and Ionic Strength
Material: Inorganic membrane, chemical modification of the ZrO2 layer of a UF membrane with cross linked Polyetherimide (PEI) Charge: positive
[13]
Single AA solutions AA mixtures Peptides (from protein hydrolysate)
NF of charged AA (single solutions and mixtures) and peptides(similar MW but different pI)
Material: ZrO2 filtering layer on a mineral support Charge: weakly negative charge at pH 8.0
[67]
Single AA solutions AA mixtures
Influence of concentration and ionic composition (salt concentration and kind of salt added) on single AA retention. Separation of AA mixtures
Separation of a mixture of 10 small peptides Influence of physicochemical conditions (ionic strength and pH) on the fractionation (permeate flux and Tr)
M5+PEI: ZrO2 modified with PEI Kerasep Solgel: microporous active layer of ZrO2
[16]
Protein hydrolysate
Effect of adjusting pH and ionic strength in the fractionation of the hydrolysate.
Flat sheet TFC membranes. Material and MWCO: PA (2.5 kDa), cellulose acetate (0.5, 0.8, 1-5 and 8-10 kDa). Charge: anionic characteristics
[69]
Single AA solutions AA mixtures
Influence of experimental conditions on the steady-state regime pH effect on retention coefficients of single AA solutions and AA mixtures Influence of ionic strength and transmembrane pressure on retention coefficients of an AA mixture
Cross-flow NF membrane Material: ceramic alumina γ with an average pore radius of 2.5 nm. Charge: zero point charge in the range of pH 8-9. Positively charged in the pH range tested.
[70]
AA mixtures
Separation performance of two different NF membranes. Influence of pH and operation pressure on the selectivity of the separation. Simulation NF process system for separation and concentration of L-Phe and L-Asp
CTF membranes with asymmetric structure Material: aromatic PA and SPS
[71]
Protein hydrolysate
Concentration polarization phenomena: effect of hydrodynamic conditions on the Tr of selected peptides from the hydrolysate
Effect of pH, concentration and physicoquemical environment (ionic strength and kind of salt added) on single AA rejection Effect of operating pressure and concentration of fermentation broth on NF (selectivity and AA rejection)
Material: SPES Charge: high negative charge at neutral pH
[14]
Protein hydrolysate
Effect of feed concentration, pH, transmembrane pressure and feed velocity in the ability of a “loose” composite NF membrane to fractionate acid, neutral and basic peptides. Evaluation of the effect of peptides fouling on sieving and electrostatic characteristics of the membrane: PEG and Effect of aggregating peptides on the fractionation of a protein hydrolysate
Flat sheet membrane Material: PA (proprietary) MWCO: 2.5 kDa Charge: negatively charged at alkaline pH
[57]
Protein hydrolysate
NaCl retention measurements.
Flat sheet membrane Material: PA (proprietary) MWCO: 2.5 kDa Charge: negatively charged at alkaline pH
[23]
Peptide mixture
Selectivity estimation in the separation peptides from lactose and effect of pH in fouling
Study solute rejection versus concentration of 5 different AA. Comparison of experimental data against a combined steric and charge rejection model.
Material: SPES MWCO: 1kDa
Table 2.
NF studies involving amino acids and peptides
Influence of concentration and ionic composition (salt concentration and type of salt added) on single amino acid retention and on the separation of amino acid mixtures was also studied to explain peptides rejection [67]. The different results show that both parameters have a negative impact on the selectivity of the membrane when size effects are not dominant. Under these conditions, the membrane seems to be more permeable to charged components due to saturation of its charged sites which makes that repulsive/attractive force between the membrane and the charged peptides become weaker.
Other studies have showed that the mixture of amino acids and their concentration affect also the behavior of NF membranes. However very few works have focused on concentrated amino acid or peptide mixtures. The most NF studies involve highly diluted amino acid solutions, which are the most likely to be found in industrial processes, and the results obtained to date are not completely understood due to at the difference in the data. For example, the results of the separation of l-glutamine (l-Gln) from Gln fermentation broth by NF, showed the effects of various experimental parameters such as transmembrane pressure, pH and concentration of broth on the rejection of l-Gln and l-glutamate (l-Glu). However, the rejection of fermentation broth from a single l-Gln or l-Glu solution was mainly caused by the complex ionic composition of the real fermentation broth [72]. Increase of I-GIn rejection was reported as a function of concentration in a concentration range from 0.3 to 3% (w/v) while the rejection of I-Glu decreased in the range from 0.1 to 0.85%.
Permeation experiments of aqueous solutions of diprotic amino acids (L-glutamine and glycine) showed different data [75]. Amino acid rejection became more concentration dependant at higher pH values due to the increased net charge of the solutes. In this high concentration regime (up to 2 M of glycine) and under alkaline conditions, an important decrease in amino acid rejection was observed in all tests.
Recent results were also found in the experiments of rejection of five amino acids by NF membranes, where experimental data were compared against a combined steric and charge rejection model [76]. Only positive charged amino acids showed good agreement with the model in all the concentration range studied while the behavior of negatively charged peptides only agree with the model at the highest concentration values and rejection of neutral amino acids was decreased due to its smaller net charge. Despite these data, the separation of bioactive peptides from natural sources and the prediction of their individual behavior require previous NF studies of complex mixed solutions.
At the other hand, the study of separation of tryptic β-casein peptides trough UF membranes showed that the separation of peptides is also affected by ionic strength by means a controlled dual mechanism: size exclusion and electrostatic repulsion [77]. Electrostatic interactions affect the peptides transport, especially if the ionic strength of the solution is low.
Another subsequent work reported the interesting potential of NF membranes for separating peptides in the range of 0.3-1 kDa [68]. Specific conditions of ionic strength and especially pH promoted the separation of peptides because the membrane and peptides showed amphoteric properties. Three categories of peptides (acid, basic, neutral) were separated according to their pI. At optimum pH 8 this led to high transmissions of basic peptides (even over 100%), intermediate transmissions for neutral peptides, and low transmissions for acid peptides. The addition of multicharged cationic and anionic species in the hydrolysate induced a markedly enhanced selectivity when the polyelectrolyte was a membrane co-ion and a complete reversion of selectivity when it was a membrane.
An additional research was later performed in order to understand the separation of peptide mixtures through NF membranes [13]. In this case, the solution tested was a mixture of 4 small peptides (4-7 residues) obtained by trypsin hydrolysis of caseinomacropeptide. From above results, it was proposed the first comprehensive approach concerning at filtration of mixtures of peptides, under two principles: (i) electro-neutrality of the solutions is always recovered, which means that all charged solute transmission are interdependent, and (ii) the number of charges along the peptide sequence, rather than the global net charge, has to be considered in order to explain the transmission of a given peptide.
Afterwards, it was investigated the potential of organic NF membranes with a MWCO between 1 and 5 kDa for the fractionation of whey protein hydrolysates. The effect of adjusting pH and ionic strength on the separation properties of the membranes was also characterized in these tests [16]. Highest selectivity between basic and acidic peptides was found at alkaline conditions without the addition of NaCl. In addition the authors demonstrated that two peptides differing by only one amino acid are transmitted differently. Consequently a single change in the amino acid sequence can affect peptides transmission.
Influence of peptide interactions on peptide separation was also established in some studies of NF membranes. The data show that the same peptide could be transmitted differently when issued from different hydrolysates, reflecting the importance of surrounding peptides, and, hence, the possible occurrence of peptide-peptide interactions [78]. Therefore hydrophobic interactions between peptides when the pH of the solution is close to their pI can lead to their aggregation and subsequent fouling of the NF membrane.
By means of NF experiments on fractionation of β-Lg tryptic hydrolysate, it was shown that peptide-peptide interactions are mainly driven by hydrophobic interactions and that some peptides are aggregated at acidic pH [14]. The morphology of these aggregates avoids the neutralization of the negative charge of the membrane surface with the alkaline peptides in the bulk. Therefore, higher permeability and higher transmission of small positive peptides is obtained under these conditions.
Furthermore peptide aggregates contribute at the polarization concentration on the membrane surface. In this case, the peptides can interact in the polarized layer during the filtration process and their transmission decreases with the time under specific conditions [79].
Other successive tests demonstrated that although physico-chemical parameters such as pH and ionic strength are the dominant ones in the case of NF membranes, operational parameters which determine permeate flux through the membrane, and in particular transmembrane pressure, have also an important influence on the retention of peptides and therefore on the selectivity of the membrane [71]. Furthermore, it should be noted that the resulting sieving properties of some NF membranes could depend on the fouled peptide layer and the composition of this layer interacting with the membrane is pH dependant [28].
The combination of membrane processes (UF and NF) was also recently used in the fractionation of whey hydrolysates to study peptides transmission [29]. The first step of this process consisted in the UF of the hydrolysate in order to obtain complete rejection of intact proteins and intermediate peptides. The resulting permeate fractions were then subjected to a fractionation by NF and a peptide fraction having a molar mass range of 5-2 kDa was isolated in this step. Transmission of peptides, amino acids and lactose were found to be mainly affected by the permeability of the fouling layer showing the effect of peptide aggregates.
