A list of representative polymers and their abbreviations.
\\n\\n
Released this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
\\n\\nWe wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'IntechOpen is proud to announce that 179 of our authors have made the Clarivate™ Highly Cited Researchers List for 2020, ranking them among the top 1% most-cited.
\n\nThroughout the years, the list has named a total of 252 IntechOpen authors as Highly Cited. Of those researchers, 69 have been featured on the list multiple times.
\n\n\n\nReleased this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
\n\nWe wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
\n'}],latestNews:[{slug:"stanford-university-identifies-top-2-scientists-over-1-000-are-intechopen-authors-and-editors-20210122",title:"Stanford University Identifies Top 2% Scientists, Over 1,000 are IntechOpen Authors and Editors"},{slug:"intechopen-authors-included-in-the-highly-cited-researchers-list-for-2020-20210121",title:"IntechOpen Authors Included in the Highly Cited Researchers List for 2020"},{slug:"intechopen-maintains-position-as-the-world-s-largest-oa-book-publisher-20201218",title:"IntechOpen Maintains Position as the World’s Largest OA Book Publisher"},{slug:"all-intechopen-books-available-on-perlego-20201215",title:"All IntechOpen Books Available on Perlego"},{slug:"oiv-awards-recognizes-intechopen-s-editors-20201127",title:"OIV Awards Recognizes IntechOpen's Editors"},{slug:"intechopen-joins-crossref-s-initiative-for-open-abstracts-i4oa-to-boost-the-discovery-of-research-20201005",title:"IntechOpen joins Crossref's Initiative for Open Abstracts (I4OA) to Boost the Discovery of Research"},{slug:"intechopen-hits-milestone-5-000-open-access-books-published-20200908",title:"IntechOpen hits milestone: 5,000 Open Access books published!"},{slug:"intechopen-books-hosted-on-the-mathworks-book-program-20200819",title:"IntechOpen Books Hosted on the MathWorks Book Program"}]},book:{item:{type:"book",id:"9201",leadTitle:null,fullTitle:"Advanced Supercritical Fluids Technologies",title:"Advanced Supercritical Fluids Technologies",subtitle:null,reviewType:"peer-reviewed",abstract:"Using SuperCritical Fluids (SCFs) in various processes is not new, because Mother Nature has been processing minerals in aqueous solutions at critical and supercritical pressures for billions of years. Somewhere in the 20th century, SCFs started to be used in various industries as working fluids, coolants, chemical agents, etc. Written by an international team of experts and complete with the latest research, development, and design, Advanced Supercritical Fluids Technologies is a unique technical book, completely dedicated to modern and advanced applications of supercritical fluids in various industries.Advanced Supercritical Fluids Technologies provides engineers and specialists in various industries dealing with SCFs as well as researchers, scientists, and students of the corresponding departments with a comprehensive overview of the current status, latest trends and developments of these technologies.Dr Igor Pioro is a professor at the University of Ontario Institute of Technology, Canada, and the Founding Editor of the ASME Journal of Nuclear Engineering and Radiation Science.",isbn:"978-1-83880-709-2",printIsbn:"978-1-83880-708-5",pdfIsbn:"978-1-83880-710-8",doi:"10.5772/intechopen.83197",price:119,priceEur:129,priceUsd:155,slug:"advanced-supercritical-fluids-technologies",numberOfPages:222,isOpenForSubmission:!1,isInWos:null,hash:"6d02d813b504c90761f9d0abca79106f",bookSignature:"Igor Pioro",publishedDate:"May 20th 2020",coverURL:"https://cdn.intechopen.com/books/images_new/9201.jpg",numberOfDownloads:3110,numberOfWosCitations:0,numberOfCrossrefCitations:3,numberOfDimensionsCitations:6,hasAltmetrics:0,numberOfTotalCitations:9,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"May 13th 2019",dateEndSecondStepPublish:"September 18th 2019",dateEndThirdStepPublish:"November 17th 2019",dateEndFourthStepPublish:"February 5th 2020",dateEndFifthStepPublish:"April 5th 2020",currentStepOfPublishingProcess:5,indexedIn:"1,2,3,4,5,6,7",editedByType:"Edited by",kuFlag:!1,editors:[{id:"15933",title:"Prof.",name:"Igor",middleName:"Leonardovich",surname:"Pioro",slug:"igor-pioro",fullName:"Igor Pioro",profilePictureURL:"https://mts.intechopen.com/storage/users/15933/images/system/15933.png",biography:"Professor Igor Pioro – Ph.D. (1983); Doctor of Technical Sciences (1992); Professional Engineer (Ontario, Canada) (2008); Fellow of ASME (2012), Canadian SME (2015), and Engineering\nInstitute of Canada (EIC) (2013); member of ANS (2004), and\nCanadian NS (2010); is an internationally recognized scientist\nwithin the areas of nuclear engineering and thermal sciences/\nengineering (https://nuclear.ontariotechu.ca/people/faculty/\ndr-igor-pioro.php). He is an author/co-author of about 500 publications. Dr Pioro\nis a Founding Editor of the ASME Journal of Nuclear Engineering and Radiation\nScience. He was a Chair of the Executive Committee of the Nuclear Engineering\nDivision of the ASME (2011-2012) and a Chair of the International Conference on\nNuclear Engineering (ICONE-20) (2011-2012). 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Rapid eye movements, dreams, skeletal muscle atonia, and autonomous-sympathetic nervous system questions the brain and its importance, and what it really means again and again with EEG signals. Therefore repeating REM waves in the brain, REM physiology and pathophysiology should be studied more in depth. We can regard narcolepsy as a type of REM physiology abnormality due to two important conditions: sleep paralysis, and dreaming phenomenon. A narcoleptic patient experiences both conditions while asleep or waking up from sleep during REM. Narcolepsy can be conceptualized as blurring of the borders of the brain while awake, sleeping or dreaming. An awake narcoleptic can feel as if sleepy and can even see dreams. In the classical sense, narcolepsy is characterized by hypersomnolence during the day associated with REM sleep phenomenon and cataplexy encompassing sleep paralysis and hypnogogic hallucinations. The fundamental pathophysiology of narcolepsy is related to a deficiency of hypocretine (orexine) which is an important component of the hypothalamic neuropeptide system.
\r\n\tHistorically the word narcolepsy was first used by Ge´lineau in 1880 to describe irresistible episodes of sleep that were repetitive with short intervals. In 1950s Kleitman was the first individual to discover REM. Since then, laboratories that can record electrophysiological signals have been developed and possibilities for diagnosing, treating and monitoring sleep disorders have increased. However, narcolepsy can still be mixed with sleep disorders and neuropsychiatric disorders.
\r\n\tThis book aims at tackling narcolepsy from both basic science and clinical science perspectives. The reader will be able to grasp physiological mechanisms on one hand while associating narcolepsy with clinical diseases on the other. In narcolepsy there are disrupted night-day and sleep-wakefulness rhythms. Once this rhythm is hindered, the individual is confronted with biological, psychological and social problems. Narcoleptics are faced with the risk of collapsing and being knocked down to the floor while in kitchen or at the park, when driving in the traffic or walking down the stairs at any given moment.
\r\n\tThis book will not only provide a resource for physicians who will be helping this group of patients, but will at the same time contribute to the pathophysiology of the disease as it contains up to date information for researchers focusing on innovations in this field.
",isbn:null,printIsbn:"979-953-307-X-X",pdfIsbn:null,doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"5b19c98934802d13418f734de27786cd",bookSignature:"Associate Prof. Murat Kayabekir",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/9780.jpg",keywords:"HLA types, Hypocretin System, Orexin Deficiency, REM Sleep, Familial Aspects, HLA-peptide, HLA DQB1*0602, Twin Studies, Sleepiness, Cataplexy, Sleep Paralysis, Hallucinations, Epworth Sleepiness Scale, SOREMPs, MSLT, CSF Hypocretin (Orexin), Behavioral Approaches, Pharmacologic, Children, Medication Side Effects",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"November 13th 2019",dateEndSecondStepPublish:"March 24th 2020",dateEndThirdStepPublish:"May 23rd 2020",dateEndFourthStepPublish:"August 11th 2020",dateEndFifthStepPublish:"October 10th 2020",remainingDaysToSecondStep:"a year",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:null,coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"265598",title:"Associate Prof.",name:"Murat",middleName:null,surname:"Kayabekir",slug:"murat-kayabekir",fullName:"Murat Kayabekir",profilePictureURL:"https://mts.intechopen.com/storage/users/265598/images/system/265598.jpg",biography:"Murat Kayabekir is an Associate Professor in the Department of Physiology at Atatürk University Medical School. He has completed Physiology training at Hacettepe University Medical School. He worked as a physiology specialist at the Sleep Disorders Centers and Electrophysiology Laboratory as a founder and director. His scientific fields of study are: neurophysiology, electrophysiology, sleep physiology and disorders, PSG and computer engineering, snoring sound analysis, sleep EEG and sleep spindles, innovative products, REM behavior disorders, narcolepsy, sleep apnea, bruxism, insomnia, and epilepsy during sleep.",institutionString:"Atatürk University",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"1",totalChapterViews:"0",totalEditedBooks:"0",institution:{name:"Atatürk University",institutionURL:null,country:{name:"Turkey"}}}],coeditorOne:null,coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"16",title:"Medicine",slug:"medicine"}],chapters:null,productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"252211",firstName:"Sara",lastName:"Debeuc",middleName:null,title:"Ms.",imageUrl:"https://mts.intechopen.com/storage/users/252211/images/7239_n.png",email:"sara.d@intechopen.com",biography:"As an Author Service Manager my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review, to approval and revision, copyediting and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. Whether that be identifying an exceptional author and proposing an editorship collaboration, or contacting researchers who would like the opportunity to work with IntechOpen, I establish and help manage author and editor acquisition and contact."}},relatedBooks:[{type:"book",id:"6550",title:"Cohort Studies in Health Sciences",subtitle:null,isOpenForSubmission:!1,hash:"01df5aba4fff1a84b37a2fdafa809660",slug:"cohort-studies-in-health-sciences",bookSignature:"R. Mauricio Barría",coverURL:"https://cdn.intechopen.com/books/images_new/6550.jpg",editedByType:"Edited by",editors:[{id:"88861",title:"Dr.",name:"R. Mauricio",surname:"Barría",slug:"r.-mauricio-barria",fullName:"R. 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Venkateswarlu",coverURL:"https://cdn.intechopen.com/books/images_new/371.jpg",editedByType:"Edited by",editors:[{id:"58592",title:"Dr.",name:"Arun",surname:"Shanker",slug:"arun-shanker",fullName:"Arun Shanker"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"878",title:"Phytochemicals",subtitle:"A Global Perspective of Their Role in Nutrition and Health",isOpenForSubmission:!1,hash:"ec77671f63975ef2d16192897deb6835",slug:"phytochemicals-a-global-perspective-of-their-role-in-nutrition-and-health",bookSignature:"Venketeshwer Rao",coverURL:"https://cdn.intechopen.com/books/images_new/878.jpg",editedByType:"Edited by",editors:[{id:"82663",title:"Dr.",name:"Venketeshwer",surname:"Rao",slug:"venketeshwer-rao",fullName:"Venketeshwer Rao"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"4816",title:"Face Recognition",subtitle:null,isOpenForSubmission:!1,hash:"146063b5359146b7718ea86bad47c8eb",slug:"face_recognition",bookSignature:"Kresimir Delac and Mislav Grgic",coverURL:"https://cdn.intechopen.com/books/images_new/4816.jpg",editedByType:"Edited by",editors:[{id:"528",title:"Dr.",name:"Kresimir",surname:"Delac",slug:"kresimir-delac",fullName:"Kresimir Delac"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"51033",title:"Conductive Polymer-Based Membranes",doi:"10.5772/63560",slug:"conductive-polymer-based-membranes",body:'\nPolymers represent a larger class of organic compounds, in terms of both diversity and industrial-scale applications. They are used in the majority of industrial branches and have contributed decisively to the last century economic development. Polymers’ impact upon the human society progress showed a positive effect, but nowadays, more attention is given to the mitigation of negative environmental impact induced by their intensive use. As a consequence of exponential growth of researches in the polymers field, the macromolecular compounds’ chemistry became a distinct science within organic chemistry, a well-defined domain, in connection with other natural sciences areas. The turning point in the development of macromolecular compounds chemistry as an exact science was the transition from semi-empiric researches to rigorous experiments marked in 1925–1930 period by Staudinger and Carothers researches [1–4] that led to highlighting of polymer structures, defining the notions of macromolecule, macromolecular chain, homologous polymeric series, etc.
