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Nanocomposite Materials Synthesis, Properties and Applications Jyotishkumar Parameswaranpillai, Nishar Hameed, Thomas Kurian, Yingfeng Yu

Synthesis of Nanomaterials

Publication details https://www.routledgehandbooks.com/doi/10.1201/9781315372310-3 A. Ramazani S.A., Y. Tamsilian, M. Shaban Published online on: 29 Jun 2016

How to cite :- A. Ramazani S.A., Y. Tamsilian, M. Shaban. 29 Jun 2016, Synthesis of Nanomaterials from: Nanocomposite Materials, Synthesis, Properties and Applications CRC Press Accessed on: 28 Sep 2021 https://www.routledgehandbooks.com/doi/10.1201/9781315372310-3

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3.3.1 On C Th 3.4.2 3.4.1 Tw 3.3.2 3.3.3 3.2.2 3.2.3 3.2.1 Ze Introduction 3 onclusion ro-Dimensional Materials...... ro-Dimensional ree-Dimensional Materials ree-Dimensional o-Dimensional Nanomaterials o-Dimensional e-Dimensional Nanomaterials e-Dimensional

...... 3.3.1.3 3.3.1.2 3.2.3.3 3.3.1.1 Sy 3.4.2.2 3.4.2.1 N 3.4.1.3 3.4.1.2 3.4.1.1 Sy 3.3.3.3 3.3.3.2 3.3.3.1 Sy 3.3.2.4 3.3.2.3 3.3.2.2 3.3.2.1 Sy 3.3.1.7 3.3.1.6 3.3.1.5 3.2.3.1 3.3.1.4 3.2.1.2 3.2.3.2 Sy Sy 3.2.1.1 Sy A. RamazaniA. S.A., Y. Tamsilian, and M. Shaban Nanomaterials of Synthesis anocoatings nthesis of Nanofilms nthesis of Nanowires nthesis of Nanorods nthesis of Nanotubes nthesis of Nanoparticles Dots nthesis of Quantum Nanoclusters...... nthesis of Metal ......

Gr Hy Mo Che Che Mi El Su Va Me Se Si Bo Ar La Mi Mo El Che Sy Sy Sy So Mi mple Hydrothermal Method mple Hydrothermal ectrophoresis-Assisted Electroless Deposition Growth Nanotube Field-Directed ectric ed-Mediated and Seedless Methods Seedless and ed-Mediated bdiffraction Laser Synthesis Laser bdiffraction nochemical Synthesis...... nochemical nthesis of Polymeric Nanoparticles nthesis of Ceramic Nanoparticles nthesis of Ceramic Nanoparticle nthesis of Metal ser Ablationser Method aphene-Based Nanocoatings c Discharge Method c Discharge por Phase Synthesis Phase por ttom-Up Chemical Synthesis ttom-Up Chemical drothermal Method Combined with a Mild Ultrasonic aMild with Combined Method drothermal crowave Method Growth Heating crowave Method Heating crowave-Assisted Synthesis...... tal–Organic Chemical Vapor Chemical Deposition Method tal–Organic lecular Seeds Self Assembly Seeds lecular lecular Layerlecular Deposition mical Vapormical Deposition mical Bath Techniquemical Treatment Subsequent with Precipitation Thermal mical ...... 44 64 64 40 6 40 6 6 6 4 66 48 65 69 38 38 38 63 72 72 37 39 73 70 70 73 73 70 62 62 62 43 71 71 71 71 75 75 74 61 0 0 0 0 6 Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 bers, wires, and rods, (c) 2D films, plates, and networks, and (c)networks, and rods, (d) nanomaterials. and 3D plates, wires, films, 2D bers, molecular scale [4]. scale molecular 3.2 Figure shows nanomaterials. physical approachesobtain to chemical and or atomic the from produced could be which nanomaterials in method approach is apopular cal using physical Bottom-up or chemi techniques. materials original dimensionof the the reducing to [2,3]. bottom-up approaches: and top-down two into main Top-downcategorized approach refers materials) (see 3.1).polycrystalline Figure powders, fibrous, including materials, sions porous nanocomposites, multilayer, nanoscale in and nanolayers,and nanocoatings),such nanofilms, as dimen and no (confined (4)three-dimensional nanowires), and nanorods, tubes, (3) (confinedin nanoscale dimensions one two-dimensional nanoparticles),and (2) (confinedsuchas nano two in nanoscale dimensions one-dimensional [1]: (1)dots, suchas in nanoscale dimensionsclusters, quantum (confinedall zero-dimensional four sections in categorized are 100 1and nanometers, between dimensionsize Nanomaterials, 3.1 38 FIGURE 3.1FIGURE uniform technique, this synthesis. solution In solid, facesand liquid, of the through existing phases inter place atthe taking mechanism separation and transfer approach phase is using ageneral This [5–8]. features molecule-like and chemical, electrical, due optical, to years recent of in attention (NPs). deal agreat nanoparticles have They and atoms metal attracted between cover distance the that anew of of category anumber nanomaterials are atoms nanoclusters(NCs)Metal containing MATERIALS ERO-DIMENSIONAL s 3.2.1 3.2 In general, several methods that have been mostly used for preparation of nanomaterials are are have that several mostly of general, for methods nanomaterials used been In preparation Wang’s such noble [9]. as approach for a general metals used synthesis of group nanocrystals