Comparison of results of NF peptides using a single amino acid solutions, amino acid mixtures and peptide mixtures, had enabled to conclude that whatever the complexity of the solution: the charge is the most important criterion for the separation of peptides having similar molecular weight. The pH value of the solution is the parameter, which has the greatest effect on the separation. Addition of salts (increase of ionic strength) could decrease the intensity of charge effects. The determination of both the membrane and the mixture characteristics are of paramount importance in order to predict and optimize the performance of NF membranes for the fractionation of complex peptide mixtures.
3.4.3. Main parameters influencing peptide fractionation using NF membranes
The interactions of peptide-peptide and peptide-membrane affect the separation process performance and thus it is difficult to predict the selectivity of the membranes when the objective is the fractionation of complex peptide mixtures. According the literature, the most important parameters that cause effect on membrane selectivity are pH, ionic strength, polarization layer and fouling.
1. The pH of solution is an important control variable in NF processes for the fractionation of complex peptide mixtures, because peptides are molecules that have at least one carboxylic group (R−COOH↔R−COO− and one amine group (R−NH3+↔R−NH2). The total number of acid and basic groups depends on its primary structure (amino acid sequence) and it determines the pH value at which the peptides have the same number of negative than positive charges, i.e., its pI. Peptides can be classified in three different groups according to their pI: acidic peptides (pI ≤ 5), neutral peptides (5 < pI ≤ 7) and basic peptides (pI > 7). Their net charge depends on the pH of the solution, as well as the charge density of the NF membrane. This last value will vary because of the ionization of its functional groups (acidic and basic).
In NF, the transmission of amino acids and peptides reaches its maximum value when the pH is equal to the pI. Under these conditions, repulsive electrostatic interactions are minimized. That way, the modification of NF membranes transmission is possible by changing the pH of the mixture.
In the case of protein hydrolysates, which composition is more complex, there will be a pH value at which the fractionation of acid, neutral and basic peptides is maximized. For example, it has been shown that the separation factor between basic and acid peptides reaches its maximum value when the pH of the mixture is alkaline [16]. However, literature published on this topic only describes the behavior of “tracer” peptides in the hydrolysate and this limits the scope of the separation factor calculated.
2. The ionic strength of peptides solution affects the selectivity of NF membranes. In an aqueous medium the increase of the ionic strength, for example by the addition of NaCl, results in a decrease of zeta potential of the NF membrane [80-83] as well as a decrease in the electrophoretic mobility of proteins and peptides [84]. According to these observations, electrostatic interactions between the membrane and the peptides become less intense, which usually leads to better transmission values of the peptides.
Several authors have demonstrated the preponderance of a selectivity based on electrostatic interactions at low ionic strength values [16, 68, 85]. The fact that electrostatic interactions membrane-peptide lose significance at high ionic strength values results in a decrease of the double selectivity size/charge in processes involving NF membranes. In addition to the effect over the charge density of the membrane, ionic strength also influences the effective hydrodynamic volume of charged proteins and peptides [86]. A charged protein is surrounded by a diffuse ion cloud, typically called the electrical double layer, and the thickness of this layer is characterized by the Debye length (LD):
LD=0.304I-1/2E2
Where I is the ionic strength (mol/L) and LD is in nm. According to equation 3 the higher the ionic strength the narrower the Debye length.
In addition, the effect of the electrical double layer could be described in terms of an increase in the effective protein radius Reff:
Reff=rs+0.045Z2LDrsE3
Where rs is the hard-sphere radius of the uncharged protein or peptide (in nm) and z is the surface charge of the protein (in electronic charge units).
Equations (3) and (4) indicate that relatively low salt concentration is needed in order to enhance the magnitude of the electrostatic interactions. However, the increase in the ionic strength leads to an increase in the transmission of charged peptides though the membrane.
This last observation, which is well known and it has been applied to explain the selectivity of several protein separation processes using UF membranes, is not usually mentioned in works involving the separation of peptides by NF membranes. The effects of the ionic strength over the charge density of the membrane and over the effective hydrodynamic volume of charged peptides are complementary and both of them contribute in the explanation of experimental results.
Variation of these parameters has been applied by some authors [86-88] to obtain good selectivity values in the fractionation of different proteins with similar sizes. The wise combination between membranes, pH and ionic strength is called HPTFF (High-performance-tangential flow filtration) and it is effective when proteins or peptides to be fractionated show different pI and when low or medium protein concentration is processed.
3. Concentration polarization and fouling is also a condition affecting the peptides separation. Physico-chemical parameters such as pH and ionic strength are of paramount importance in NF processes because they modulate the electrostatic interactions on which the selectivity of these membranes is supported. In addition electrostatic interactions may partly explain the distribution of a peptide between the whole solution and the membrane interface [89-90]. However, when using porous membranes, peptides are involved in a convective transport flux and its rejection is therefore the result of (i) electrostatic interactions between the membrane and the peptides plus (ii) a steric mechanism through the porous. In this sense, hydrodynamic parameters have influence in peptide rejection [91]. Thus, for example, when the MWCO of the membrane and the molecular weight of the peptide have similar values or in the presence of electrostatic interactions, an increase in transmembrane pressure will result in an increase of amino acid retention.
Concentration polarization is one of the consequences of selective solute transport through membranes. The constituents of the solution that are retained by the membrane tend to accumulate over its surface and this creates a concentration gradient in the area called polarization boundary layer. This phenomenon is quickly established at the beginning of the process and leads to a modification in the efficiency of membrane processes as well as a change in the composition of the permeate stream. The management of hydrodynamic conditions could minimize its effects. In addition size exclusion properties related to the pore size of the membrane could be completely modified due to pore blocking by the peptides. Fouling is a general term for any accumulation of deposits and materials over the membrane surface or within the pores. Two kinds of fouling can be defined: reversible fouling, the one which can be reduced by adjusting hydrodynamic conditions (velocity or transmembrane pressure), and irreversible fouling, which effect can´t be avoid by cleaning procedures.
In practice, the series resistance model is widely used for fouling quantification in membrane processes. This approach derives from Darcy’s phenomenological equation. The clean water flux rate (JW) through a membrane is defined by equations (5).
Jw=PTμwRME4
\n\t\t\t\t\t
Where PT is the transmembrane pressure, μW the water viscosity and RM the intrinsic resistance of the membrane.
The measurement of water flux rate through the same membrane after being used (JW’) can be expressed as:
JW’ = PTμw(RM+Rf)
Equation 6 allows the calculation of the resistance associated to fouling (Rf).
Studies involving peptides transmission or retention don´t usually take into account the polarization and fouling phenomena but it has been demonstrated that these phenomena are crucial in the case of protein hydrolysates, especially at acid pH values [16, 68]. Complex peptide mixtures contain peptides, which with different physicochemical characteristics (pI, hydrophobicity, charge) promote the creation of strong interactions with filtration membranes [92-93].
4. Future potential of peptides fractionation by means of membrane techniques
Currently, conventional membrane separation techniques can be employed to obtain peptide fractions in purified form with higher functionality and higher nutritional value. Special properties of the NF membranes make possible novel peptide separations. However, the specific separation of one or more peptides from a raw hydrolysate is a difficult subject because ionic interactions between peptides and membranes can markedly influence on peptides fractionation. In addition these pressure-driven processes involve the accumulation of particles on membrane leading formation of a fouling and to the modification of the membrane transport selectivity. Therefore, it is clear that NF still has to grow more in terms of understanding, materials, and process control. In addition modeling studies are necessary to predict of the process performance in all circumstances.
Alternatively the application of an external electrical field, which acts as an additional driving force to the pressure gradient, can be seen as a technique that could improve the efficiency of the conventional membrane processes for the separation of charged bioactive molecules. In this sense, two different configurations can be distinguished: electrically-enhanced filtration, which can be used with conventional pressure driven membrane filtration, and forced-flow membrane electrophoresis, which is conducted in an electrophoretic cell. Intensive researches on these membrane processes have been carried out including electromembrane filtration (EMF) [94-95], electrodialysis with UF membranes (EDUF) [96-99] and forced-flow electrophoresis (FFE) [100] for the separation of charged bioactive molecules.
EDUF couples size exclusion capabilities of UF membranes with the charge selectivity of electrodyalysis (ED) allowing separation of molecules according to their electric charges and to their molecular mass (membrane filtration cut-off). The feasibility of peptide fractionation by EDUF was demonstrated notably with β-Lg tryptic hydrolysate solutions and was suggested to improve the separation between basic and neutral peptides [97]. Actually, EDUF process also allowed a selective and a simultaneous separation of anionic and cationic peptides presents in an uncharacterized concentrated polypeptide mixture of snow crab by-products hydrolysate [101].
Recently a comparative study on NF and EDUF was performed in terms of flux and mass balance [102]. The results showed that NF provides a greater mass flux while when using EDUF a wider range of peptides and more polar amino acids are recovered. EDUF can be seen to be a promising separation technology, but further scale-up developments will be necessary to confirm its feasibility at large scale.