\nPolymers led to rapid development of plastic materials science due to their specific properties: chemical stability on acids, bases and solvents (higher than gold and platinum in some cases), high thermal stability, elasticity, plasticity, excellent mechanical strength, non-permeability to gases, low density, electrical insulation properties and also electroconductive properties. The latest characteristics referring to electroconductivity was thoroughly studied during the last 60 years, leading to the development of a new polymer chemistry subdomain, and dedicated to conductive polymers. The results, reported within research works focussed on conductive polymers, materialized in two Nobel prizes in chemistry [5]:
\nRudolph A. Marcus (1992) for his works on electron transfer theory in redox processes, with direct applications in biopolymers science and
Alan J. Heeger, Alan G. Mac Diarmid and Hideki Shirakawa (2000) for development of intrinsic electroconductive polymers through researches related to polyacetylene.
At the same time, with macromolecular compound chemistry, a new domain related to the preparation and use of membrane-type advanced materials was developed. Membrane science developed continuously as an interdisciplinary science in which polymers have a central role. With the progress of research works dedicated to conductive polymers, researches on conductive polymers membranes preparation and their application were also initiated and developed.
\nClassification of conductive polymers can be done based on various criteria. The most important criterion is related to the electric charge movement type which depends on the polymer chemical structure. Thus, two groups of electronic conductive polymers are formed:
\nRedox polymers: polymers that possess redox potential within their structure groups (reduction/oxidation capacity);
Intrinsic electroconductive polymers: polymers with conjugated п-п or p-п systems.
In the case of redox polymers, the movement of electrons is realized through reversible chemical reactions “donor-acceptor” type, in accordance with Eq. (1):\n
where “n” is the number of transferred electrons.
\nThe standard potential (E0) is determined by Eq. (2):\n
where F is the Faraday constant and ΔG0 is the standard Gibbs free energy, calculated in accordance with Eq. (3):\n
In the case of redox polymers, the essential condition needed for continuous electron transport, which defines the “electronic conductive polymer” property, is that groups with redox potential have to be distributed one next to the other within the macromolecular structure (its spatial configuration) in such a way that electron jump between groups is possible (Figure 1).
\nElectric charges movement within redox polymers.
Such polymers are those based on substituted nitro-styrene, quinones, dopamines and polymers which have within structure coordinative ligands based on Ir, Co, Re, Ru or Os [6].
\nThe electrons transport principle of intrinsic electroconductive polymers consists of electrons transfer from п type bonds to nearby simple σ bonds, due to repulsion effect of same type charges.
\nThe mandatory condition is that double bonds alternate with the simple ones (conjugated п-п systems), as shown in Figure 2.
\nElectric charges movement in “π-π” conjugated systems.
The same principle applies to the continuous transport of electrons in the case of polymers which contains heteroatoms N, S or O types within the macromolecular chain. Heteroatoms must be bonded to C atom that is involved in a double bond. Practically, non-participating p electrons of the heteroatom move to σ single bond, and through electrostatic repulsion effect, they further induce the movement of п electrons from the nearby double bond. That type of electrons transport is specific to conjugated p-п systems (Figure 3).
\nIntrinsic conductive polymers have the capacity to conduct electricity better than the majority of plastic materials which do not contain conjugated electron systems. For example, polyacetylene has a conductivity of 10−8–10−7 S m−1 in the form of “cis” isomer and 10−2–10−3 S m−1 in the form of “trans” isomer, compared with Teflon which has a conductivity of 10−16 S m−1. However, compared with the conductivity of metals with best electric properties (Ag and Cu), which is of order 108 S m−1, the conductivity of these polymers is very low, having semiconductor properties. Through doping process, similar with that applied to classic inorganic semiconductors, the conductivity of intrinsic conductive polymers significantly grows, being closer to metals properties. Thus, polyacetylene doping with halogen vapour made (Cl, Br, I) the conductivity grow up to 105 S m−1 [5].
\nElectric charges movement in “p-π” conjugated systems.
Doping process involves the introduction of atoms capable of extracting or providing electrons to polymer’s conjugated system, within its macromolecular chain. Introduction of such defects within the structure of macromolecule results in a more rapid jumping of electrons from created polar centres, assuring a better conductivity for the polymer. Usually, two distinct doping processes are applied [5]: oxidative doping (or p-doping) through which electrons are abstracted from the structure of polymer and reductive doping (or n-doping) through which electrons are introduced within the structure of polymer.
\nThe two mentioned reactions are the processes for polyacetylene in Eqs (4) and (5):\n
Oxidative doping\n
In the first case, iodine is abstracting electrons from double bonds and in the second case, sodium atoms are releasing electrons to the double bonds bond resulting in their polarization. Both electric charges are migrating within the polymeric chain, adding the electric conductivity property, as shown in Eqs (4) and (5).
\nDoped intrinsic conductive polymers are obtained through one of the two main methods: chemical or electrochemical [7, 8]. Through chemical synthesis processes, monomers are polymerized/polycondensated by mixing with specific oxidative reagents such as ferric chloride or ammonium persulphate, at a specific pH. The method presents two main advantages compared with the electrochemical method: can be used to obtain polymeric powders or films that can be further processed and used at industrial level and can be used also in the synthesis of conductive polymers via electrochemical methods. Drawbacks of the methods are related to the fact that is highly sensitive, being dependent on reaction conditions (solvent nature, solvent and reagents purity, reagents’ molar ratios, temperature, mixing mode and speed, reaction time, etc.). Electrochemical synthesis method is based on polymerization/polycondensation of monomers dissolved in a specific solvent through appliance of electricity between two electrodes. The monomer solution also contains the doping agent. Through this method, polymeric films (nanometers order thickness) with controlled/predefined structure are obtained. Electrochemical synthesis can be realized through three techniques: galvanostatic, potentiostatic and potentiodynamic [8]. The method presents the following disadvantages: limited polymer doping, conductive polymer quantity and polymeric film size are limited by electrode geometry and surface, difficulties in appliance for composite materials preparation (compared with the chemical synthesis).
\nNo. | \nChemical name | \nAbbreviation | \n
---|---|---|
1 | \nPolyacetylene | \nPAc | \n
2 | \nPolyaniline | \nPANI | \n
3 | \nPolypyrrole | \nPPy | \n
4 | \nPolythiophene | \nPTh | \n
5 | \nPoly(p-phenylene) | \nPPP | \n
6 | \nPolyazulene | \nPAZ | \n
7 | \nPolyfuran | \nPFu | \n
8 | \nPolyisopren | \nPIP | \n
9 | \nPolybutadiene | \nPBD | \n
10 | \nPoly(isothianaphtene) | \nPITN | \n
11 | \nPoly(α-naphthylamine) | \nPNA | \n
A list of representative polymers and their abbreviations.
At the 2014 year level, more than 25 intrinsic conductive polymers [8] were known and used in various applications: electrochemical sensors [9–11]; gas sensors [12]; biosensors for medicine, food industry and environmental monitoring [13–15]; functionalized biomaterials with application in medicine [8, 16]; corrosion inhibitors [17]; fuel cells [18], etc. One of the main applications of conductive polymers is the development of optoelectronic devices based on electroluminescence phenomenon (field-effect transistors, FET; photodiodes; and light-emitting diodes, LEDs) [19]. The most representative polymers from those classes and their abbreviations are presented in Table 1.
\nFor each basic polymer, a larger number of derivatives with electroconductive properties suitable for various applications were studied, and the research results were reported within the literature.
\nMany of the listed conductive polymers can be used for the preparation of polymeric membranes used in advanced separation processes, which is presented in the next section.
\nMembranes are advanced materials used for separation of compounds of sizes between 0.1 nm and 1 µm (from suspensions, dissolved macromolecules to simple or complex ions) from liquid and gaseous mixtures. It is difficult to find a membrane definition that covers simultaneously the issues related to its structure, separation mechanism and utilization domain. A generally accepted definition presented within the literature is as follows: membrane is a selective barrier which actively or passively participates to the mass transfer between the phases separated by it [20]. The membrane selectivity is determined by the material from which it is made, its structure (form, dimensions and pores distribution) and the force responsible for the separation process.
\nMembranes are classified based on material type and nature, structure and application domain. Based on these criteria, membranes are as follows:
\nDepending on material nature: natural or synthetic;
Depending on material type: polymeric or inorganic;
Depending on structure: porous or dense (non-porous);
Depending on utilization domain: microfiltration (MF), ultrafiltration (UF), nanofiltration (NF), reverse osmosis (RO), dialysis (D), electro-dialysis (ED), membrane distillation (MD), pervaporation (PV) and electro-osmosis (EO).
Considering the pores’ form and distribution within the porous or non-porous membranes, they can be classified as
\nSymmetric structure: straight or inclined cylindrical pores, uniformly distributed of mono-disperse microspherulites;
Asymmetric structure: micropores with variable diameters forming a very thin layer 0.1–1 µm named active layer and non-regulated macropores forming the macroporous layer 100–200 µm;
Composite structure: an active compact symmetric or asymmetric layer, an intermediary layer and a macroporous layer.
Depending on the separation surface, geometry membranes are plane, tubular hollow fibre type (inner diameter <0.5 mm), tubular capillary type (0.5 mm < inner diameter < 5 mm) and tubular type (inner diameter > 5 mm).
\nThere are five main methods for membrane preparation: sintering, lamination, irradiation, phase inversion and deposition on thin layers [21]. Among them, phase inversion is the most commonly used method and is applied for membrane preparation at both laboratory and industrial level. Phase inversion concept was introduced in the literature by Kesting [22], and the concept implies transformation of one homogeneous polymeric solution in a two-phase system: one rich in polymer which forms the continuous part of porous membrane and other lacking polymer which fills the pores from membrane structure. The process has three main stages: polymer solubilization in a suitable solvent, skinning of polymer solution on a plane or tubular surface and polymer precipitation (phase inversion). The stage responsible for membrane structure is the precipitation one. Frequently, one of the following techniques for polymer transformation from liquid to solid phase is used: vapour phase precipitation [23], controlled evaporation precipitation [24], thermal precipitation [25] and immersion precipitation [26, 27]. Through phase inversion and immersion-precipitation techniques, membranes from various polymers are obtained: polysulphone, polyether sulphone, nylon 6,6, cellulose derivatives, polycarbonate, polyphenylenoxide, polyimides, polyamides, etc. These are used in both base form and modified (functionalized) form via various chemical reactions [28, 29].
\nMembrane processes are determined by the membrane structure and differentiated after the transport mechanism of chemical species through the membrane. Passing of one component from one side of the membrane to the other is defined as permeation, which is dependent on the driving force that generates it. After this criterion, membrane processes are classified as follows:
\nMicrofiltration, ultrafiltration and reverse osmosis (driving force—pressure gradient);
Pervaporation, gas permeation, dialysis, separation through liquid membranes (driving force—concentration gradient);
Thermo-osmosis and membrane distillation (driving force—temperature gradient);
Electrodialysis and electro-osmosis (driving force—electric potential gradient).