INTRODUCTION Z y n

thesis ( S ee color insert. ee

(c) (a) of M etal N ) Classification of nanomaterials (b) and (a)clusters, 0Dnanofi spheres 1D nanomaterials of ) Classification a n o c lusters (d (b ) ) Nanocomposite Materials Nanocomposite - - - - - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 Journal of Nanomaterials of V. Journal Padavettan, I. Rahman, serum albumin (BSA) as the reducing agent and the stabilizer which is reacted with HAuCl with which is reacted (BSA) stabilizer agent the reducing albumin and the as serum for 6 microwave-assistedstep MWI with technique uniform. is rapid and method conventional to this is that comparison heating in MWI cost-effectiveness and environment-friendly features, [15–17]. advantage of main the Furthermore, heating, such low as superiorities of several uniform consumption, because energy outstanding rials the synthesis is one methods of nanomate mostfor of significant the Microwave (MWI) irradiation 3.2.1.1 [14]. by techniques controlled different could be synthesis processes conditionsreaction and the Also of nanomaterial. kind of for this preparation stabilizers agents reducing and appropriate are AuNCs. precursors Consequently, luminescent small synthesize to applied be thiol-containing a strong reducing agenta strong reducing such NaBH as (AuNPs)tion Au to nanoparticles Au have atoms the tendency because aggregation to when agreat applied for preparation of uniform luminescent AuNCs with high quality. AuNCs high with luminescent of forapplied uniform preparation have 2 under size aparticle goldluminescent nanoclusters(AuNCs) which nanomaterials anew of category luminescent are stability. chemical that note to photophysical It is astonishing interesting and outstanding features, facile synthesis, nontoxicity, such their as due some to interest properties good received particular Au Pd, and NCsnanoclusters such Ag, [10–12], Cu, as Pt, gold but them, between nanoclustershave situations. or atmospheric hydrothermal under of 20–200°C temperatures atvarious ethanol via reduction of using were noble the ions produced metal or nanocrystals, dots, noble quantum metal 3.2 FIGURE and uniform heating; thus, it can speed up the synthesis of up nanomaterials. the speed it thus, heating; can uniform and power [21,22]. irradiation the by controlling minutes microwave-assisted The provides method fast by coworkers Liu and was reported [20]. some to time reaction we addition, the In could reduce of polyelectrolyte, presence acommon (PMAA-Na), salt the acid sodium in rescent polymethacrylic AuNCs [19]. (5 cycle per lysozyme-directed heating the power min the with prepare to of W) 90 using microwaves.processes et al. eight applied Chen cycles For instance, of consecutive microwave [18]. temperature the maintain to heating of alternative direct an as 37°C MWI via simple conditions (pH was particularly reaction under the method, Au this precursor. In Synthesis of Nanomaterials Synthesis Yue coworkers extremely and fluorescent prepared 16 containing AuNCs gold using atoms a one- It is well known that sodium Itborohydride (NaBH is well sodium that known Up now, to synthesis of considerable several atthe made noble attempts researchers metal many A very rapid and strong microwave-assisted rapidA very and synthesis of fluo Ag high nanoclusters with green 1 to several from hours reduced be can time reaction Moreover, the method this in Microwave-Assisted Synthesis Microwave-Assisted