EMF combines the separation mechanisms of membrane filtration and electrophoresis. Ion exchange membranes are replaced by UF in a conventional electrodialysis cell. In electrophoretic separators, a porous membrane is used to put into contact two flowing liquids between which an electrically driven mass transfer takes place. During this process the mass transport is affected by electrostatic interactions taking place at the membrane solution interface. The perspectives in the field of peptide fractionation will be the complete understanding of the interactions of peptides and membrane as well as the development of new membrane materials of gels limiting or increasing these interactions to improve the selectivity and the yield of production of specific peptides [100].
\n',keywords:null,chapterPDFUrl:"https://cdn.intechopen.com/pdfs/42422.pdf",chapterXML:"https://mts.intechopen.com/source/xml/42422.xml",downloadPdfUrl:"/chapter/pdf-download/42422",previewPdfUrl:"/chapter/pdf-preview/42422",totalDownloads:2969,totalViews:284,totalCrossrefCites:4,totalDimensionsCites:9,hasAltmetrics:0,dateSubmitted:"January 18th 2012",dateReviewed:"September 21st 2012",datePrePublished:null,datePublished:"January 30th 2013",dateFinished:null,readingETA:"0",abstract:null,reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/42422",risUrl:"/chapter/ris/42422",book:{slug:"bioactive-food-peptides-in-health-and-disease"},signatures:"Claudia Muro, Francisco Riera and Ayoa Fernández",authors:[{id:"85654",title:"Dr.",name:"Claudia",middleName:null,surname:"Muro",fullName:"Claudia Muro",slug:"claudia-muro",email:"cmuro@ittoluca.edu.mx",position:null,institution:{name:"Instituto Tecnológico de Toluca",institutionURL:null,country:{name:"Mexico"}}},{id:"94458",title:"Dr.",name:"Francisco",middleName:null,surname:"Riera Rodríguez",fullName:"Francisco Riera Rodríguez",slug:"francisco-riera-rodriguez",email:"far@uniovi.es",position:null,institution:{name:"University of Oviedo",institutionURL:null,country:{name:"Spain"}}},{id:"167650",title:"Dr.",name:"Ayoa Fernández",middleName:null,surname:"Martínez",fullName:"Ayoa Fernández Martínez",slug:"ayoa-fernandez-martinez",email:"ayoafm@hotmail.com",position:null,institution:null}],sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Overview of techniques used for peptide fractionation",level:"1"},{id:"sec_3",title:"3. Membrane technology applied to peptide fractionation",level:"1"},{id:"sec_3_2",title:"3.1. Enzymatic membrane reactor equipped with membranes: first step to peptide fractionation ",level:"2"},{id:"sec_4_2",title:"3.4. NF membranes and peptide fractionation",level:"2"},{id:"sec_4_3",title:"3.4.1. NF transport mechanism",level:"3"},{id:"sec_5_3",title:"Table 2.",level:"3"},{id:"sec_6_3",title:"3.4.3. Main parameters influencing peptide fractionation using NF membranes",level:"3"},{id:"sec_9",title:"4. 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Selective Isolation of Cationic Amino Acids and Peptides by Electro-Membrane Filtration. Le Lait 2002801175185\n\t\t\t'},{id:"B96",body:'LapointeJ. FGauthierS. FPouliotYBouchardCSelective Separation of Cationic Peptides from a Tryptic Hydrolysate of β-Lactoglobulin by Electrofiltration. Biotechnology and Bioengineering 2006942223233\n\t\t\t'},{id:"B97",body:'PoulinJ. FAmiotJBazinetLSimultaneous Separation of Acid and Basic Bioactive Peptides by Electrodialysis with Ultrafiltration Membrane. Journal Biotechnology 20061233314328\n\t\t\t'},{id:"B98",body:'PoulinJ. FAmiotJBazinetLImpact of Feed Solution Flow Rate on Peptide Fractionation by Electrodialysis with Ultrafiltration Membrane. Journal of Agricultural Food Chemistry 200756620072011\n\t\t\t'},{id:"B99",body:'PoulinJ. FAmiotJBazinetLImproved Peptide Fractionation by Electrodialysis with Ultrafiltration Membrane: Influence of Ultrafiltration Membrane Stacking and Electrical Field Strength. Journal Membrane Science 200729918390\n\t\t\t'},{id:"B100",body:'BazinetLFirdaousLMembrane Processes and Devices for Separation of Bioactive Peptides. Recent Patents on Biotechnology 2009316172\n\t\t\t'},{id:"B101",body:'DoyenABaulieuLSaucieraLPouliotYBazinetLDemonstration of in Vitro Anticancer Properties of Peptide Fractions from a Snow Crab by-Products Hydrolysate after Separation by Electrodialysis with Ultrafiltration Membranes. Separation and Purification Technology 2011783321329'},{id:"B102",body:'LangevinM. ERobletCMoresoliCRamassamyCBazinetLComparative Application of Pressure and Electrically-Driven Membrane Processes for Isolation of Bioactive Peptides from Soy Protein Hydrolysate. Journal Membrane Science 2012\n\t\t\t'}],footnotes:[],contributors:[{corresp:null,contributorFullName:"Claudia Muro",address:null,affiliation:'
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1. Introduction
After discovering graphene in 2004, the two-dimensional (2D) materials have drawn significant attention in broad applications due to their unique physicochemical properties. The 2D materials such as transition metal dichalcogenides (TMDs), phosphorene and bismuthine, etc., which consists of a one-atom-thick monolayer network can exhibit different chemical and physical properties, including the electrical and thermal conductivity, magnetic, photonic and catalytic properties when compared to their bulk counterparts [1]. Over the past few years, the enormous 2D family materials like graphene [2, 3], molybdenum disulphide (MoS2) [4, 5], tungsten disulphide (WS2) [6, 7], graphitic carbon nitride (g-C3N4) [8] and recently MXene [9, 10] have been investigated for various applications in electronic, energy, catalysis and electrochemical applications. However, the electrochemistry investigation of those materials is yet to be explored in detail. The limitation in the bandgap of these materials has hindered their performance in practical applications. Therefore, exploring a new novel 2D material is highly recommended, especially for the future electrochemical energy conversion, storage, and biosensors applications. Recently, silicon (Si) based one-atom-thick layered material named siloxene has been investigated for electrochemical energy and sensing applications, including supercapacitors, batteries, and dopamine sensors [1, 11, 12, 13].
Siloxene is a direct bandgap material that was discovered by Wohler in 1863. It can be obtained through the deintercalation of calcium and exfoliation from the Zintl phase of calcium silicide (CaSi2) powder [14, 15, 16]. Different from the graphene planner structure, siloxene possesses a low-buckled structure due to its double band role. As a result of the surface-terminated functional groups with Si chain and the mixed sp2 and sp3 hybridization, siloxene can provide several advantages in the electrochemical energy and sensor applications [1, 11, 12, 17].
1.1 Synthesis of siloxene and its structural types
Siloxene is prepared by deintercalation of Ca2+ from CaSi2 under concentrated hydrochloric acid. Briefly, the required amount of CaSi2 powder and HCl acid stirred in the ice-cold condition under the inert gas atmosphere for 2-4 days (Figure 1). During this reaction, the deintercalation of Ca layers and functionalization of Si sheets can be occurred simultaneously and formed the siloxene structure. The following equation can describe the common formation mechanism of siloxene from CaSi2 [11].
Figure 1.
Siloxene synthesis process (reproduced from [11] with permission from Elsevier).
3CaSi2+6HCl+3H2O→Si6O3H6+3CaCl2+3H2↑E1
In general, the siloxene stoichiometric ratio of Si:H:O is 2:2:1. Based on the exfoliation and deintercalation conditions such as reaction time, the concentration of the acidic medium, and temperature, siloxene can be classified into two major types. (1) Weiss, and (2) Kautsky type siloxene structures [18]. In Weiss type siloxene (Si6(OH)3H3), the six-membered Si6 rings connected with alternative Si-H and Si-OH bonds, whereas Kautsky type siloxene (Si6O3H6), the Si6 rings connected by Si-O-Si bridge (Figure 2). It is noteworthy that the crystalline silicon (common impurity) in CaSi2 may affect the siloxene structure formation [19], which deviates from the structures mentioned above.
Figure 2.
Different types of Siloxene structure [19].
2. Electrochemical application of siloxene
Due to the unique 2D structure and the abundant functional groups of siloxene, it can be applied in various applications such as optoelectronics, catalysis, water splitting, etc. Theoretical investigations of the siloxene have shown the high possibilities in different electrochemical applications [20]. However, because of limited knowledge of siloxene’s electrochemistry, only a few works have been reported on the electrochemical application of siloxene so far. The siloxene has been mainly employed in supercapacitors and batteries as an electrode material and detection of biomarkers in electrochemical biosensors.