Practical realization of membrane separation processes involves specific installations for each application field, in which the core element is represented by the equipment that contains the membrane, named membrane module. Depending on membrane shape there are two types of modules: plane and tubular. Plane membranes can be used in various geometries within modules similar to classic plate filters. Plane membranes can also be used within filter modules with both spiral and folded configurations. Tubular membranes can be used within tubular, capillary or hollow fibre modules.
\nMembranes and membrane process applications cover a vast area: treatment of water intended for human consumption from various sources (surface water including marine water, ground water), wastewater treatment, separation and concentration of proteins and enzymes from various natural and biosynthesis media, preparation of ultrapure water, development of medical devices (artificial kidneys, artificial lungs), development of sensors and biosensors with multiple applications, gas separations, fuel cells, ultrapure compounds via membrane distillation and pervaporation, etc.
\nRecent works in the field of membranes and membrane processes are focussing on obtaining cost reduction, improvement of separation characteristics (flow rate, selectivity, limitation of clogging) and extension of application domains at industrial scale [30]. Among these domains, the use of conductive polymer-based membranes is envisaged.
\nMembranes based on conductive polymers represent a new class of advanced materials that can be used for separation or for interphase transfer processes of some chemical species based on their electrical properties. These membranes can be obtained through the previously described processes for preparation of classic membranes, their particularities being linked to polymers’ “doping” methods in order to improve their conductive properties. Membranes of this type are obtained mainly from the polymers mentioned within Table 1, but considering the number of citations from the literature, the most used polymers are polyaniline (PANI) and polypyrrol (PPy). Apart from these polymers, during the last period, the use of functionalized polyetheretherketone (PEEK) as conductive polymer and of a considerable number of other polymers in fuel cells were thoroughly researched. Based on these facts, three main classes of conductive polymer-based membranes are presented. All the above-mentioned polymers have physical-chemical properties that do not allow the preparation of membranes using only the specific polymer but only in combination with other polymers. Such membranes usually lack conductive properties but have excellent mechanical strengths. Therefore, the majority of conductive polymer-based membranes are “composite membranes”.
\nPolyaniline (PANI) is a macromolecular compound obtained through oxidative polymerization of aniline in accordance with Eq. (6):\n
In its structure, there are structural units formed from benzene rings linked through aminic groups (-NH-) and structural units formed from a benzene ring linked with a quinone diimine. The ratio of the two structural units within polymeric chain is varying depending on its degree of oxidation. There are three particular structures of the polyaniline, which differentiate among them the function of the two structural units’ ratio (Figure 4).
\nStructural PANI forms. (a) Leucoemeraldine base, (b) pernigraniline base and (c) emeraldine base.
Thus, in the limit case of PANI containing only structural units formed from benzene rings linked through aminic groups (x = 1), the compound is named PANI-leucoemeraldine base (Figure 4a), and in the limit case in which within the structure are only structural units formed from one benzene ring linked with a quinone diamine (x = 0), the compound is named PANI-pernigraniline base (Figure 4b). The third particular case is that in which within the macromolecular compound structure, the proportions of the two structural units are equal (x = 0.5), the compound being named PANI-emeraldine base (Figure 4c). Through treatment of these forms with acids or bases (“doping”), the polymer reversible passes from one form to other and gains electroconductive properties.
\nPANI in the base form has properties that do not allow obtaining simple membranes (low solubility in the majority of solvents commonly used for membranes preparation, low plasticity, thermal instability at temperatures above 160°C, etc.). For this reason, PANI-based membranes are obtained through blends with other polymer (usually chemically inert) suitable for membranes preparation. Composite membranes based on PANI with conductive properties are obtained. There are a large number of inert polymers used for PANI-based composite membranes preparation, the most used being cellulose and its derivatives, polysulphone, polystyrene and polypropylene.
\nPANI-based composite membranes are used in the majority of domains mentioned for conductive polymers, mainly for selective separation processes of some chemical species from complex liquid solutions, selective separation of gases, development of biosensors, electric and electronic devices (LED, photovoltaic cells), anticorrosive films and fabrication of antistatic textile materials.
\nThe most recent scientific researches on preparation and specific applications of PANI-based composite membranes are presented in the following paragraphs.
\nFibre-type cellulose was used in nanocomposites fabrication through oxidative in situ polymerization of aniline within fibres microstructure [31]. Polymerization was made in oxidative conditions using ammonium peroxydisulphate in hydrochloric acid aqueous solutions in which cellulose fibres impregnated with aniline are suspended. From the fibres separated at the end of the process, which contain PANI in their microporous structure, polymeric films were obtained via phase inversion process. Similarly, a composite material using nanofibrils bacterial cellulose as support material for PANI was obtained [32]. Research works showed the growth of PANI content within the composite material at the same time with the increase of its electric conductivity, with the prolonged reaction time from 30 to 90 min. Prolonging reaction time more than 90 min resulted in a decrease of electric conductivity due to aggregation of PANI particles and creation of discontinuities within nanocomposite structure. At the optimum time, a nanomaterial with the best conductivity of cca. 5.0 S m−1 was obtained. Using this composite material, a flexible film (conductive membranes) that synergetically combines PANI conductive properties with mechanical strength (Young’s modulus is 5.6 GPa and tensile strength is 95.7 MPa) provided by bacterial cellulose is obtained. The membranes obtained are applied in the field of electrochemical sensors, flexible electrodes and flexible displays. Compared with the processes in which first a nanocomposite material is obtained and then is used for conductive membrane preparation following a classic technique (phase inversion through immersion-precipitation technique), research works were conducted with the aim to obtain PANI-based composite conductive membranes following the next sequence: first, a semipermeable cellulose membrane is obtained and then on its surface, a thin layer of PANI is applied [33]. Deposition of the thin layer at membrane interface is realized via in situ polymerization of aniline with oxidative mixture containing ammonium peroxydisulphate in hydrochloric acid aqueous solutions. An aniline conversion of 80% was obtained after 24 h reaction time. At the end of the process, residual aniline was found on the active side of PANI membranes and secondary reaction products (ammonium hydrogen sulphate) obtained from ammonium peroxydisulphate were found on both sides of the membrane.
\nCellulose esters are representing another class of polymeric materials used as support in preparation of PANI-based composite membranes. Investigations on PANI deposition on the surface of some microporous cellulose ester membranes were performed using two distinct techniques: deposition of PANI layer on membrane surface through in situ aniline polymerization in liquid phase or aniline polymerization in vapour phase [34, 35].
\nIn situ polymerization of aniline in liquid phase was performed through dipping of one membrane from cellulose esters mixture in an aniline solution (PANI monomer) and FeCl3 as oxidant [34]. In other experimental variant, aniline polymerization in liquid phase is made by immersion of pre-formed cellulose esters membrane in a solution that contains aniline and HCl followed by the addition (at a certain time) of oxidative agent such as ammonium peroxydisulphate solution [35]. Aniline polymerization in vapour phase is done by soaking cellulose ester-based membrane in a solution of aniline and HCl and maintaining it in a closed tank with an oxidizing agent (ammonium peroxydisulphate and HCl solution)-saturated vapour atmosphere heated at 65–70°C [34, 35]. Cellulose acetate—PANI composite membranes with electric conductivities from 10−3 and 11 S m−1 \n(using the liquid phase polymerization) [34] and respectively 98 Sm-1 (using the vapour phase polymerization) [35] were obtained.
\nPolysulphone (Psf) is another frequently used polymer in the preparation of polymeric membranes used in membrane processes based on gradient pressure driving forces (microfiltration, ultrafiltration, reverse osmosis). This diversity of uses is due to polymers physical-chemical characteristics (chemical inertness, very good plasticity, excellent solubility in usual solvents used within phase inversion process, good mechanical strength, etc.). Psf is used as a substrate for the preparation of Psf–PANI composite membranes designed for advanced separation of compounds with polar groups from various mixtures, capitalizing the conductive properties of PANI from their structure.
\nWithin the Psf – PANI composite membranes, PANI is present in the whole membrane’s microporous structure, not only on surface. Preparation method is also a specific one and is differentiating from those already described. Thus, research works aimed to prepare Psf–PANI composite membranes through simultaneous formation of Psf-base membrane and aniline polymerization in oxidative conditions within membranes under formation pores [36]. Practically, the process consists of solubilization of Psf polymer within a specific solvent (N-methyl-pyrolidone or dimethylformamide) and aniline (PANI monomer), skinning of polymeric solution on a plane surface and immersion of polymeric film within an oxidative coagulation solution (ammonium peroxydisulphate and HCl). As the phase inversion process advances, Psf membrane is formed and within its pores PANI resulted from aniline polymerization in oxidative conditions.
\nSix types of composite membranes were obtained, using three polymeric solutions with 10, 12 and 14% Psf and two types of coagulants (distilled water and distilled water with 1.9% aniline). In all polymeric solutions, Psf was dissolved in a mixture of N-methylpyrrolidone and aniline. Obtained membranes were characterized from the point of view of flow and electroconductive properties through flows determination for solutions with variable pH (1, 3, 5, 7, 9 and 11), and selective separation properties were emphasized via determination of retention degree for standard proteins (albumin from bovine serum—BSA). BSA separation experiments proved that membranes obtained through coagulation from water and aniline solution present higher flows and retention degree compared to the membranes obtained by coagulation with only distilled water. For example, membranes obtained from 10% solution coagulated with water and aniline present a flow of 151.2 L/m2h at pH = 4.9 and 196.3 L/m2h at pH = 7.4 compared with membranes obtained from the same solution but coagulated in distilled water that showed a flow of 140.1 L/m2h at pH = 4.9 and 189.4 L/m2h at pH = 7.4. Retention degrees for membranes coagulated in water and aniline varied between 81.84 and 92.16% compared with 75.36–81.4% determined for membranes coagulated in distilled water.
\nThrough this process composite membranes with conductive properties are obtained, having separation characteristics superior to those obtained using similar polymeric conditions that contains only Psf. Performed research emphasized the dependence of Psf/aniline ratio from polymeric solution and structural and hydrodynamic characteristics of Psf–PANI composite membranes.
\nIn order to diminish the errors at laboratory level, mainly the manual skinning of polymeric solution and variation during the phase inversion process of the coagulation solution composition, Psf–PANI-based composite membrane preparation was studied in a steady-state installation [37]. That induces a modification of composite membrane preparation technology such that in one tank Psf membrane forming takes place. Psf membrane has in its pre-formed pores a certain quantity of aniline, and finalization of its structure is made in a reaction tank filled with oxidative mixture in which polymerization of aniline from pores occurs.
\nUsing a 10% Psf solution (MW = 22,000 Da) dissolved in a mixture of N-methylpyrrolidone and aniline, membranes in a continuous system in the following working conditions were prepared: thickness of the polymeric film is equal to 0.2 mm, speed of the carrier in the tanks is equal to 1 m/min, temperature of the oxidative solution is equal to 25°C and reaction time is equal to 2 h. Characterization via distilled water flow for nine samples from the same membrane led to a maximum relative deviation of flow values of 2.45%, proving that through this approach, Psf–PANI composite membranes with reproducible hydrodynamic and conductive properties both in the entire surface and from one batch to other are obtained.