( See color insert. See Ph ysical me nm and contain about 100 gold contain and [13]. atoms nm Various have methods been ) Physical and chemical approach to produce nanomaterials. (Adapted from from (Adapted nanomaterials. produce to approach chemical ) Physical and th od 4 is utilized. Therefore, partially weak reducing agents reducing could weak Therefore, partially is utilized. , 1, 2012, 1–15.) 4 ) is used normally for reduction of normally HAuCl ) is used h with powerh with of 700 Chemical meth W. bovine utilized They od h with modified modified h with 12) at = 12) 4 4 as an an as solu 39 - - - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 was exposed to ultrasonic irradiation (50 irradiation was exposed ultrasonic to condition;mixture agentfinally, agent reducing this the in and where BSA astabilizing as acted 0.50 then vigorous stirring, rescent AuNCs [14]. preparing AuNCs, for example:preparing 2 less than Ag 3.3c nanoclusters resulting are Figure e, the in and illustrated Figure 3.3a fortion 2 Ar was with purged reagent best Ag produce nanoclusters to [25]. the as solu The reported whichbeen has PMAA, dark red (180 red dark nanoparticles. for avoid Agylate stability afford nanoclustersand groups of nanoclusterslarge to growth extra is apreferablePMAA capping agent for synthesisof Ag nanoclusters [26,27]. carbox charged The carboxylic which acid groups, have tendency silver to agreat ions silver and therefore, surfaces; contains agent. PMAA lyte, polymethylacrylic It that should noted acid (PMAA), be astabilizer as gation [25] Xu of asimple et al. Ag Ag nanoclusters formlarge to used nanoparticles. polyelectro acid units) Ag to study, solution. this PMAA of ratio aqueous molar carboxylate In (from the groups methacrylic the with aqueous AgNO aqueous with briefly, method, this 250 In synthesis method. water-soluble silver (AgNCs) nanoparticles by Liu [23]. et al. onochemical Synthesis [23]. purity high with NPs it uniform ditions, monosize and and produces con reaction the controlto easy advantages suchas significant harmless, reaction, has fast method This approach for nanomaterials. synthesizing important additional is an method sonochemical The 3.2.1.2 40 rial with diameters in the range of range 1–12 the in diameters with (10–50 nanometers rial atoms). (smaller Atsizes such small than of mate asemiconducting or nanocrystals particles spherical and small are semiconductors talline - bioanalysis, colloidal nanocrys in attention received optoelectronics. These bioimaging, great and have that (QDs) dots luminescence high very Semiconductor with quantum nanoparticles are s 3.2.2 molecular-weight cutoffs (MWCO) dialysis bag. fordence formationof AgNCs the [24].dialysis AgNCsDa via solution The using 7000 is purified color the colloid of the period, solutionthis colorless from changed yellow, to providing evi clear in this figure, figure, Au this in • of for used synthesismentioned above, methods be may also addition the to In techniques other • To solution Ag nanoclusters, afresh synthesize of AgNO • In this work, the BSA-stabilized AgNCs were synthesized by a facile, fast, green sonochemical work, BSA-stabilized AgNCs by sonochemical the were afacile, this synthesized fast, green In following, highly the example byIn method an of sonochemical preparing explain wethe will Sonochemical reduction ofSonochemical Ag illustrates a schematic of different methods for preparation of for 3.4AuNCs. a schematic of methods preparation Figure it different As is illustrates shown