2.1 Supercapacitors
2.1.1 Siloxene based supercapacitors
Though siloxene was discovered in 1863, it has recently received considerable attention in the electrochemical energy storage application. The researchers have been focused on siloxene based electrode materials for energy storage and conversion application. Due to the increases in energy consumption and the non-renewable sources decreasing gradually, the development of high-efficiency energy storage devices is highly demanded. Electrochemical or supercapacitors are the perfect choice for high-performance devices as the results of its high-power density and long cyclic lifetime [21]. Compared with the commercial activated carbon-based supercapacitors, the integration of Si-based materials with the current microelectronic technology can lead to higher performance in energy storage devices because of its high theoretical capacity (3579 mA hg−1). However, Si-based materials such as silicon carbide (SiC), Si nanowire, porous silicon have been employed as electrode materials in supercapacitor application, the functionalization of the one-atom-thick Si layers with interconnected Si6 rings can accommodate the better performance in supercapacitors [1].
Krishnamoorthy et al. have reported the siloxene based symmetric supercapacitor (SSC) application in 2018 [1]. The Kautsky-type of siloxene structure prepared by deintercalation of calcium from CaSi2 and confirmed its Si-O-Si bridges Si6 rings interconnection by Fourier transform infrared spectroscopy. The capacitance behavior of the siloxene has been studied in tetraethylammonium tetrafluoroborate (TEABF4) electrolyte under optimal conditions. Interestingly, the operating potential window (OPW) of the siloxene-SSC device was determined from 0 to 3.0 V. This result confirms the excellent electrochemical stability of the SSC device even at a higher voltage window. The fabricated SSC device showed unique capacitance behavior with an energy density of 5.08 W h kg−1 (areal energy density of 9.82 mJ cm−2) and about 98% of capacitance retention even after 10 k cycles (Figure 3). The ion diffusion and the electron transfer rate were significantly enhanced by the conductive hexagonal Si frameworks in the siloxene during the electrochemical redox reactions. Also, the high surface area and the larger interlayer spacing between the siloxene sheets were enabled fast ion transport and improved the electrochemical performance of the SSC device.
Figure 3.
(a, b) Ragone plot and cyclic stability of p-siloxene SSC device; (c) structure of p-siloxene [1]; (d, e) Ragone plot and cyclic stability of HT- siloxene SSC device; (f) structure of HT-siloxene (reproduced from [23] with permission from ACS).
It is well known that the reduced graphene oxide (rGO) can increase the electroactive sites for the electrochemical reactions than bare graphene oxide (GO) because of its higher electronic conductivity [22]. The electrical conductivity of siloxene sheets may decrease when a higher amount of the oxygen functional groups is attached on its edge/basal surface; thus, the reduction of oxygen functional groups in siloxene enhances the active sites for electrochemical redox reactions due to its better conductivity. In this scenario, Parthiban et al. have investigated the removal of oxygen functional groups in pristine siloxene (p-siloxene) at high temperatures and obtained reduced siloxene sheets (denoted as HT-siloxene). Calcinating siloxene sheets removed the functional groups at edge/basal planes of siloxene at 900°C, which led to the formation of reduced siloxene sheets [23]. Interestingly, the calcination process has decomposed the oxygen functional groups at edge/basal planes of siloxene and preserved the Si6 rings’ connection with oxygen atom without affecting the 2D layer structure. The obtained HT-siloxene possessed a higher electrical conductivity than p-siloxene resulting in improved electrochemical performance. The specific capacitance of the HT-siloxene increased almost 1.71 times higher than that of p-siloxene. The maximum energy density of the HT-siloxene SSC device has been achieved by about 6.64 Wh kg−1, higher than p-siloxene (3.89 Wh kg−1) due to its lower equivalent series resistance and better electrical conductivity. The complete removal of the oxygen functional groups in p-siloxene enhanced the energy density of SSC. It also increased the cyclic stability of the SSC (96.3% after 10000 cycles), as shown in Figure 3.
Another fascinating strategy has been developed by Kim and co-workers recently that dry reforming methane (DRM) recycled siloxene/Ni foam catalyst towards supercapacitor applications. The siloxene coated Ni foam was initially utilized for DRM reactions for producing H2 and CO gas by CO2 reduction. After the DRM reaction, the siloxene/Ni foam catalyst has employed as electrode material in SSC [24]. The regeneration of carbon during the DRM reactions deposited on the siloxene/Ni foam catalyst and could improve the electrochemical performance. Compared to the p-siloxene and HT-siloxene, the carbon-coated siloxene/Ni foam exhibited superior performance in the supercapacitor. A maximum energy density of 30.81 Wh kg−1 was achieved for carbon/siloxene/Ni foam-based SSC, indicates the remarkable performance enhancement. Thus, utilizing spent siloxene catalysts to supercapacitor can be an effective approach for waste-to-energy applications. Besides, the direct use of the siloxene in a supercapacitor, siloxene was also confirmed as a flexible template for fabricating silicon oxy-carbide (SiOC). Carbothermal conversion of siloxene to SiOC has been proposed by Pazhamali and co-works [12]. Mixing siloxene and sodium alginate at 900°C led to the formation of SiOC. Since the SiC-based electrodes can intensify the cycling stability and areal capacitance in supercapacitors, the SiOC electrodes were expected to improve the stability of the SSC device than siloxene based SSC. The SiOC based SSC device delivered an excellent electrochemical performance with an energy density of 20.89 Wh kg−1, which is higher than that of p-siloxene. However, the cyclic stability of SiOC supercapacitor decreased to 92.8% after 5000 cycles. As pointed out in the previous paragraph, the removal of oxygen functional groups can improve the SSC performance; the complete reduction of oxygen in SiOC may help to facilitate the fast ion transport and wettability of the electrode during the long cyclic time.
2.1.2 Siloxene composite supercapacitor
Making composite electrodes is an efficient approach to increase the supercapacitor’s electrochemical performance due to its synergistic behavior [25]. The specific capacitance of siloxene is restricted because of its aggregation effect; consequently, the layers agglomerations generate poor utilization of the pores and the lower specific surface area. Thus, introducing a spacer material such as metal oxides or carbon between the siloxene sheets can enhance the accessible sites for the electrochemical reactions. Meng and co-works have reported the construction of a three-dimensional (3D) architecture of siloxene-reduced graphene oxide hydrogel (SGH) through a simple hydrothermal method (Figure 4) [26].
Figure 4.
Synthesis of siloxene-reduced graphene oxide hydrogel and its specific capacitance plot [26].
The hybrid structure of SGH has increased the specific surface area and facilitated the electrolyte ions transportation, resulting in improved capacitive performance. As compared to bare siloxene electrode specific capacitance (23 F g−1), the SGH with 1:3 ratio composite electrode exhibited a maximum specific capacitance of 520 F g−1 at a current density of 1 A g−1. However, the EDLC of the graphene in SGH has contributed significantly to the capacitive enhancement of siloxene-graphene composite. Though graphene could facilitate the capacitance performance, the surface oxygen-functional groups of siloxene provided pseudocapacitance and improved the wettability of the electrode, results in an excellent rate capability and outstanding cyclic stability.
2.2 Siloxene application in batteries
Like supercapacitors, rechargeable batteries (e.g., lithium-ion batteries, sodium-ion batteries, lead-acid, etc.) are primary power sources for large-scale portable and wearable electronic devices. They have received significant consideration due to their high energy density and long cyclic stability [27, 28]. However, the current battery technologies cannot meet the advanced application requirement as the result of confined energy storage capacity. Thus, the development of commercial electrodes in the existing technologies is highly needed.