\nOther polymers studied as support materials in order to develop composite membranes based on PANI, with conductive polymers, are polystyrene [38, 39] and polypropylene [40]. Thus, from blends containing PANI and polystyrene in various ratios, dissolved in N-methyl-2-pyrrolidone, flexible polymeric films were obtained via phase inversion process, phase changing taking place through precipitation in vapour phase [38]. The particularity of the method consists in the fact that PANI was obtained in a separate oxidative polymerization process: a reaction media formed from aniline and alcoholic solution of 0.1 M H2SO4 in a volumetric ratio of 1/25 is cooled to −5°C; a solution containing ammonium peroxydisulphate as initiator is slowly added in a 2-h period within the reaction mixture; obtained PANI polymer is filtered and washed with acetone and a solution of 0.1 M NH4OH and mixed for 24 h; after that the polymer is filtered again, washed with distilled water and dried at 60°C for 24h. After drying, PANI and polystyrene are dissolved in N-methyl-2-pyrrolidone, the solution being coated on a support that is heated in an oven at 60°C for 24 h. Finally, the composite membrane obtained is removed from the support and subjected to doping process by immersing in a 5 M HCl solution for 9 min and dried afterwards [38].
\nObtained polystyrene-PANI composite membranes present conductive properties depending on polystyrene/PANI ratio within the solution.
\nPolystyrene is used also in functionalized sulphonated form for the preparation of PANI-based composite materials [39]. Both polymers are obtained simultaneously in the same reaction environment consisting of aniline (PANI monomer), 4-styrene sulphonic acid sodium salt hydrate (sulphonated polystyrene monomer), ammonium peroxydisulphate and HCl (for oxidative polymerization).
\nThe working procedure is the following: within a 3.47 mM aqueous solution of 4-styrene sulphonic acid sodium salt hydrate, heated at 80°C, the oxidant ammonium peroxydisulphate (aqueous solution 4.86 M) was added drop wise in a volumetric ration of 1/7 to styrene solution, under mixing for 1 h; after that an aqueous solution of aniline chlorhydrate 0.58 M (volumetric ratio of 1/8 to mixture) is added and after another 15 min a new quantity of 4-styrene sulphonic acid sodium salt hydrate (aqueous solution with a concentration of 0.72 M in a ratio of 1/9 to reaction media) was added drop wise; the reaction media is maintained under mixing at 80°C for 3 h, and afterwards the temperature drops to ambient temperature in a 24-h period. The composite polymer is precipitated in iso-propanol for 24 h without mixing and is washed with ethanol and dried at 70°C.
\nObtained composite material contains in its structure PANI and sulphonated polystyrene macromolecular linked with chemical bonds (ionic bonds) through diimino protonated groups of PANI and sulphonic groups of sulphonated polystyrene. Due to these bonds, the conductive capacity of the composite material is lower compared with the above-presented composite materials, being practically a semiconductor. This composite material is used for polymeric membranes preparation through classic processes, dense films for antistatic packages, anticorrosive material or semiconductors.
\nPolypropylene is used as support material for preparation of PANI-based composite materials in the form of microporous membrane film through biaxial stretching technique [40]. PANI is formed within the polypropylene pores membrane through soaking of polymeric film in aniline followed by aniline oxidative polymerization using ammonium peroxydisulphate and HCl. Polypropylene—PANI composite membranes maintain the microporous structure of the support polymer, with various pores diameters and present conductive properties. These composite membranes are used in selective separation of chemical species from various liquid media through microfiltration, ultrafiltration, nanofiltration and reverse osmosis.
\nBesides polymeric materials, inorganics can be used as support for PANI-based composite materials. Thus, zeolites were used for new zeolite-PANI composite materials preparation due to their microporous structure and adsorption capacities [41]. Method consists of polymerization of aniline retained within zeolite matrix (Molecular Sieve 13X – SUPELCO Analytical) in oxidative conditions similar to those described previously (ammonium peroxydisulphate and HCl). The composite material is included within a quartz filter structure resulting in an inorganic-organic membrane with ultrafiltration flow rate properties. Conductive properties of these membranes (due to the PANI inclusion within their structure) allow separation of chemical species with high pollution potential from wastewater, such as heavy metals ions (Pb, Cu, Zn) and phenol derivatives (phenol, aminophenols or nitrophenols). Thus, retention degrees determined for heavy metal ions were 72.59% for Pb2+, 87.48% for Zn2+ and 99.55% for Cu2+. Phenol derivatives from wastewater were removed using these composite materials with efficiencies above 98% (phenol, 98.15%; aminophenol, 99.78%; nitrophenol, 99.23%).
\nPolypyrrol (PPy) is a polymer obtained by pyrrol oxidation (Py) in the form of a black powder. This polymer has poor mechanical strength and thus low processibility. Its conductive properties in natural state are very low, and it is rapidly oxidized in contact with air, changing its properties. PPy conductivity is given by the existence within its structure of π conjugated electron systems (from pyrrol ring) with p electrons available at N atom from pyrrol ring. This property is significantly improved by PPy “doping” with anions such as chloride, sulphate, perchlorate, dodecylsulphate and other organic compounds. Doped PPy is a polymer characterized by good chemical and thermal stability and better conductivity compared with other conductive polymers. Disadvantages related to PPy mechanical strength, plasticity and elasticity are improved both through doping process and by inclusion (as doped form, similar with PANI) within the polymeric and inorganic composite materials structure. PPy-based composite materials are frequently used as membranes within the processes in which driving force is no longer the pressure gradient but concentration gradient (gas separation from complex mixtures and pervaporation) and electric potential gradient (electro-dialysis).
\nDuring the last period, the research works related to PPy-based composite materials studies are focussed on their application in electro-analysis, medical field (systems for controlled release of drugs and use as biomaterial for artificial muscles) and antistatic and anticorrosive protection.
\nPPy polymerization in PPy-based composite materials is done through two methods: polymerization through chemical oxidation and electrochemical polymerization [42].
\nAmmonium peroxydisulphate, hydrogen peroxide and various compounds based on transitional metals salts (Fe2+; Cu2+; Cr6+; Mn2+; etc.) are frequently used as oxidative agents for the polymerization through chemical oxidation.
\nThe process is presented in Eq. (7):
\nPPy polymeric chain can contain Py linked with three types of dimer sequences [8], presented in Figure 5.
\nAddition within the chemical oxidation reaction media of surfactants such as sodium dodecylbenzensulphonate and sodium alkylsulphonate and alkylnaphtalenesulphonate results in an increase of electric conductivity of the composite material and Py polymerization efficiency [42]. Electrochemical polymerization is performed in conditions mentioned within Section 1.2 based on application of an electric current between two electrodes immersed in a Py solution that contains also the dopant, in accordance with Eq. (8):
\nwhere C− is counterion.
\nDimer sequences within PPy structure. (a) α,α’, (b) α,β’ and (c) β,β’
The Py chemical oxidative polymerization was applied to obtain membranes with high permeability for gas separation. Membranes were obtained through the technique of deposition in thin layers through interfacial polymerization [43, 44]. A freestanding polymeric film, 200–300 nm thick, was obtained by Py polymerization on an inert glass support through mixing of oxidative agent aqueous solutions containing ferrous chloride (0.4 M) and ferric chloride (0.5 M) with a solution of Py dissolved in an organic solvent (n-hexane) [43]. The membranes were prepared by pouring a solution of polydimethylsiloxane dissolved in n-hexane on PPy surface, after oxidant excess removal and polymeric film washing with methanol. The contact between components was maintained for 24 h and after that the composite membrane was annealed in air at 80°C for 15 min. Finally, the composite membrane is removed from the glass surface by simple washing with water. Obtained composite membranes present high selectivity for separation of oxygen and nitrogen from various mixtures, separation ratios O2/N2 of 17.2 being reported. The permeability for O2 was 40.2 barrer. Using the same method of interfacial polymerization through chemical oxidation of Py or its derivatives (N-methylpyrrole), PPy-based conductive composite membranes with applications in the field of gas separation and pervaporation were obtained on a surface of microporous membrane supports [44]. Polymerization was performed at chamber temperature for 4 h using an aqueous 0.5 M Py solution and ferric chloride solutions (0.5, 1, 2 or 3M) as oxidative agent. The obtained membranes were washed with deionized water and stored in a 1 M HCl solution, and the operation was repeated daily for a week. In the final, membranes were stored in deionized water prior to characterization and use.
\nThe Py chemical oxidative polymerization was used also for the preparation of PPy-based composite membranes having pre-formed membranes from sulphonated poly(styrene-co-divinylbenzene) as support, with its biotechnological applications and applications in wastewater treatment through electro-dialysis [45]. PPy polymer was formed through chemical oxidation within the structure of a commercial membrane with cationic exchange properties (Selemion CMT, manufactured by Asahi Glass Co.). The process consists of immersion of commercial membrane soaked in a ferric chloride oxidant solution in a Py aqueous solution at chamber temperature for about 4 h.
\nSimilar properties related to ion exchange and possibility to apply in electro-dialysis also present PPy-based membranes obtained via Py chemical oxidative polymerization within the microporous structure of some inert polymeric supports [46] or inorganic supports [47]. In the first case [46], composite membrane is formed in one single stage through phase inversion techniques and chemical oxidation reactions. A solution of polysulphone and PPy dissolved in a N,N-dimethylformamide/methanol solvent system is coated on a plane surface and then immersed in a ferric chloride oxidant solution. At the same time, with formation of microporous polysulphone support, the chemical oxidative polymerization of Py within the preformed pores takes place. In the second case [47], the process consists of polymerization of adsorbed Py into silica through chemical oxidation, resulting in PPy inorganic-organic composite membranes.
\nPPy obtained through chemical oxidative polymerization is used as base material for medical devices [48, 49] due to its conductive properties. Py polymerization takes place in controlled conditions, a special attention being given to PPy doping and modification in order to be biocompatible. On PPy structure are engrafted biomolecules or cells (mammalian cells, endothelial cells, mesenchymal stem cells, etc.) through adsorption of covalent bonding [48]. Other studies emphasized the use of PPy incorporated in poly(ε-caprolactone) and gelatin nanofibres for cardiac tissues [49]. Performed experiments proved that increase of PPy concentration up to 30% within the composite material resulted in a reduction of average diameter of fibres from 239 ± 37 to 191 ± 45 nm, at the same time, with an increase of about six times of tensile modulus (7.9 ± 1.6 MPa initial and 50.3 ± 3.3 MPa after introduction of PPy).
\nOther applications of PPy-based composite membranes prepared through Py chemical oxidation is in the antistatic and anticorrosive materials field. Polyethylene used as natural [50] or modified [51] polymer constitutes an excellent polymeric material for the preparation of PPy composite membranes due to its properties (good mechanical strength, plasticity, elasticity) needed for membranes preparation. Thus, within the pores of polymeric films obtained through melt extrusion with subsequent annealing, uniaxial extension and thermal fixation, PPy was deposited through Py chemical oxidative polymerization [50]. Using another technique [51], polyethylene polymeric film is modified through engraftment within its structure of another polymer realized through acrylic acid irradiation with γ rays. Obtained material is highly hydrophilic which contributes to a better Py retention through surface adsorption that is further polymerized through chemical oxidation using iron chloride (III) or ammonium peroxydisulphate. Performed researches [51] were focussed on increase of electric conductivity of the composite material through increase of Py concentration within the reaction media from 0.3 to 0.9 M, but obtained results proved that this was insignificant (from 162 to 166 S m−1). Introducing a new Py polymerization phase resulted in an increase of electric conductivity from 166 to 543 S m−1.
\nPPy obtained via electrochemical method has similar application with those of PPy obtained through chemical oxidation.
\nThus, PPy membrane formed on stainless steel net is used for separation of ethanol and cyclohexane mixtures through pervaporation [52]. Electrochemical polymerization takes place in a four-cell installation with porous glass walls and three electrodes. One of the electrodes is made from stainless steel net obtained through weaving of stainless steel fibre with 25 or 18 µm diameter. Within the cell that contains this electrode, a solution of 0.1M Py, acetonitrile as solvent and a doping agent (Me4NBF4 0.05 M, Bu4NBF4 0.1 M or Bu4NPF6 0.1 M) are administered. Formed pervaporation membranes were tested in a specific installation and are proved to be selective for ethanol, permeation being dependent on Py polymerization degree and dopant type.