molecules, such as dendrimers, thiols, and Au and thiols, molecules, such dendrimers, as E P agent for preparation of AuNCs from Au(III) precursors. agent of for AuNCsAu(III) from preparation M solution to a microemulsion containing methanol, thiolates, and HAuCl and thiolates, methanol, solution amicroemulsioncontaining to stirring [29–32]. The microemulsion method will be explained in detail in the next the section. in [29–32]. detail in explained be stirring will microemulsionmethod The

hotoreductive synthesis hotoreductive tching-based technique tching-based icroemulsion method icroemulsion S y n , under sonication, the first colorless first sonication, the , under solution slowly (90 changesto pink thesis

m in). Ag producing nanoclusters have The (Figure 3.3b). fluorescence ahigh As it is + 3 was 1:1. pH was the adjusted 4.5 to due Then coil formationof to compacted +

precursors and appropriate stabilizer agents are essential for essential synthesisof agents fluo are stabilizer appropriate and precursors of 3 solution (1 Q ua n

m tum : In this method, AuNCs is obtained by adding aqueous NaBH aqueous by adding AuNCs is obtained method, this : In L, mol/L NaOH was added to the solution NaOH the to was added adjust to mol/L pH 12, to L, the : In this method, the AuNPs are etched with extra amounts of amounts extra with etched are AuNPs the method, this : In

: In this technique, ultraviolet technique, lightis employed this : In areducing as h a

m + D needs the use of use atemplate the or capping agent avoid to needs aggre the L, 100 L, nd then sonicated for a different period of time. As shown of As fortime. in period sonicated adifferent nd then ots

m

W mol/L), reacting at ambient temperature for 5 mol/L), at ambient temperature reacting /cm

m g of BSA was dissolved 9 in 2 ) under low temperature (15°C) low) under temperature for 4 3 + ions to form the AuNCs ions [28]. formthe to 3 as Ag as + precursor was mixed with an an with was mixed precursor Nanocomposite Materials Nanocomposite

nm in diameter [25]. diameter in nm

m 4 L water and mixed mixed L water and under vigorous under

m in) then and

h

m . During . During in with with in 4

------Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 Trends in Analytical Chemistry Q. Song, Trends Analytical in containing PMAA and AgNO and PMAA containing FIGURE 3.4 FIGURE [35]. approaches synthetic well-established their CdTe/ZnS, and core/shell have CdSe/ZnS analogs, received most QDs among due attention to the confinement effects [33,34]. quantum to solids due exciton of dimensions bulk the from the differently act radius), Bohr nanocrystals these 3.3 FIGURE Synthesis of Nanomaterials Synthesis sters from different lengths of sonication: (c) of sonication: lengths different 60 from sters Chemical Society American nanoclusters, fluorescent of highly synthesis Sonochemical Suslick, S. Kenneth Xu Hangxun, from QDs have been prepared from a wide range of semiconductor materials. CdSe, CdTe, awide of range from semiconductor materials. QDs have their prepared and been (c)

300 Absorbance (a.u.) (a) Au

400 Cl ( ( See color insert. See See color insert. See – 4 , 4, 3209–3214. Society.) Chemical 2010 Copyright American Wa veleng 500 + 60 min th (nm) St 3 20 nm in different length of sonication time; TEM images of as prepared Ag nanoclu prepared of as images TEM time; of sonication length different in abilizers 600 ) Synthesis of gold nanoclusters (AuNCs). of gold) Synthesis nanoclusters Y. M. Cui, from (Adapted Zhao, ) (a) UV–vis spectra and (b) fluorescence emission spectra of the solution the of ) (a) spectra (b) emission and fluorescence UV–vis spectra (d )( , 57, 2014, 73–82.) 700 2 nm 120 min 150 min 180 min 10 min 20 min 30 min 45 min 60 min 90 min 0 min min, (d) min, 90 V 800 Photore igorous stirring Ultra Microwa incubate Fluorescence intensity (104 cps) sound duction 0 1 2 3 4 5 min, and (e) and min, 180 ve 400 (b 90 min ) 20 nm 500 Wa