The theoretical capacity of silicon (Si) is 4200 mA hg−1 [29], which is higher than the capacity of graphite (372 mA hg−1), has considered being an active anode material for the future lithium-ion batteries (LIBs). However, the severe capacity degradation and the high-volume change during the lithiation-delithiation process may lead to lower Coulombic efficiency. Making 2D Si nanosheets with oxygen functional groups provides a high specific surface area, resulting in fast lithium storage and preventing volume changes. As mentioned in the previous section, the siloxene oxidation level can be controlled by the various synthesis conditions such as temperature, oxidants, concentrations, etc. The oxidation level may influence the lithiation-delithiation process. Xu and co-workers have demonstrated the siloxene preparation with different oxidation levels in the various oxidants and the temperature [30]. Three types of siloxene oxidation level have been achieved by altering the oxidants and temperature: (i) CuCl2 aqueous solution used to prepare fully oxidized siloxene nanosheet (FO-SNS) at room temperature; (ii) partially oxidized siloxene nanosheet (PO-SNS) made in SnCl2 ethanol solution at 60°C and (iii) hardly oxidized siloxene nanosheet (HO-SNS) synthesized in a LiCl-KCl molten salt at 400°C (Figure 5(i)). The FO-SNS, PO-SNS, and HO-SNS electrodes delivered the lithiation capacity of 298, 1218, and 1450 mA hg−1. Besides, the HO-SNS presented a higher Coulombic efficiency of 66%, which is higher than FO-SNS (24%) and PO-SNS (56%). The improved performance of HO-SNS has associated with the presence of a higher atomic percentage (64%) of bulk Si (Si0) and the lower percentage (7%) of SiO2 (Si4+) in HO-SNS, which were estimated from the XPS analysis (Figure 5(ii)). Besides, the hierarchical nanostructure of HO-SNS could buffer the volume expansion and contribute to the good rate performance. Fu and co-workers have remarked that bare siloxene is an unsuitable anode material for LIBs due to its inadequate electrochemical capacity, resulting in the lower Coulombic efficiency. However, Si- derivatives such as silicon suboxides (SiOx), carbon-coated SiO2, etc., from siloxene can meet higher capacity requirements with satisfactory Coulombic efficiency. Fu et al., have demonstrated the carbon-coated 2D SiOx nanocomposites (nano-Si/α-SiO2) from siloxene to moderate the volume expansion during the electrochemical lithiation-delithiation process [31]. The carbon-coated nano-Si/α-SiO2 anode materials showed the limited volume change, fast electrons transport, and more significant Li-ion kinetics, resulting in high initial Coulombic efficiency (72.5%) with a capacity of 946 mA hg−1. On the other hand, the value of x in SiOx can influence Li storage’s electrochemical performance. Thus, controlling the oxidation level of the SiOx is a crucial process to achieve higher capacity than bare Si structures. Many previous studies showed that SiOx with x = 1.0 presented the specific capacity value higher than 1000 mA hg−1 [32]. However, unsatisfactory cyclic life has limited its practical usage. Thus, turning the oxygen content in SiOx is a proper way to improve the electrochemical performance in LIBs. After investigating carbon-coated nano-Si/α-SiO2, Fu and co-workers have prepared siloxene with different levels of oxidation in SiOx and used as anode material for LIB. They controlled the SiOx oxidation level in the siloxene via stepwise oxidizing of the siloxene precursor at various times [32]. SiOx with four different oxidation levels, such as SiO1.01, SiO1.25, SiO1.47, and SiO1.78 has been tailored through siloxene oxidation and investigated their Li-storage capacity. The sample SiO1.47 exhibited optimal electrochemical behavior due to the synergistic effect of electrical conductivity and Li-ion diffusivity. The higher oxygen level in SiOx caused a larger polarization effect, resulting in the poor Coulombic efficiency and smaller reversible capacity.
Figure 5.
(i) SEM images of (a, b) FO-SNS, (c, d) PO-SNS, (e, f) HO-SNS; (ii) XPS spectrum of siloxene samples at different oxidation (reproduced from [30] with permission from Springer).
Similar to the graphene-siloxene composite electrode in supercapacitors, the incorporation of siloxene sheets between the graphene layers enhances the specific surface area, facilitating the fast Li-storage. In the siloxene-graphene (SiG) composite, the siloxene sheets have provided higher Li-storage, and the encapsulated graphene sheets prevented the volume expansion during lithium insertion-extraction process. SiG anode material exhibited the initial cycle charge and discharge capacities of 3016 mA hg−1 and 3880 mA hg−1 with a capacity decay of 78%, which were higher than the bare siloxene and graphene electrodes. The synergistic effect of graphene and siloxene and the excellent electrical conductivity of graphene in the composite contributed to the higher electrochemical performance for LIBs [29].
2.3 Siloxene based electrochemical sensor
The 2D siloxene sheets not only possessed the excellent electrochemical characteristics towards electrochemical energy application. Besides, due to the large surface area and the unique 2D structure of siloxene, the heterogeneous electron transfer (HET) is high, which beneficial for selective electrochemical bio-marker detections. We have recently demonstrated the siloxene-based novel electrochemical dopamine sensor and obtained remarkable achievements in dopamine detection by the siloxene modified sensor [11]. Dopamine (DA) is an important neurotransmitter that plays a crucial role in the central nervous system and cardiovascular systems. A variety of materials have been employed for electrochemical DA detection in the past decades. However, the high selectivity of DA is limited to the existing materials. As a result of high HET rates, large surface area, and improved mass transportation, siloxene possessed high selectivity for DA detection (Figure 6). Siloxene modified glassy carbon electrode showed a well-defined redox peak in the cyclic voltammetry technique towards DA detection. Excellent linearity has been achieved for the siloxene electrode in the presence of a different concentration of DA, and the modified electrode exhibited a detection limit of 0.327 μM. Besides, the proposed sensor revealed a wide linear range from 10 to 1100 μM (Figure 6(b)).
Figure 6.
(a-d) Electrochemical differential pulsed voltammetry response and linear range of siloxene modified electrode for DA detections (reproduced from [11] with permission from Elsevier).
The DA detection performance by the 2D siloxene sheets is remarkably higher than that of other reported 2D graphene and g-C3N4 modified electrodes. Siloxene sheets owned a higher response for the detection limit and showed high selectivity for DA detection. The stronger π-π interaction between the siloxene planar structure and the dopamine phenyl structure enables faster electron transportation during the DA oxidation process, making the high selectivity characteristic of the siloxene modified electrode. On the other hand, the π-π interaction of the siloxene structure with other biomolecules such as ascorbic acid, uric acid, etc., is weak, resulting in the inactive oxidation. However, the thickness of the siloxene sheets can affect the electron conduction during the electrochemical reactions similar to graphene [33]. Reducing the size and the layer thickness of siloxene could tremendously enhance its performance for DA detection.
3. Summary and future research direction
In conclusion, this chapter deals with the comprehensive review of the raising star 2D siloxene based electrochemical energy and sensor applications. The siloxene synthesis process and the siloxene structure affecting parameters have been reviewed in detail. The functional groups in siloxene and the oxidation level can be varied at different synthesis times and the annealing temperature. Compared to pristine siloxene, high temperature treated siloxene possessed an excellent performance in the electrochemical supercapacitors because of its reduced functional groups. Besides, the siloxene and its composite have been used as anode materials for LIBs and showed a significant capacity and Coulombic efficiency. Li-storage has influenced by the oxidation level in siloxene due to the presence of different atomic percentages of Si functional groups. However, both supercapacitors and LIBs applications, siloxene derivatives such as SiOx, SiOC showed improved performance as the results of its better electrical conductivity and Li-ion diffusivity compared to the bare siloxene. The reported siloxene works have focused on the performance of siloxene in supercapacitors and LIBs. But many works failed to investigate the insight of the electrochemistry of siloxene and its derivatives for better energy density, capacity, and cyclic stability. Thus, the research direction should be focused more on the study of electrochemistry of siloxene. On the other hand, the 2D siloxene sheets proved as a novel electrochemical sensor for highly selective dopamine detection. Moreover, the size and thickness of the layer can influence the HET rate, specific surface area, and active sites for DA detection, which need to be optimized in the near future.
Acknowledgments
This work was supported in part by the National Natural Science Foundation of China (Project No. 51950410598), in part by Shenzhen Science and Technology Innovation Committee (Projects No. JCYJ20170412154426330), and in part by Guangdong Natural Science Funds (Project No.: 2016A030306042 and 2018A050506001). Also, this work was supported by the Major Program of Guangdong Basic and Applied Research (No. 2019B030302009).