\nUsing a similar method, electrochemical polymerized PPy deposited onto platinum sputter-coated polyvinylidene filters was obtained [53]. Process was realized through introduction within the cell containing filters of a Py aqueous solution containing as doping agents 8-hydroxyquinoline-5-sulphonic acid (HQS) or 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline disulphonic acid (BCS). PPy/BCS-type conductive membranes are permeable to a series of ions such as Co2+, Ni2+, Zn2+, K+, Mg2+, Ca2+, Mn2+, Fe3+ and Cu2+. PPy/HQS conductive membranes are not permeable to all above-mentioned ions, significant results being obtained only for K+, Co2+ and Cu2+. Moreover, ion fluxes are much higher (more than 10 times in case of Cu2+) for PPy/BCS compared with PPy/HQS membranes. Conductive membranes with permeability for Na+, K+, Ca2+ and Mg2+ ions were obtained in similar conditions with those described above with the difference that PPy was deposited onto platinum sputter-coated polyvinylidene fluoride filters and polystyrenesulphonate/dodecylbenzenesulphonate (1%) or polyvinylphosphate/dodecylbenzenesulphonate systems were used for doping [54]. It was proved that ions transport fluxes are varying in the following order: Na+ > K+ > Ca2+ >Mg2+.
\nAnother domain that was thoroughly studied in the last period and uses PPy polymers obtained in the form of membrane films via electrochemical polymerization is that of electro-analysis. Through deposition of PPy membrane on the Al2O3 surface of one electrode, amperometric sensors with multiple uses in the field of analytical chemistry is obtained [55]. PPy membrane is prepared through electrochemical polymerization of Py on the electrode surface using an aqueous solution 0.2 M Py and 0.1 M KCl (dopant) or 0.1 M Py and 0.5 M K4[Fe(CN)6] (dopant).
\nPPy based membranes applications within fuel cells domain should be mentioned also. The conductive polymers applications in the field of fuel cells are presented within the next section.
\nFuel cells are devices that generate electricity based on the free energy of a chemical reaction. A classical fuel cell consists of a porous anode fed with gas fuel that after oxidation led to electrons release; a porous cathode fed with oxidant, which generates protons and an electrolyte located between the two electrodes; and two bipolar plates and electric connectors that are linking electrodes through an exterior circuit. Chemical reactions for a classic combustion cell are presented in Eqs (9–11).\n
where E = electrical energy and H = heat.
\nType of fuel cell | \nOperating temperature (°C) | \nElectrolyte | \nReaction At the anode (A) At the cathode (C) | \n
---|---|---|---|
AFCs | \n60–90 | \nKOH (liquid) | \n(A) H2 + 2HO− = 2H2O + 2e− (C) 1/2O2 + H2O + 2e- = 2HO− | \n
PEMFCs | \n60–120 | \nPolymer–SO3H (solid) | \n(A) H2 = 2H+ + 2e− (C) 1/2O2 + 2H+ + 2e− = H2O | \n
DMFCs | \n60–120 | \nPolymer-+NR3 (liquid) | \n(A) CH3OH + 6HO- = CO2 + 5H2O + 6e− (C) 3/2O2 + 3H2O + 6e− = 6HO− | \n
PAFCs | \n160–220 | \nPhosphoric acid H3PO4 (liquid) | \n(A) H2 = 2H+ + 2e− (C) 1/2O2 + 2H+ + 2e− = H2O | \n
MCFCs | \n600–800 | \nMolten salt Li2CO3/K2CO3 (liquid) | \n(A) H2 + CO32− = H2O + CO2 + 2e− (C) 1/2O2 + CO2 + 2e- = CO32− | \n
SOFCs | \n800–1000 | \nCeramic ZrO2/Y2O3 (solid) | \n(A) H2 + O2− = H2O + 2e− (C) 1/2O2 + 2e- = O2− | \n
Main combustion cell type’s characteristics.
These devices present large spectra of applications due to the fact that global efficiencies obtained for electricity are higher than those of classical systems (thermic engines or hydroelectric turbines). At the same time, the effects induced upon the environment are less harmful than those produced by other electricity-producing systems such as fossil fuels burning.
\nFuel cells can be classified based on two main criteria: electrolyte nature (charge carriers HO−, H+, CO32− or O2−) and operation temperature. Based on the latter criterion, fuel cell types are: low temperature—alkaline fuel cells (AFCs—T < 100°C), polymer electrolyte fuel cells (PEMFCs—T = 60–120°C), direct methanol fuel cells (DMFCs—T = 60–120°C), phosphonic acid fuel cells (PAFCs—T = 160–220°C) and high temperature—molten carbonate fuel cells (MCFCs—T = 600–800°C), solid oxide fuel cells (SOFCs—T = 800–1000°C).
\nTable 2 is summarizing the main combustion cell types depending on operating temperature, electrolyte nature, anode (A) and cathode (C) reactions.
\nConductive polymer membranes are thoroughly studied due to advantages offered by the fact that they function both as solid electrolytes and as selective separation barriers for the species implied in electricity generation within the fuel cells.
\nFirst applications were based on preparation and inclusion within the fuel cells structure of protons exchange membranes—Nafion, obtained from persulphonic acid and PTFE by Dupont Company 30 years ago. Nowadays researches are focussed on preparation of conductive polymers membranes with improved electric and mechanical properties. The most recent researches in preparation of both conductive membranes with protons exchange properties, applicable in PEMFCs, and conductive membranes applicable to AFCs are reviewed in the following paragraphs.
\nIn a study dedicated to this domain [56] are emphasized the large number of composite membranes based on conductive polymers used for fabrication of high temperature proton exchange membrane fuel cells. Both organic composite membranes based on polymers with electric properties such as sulphonated poly (p-phenylene), sulphonated poly(ether ether ketone), sulfonated polysulfone, sulfonated poly (arylene ether sulfone), sulfonated poly(aryl ether ether nitrile), sulfonated poly(sulphide ketone), and organic-inorganic composite membranes such as fluorinated polymer/SiO2, polyalkoxysilane/phosphotungstic acid, Nafion/PTFE/zirconium phosphate, Nafion/TiO2 and Nafion/SiO2 are reviewed.
\nOne of the most studied polymers for organic composite membranes with applications in fuel cells is poly(ether ether ketone) (PEEK), which is used in base or modified form. Thus, from sulfonated poly(ether ether ketone) (SPEEK), asymmetric microporous membranes can be obtained via phase inversion method and immersion-precipitation technique. The SPEEK polymer was obtained by dissolving PEEK in concentrated H2SO4 added in a proportion of 5 wt%, at room temperature, reaction media being maintained by mixing for 24 h. From the resulted solution, a membrane was prepared by coating on a plane glass surface, followed by immersion in a coagulation bath containing distilled water (phase inversion method, immersion-precipitation technique). The obtained membrane is modified through in situ polymerization (within membrane pores) of Py doped with iron chloride and cerium sulphate [57]. Electroconductive properties of PPy from composite membrane structure (ionic conductivity of 0.34 S m−1) made the membrane suitable for fuel cells.
\nComposite membranes are obtained, using SPEEK as base material, through inclusion within its structure of heteropolycompounds based on tungsten, molybdenum or wolfram [58]. Obtained composite membranes present a conductivity of 1 S m−1 at chamber temperature and 10 S m−1 at 100°C temperature, being used in PEMFC-type fuel cells.
\nOther studies on SPPEK applications for fuel cells showed that it can be functionalized with quaternary amine hydroxide and imidazolium hydroxide [59] (resulting membranes with 10−3 S m−1 conductivity) or by PANI inclusion within membrane structure [60].
\nPolysulfone [61] and poly(1,4-phenylene ether ether sulfone) [62] are other polymeric materials that can be used to obtain composite membranes with conductive properties for fabrication of fuel cells. Using polysulfone, asymmetric membranes can be obtained via classical process of phase inversion and afterwards functionalized through incorporating acrylamide-based ionomers having proton-conducting sulphonics groups. Incorporation process of the new polymer is based on photopolymerization [61]. At the surface of membranes prepared from poly(1,4-phenylene ether ether sulfone) modified through addition of tungstophosphoric acid, a layer of PPy polymer is applied via chemical oxidation, resulting in composite membranes used for fabrication of DMFC [62]-type fuel cells.
\nFuel cells protons exchange composite membranes, which can be used at temperature above 100°C, were obtained from poly(2,6-dimethyl-1,4-phenylene oxide), N-(3-aminopropyl)-imidazole and metal – organic frameworks [63].
\nComposite membranes with applications at high temperatures, for fuel cells, are obtained also from bi-functionalized copolymer prepared through radical copolymerization, having SiO2 [64] within in its structure.
\nAnother point of interest within the literature is represented by preparation of membranes for alkaline fuel cells. Studies performed in this domain [65, 66] classify conductive membranes for preparation of AFCs in heterogeneous and homogeneous membranes, each with their specific polymers and preparation methods. One of the most recent researches related to membranes for alkaline fuel cells is focussing on preparation of high ionic conductivity membrane from crosslinked poly(arylene ether sulphones) [67].
\nBesides traditional methods for preparation of polymeric membranes with conductive polymers (phase inversion, lamination, irradiation, etc.), a new technique was recently developed—plasma techniques both for plasma polymerization and for plasma modification of membrane surfaces [68]. Proton exchange membrane for PEMFCs and membranes for alkaline fuel cells (AFCs) can be obtained using this technique.
\nConductive polymers themselves are not forming membranes that can be used in various processes due to low mechanical strength, lack of elasticity and plasticity. For this reason, conductive polymer-based membranes are mainly composite membranes.
\nPreparation methods of composite membranes based on conductive polymers are similar to those used for simple membranes (sintering, lamination, irradiation, phase inversion, deposition on thin layers) for the formation of support polymer that confers mechanical strength and elasticity. Chemical oxidation polymerization and electrochemical polymerization are used for the inclusion within the support structure of a polymer with conductive properties. There are three ways for preparation of composite membranes presented within the literature:
\nConductive polymer is formed at the same time with support membrane; in this case, the composite membrane contains the conductive polymer in all its structure;
Conductive polymer is formed after support membrane preparation and its soaking in monomer solution followed by polymerization through chemical oxidation; in this case, composite membrane contains conductive polymer in all microporous structure;
Conductive polymer is formed only after preparation of support membrane through deposition on its surface of conductive polymeric film; in this case, composite membrane contains in its structure two different layers—sandwich type.
Conductive properties of polymers that contain conjugated electrons systems (п-п or p-п) are low compared with metals, being at the level of semiconductors. In order to obtain polymers with better conductive properties, “doping” technique is used, through introduction within polymeric chain of atoms or groups of atoms that creates “defects” within macromolecule structure as a result having more rapid “jumping” of electrons between polar centres. Doping process takes place simultaneously with conductive polymer formation within the composite membrane structure, through dopants addition within monomer solution. Doping process takes place with conductive polymer preparation in some rare cases.
\nConductive polymer-based composite membranes are used in membrane processes that generally use concentration gradient (pervaporation and gas separation) and electric potential gradient (electro-dialysis) as driving forces. There are also cases in which these membranes are used in processes that uses pressure gradient (MF, UF, RO). Many researches are focussed on conductive polymer-based composite membranes’ use for fuel cells.