e) Excitation spectrum veleng min. (Reprinted with permission permission with (Reprinted min. Fluorescenc 600 th (nm) 180 150 60 45 20 30 90 10 0 Au 120 NC e s 700 1 cm 180 min 20 nm 800 41 - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 flask is then adjusted at 300°C under 1 atm of argon. One milliliter of Me milliliter argon. One under 1atm of adjustedthen at 300°C flask is for 20 1 torr at vessel reaction 200°C to the in heating via purged and below of is dried TOPO [36]. grams Fifty solvents. (TOPO)phineoxide solutions solventscoordinating wereagents as known used stabilizer and S, Te Se, as and used respectively. sources, tri-noctylphos (TOP)- and tri-n-octylphosphine Mixed lation was dispersed in 25 in lation was dispersed Then floccu usingcentrifugation. thenseparated were and supernatant flocculate The crystallites. 20 adding and 1.5 from ranging of sizes aseries with nanoparticles CdSe time, aging on the Depending aged at230–260°C. and to raised gradually is temperature the and to 180°C. flask reaction the to is restored perature Heating at 440–460 feature absorption an with solution orange an reagents in of results rapid introduction these The its content is strongly stirred. box is rapidly and removed dry the vessel. reagent from reaction holding mixture the syringe The box. is removed heat The the dry from Two the in asyringe to added and mixed solutions then are solution or organic/aqueous solution interfaces. The hydrophilic chains are turned to the aqueous aqueous to the turned solution are or organic/aqueous solutionchains hydrophilic The interfaces. hydrophobic dissolvedand are asolvent, into chains, self-assemble typically they atair/aqueous following. the of is in explained micelles formation The micelles. reagents inside the the among occur reactions technique, this In perature. [40]. biomolecules colloid’s the both facilitate ligands forThese attachment of apoint solubility as act chemical and required. are coating organic functional hetero athick in nanocrystals or by these encapsulating ligands solutions using aqueous to modification therefore, transfer hydrophilic phase surface with 3.5 Figure [39]. in ofis illustrated TOP/TOPO method mary semiconducting, gaps whichwider (e.g., different band with has core CdS) and [37,38]. ZnS Asum spectrum. tion absorp optical of the by sharpening indicated as distribution size of the narrowing no further until size-selective dispersion and is repeated precipitation methanol with This nanocrystallites. CdSe of enriched precipitate a produce to centrifugation by flocculate separated were and supernatant ent solution. Subsequently, persists.Finally, opalescence dispersion until the to was added methanol flowing nanoparticles. CdSe ofTOP/TOPO capped free with methanol productthe followed TOPO.of 300 produces washing Afinal drying by vacuum andremove crystallites excessandthe TOP flocculate to supernatant the to was added methanol next the step, In 25 by centrifugation. additional was precipitate obtained a gray oxide, pyrolysis TOP/TOPO with precursors. of organometallic of 8%–11% distributions size and cores phosphine line phosphine/trioctyl of trioctyl using amixture [36] Bawendi crystal when of highly the QDsQDs with happened CdSe preparation reported group offluorescent highly colloidal preparation in breakthrough actual the suitable air-stable precursors, 42 ((TMS) of TOP in the dry box, 10.0 and dry of the TOP in The process for synthesizing of TOP/TOPO capped CdSe nanocrystallites is briefly outlined is briefly outlined nanocrystallites CdSe for of process TOP/TOPO capped synthesizing The Produced colloidal dispersion is purified by cooling to 60°C, above 60°C, to the meltingcooling by point TOPO,of colloidal dispersion is purified Produced When surfactants or block polymers, which generally contain two parts of head hydrophilic or block two parts polymers, which contain generally surfactants When prevalent is another approach offor microemulsion method QDs at tem room The preparation notsoluble; aqueous are procedure using this synthesized are QDs that It that should noted be native reagents coat to the was used CdSe suitable with joined organometallic method A similar 1-butanol anhydrous in subsequently formatranspar to dispersed are nanocrystals CdSe These Dimethylcadmium (Me Dimethylcadmium example method. an general exemplify to as following, the the report In this use we will using media of aqueous QDs in on preparation However, reports and efforts frequent are there 2 S), selenide (TOPSe), (TOPTe) trioctylphosphine telluride trioctylphosphine and were