\n',keywords:"siloxene, electrochemistry, functional groups, active sites",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/73498.pdf",chapterXML:"https://mts.intechopen.com/source/xml/73498.xml",downloadPdfUrl:"/chapter/pdf-download/73498",previewPdfUrl:"/chapter/pdf-preview/73498",totalDownloads:80,totalViews:0,totalCrossrefCites:0,dateSubmitted:"June 3rd 2020",dateReviewed:"September 9th 2020",datePrePublished:"October 7th 2020",datePublished:null,dateFinished:null,readingETA:"0",abstract:"After discovering graphene, the two-dimensional materials have gained considerable interest in the electrochemical applications, especially in energy conversion, storage, and bio-sensors. Siloxene, a novel two-dimensional low-buckled structure of Si networks with unique properties, has received the researcher’s attention for a wide range of applications. Though the electronic and optical properties of siloxene have been explored in detail previously, there is a lack of electrochemistry studies of siloxene as the result of material degradation, and the investigation is still open-ended to enhance the electrochemical application. Recently, siloxene has been used for supercapacitor, lithium-ion batteries, and dopamine bio-marker detections. This chapter highlights the recent development of siloxene synthesis and its electrochemical properties in energy and sensor applications. The plannar Si structure with Si6 rings interconnected with different oxygen, hydroxyl functional groups, and large interlayer spacing of siloxene sheets can promote the active sites for enhanced electrochemical performance. This chapter provides the current state-of-the-art in the field and a perspective for future development in the electrochemistry field of siloxene.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/73498",risUrl:"/chapter/ris/73498",signatures:"Rajendran Ramachandran, Zong-Xiang Xu and Fei Wang",book:{id:"10414",title:"Novel Nanomaterials",subtitle:null,fullTitle:"Novel Nanomaterials",slug:null,publishedDate:null,bookSignature:"Dr. Karthikeyan Krishnamoorthy",coverURL:"https://cdn.intechopen.com/books/images_new/10414.jpg",licenceType:"CC BY 3.0",editedByType:null,editors:[{id:"278690",title:"Dr.",name:"Karthikeyan",middleName:null,surname:"Krishnamoorthy",slug:"karthikeyan-krishnamoorthy",fullName:"Karthikeyan Krishnamoorthy"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}},authors:null,sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_1_2",title:"1.1 Synthesis of siloxene and its structural types",level:"2"},{id:"sec_3",title:"2. Electrochemical application of siloxene",level:"1"},{id:"sec_3_2",title:"2.1 Supercapacitors",level:"2"},{id:"sec_3_3",title:"2.1.1 Siloxene based supercapacitors",level:"3"},{id:"sec_4_3",title:"2.1.2 Siloxene composite supercapacitor",level:"3"},{id:"sec_6_2",title:"2.2 Siloxene application in batteries",level:"2"},{id:"sec_7_2",title:"2.3 Siloxene based electrochemical sensor",level:"2"},{id:"sec_9",title:"3. Summary and future research direction",level:"1"},{id:"sec_10",title:"Acknowledgments",level:"1"}],chapterReferences:[{id:"B1",body:'Krishnamoorthy K, Pazhamalai P, Kim S-J. Two-dimensional siloxene nanosheets: novel high-performance supercapacitor electrode materials, Energy Environ. Sci., 2018:11:1595-1602. DOI: https://doi.org/10.1039/C8EE00160J'},{id:"B2",body:'Ramachandran R, Felix S, Joshi GM, Raghupathy BPC, Jeong SK, Grace AN. 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Engg. J., 2020:387:123886. DOI: https://doi.org/10.1016/j.cej.2019.123886'},{id:"B13",body:'Loaiza LC, Monconduit L, Seznec V. Siloxene: A potential layered silicon intercalation anode for Na, Li and K ion batteries, J. Power Source, 2019:417:99-107. DOI: https://doi.org/10.1016/j.jpowsour.2019.02.030'},{id:"B14",body:'Nakano H, Ishii M, Nakamura H. Preparation and structure of novel siloxene nanosheets, Chem. Commun., 2005:2945-2947. DOI: https://doi.org/10.1039/B500758E'},{id:"B15",body:'Li S, Wang H, Li D, Zhang X, Wang Y, Xie J, Wang J, Tian Y, Ni W, Xie Y. Siloxene nanosheets: a metal-free semiconductor for water splitting, J. Mater. Chem. A 2016:4:15841-15844. DOI: 10.1039/c6ta07545b'},{id:"B16",body:'Kong X, Liu Q , Zhang C, Peng Z, Chen Q. Elemental two-dimensional nanosheets beyond graphene, Chem. Soc. Rev., 2017:46:2127-2157. DOI: 10.1039/c6cs00937a'},{id:"B17",body:'Zhang W, Sun L, Vianney JM, Nsanzimana, Wang X. Lithiation/Delithiation Synthesis of Few Layer Silicene Nanosheets for Rechargeable Li–O2 Batteries, Adv. Mater., 2018:30:1705523. DOI: 10.1002/adma.201705523'},{id:"B18",body:'Yamanaka S, Matsu-ura H, Ishikawa M. New deintercalation reaction of calcium from calcium disilicide synthesis of layered polysilane, Mater. Res. Bull., 1996:31:307-316. DOI: https://doi.org/10.1016/0025-5408(95)00195-6'},{id:"B19",body:'Dahn JR, Way BM, Fuller E. Structure of siloxene and layered polysilane (Si6H6), Phys. Rev. B 1993:48(24):17872-17877. DOI: http://dx.doi.org/10.1103/PhysRevB.48.17872'},{id:"B20",body:'Rosli NF, Rohaizad N, Sturala J, Fisher AC, Webster RD, Pumera M. Siloxene, Germanane, and Methylgermanane: Functionalized 2D Materials of Group 14 for Electrochemical Applications, Adv. Funct. Mater. 2020:30:1910186. DOI: https://doi.org/10.1002/adfm.201910186.'},{id:"B21",body:'Ramachandran R, Lan Y, Xu Z-X, Wang F. Construction of NiCo-Layered Double Hydroxide Microspheres from Ni-MOFs for High-Performance Asymmetric Supercapacitors, ACS Appl. Energy Mater. 2020:3:6633-6643. DOI: https://dx.doi.org/10.1021/acsaem.0c00790'},{id:"B22",body:'Ramachandran R, Saranya M, Velmurugan V, Raghupathy BPC, Jeong SK, Grace AN. Effect of reducing agent on graphene synthesis and its influence on charge storage towards supercapacitor applications, Appl. Energy 2015:153:22-31. DOI: http://dx.doi.org/10.1016/j.apenergy.2015.02.091'},{id:"B23",body:'Pazhamalai P, Krishnamoorthy, Sahoo S, Mariappan VK, Kim S-J. Understanding the Thermal Treatment Effect of Two-Dimensional Siloxene Sheets and the Origin of Superior Electrochemical Energy Storage Performances, ACS Appl. Mater. Interfaces 2019:11:624-633. DOI: 10.1021/acsami.8b15323'},{id:"B24",body:'Krishnamoorthy K, Sudhakaran MSP, Pazhamalai P, Mariappan VK, Mok YS, Kim S-J. A highly efficient 2D siloxene coated Ni foam catalyst for methane dry reforming and an effective approach to recycle the spent catalyst for energy storage applications, J. Mater. Chem. A 2019:7:18950-18958. DOI: https://doi.org/10.1039/C9TA03584B'},{id:"B25",body:'Ramachandran R, Saranya M, Grace AN, Wang F. MnS nanocomposites based on doped graphene: simple synthesis by a wet chemical route and improved electrochemical properties as an electrode material for supercapacitors, RSC Adv. 2017:7:2249-2257. DOI: 10.1039/c6ra25457h'},{id:"B26",body:'Meng Q , Du C, Xu Z, Nie J, Hong M, Zhang X, Chen J. Siloxene-reduced graphene oxide composite hydrogel for supercapacitors, Chem. Engg. J. 2020:393:124684. DOI: https://doi.org/10.1016/j.cej.2020.124684'},{id:"B27",body:'An Y, Tian Y, Wei C, Jiang H, Xi B, Xiaong S, Feng J, Qian Y. Scalable and Physical Synthesis of 2D Silicon from Bulk Layered Alloy for Lithium-Ion Batteries and Lithium Metal Batteries, ACS Nano. 2019:13:13690-13701. DOI: 10.1021/acsnano.9b06653'},{id:"B28",body:'Zhang X, Li L, Fan E, Xue Q , Bian Y, Wu F, Chen R. Toward sustainable and systematic recycling of spent rechargeable batteries, Chem. Soc. Rev. 2018:47:7239-7302. DOI: https://doi.org/10.1039/C8CS00297E'},{id:"B29",body:'Kumar KT, Reddy MJK, Sundari GS, Raghu S, Kalaivani RA, Ryu SH, Shanmugharaj AM. Synthesis of graphene-siloxene nanosheet based layered composite materials by tuning its interface chemistry: An efficient anode with overwhelming electrochemical performances for lithium-ion batteries, J. Power Sources 2020:450:227618. DOI: https://doi.org/10.1016/j.jpowsour.2019.227618'},{id:"B30",body:'Xu K, Ben L, Li H, Huang X. Silicon-based nanosheets synthesized by a topochemicalreaction for use as anodes for lithium ion batteries, Nano Res. 2015:8:2654-2662. DOI: 10.1007/s12274-015-0772-4'},{id:"B31",body:'Fu R, Zhang K, Zaccaria RP, Huang H, Xia Y, Liu Z. Two-dimensional silicon suboxides nanostructures with Si nanodomains confined in amorphous SiO2 derived from siloxene as high performance anode for Li-ion batteries, Nano Energy 2017:39:546-553. DOI: http://dx.doi.org/10.1016/j.nanoen.2017.07.040'},{id:"B32",body:'Fu R, Li Y, Wu Y, Shen C, Fan C. Controlling siloxene oxidization to tailor SiOx anodes for high performance lithium ion batteries, J. Power Sources 2019:432:65-72. DOI: https://doi.org/10.1016/j.jpowsour.2019.05.071'},{id:"B33",body:'Hu Y, Li X, Geng D, Cai M, Li R, Sun X. Influence of paper thickness on the electrochemical performances of graphene papers as an anode for lithium ion batteries, Electrochim. Acta 2013:91:227-233. DOI: https://doi.org/10.1016/j.electacta.2012.12.106'}],footnotes:[],contributors:[{corresp:null,contributorFullName:"Rajendran Ramachandran",address:null,affiliation:'
SUSTech Academy for Advanced Interdisciplinary Studies, Southern University of Science and Technology, China
School of Microelectronics, Southern University of Science and Technology, China
Department of Chemistry, Southern University of Science and Technology, China
School of Microelectronics, Southern University of Science and Technology, China
Engineering Research Center of Integrated Circuits for Next-Generation Communications, Ministry of Education, China