\nThe incidence of microbial attack in different sectors such as food, textiles, medicine, water disinfection, and food packaging leads to a constant trend in the search for new antimicrobial substances. The increased resistance of some bacteria to some antibiotics and the toxicity to the human body of some organic antimicrobial substances has increased the interest in the development of inorganic antimicrobial substances. Among these compounds, metal and metal oxide compounds have attracted significant attention due to their broad-spectrum antibacterial activities. On the other hand, nanoscale materials are well known thanks to their increased properties due to their high surface area-to-volume ratio. Antimicrobial NPs have shown excellent and different activities from their bulk properties [1, 2].
\nDuring last decades, metal oxide nanoparticles, such as zinc oxide (ZnO), manganese oxide (MgO), titanium dioxide (TiO2), and iron oxide (Fe2O3), have been extensively applicable thanks to their unique physiochemical properties in biological applications. Among metal oxide antimicrobial agents, TiO2 is a valuable semiconducting transition metal oxide material and shows special features, such as easy control, reduced cost, non-toxicity, and good resistance to chemical erosion, that allow its application in optics, solar cells, chemical sensors, electronics, antibacterial and antifungal agents [3]. In general, TiO2 nanoparticles (TiO2 NPs) present large surface area, excellent surface morphology, and non-toxicity in nature. Several authors have reported that TiO2 NPs have been one of the most studied NPs thanks to their photocatalytic antimicrobial activity, exerting excellent bio-related activity against bacterial contamination [4, 5, 6, 7].
\nAntimicrobial activity of nanoparticles is highly influenced by several intrinsic factors such as their morphology, size, chemistry, source, and nanostructure [8, 9, 10, 11]. Specifically, antimicrobial activity of TiO2 NPs is greatly dependent on photocatalytic performance of TiO2, which depends strongly on its morphological, structural, and textural properties [12]. Several TiO2 NPs have been developed through different methods of synthesis. Specifically, in this chapter, eco-friendly synthesis based on biological sources, such as natural plant extracts and metabolites from microorganisms, which have resulted in TiO2 NPs with different size, shape, morphology, and crystalline structures will be presented. Titanium dioxide produces amorphous and crystalline forms and primarily can occur in three crystalline polymorphous: anatase, rutile, and brookite. Studies on synthesis have stated that the crystalline structure and morphology of TiO2 NPs is influenced by process parameters such as hydrothermal temperatures, starting concentration of acids, etc. [13]. The crystal structures and the shape of TiO2 NPs are both the most important properties that affect their physicochemical properties, and therefore their antimicrobial properties [14]. Regarding the crystal structures, anatase presents the highest photocatalytic and antimicrobial activity. Some works have shown that anatase structure can produce OH˙ radicals in a photocatalytic reaction, and as it will be clearly explained below, bacteria wall and membranes can be deadly affected [15, 16].
\nThe potential health impact and toxicity to the environment of NPs is currently an important matter to be addressed. Several works have confirmed that metal oxide NPs conventionally synthesized using chemical methods, such as sol–gel synthesis and chemical vapor deposition, have shown different levels of toxicity to test organisms [17, 18, 19, 20]. In recent years, researchers have emphasized on the development of nanoparticles promoted through environmental sustainability and processes characterized by an ecological view, mild reaction conditions, and non-toxic precursors. Due to this growing sensitivity toward green chemistry and biological processes, ecological processes are currently being investigated for the synthesis of non-toxic nanoparticles.
\nThese biological methods are considered safe, cost-effective, biocompatible, non-toxic, sustainable, and environmentally friendly processes [20]. Furthermore, it has been described that chemically synthesized NPs have exhibited less stability and added agglomeration, resulting in biologically synthesized NPs that are more dispersible, stable in size, and the processes consuming less energy [21].
\nThese biosynthetic methods, also called “green synthesis,” use various biological resources available in nature, including live plant [22], plant products, plant extracts, algae, fungi, yeasts [23], bacteria [24], and virus for the synthesis of NPs. Among these methods, the processes that use plant-based materials are considered the most suitable for large-scale green synthesis of NPs with respect to their ease and safety [25]. On the other hand, the reduction rate of metal ions in the presence of the plant extract is much faster compared to microorganisms, and provides stable particles [26]. Plants contain biomolecules that have been highly studied by researchers like phenols, nitrogen compounds, terpenoids, and other metabolites. It is well known that the hydroxyl and carboxylic groups present in these biocompounds act as stabilizers and reducing agents due to their high antioxidant activity [12]. Thus, plant extracts have been studied as one of the best green alternatives for metal oxide nanoparticles synthesis [27]. In recent years, TiO2 nanoparticles have been obtained by using different plant extracts, but not all of them have been studied for their antimicrobial activity. Table 1 presents a compilation of synthesized TiO2 nanoparticles from green synthesis by using plant extracts that were tested against different microorganisms.
\nSource | \nTitanium precursor | \nSize (nm) | \nShape/crystal structure | \nTarget microorganism (method) | \n
---|---|---|---|---|
\nAzadirachta indica leaves extract [28] | \nTiO2\n | \n25–87 (SEM) | \nSpherical/anatase-rutile | \n\nS. typhi, E. coli, and K. pneumoniae (broth micro dilution method) | \n
\nPsidium guajava leaves extract [29] | \nTiO(OH)2\n | \n32.58 (FESEM) | \nSpherical shape and clusters/anatase-rutile | \n\nS. aureus and E. coli (agar diffusion) | \n
\nVitex negundo Linn leaves extract [30] | \nTi{OCH(CH3)2}4\n | \n26–15 (TEM) | \nSpherical and rod shaped/tetragonal phase anatase | \n\nS. aureus and E. coli (agar diffusion) | \n
\nMorinda citrifolia leaves extract [31] | \nTiCl4\n | \n15–19 (SEM) | \nQuasi-spherical shape/rutile | \n\nS. aureus, B. subtilis, E. coli, P. aeruginosa, C. albicans, A. niger (agar diffusion) | \n
\nTrigonella foenum-graecum leaf extract [21] | \nTiOSO4\n | \n20–90 (HR-SEM) | \nSpherical/anatase | \n\nE. faecalis, S. aureus, S. faecalis, B. subtilis., Y. enterocolitica, P. vulgaris, E. coli, P. aeruginosa, K. pneumoniae, and C. albicans (agar diffusion) | \n
Orange peel extract [32] | \nTiCl4\n | \n20–50 (SEM) | \nIrregular and angular structure with high porous net/anatase | \n\nS. aureus, E. coli, and P. aeruginosa (agar diffusion) | \n
\nGlycyrrhiza glabra root extracts [33] | \nTiO2\n | \n60–140 (FESEM) | \nSpherical shape/anatase | \n\nS. aureus and K. pneumoniae (agar diffusion) | \n
Synthesis of TiO2 NPs by using plant extracts.
Different factors need to be evaluated in this research field in order to obtain TiO2 NPs with better properties and to maintain their biocompatibility. It has been shown that nanoparticles obtained from green synthesis can have a better morphology and size translated into better antimicrobial activity. Mobeen and Sundaram have obtained TiO2 NPs from titanium tetrachloride precursor through a chemical and a green synthesis method. Sulfuric acid and ammonium hydroxide were used in the chemical-based method and, in the green synthesis, those chemical reagents were replaced by an orange peel extract [32]. The nanoparticles obtained by using the natural extract presented a well-defined and smaller crystalline nature (approx. 17.30 nm) compared to the nanoparticles synthesized through the chemical method (21.61 nm). Both methods resulted in anatase crystalline structures, and, when evaluating the antimicrobial activity, the more eco-friendly NPs revealed higher bactericidal activity against Gram-positive and Gram-negative bacteria compared to the chemically synthesized nanoparticles.
\nBavanilatha et al. have also detailed TiO2 NPs green synthesis with Glycyrrhiza glabra root extract. Antibacterial activity against Staphylococcus aureus and Klebsiella pneumonia were investigated and in vivo toxicity tests using the zebrafish embryonic model (Danio rerio) were also carried out [33]. Results have demonstrated their biocompatibility because healthy embryos of adult fish to different variations of NP and no distinctive malformations were observed at every embryonic stage with respect to embryonic controls.
\nSubhapriya and Gomathipriya have biosynthesized TiO2 NPs by using a Trigonella foenum-graecum leaf extract, obtaining spherical NPs and their size varied between 20 and 90 nm, and their antimicrobial activity was evaluated through the standard method of disc diffusion [21]. The NPs showed significant antimicrobial activity against Yersinia enterocolitica (10.6 mm), Escherichia coli (10.8 mm), Staphylococcus aureus (11.2 mm), Enterococcus faecalis (11.4 mm), and Streptococcus faecalis (11.6 mm). Results confirmed developed TiO2 NPs as an effective antimicrobial drug that can lead to the progression of new antimicrobial drugs.
\nSpherical TiO2 NPs were synthesized from plants, in particular by applying a Morinda citrifolia leaf extract, and through advanced hydrothermal method [31]. Developed TiO2 NPs showed a size between 15 and 19 nm in an excellent quasispherical shape. In addition, their antimicrobial activity was tested against human pathogens, such as Staphylococcus aureus, Escherichia coli, Bacillus subtilis, Pseudomonas aeruginosa, Candida albicans, and Aspergillus niger. TiO2 NPs exhibited interesting antimicrobial activity, principally against Gram-positive bacteria.
\nIn addition to plants, other organisms can produce inorganic compounds at an intra or extracellular level. The synthesis of TiO2 NPs through microorganisms, including bacteria, fungi, and yeasts, also meets the requirements and the exponentially growing technological demand toward eco-friendly strategies, by avoiding the use of toxic chemicals in the synthesis and protocols [34]. The metabolites generated by microorganism present bioreducing, capping, and stabilizing properties that improve the NPs synthesis performance. Jayaseelan et al. have stated glycyl-L-proline, one of the most abundant metabolite from Aeromonas hydrophilia bacteria, as the main compound that acted as a capping and stabilizing agent during TiO2 NPs green synthesis [35]. Moreover, the interest in fungi in green synthesis of metal oxide nanoparticles has increased over last years. Fungi enzymes and/or metabolites also present intrinsically the potential to obtain elemental or ionic state metals from their corresponding salts [34, 36]. Different works based on the green synthesis of TiO2 NPs from bacteria and fungus are presented in Table 2. Some of them have been synthesized with antimicrobial and antifungal purposes, and their target microorganisms are also declared.
\nMicroorganism | \nTitanium precursor | \nSize (nm) | \nShape/crystal structure | \nTarget microorganisms (method) | \n
---|---|---|---|---|
\nAeromonas hydrophilia [46] | \nTiO(OH)2\n | \n28–54 (SEM) ~ 40.5 (XRD) | \nSpherical/uneven | \n\nS. aureus, S. pyogenes (agar diffusion) | \n
\nAspergillus flavus [34] | \nTiO2\n | \n62–74 (TEM) | \nSpherical/anatase and rutile | \n\nE. coli, P. aeruginosa, K. pneumoniae, B. subtilis (agar diffusion and MIC) | \n
\nBacillus mycoides [37] | \nTitanyl hydroxide | \n40–60 (TEM) | \nSpherical/anatase | \n\nE. coli (toxicity) | \n
\nBacillus subtilis [38] | \nK2TiF6\n | \n11–32 (TEM) | \nSpherical | \nAquatic biofilm | \n
\nFusarium oxysporum [36] | \nK2TiF6\n | \n6–13 (TEM) | \nSpherical/brookite | \n— | \n
\nLactobacillus sp. [51] | \nTiO(OH)2\n | \n~ 24.6 (TEM) | \nSpherical/anatase-rutile | \n— | \n
\nPlanomicrobium sp. [39] | \nTiO2\n | \n100–500 (SEM) | \nIrregular/pure crystalline | \n\nB. subtilis, K. planticola, Aspergillus niger (agar diffusion) | \n
\nPropionibacterium jensenii [52] | \nTiO(OH)2, 300°C | \n15–80 (FESEM) | \nSpherical | \n— | \n
\nSaccharomyces cerevisiae [51] | \nTiO(OH)2\n | \n~ 12.6 (TEM) | \nSpherical/anatase-rutile | \n\n—\n | \n
Examples of TiO2 NPs synthesis through microorganisms, both bacteria and fungus strains.
Two important factors that affect NPs synthesis are the type of microorganisms and their source. Some microorganisms widely used in the food industry are Lactobacillus, a bacterium used in dairy products and as a probiotic supplement, and Saccharomyces cerevisiae, a yeast commonly used in bakery. Jha et al. have investigated the effectiveness of both microorganisms to synthesize TiO2 NPs. A comparison between synthesis through Lactobacillus from yogurt and probiotic tablets resulted in different NP sizes: a particle size of 15–70 nm for yogurt, and 10–25 nm for tablets. This difference was due to the purity of the bacteria [40]. In general, TiO2 NP synthesis through microorganisms has not provided stable sizes, being not industrially scalable compared to the synthesis of nanoparticles from plants.
\nHarmful bacteria, such as Staphylococcus aureus, Burkholderia cepacia, Pseudomonas aeruginosa, Clostridium difficile, Klebsiella pneumoniae, Escherichia coli, Acinetobacter baumannii, Mycobacterium tuberculosis, and Neisseria gonorrhoeae, are responsible for bacterial infections that can cause serious diseases in humans year after year [40]. The principal solution is the use of antibiotics, antimicrobial and antifungal agents. Nevertheless, in recent years there has been an increase in the resistance of several bacterial strains to these substances, and therefore there is currently a great interest in the search for new antimicrobial substances. The antimicrobial nanoparticles have been studied due to their high activity, specifically the metal oxide nanoparticles [41, 42, 43]. In this sense, titanium dioxide nanoparticles are one of the antimicrobial NPs whose study has gained interest during last years.
\nTiO2 is a thermally stable and biocompatible chemical compound with high photocatalytic activity and has presented good results against bacterial contamination [44]. Table 3 presents some research including the antimicrobial capacity of TiO2 NPs.
\nMicroorganism | \nNPs | \nResults | \n
---|---|---|
Methicillin-resistant Staphylococcus aureus [45] | \nFe3O4-TiO2 core/shell magnetic NPs | \nThe survival ratio [%] of bacteria decreased from 82.40 to 7.13%. | \n
\nStaphylococcus saprophyticus [45] | \nFe3O4-TiO2 core/shell magnetic NPs | \nThe survival ratio [%] of bacteria decreased from 79.15 to 0.51%. | \n
\nStreptococcus pyogenes[57] | \nFe3O4-TiO2 core/shell magnetic NPs | \nThe survival ratio [%] of bacteria decreased from 82.87 to 4.45%. | \n
\nEscherichia coli [46] | \nTiO2 nanotubes ~ 20 nm | \n97.53% of reduction | \n
\nStaphylococcus aureus [46] | \nTiO2 nanotubes ~ 20 nm | \n99.94% of reduction | \n
\nBacillus subtilis [47] | \nTiO2 NPs co-doped with silver (19–39 nm) | \n1% Ag-N-TiO2 had the highest antibacterial activity with antibacterial diameter reduction of 22.8 mm | \n
\nMycobacterium smegmatis [48] | \nCu-doped TiO2NPs ~20 nm | \nThe percentage of inhibition was around 47% | \n
\nPseudomonas aeruginosa [49] | \nTiO2 NPs 10–25 nm | \nAlthough it was not completely euthanized, their survival was significantly inhibited. | \n
\nShewanella oneidensis MR-1 [48] | \nCu-doped TiO2 NPs ~20 nm | \nThe percentage of inhibition was around 11% | \n
TiO2 nanoparticles against different microorganisms and their antimicrobial activities.
The principal factors differentiating the antimicrobial activity between TiO2 NPs were their morphology, crystal nature, and size. According to López de Dicastillo et al. [11], hollow TiO2 nanotubes presented interesting antimicrobial reduction thanks to the enhancement of specific surface area. This fact can be explained by the nature of titanium dioxide, and one of the main mechanisms of its action is through the generation of reactive oxygen species (ROS) on its surface during the process of photocatalysis when it exposed to light at an appropriate wavelength. It is important to highlight that some research works have evidenced antimicrobial activity of TiO2 NPs increased when they were irradiated with UV-A light due to the photocatalytic nature of this oxide. The time of irradiation varied between 20 min [45] and 3 hours [50].
\nTitanium dioxide nanoparticles (TiO2 NPs) are one of the most studied materials in the area of antimicrobial applications due to its particular abilities, such as bactericidal photocatalytic activity, safety, and self-cleaning properties. The mechanism referred to the antimicrobial action of TiO2 is commonly associated to reactive oxygen species (ROS) with high oxidative potentials produced under band-gap irradiation photo-induces charge in the presence of O2 [51]. ROS affect bacterial cells by different mechanisms leading to their death. Antimicrobial substances with broad spectrum activity against microorganisms (Gram-negative and Gram-positive bacteria and fungi) are of particular importance to overcome the MDR (multidrug resistance) generated by traditional antibiotic site-specific.
\nThe main photocatalytic characteristic of TiO2 is a wide band gap of 3.2 eV, which can trigger the generation of high-energy electron–hole pair under UV-A light with wavelength of 385 nm or lower [52]. As mentioned above for bulk powder, TiO2 NPs have the same mechanism based on the ROS generation with the advantage of being at nanoscale. This nanoscale nature implies an important increase of surface area-to-volume ratio that provides maximum contact with environment water and oxygen [53] and a minimal size, which can easily penetrate the cell wall and cell membrane, enabling the increase of the intracellular oxidative damage.
\nBacteria have enzymatic antioxidant defense systems like catalases and superoxide dismutase, in addition to natural antioxidants like ascorbic acid, carotene, and tocopherol, which inhibit lipid peroxidation or O-singlet and the effects of ROS radicals such as OH2˙− and OH˙. When those systems are exceeded, a set of redox reactions can lead to the death cell by the alteration of different essential structures (cell wall, cell membrane, DNA, etc.) and metabolism routes [54]. In the following sections, several ways that cellular structures were affected in the presence of TiO2 NPs will be described. In order to understand the genome responses of bacteria to TiO2-photocatalysis, some biological approaches related to expression of genes encoding to defense and repair mechanism of microorganism will explained below. Different mechanisms and processes of antimicrobial activity of TiO2 NPs are represented as a global scheme in Figure 1.
\nScheme of main antimicrobial activity-based processes.
ROS are responsible for the damage by oxidation of many organic structures of microorganisms. One of them is the cell wall, which is the first defense barrier against any injury from the environment, thus being the first affected by oxidative damage. Depending on the type of microorganism, the cell wall will have different composition; that is, in fungi and yeast, cell walls are mainly composed of chitin and polysaccharides [55], Gram-positive bacteria contain many layers of peptidoglycan and teichoic acid, and Gram-negative bacteria present a thin layer of peptidoglycan surrounded by a secondary lipid membrane reinforced with transmembrane lipopolysaccharides and lipoproteins [56]. Thus, the effect of TiO2 NPs will be slightly different depending type of microorganism.
\nIt has been studied that the composition of the cell wall in Pichia pastoris (yeast) changed in the presence of TiO2, increasing the chitin content in response to the ROS effects [57]. The cell wall of Escherichia coli (Gram-negative) composed of lipo-polysaccharide, phosphatidyl-ethanolamine, and peptidoglycan has been reported to be sensitive to the peroxidation caused by TiO2 [58]. The damage can be quantified by assessing the production of malondialdehyde (MDA), which is a biomarker of lipid peroxidation, or through ATR-FTIR of the supernatant of cell culture, which evidenced the way that porins and proteins on the outer membrane were affected, probably as a result of greater exposure to the surface of TiO2 [59]. In fungi, the release of OH˙ captured hydrogen atoms from sugar subunits of polysaccharides, which composed the cell wall, leading to the cleavage of polysaccharide chain and the exposition of cell membrane [60].
\nIn terms of genetic issues, there is evidence that the bacteria change the level expression of certain genes encoding for proteins involved in lipopolysaccharide and peptidoglycan metabolism, pilus biosynthesis, and protein insertion related to the cell wall which values were lower-expressed after exposition to TiO2 NPs [61].
\nThe second usual cellular target of most of antibiotics is the cell membrane mainly composed by phospholipids, which grant the cell a non-rigid cover, permeability, and protection. Most of the studies with TiO2 NPs have been focused to the loss of membrane integrity caused by oxidation of phospholipids due to ROS such hydroxyl radicals and hydrogen peroxide [62, 63], which led to an increase in the membrane fluidity, leakage of cellular content, and eventually cell lysis.
\nGram-positive bacteria present only one membrane protected by many layers of peptidoglycan, whereas Gram-negative bacteria are composed by two membranes, inner and outer, and a thin layer of peptidoglycan between them. The outer membrane is exposed, thus, more liable to mechanical breakage due to the lack of peptidoglycan protective cover, like in Gram-positive bacteria [64]. Some studies have demonstrated a better antimicrobial performance of TiO2 NPs against Gram-positive bacteria [65] while others reported that Gram-negative bacteria were more resistant [66, 67]. It can be concluded that the bacterial inactivation effectiveness depends mainly on the resistant capacity of cell wall structures and the damage level of ROS generation [68].
\nIn contrast with the lower expression of genes related to the cell wall seen before, the level expression of genes encoding for enzymes involved in metabolism of lipid essential for the cell membrane structure, are over-expressed [61]. It would be concluded that cells compensate the initial cell wall damage by reinforcing the second defense barrier, the cell membrane, in a way to provide support against the oxidation produced by ROS.
\nIn fungi, the biocidal effect is not quite different. In the presence of TiO2 NPs and UV light, hydroxyl radicals, hydrogen peroxide, and superoxide anions initially promote oxidation of the membrane, leading to an unbalance in the cell permeability, even decomposition of cell walls [69]. This oxidation can inhibit cell respiration by affecting intracellular membranes in mitochondria. Studies have demonstrated biocidal effects on Penicillium expansum [70], but there is still research on other strains.
\nBeyond the relatively well-studied initial lipoperoxidation attack of TiO2 NPs on the outer/inner cell membrane of the microorganism, specific mechanisms are still aimed of being solved.
\nAs the oxidative damage generates lipoperoxidation of cell membranes due to their lipid nature, the respiratory chain, which takes place in the double-membrane mitochondria, is also affected. This organelle is a natural source of ROS in aerobic metabolism because superoxide anions are produced in the electron transfer respiratory chain process. Mitochondria can control this fact by converting them into H2O2 by superoxide dismutase (SOD), and finally into water by glutathione peroxidase and catalase [71]. The presence of TiO2 NPs increases the production of ROS at levels that this enzymatic defense mechanism cannot attenuate the damage, even a dysregulation in electron transfer through the mitochondrial respiratory chain implies an increase in ROS generation [72].
\nThe genetic approaches have indicated that changes in level expression in genes related to the energy production in mitochondria prioritize the most efficient pathway to uptake oxygen, which is through ubiquinol coenzyme [61]. This coenzyme presented a higher capacity to exchange electrons, while the coenzyme-independent oxygen uptake pathways were expressed at lower level.
\nDamage at molecular level in DNA affects all regulatory microorganism metabolism, replication, transcription, and cell division. DNA is particularly sensitive to oxidative damage because oxygen radicals, specially OH˙ produced by Fenton reaction [73], may attack the sugar-phosphate or the nucleobases and cause saccharide fragmentation aimed to the strand break [74].
\nDNA strand modifications are more lethal than base modifications (punctual mutation). Mitochondrial DNA is more vulnerable to oxidative damage than nuclear DNA because it is closer to a major cellular ROS source [75].