'}],corrections:null},book:{id:"10414",title:"Novel Nanomaterials",subtitle:null,fullTitle:"Novel Nanomaterials",slug:null,publishedDate:null,bookSignature:"Dr. Karthikeyan Krishnamoorthy",coverURL:"https://cdn.intechopen.com/books/images_new/10414.jpg",licenceType:"CC BY 3.0",editedByType:null,editors:[{id:"278690",title:"Dr.",name:"Karthikeyan",middleName:null,surname:"Krishnamoorthy",slug:"karthikeyan-krishnamoorthy",fullName:"Karthikeyan Krishnamoorthy"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}}},profile:{item:{id:"143055",title:"Dr.",name:"Kohsuke",middleName:null,surname:"Yanai",email:"kyanai@hitachi.co.in",fullName:"Kohsuke Yanai",slug:"kohsuke-yanai",position:null,biography:null,institutionString:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",totalCites:0,totalChapterViews:"0",outsideEditionCount:0,totalAuthoredChapters:"1",totalEditedBooks:"0",personalWebsiteURL:null,twitterURL:null,linkedinURL:null,institution:null},booksEdited:[],chaptersAuthored:[{title:"Analysis and Learning Frameworks for Large-Scale Data Mining",slug:"analysis-and-learning-frameworks-for-large-scale-data-mining",abstract:null,signatures:"Kohsuke Yanai and Toshihiko Yanase",authors:[{id:"143055",title:"Dr.",name:"Kohsuke",surname:"Yanai",fullName:"Kohsuke Yanai",slug:"kohsuke-yanai",email:"kyanai@hitachi.co.in"},{id:"157433",title:"Dr.",name:"Toshihiko",surname:"Yanase",fullName:"Toshihiko Yanase",slug:"toshihiko-yanase",email:"toshihiko.yanase.gm@hitachi.com"}],book:{title:"Advances in Data Mining Knowledge Discovery and Applications",slug:"advances-in-data-mining-knowledge-discovery-and-applications",productType:{id:"1",title:"Edited Volume"}}}],collaborators:[{id:"11865",title:"Prof.",name:"Mofizur",surname:"Rahman",slug:"mofizur-rahman",fullName:"Mofizur Rahman",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"104698",title:"Mr.",name:"Roberto",surname:"Oliveira",slug:"roberto-oliveira",fullName:"Roberto Oliveira",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"Federal University of Para",institutionURL:null,country:{name:"Brazil"}}},{id:"107224",title:"Dr.",name:"Dost",surname:"Khan",slug:"dost-khan",fullName:"Dost Khan",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/107224/images/1095_n.jpg",biography:"Receive PhD from School of Innovative Technologies and Engineering (SITE), University of Technology, Mauritius (UTM). M.Sc. (Computer Science) from BZU, Multan, Pakistan. Assistant Professor and Head Department of Computer Science & IT at The Islamia University of Bahawalpur, Pakistan.",institutionString:null,institution:{name:"Islamia University of Bahawalpur",institutionURL:null,country:{name:"Pakistan"}}},{id:"119486",title:"Dr.",name:"Nawaz",surname:"Mohamudally",slug:"nawaz-mohamudally",fullName:"Nawaz Mohamudally",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/119486/images/system/119486.jpeg",biography:"Dr. Nawaz Mohamudally graduated in telecommunications from the University of Science and Technology of Lille I in France. He is presently an Associate Professor at the University of Technology, Mauritius, where he has occupied the posts of Head of School of Business Informatics and Software Engineering and recently the Chairman of the Research Degrees Committee. He was formerly the Chairman of the Internet Management Committee at the national level and a member of the Mauritius Academy of Science and Technology. He is an academic researcher and practitioner in the fields of pervasive computing and data science. His latest ongoing research and development work with the industry is on customers behaviors insights. He is the recipient of the Outstanding Contribution in Education award from Stars of The Industry-Indo-African Forum and Best Professor in Industrial Systems Engineering from Africa Leadership Awards.",institutionString:"University of Technology",institution:{name:"University of Technology, Mauritius",institutionURL:null,country:{name:"Mauritius"}}},{id:"130685",title:"Prof.",name:"Dilek",surname:"Karahoca",slug:"dilek-karahoca",fullName:"Dilek Karahoca",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"Bahçeşehir University",institutionURL:null,country:{name:"Turkey"}}},{id:"139542",title:"Prof.",name:"Adem",surname:"Karahoca",slug:"adem-karahoca",fullName:"Adem Karahoca",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/139542/images/system/139542.jpg",biography:"Dr. Adem Karahoca received his B.Sc. degree in Mathematical Engineering from Istanbul Technical University, M.Sc. and Ph.D. degrees in Software Engineering from Istanbul University. His research interests and expertise include mobile telecommunication software, data mining, management information systems, bioinformatics, information systems, business intelligence, computers in education, and human computer interaction. He has written 26 IT related books and book chapters. He has supervised different variety of IT research and application projects. He is currently working on data mining applications in medicine.",institutionString:null,institution:{name:"Bahçeşehir University",institutionURL:null,country:{name:"Turkey"}}},{id:"140708",title:"Dr.",name:"Jie",surname:"Gao",slug:"jie-gao",fullName:"Jie Gao",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"141999",title:"Mr.",name:"Dewan",surname:"Farid",slug:"dewan-farid",fullName:"Dewan Farid",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"United International University",institutionURL:null,country:{name:"Bangladesh"}}},{id:"155452",title:"Prof.",name:"Mohammad",surname:"Zahidur Rahman",slug:"mohammad-zahidur-rahman",fullName:"Mohammad Zahidur Rahman",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"155701",title:"M.Sc.",name:"Erdem",surname:"Alparslan",slug:"erdem-alparslan",fullName:"Erdem Alparslan",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/155701/images/3240_n.jpg",biography:null,institutionString:null,institution:null}]},generic:{page:{slug:"our-story",title:"Our story",intro:"
The company was founded in Vienna in 2004 by Alex Lazinica and Vedran Kordic, two PhD students researching robotics. While completing our PhDs, we found it difficult to access the research we needed. So, we decided to create a new Open Access publisher. A better one, where researchers like us could find the information they needed easily. The result is IntechOpen, an Open Access publisher that puts the academic needs of the researchers before the business interests of publishers.
",metaTitle:"Our story",metaDescription:"The company was founded in Vienna in 2004 by Alex Lazinica and Vedran Kordic, two PhD students researching robotics. While completing our PhDs, we found it difficult to access the research we needed. So, we decided to create a new Open Access publisher. A better one, where researchers like us could find the information they needed easily. The result is IntechOpen, an Open Access publisher that puts the academic needs of the researchers before the business interests of publishers.",metaKeywords:null,canonicalURL:"/page/our-story",contentRaw:'[{"type":"htmlEditorComponent","content":"
We started by publishing journals and books from the fields of science we were most familiar with - AI, robotics, manufacturing and operations research. Through our growing network of institutions and authors, we soon expanded into related fields like environmental engineering, nanotechnology, computer science, renewable energy and electrical engineering, Today, we are the world’s largest Open Access publisher of scientific research, with over 4,200 books and 54,000 scientific works including peer-reviewed content from more than 116,000 scientists spanning 161 countries. Our authors range from globally-renowned Nobel Prize winners to up-and-coming researchers at the cutting edge of scientific discovery.
\\n\\n
In the same year that IntechOpen was founded, we launched what was at the time the first ever Open Access, peer-reviewed journal in its field: the International Journal of Advanced Robotic Systems (IJARS).
\\n\\n
The IntechOpen timeline
\\n\\n
2004
\\n\\n
\\n\\t
Intech Open is founded in Vienna, Austria, by Alex Lazinica and Vedran Kordic, two PhD students, and their first Open Access journals and books are published.
\\n\\t
Alex and Vedran launch the first Open Access, peer-reviewed robotics journal and IntechOpen’s flagship publication, the International Journal of Advanced Robotic Systems (IJARS).
\\n
\\n\\n
2005
\\n\\n
\\n\\t
IntechOpen publishes its first Open Access book: Cutting Edge Robotics.
\\n
\\n\\n
2006
\\n\\n
\\n\\t
IntechOpen publishes a special issue of IJARS, featuring contributions from NASA scientists regarding the Mars Exploration Rover missions.
\\n
\\n\\n
2008
\\n\\n
\\n\\t
Downloads milestone: 200,000 downloads reached
\\n
\\n\\n
2009
\\n\\n
\\n\\t
Publishing milestone: the first 100 Open Access STM books are published
\\n
\\n\\n
2010
\\n\\n
\\n\\t
Downloads milestone: one million downloads reached
\\n\\t
IntechOpen expands its book publishing into a new field: medicine.
\\n
\\n\\n
2011
\\n\\n
\\n\\t
Publishing milestone: More than five million downloads reached
\\n\\t
IntechOpen publishes 1996 Nobel Prize in Chemistry winner Harold W. Kroto’s “Strategies to Successfully Cross-Link Carbon Nanotubes”. Find it here.
\\n\\t
IntechOpen and TBI collaborate on a project to explore the changing needs of researchers and the evolving ways that they discover, publish and exchange information. The result is the survey “Author Attitudes Towards Open Access Publishing: A Market Research Program”.
\\n\\t
IntechOpen hosts SHOW - Share Open Access Worldwide; a series of lectures, debates, round-tables and events to bring people together in discussion of open source principles, intellectual property, content licensing innovations, remixed and shared culture and free knowledge.
\\n
\\n\\n
2012
\\n\\n
\\n\\t
Publishing milestone: 10 million downloads reached
\\n\\t
IntechOpen holds Interact2012, a free series of workshops held by figureheads of the scientific community including Professor Hiroshi Ishiguro, director of the Intelligent Robotics Laboratory, who took the audience through some of the most impressive human-robot interactions observed in his lab.
\\n
\\n\\n
2013
\\n\\n
\\n\\t
IntechOpen joins the Committee on Publication Ethics (COPE) as part of a commitment to guaranteeing the highest standards of publishing.
\\n
\\n\\n
2014
\\n\\n
\\n\\t
IntechOpen turns 10, with more than 30 million downloads to date.
\\n\\t
IntechOpen appoints its first Regional Representatives - members of the team situated around the world dedicated to increasing the visibility of our authors’ published work within their local scientific communities.
\\n
\\n\\n
2015
\\n\\n
\\n\\t
Downloads milestone: More than 70 million downloads reached, more than doubling since the previous year.
\\n\\t
Publishing milestone: IntechOpen publishes its 2,500th book and 40,000th Open Access chapter, reaching 20,000 citations in Thomson Reuters ISI Web of Science.
\\n\\t
40 IntechOpen authors are included in the top one per cent of the world’s most-cited researchers.
\\n\\t
Thomson Reuters’ ISI Web of Science Book Citation Index begins indexing IntechOpen’s books in its database.
\\n
\\n\\n
2016
\\n\\n
\\n\\t
IntechOpen is identified as a world leader in Simba Information’s Open Access Book Publishing 2016-2020 report and forecast. IntechOpen came in as the world’s largest Open Access book publisher by title count.
\\n
\\n\\n
2017
\\n\\n
\\n\\t
Downloads milestone: IntechOpen reaches more than 100 million downloads
\\n\\t
Publishing milestone: IntechOpen publishes its 3,000th Open Access book, making it the largest Open Access book collection in the world
We started by publishing journals and books from the fields of science we were most familiar with - AI, robotics, manufacturing and operations research. Through our growing network of institutions and authors, we soon expanded into related fields like environmental engineering, nanotechnology, computer science, renewable energy and electrical engineering, Today, we are the world’s largest Open Access publisher of scientific research, with over 4,200 books and 54,000 scientific works including peer-reviewed content from more than 116,000 scientists spanning 161 countries. Our authors range from globally-renowned Nobel Prize winners to up-and-coming researchers at the cutting edge of scientific discovery.
\n\n
In the same year that IntechOpen was founded, we launched what was at the time the first ever Open Access, peer-reviewed journal in its field: the International Journal of Advanced Robotic Systems (IJARS).
\n\n
The IntechOpen timeline
\n\n
2004
\n\n
\n\t
Intech Open is founded in Vienna, Austria, by Alex Lazinica and Vedran Kordic, two PhD students, and their first Open Access journals and books are published.
\n\t
Alex and Vedran launch the first Open Access, peer-reviewed robotics journal and IntechOpen’s flagship publication, the International Journal of Advanced Robotic Systems (IJARS).
\n
\n\n
2005
\n\n
\n\t
IntechOpen publishes its first Open Access book: Cutting Edge Robotics.
\n
\n\n
2006
\n\n
\n\t
IntechOpen publishes a special issue of IJARS, featuring contributions from NASA scientists regarding the Mars Exploration Rover missions.
\n
\n\n
2008
\n\n
\n\t
Downloads milestone: 200,000 downloads reached
\n
\n\n
2009
\n\n
\n\t
Publishing milestone: the first 100 Open Access STM books are published
\n
\n\n
2010
\n\n
\n\t
Downloads milestone: one million downloads reached
\n\t
IntechOpen expands its book publishing into a new field: medicine.
\n
\n\n
2011
\n\n
\n\t
Publishing milestone: More than five million downloads reached
\n\t
IntechOpen publishes 1996 Nobel Prize in Chemistry winner Harold W. Kroto’s “Strategies to Successfully Cross-Link Carbon Nanotubes”. Find it here.
\n\t
IntechOpen and TBI collaborate on a project to explore the changing needs of researchers and the evolving ways that they discover, publish and exchange information. The result is the survey “Author Attitudes Towards Open Access Publishing: A Market Research Program”.
\n\t
IntechOpen hosts SHOW - Share Open Access Worldwide; a series of lectures, debates, round-tables and events to bring people together in discussion of open source principles, intellectual property, content licensing innovations, remixed and shared culture and free knowledge.
\n
\n\n
2012
\n\n
\n\t
Publishing milestone: 10 million downloads reached
\n\t
IntechOpen holds Interact2012, a free series of workshops held by figureheads of the scientific community including Professor Hiroshi Ishiguro, director of the Intelligent Robotics Laboratory, who took the audience through some of the most impressive human-robot interactions observed in his lab.
\n
\n\n
2013
\n\n
\n\t
IntechOpen joins the Committee on Publication Ethics (COPE) as part of a commitment to guaranteeing the highest standards of publishing.
\n
\n\n
2014
\n\n
\n\t
IntechOpen turns 10, with more than 30 million downloads to date.
\n\t
IntechOpen appoints its first Regional Representatives - members of the team situated around the world dedicated to increasing the visibility of our authors’ published work within their local scientific communities.
\n
\n\n
2015
\n\n
\n\t
Downloads milestone: More than 70 million downloads reached, more than doubling since the previous year.
\n\t
Publishing milestone: IntechOpen publishes its 2,500th book and 40,000th Open Access chapter, reaching 20,000 citations in Thomson Reuters ISI Web of Science.
\n\t
40 IntechOpen authors are included in the top one per cent of the world’s most-cited researchers.
\n\t
Thomson Reuters’ ISI Web of Science Book Citation Index begins indexing IntechOpen’s books in its database.
\n
\n\n
2016
\n\n
\n\t
IntechOpen is identified as a world leader in Simba Information’s Open Access Book Publishing 2016-2020 report and forecast. IntechOpen came in as the world’s largest Open Access book publisher by title count.
\n
\n\n
2017
\n\n
\n\t
Downloads milestone: IntechOpen reaches more than 100 million downloads
\n\t
Publishing milestone: IntechOpen publishes its 3,000th Open Access book, making it the largest Open Access book collection in the world
\n
\n"}]},successStories:{items:[]},authorsAndEditors:{filterParams:{sort:"featured,name"},profiles:[{id:"6700",title:"Dr.",name:"Abbass A.",middleName:null,surname:"Hashim",slug:"abbass-a.-hashim",fullName:"Abbass A. Hashim",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/6700/images/1864_n.jpg",biography:"Currently I am carrying out research in several areas of interest, mainly covering work on chemical and bio-sensors, semiconductor thin film device fabrication and characterisation.\nAt the moment I have very strong interest in radiation environmental pollution and bacteriology treatment. The teams of researchers are working very hard to bring novel results in this field. I am also a member of the team in charge for the supervision of Ph.D. students in the fields of development of silicon based planar waveguide sensor devices, study of inelastic electron tunnelling in planar tunnelling nanostructures for sensing applications and development of organotellurium(IV) compounds for semiconductor applications. I am a specialist in data analysis techniques and nanosurface structure. I have served as the editor for many books, been a member of the editorial board in science journals, have published many papers and hold many patents.",institutionString:null,institution:{name:"Sheffield Hallam University",country:{name:"United Kingdom"}}},{id:"54525",title:"Prof.",name:"Abdul Latif",middleName:null,surname:"Ahmad",slug:"abdul-latif-ahmad",fullName:"Abdul Latif Ahmad",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"20567",title:"Prof.",name:"Ado",middleName:null,surname:"Jorio",slug:"ado-jorio",fullName:"Ado Jorio",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"Universidade Federal de Minas Gerais",country:{name:"Brazil"}}},{id:"47940",title:"Dr.",name:"Alberto",middleName:null,surname:"Mantovani",slug:"alberto-mantovani",fullName:"Alberto Mantovani",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"12392",title:"Mr.",name:"Alex",middleName:null,surname:"Lazinica",slug:"alex-lazinica",fullName:"Alex Lazinica",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/12392/images/7282_n.png",biography:"Alex Lazinica is the founder and CEO of IntechOpen. After obtaining a Master's degree in Mechanical Engineering, he continued his PhD studies in Robotics at the Vienna University of Technology. Here he worked as a robotic researcher with the university's Intelligent Manufacturing Systems Group as well as a guest researcher at various European universities, including the Swiss Federal Institute of Technology Lausanne (EPFL). During this time he published more than 20 scientific papers, gave presentations, served as a reviewer for major robotic journals and conferences and most importantly he co-founded and built the International Journal of Advanced Robotic Systems- world's first Open Access journal in the field of robotics. Starting this journal was a pivotal point in his career, since it was a pathway to founding IntechOpen - Open Access publisher focused on addressing academic researchers needs. Alex is a personification of IntechOpen key values being trusted, open and entrepreneurial. 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