\nBesides the enzymatic detoxification system (SOD, glutathione and catalase), DNA injuries are covered by a set of structures related to post-translational modification, protein turnover, chaperones (related to folding), DNA replication and repair, which are significantly over-expressed in the presence of TiO2 NPs [61].
\nIron is an essential ion for cell growth and survival, but it can turn potentially toxic if some malfunction in homeostatic regulation occurs (i.e., Fenton reaction that produces ROS). Bacteria are able to regulate iron concentration in order to maintain it in a physiological range [76]. This regulation involves directly siderophores to active transport of iron in cell [77], whose coding genes related to siderophore synthesis and iron transport protein are significantly lower-expressed in the presence of TiO2 NPs, decreasing the ability to assimilate and transport it, leading to cell death [61]. The loss of homeostasis regulation was confirmed by ICP-MS analysis, which revealed that the presence of TiO2 NPs significantly reduced the cellular iron level in Pseudomonas brassicacearum, directly proportional to the cell viability [78].
\nRegarding the functions related to Pi group (PO4\n3−) uptake, major differences were found in the expression of set of genes contained in Pho regulon, which were significantly lower when compared to the control [61]. The Pho regulon is a regulatory network in bacteria, yeast, plants, and animals, related to assimilation of inorganic phosphate, merely available in nature, and essential to nutritional cross-talk, secondary metabolite production, and pathogenesis [79].
\nThis suggested that the microorganisms were highly deficient in phosphorus uptake and metabolism in the presence of TiO2 NPs. It should be also noted that the Pho regulon has been reported to regulate biofilm synthesis capacity and pathogenicity [80].
\nTiO2 NPs can directly oxidize components of cell signaling pathways and even change the gene expression by interfering with transcription factors [81]. There is evidence to confirm the interference of TiO2 NPs in biosynthesis pathways of signaling molecules that bind lipopolysaccharide, stabilize and protect the cell wall against oxidative damage [82]. Moreover, a significant decrease in the synthesis of quorum-sensing signal molecule related to functions like pathogenesis and biofilm development was observed. This was corroborated through Scanning Electron Microscopy (SEM) images of bacteria (P. aeruginosa) growth in the presence of TiO2 NPs without UV irradiation. Cells appeared mainly non-aggregated and dispersed in the substratum, compared with controls without NPs where cells were mainly aggregated by lateral contact. This suggested that TiO2 NPs not only affected microorganisms by oxidative damage, but also bacteria aggregation and biofilm formation, which directly influenced in pathogenicity [83].
\nIn plants and algae, ROS can act as signaling intermediates in the process of transcription factor controlling stress response by H2O2, which is activated by a GSH peroxidase, and not by peroxides directly. But there is still lack of research in this area [84].
\nThe control of morphology and crystal structure of TiO2 NPs is the most important factor to enhance their antimicrobial activity. The appropriate design based on desirable surface properties given by shaped nanoparticles can improve effectiveness that is also dependent on the type of bacteria. The route of synthesis of TiO2 NPs is also a key factor. Recent works have revealed more eco-friendly synthesis methods, principally based on plant-based compounds and microorganisms, such as bacteria and fungus. Antimicrobial activity of different TiO2 NPs against Gram-positive and Gram-negative bacteria including antibiotic-resistant strains has been confirmed in different works.
\nSpecific studies on antimicrobial mechanisms have evidenced that microorganism exposed to photocatalytic TiO2 NPs exhibited cell inactivation at regulatory network and signaling levels, an important decrease in the activity of respiratory chain, and inhibition in the ability to assimilate and transport iron and phosphorous. These processes with the extensive cell wall and membrane alterations were the main factors that explain the biocidal activity of TiO2 NPs.
\nThe authors acknowledge the financial support of CONICYT through the Project Fondecyt Regular 1170624 and “Programa de Financiamiento Basal para Centros Científicos y Tecnológicos de Excelencia” Project FB0807, and CORFO Project 17CONTEC-8367.
\nThe authors declare no conflict of interest.
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\\n\\nDISCLAIMER: Neither the CC BY 3.0 license, nor any other license IntechOpen currently uses or has used before, applies to figures and tables reproduced from other works, as they may be subject to different terms of reuse. In such cases, if the copyright holder is not noted in the source of a figure or table, it is the responsibility of the User to investigate and determine the exact copyright status of any information utilised. Users requiring assistance in that regard are welcome to send an inquiry to permissions@intechopen.com.
\\n\\nAll rights to Books and all other compilations published on the IntechOpen platform and in print are reserved by IntechOpen.
\\n\\nThe copyright to Books and other compilations is subject to separate copyright from those that exist in the included Works.
\\n\\nAll Long Form Monographs/Compacts are licensed under the Creative Commons Attribution-NonCommercial 4.0 International (CC BY-NC 4.0) license granted to all others.
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\\n\\nAll Video Lectures under IntechOpen's production are subject to copyright and are property of IntechOpen, unless defined otherwise, and are licensed under the Attribution-NonCommercial-NoDerivatives 4.0 International (CC BY-NC-ND 4.0) license. This grants all others the right to:
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\\n\\nPolicy last updated: 2016-06-08
\\n"}]'},components:[{type:"htmlEditorComponent",content:'Copyright is the term used to describe the rights related to the publication and distribution of original Works. Most importantly from a publisher's perspective, copyright governs how Authors, publishers and the general public can use, publish, and distribute publications.
\n\nIntechOpen only publishes manuscripts for which it has publishing rights. This is governed by a publication agreement between the Author and IntechOpen. This agreement is accepted by the Author when the manuscript is submitted and deals with both the rights of the publisher and Author, as well as any obligations concerning a particular manuscript. However, in accepting this agreement, Authors continue to retain significant rights to use and share their publications.
\n\nHOW COPYRIGHT WORKS WITH OPEN ACCESS LICENSES?
\n\nAgreement samples are listed here for the convenience of prospective Authors:
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\n\nWork - a Chapter, including Conference Papers, and any and all text, graphics, images and/or other materials forming part of or accompanying the Chapter/Conference Paper.
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\n\nIntechOpen - Registered publisher with office at 5 Princes Gate Court, London, SW7 2QJ - UNITED KINGDOM
\n\nIntechOpen platform - IntechOpen website www.intechopen.com whose main purpose is to host Monographs in the format of Book Chapters, Long Form Monographs, Compacts, Conference Proceedings and Videos.
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\n\nTERMS
\n\nAll Works published on the IntechOpen platform and in print are licensed under a Creative Commons Attribution 3.0 Unported License, a license which allows for the broadest possible reuse of published material.
\n\nCopyright on the individual Works belongs to the specific Author, subject to an agreement with IntechOpen. The Creative Common license is granted to all others to:
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\n\nAll Works are published under the CC BY 3.0 license. However, please note that book Chapters may fall under a different CC license, depending on their publication date as indicated in the table below:
\n\n\n\n
LICENSE | \n\t\t\tUSED FROM - | \n\t\t\tUP TO - | \n\t\t
\n\t\t\t Creative Commons Attribution-NonCommercial-ShareAlike 3.0 Unported (CC BY-NC-SA 3.0) \n\t\t\t | \n\t\t\t\n\t\t\t 1 July 2005 (2005-07-01) \n\t\t\t | \n\t\t\t\n\t\t\t 3 October 2011 (2011-10-03) \n\t\t\t | \n\t\t
Creative Commons Attribution 3.0 Unported (CC BY 3.0) | \n\t\t\t\n\t\t\t 5 October 2011 (2011-10-05) \n\t\t\t | \n\t\t\tCurrently | \n\t\t
The CC BY 3.0 license permits Works to be freely shared in any medium or format, as well as the reuse and adaptation of the original contents of Works (e.g. figures and tables created by the Authors), as long as the source Work is cited and its Authors are acknowledged in the following manner:
\n\nContent reuse:
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\n\nReposting & sharing:
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\n\nRepublishing – More about Attribution Policy can be found here.
\n\nThe same principles apply to Works published under the CC BY-NC-SA 3.0 license, with the caveats that (1) the content may not be used for commercial purposes, and (2) derivative works building on this content must be distributed under the same license. The restrictions contained in these license terms may, however, be waived by the copyright holder(s). Users wishing to circumvent any of the license terms are required to obtain explicit permission to do so from the copyright holder(s).
\n\nDISCLAIMER: Neither the CC BY 3.0 license, nor any other license IntechOpen currently uses or has used before, applies to figures and tables reproduced from other works, as they may be subject to different terms of reuse. In such cases, if the copyright holder is not noted in the source of a figure or table, it is the responsibility of the User to investigate and determine the exact copyright status of any information utilised. Users requiring assistance in that regard are welcome to send an inquiry to permissions@intechopen.com.
\n\nAll rights to Books and all other compilations published on the IntechOpen platform and in print are reserved by IntechOpen.
\n\nThe copyright to Books and other compilations is subject to separate copyright from those that exist in the included Works.
\n\nAll Long Form Monographs/Compacts are licensed under the Creative Commons Attribution-NonCommercial 4.0 International (CC BY-NC 4.0) license granted to all others.
\n\nCopyright to the individual Works (Chapters) belongs to their specific Authors, subject to an agreement with IntechOpen and the Creative Common license granted to all others to:
\n\nUnder the following terms:
\n\nThere must be an Attribution, giving appropriate credit, provision of a link to the license, and indication if any changes were made.
\n\nNonCommercial - The use of the material for commercial purposes is prohibited. Commercial rights are reserved to IntechOpen or its licensees.
\n\nNo additional restrictions that apply legal terms or technological measures that restrict others from doing anything the license permits are allowed.
\n\nThe CC BY-NC 4.0 license permits Works to be freely shared in any medium or format, as well as reuse and adaptation of the original contents of Works (e.g. figures and tables created by the Authors), as long as it is not used for commercial purposes. The source Work must be cited and its Authors acknowledged in the following manner:
\n\nContent reuse:
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\n\nReposting & sharing:
\n\nOriginally published in {full citation}. Available from: {DOI}
\n\nAll Book cover design elements, as well as Video image graphics are subject to copyright by IntechOpen.
\n\nEvery reproduction of a front cover image must be accompanied by an appropriate Copyright Notice displayed adjacent to the image. The exact Copyright Notice depends on who the Author of a particular cover image is. Users wishing to reproduce cover images should contact permissions@intechopen.com.
\n\nAll Video Lectures under IntechOpen's production are subject to copyright and are property of IntechOpen, unless defined otherwise, and are licensed under the Attribution-NonCommercial-NoDerivatives 4.0 International (CC BY-NC-ND 4.0) license. This grants all others the right to:
\n\nShare — copy and redistribute the material in any medium or format
\n\nUnder the following terms:
\n\nUsers wishing to repost and share the Video Lectures are welcome to do so as long as they acknowledge the source in the following manner:
\n\n© {year} IntechOpen. Published under CC BY-NC-ND 4.0 license. Available from: {DOI}
\n\nUsers wishing to reuse, modify, or adapt the Video Lectures in a way not permitted by the license are welcome to contact us at permissions@intechopen.com to discuss waiving particular license terms.
\n\nAll software used on the IntechOpen platform, any used during the publishing process, and the copyright in the code constituting such software, is the property of IntechOpen or its software suppliers. As such, it may not be downloaded or copied without permission.
\n\nUnless otherwise indicated, all IntechOpen websites are the property of IntechOpen.
\n\nAll content included on IntechOpen Websites not forming part of contributed materials (such as text, images, logos, graphics, design elements, videos, sounds, pictures, trademarks, etc.), are subject to copyright and are property of, or licensed to, IntechOpen. Any other use, including the reproduction, modification, distribution, transmission, republication, display, or performance of the content on this site is strictly prohibited.
\n\nPolicy last updated: 2016-06-08
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