m

in, and then it was purged with argon intermittently. The temperature of the reaction reaction of the it temperature intermittently. then argon was with purged The and in, m

L of anhydrous methanol, which results in the reversible the which in results L of methanol, anhydrous the nano flocculation of nm to 11.5 to nm

m 2

Cd) was utilized as the Cd precursor and bis(trimethylsily1)sulfide and precursor Cd the as Cd) was utilized nm in diameter are prepared. are diameter in nm L of anhydrous 1-butanol and a clear solution of nanocrystallites and and L of 1-butanol anhydrous solution aclear and of nanocrystallites

m L of 1.0

n - tem in by a sudden decrease accompanied is also This m.

M T OPSe stock solution 15.0 to is added Nanocomposite Materials Nanocomposite 2 Cd is added to 25.0 to is added Cd

m L of anhydrous

m L of TOP.

m m L g ------Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 Synthesis of Nanomaterials Synthesis The first group includesliquid-phasegroup approaches, the which in employsolvents. first processes The chemical major collections. (NPs)three classified forinto could be nanoparticles procedures preparation The s 3.2.3 of concentrations reagents [42]. and temperature, factors such time, reaction other as and concentration by surfactant adjusting of the we nanoparticles feature could control method, size, shape, and this In surfactant. of presence the the in could happen nucleation nanoparticles of the the growth hand, and bigger into other avoids aggregating or polymer the sizes. that On and growing particles surfactant the of presence a the in ions decomposition reagent or the of could occur metal a single organometallic example, reduction of an as the resources, of reaction suitable the initial needs emulsion technique (CTAB),bromide (SDS) dodecyl sulfate or sodium ortriton-X. such aerosol (AOT), OT as achieved be surfactant might using added cetyl trimethyl-ammonium solutions organic different in emulsion. the water Nanoscale dispersed droplets create to mixed are of for such long-chainattention liquids QDs, water alkane which as and two preparation immiscible employed reversebe received most The process the micelle of nanoparticles. for preparation the solventspolar of water. such could instead alcohol applied as could method microemulsion be The (oil-in-water emulsion) or inverse (water-in-oil microemulsions emulsion). some conditions, In other solution microemulsions solution organic aqueous of an an in normal which considered as could be solutions. aqueous of and organic Finally,dropletsliquid of fine amicroemulsionis adistribution interface atthe or block self-assemble they polymers remain amount, Surfactants micelles. create to a critical or block than polymers is higher surfactants solution. of concentration the the When 3.5 FIGURE 2006, 207–218.)2006, Chemistry Trends Analytical in A. Sanz-Medel, R. Pereiro, Costa-Fernandez, M. from fication. (Adapted modi (b) and (a) surface synthesis precursor. as of use CdO onthe Nanoparticle QD based of aluminescent TO

These micelles are thermodynamically stable and couldstable behave [41]. and “nanoreactors” as thermodynamically are micelles These micro The CdO HP (a)

+ + T (b PO hermomete A P ) O

QD y P r Nucl n

thesis 320°C Argon O ( P See color insert. See ea P tion Syr

TO T

of i CdS nge OP/T (in CH P- N

e QDs Se

a T OP n hermomete 4 ) oparti O

) Schematic illustration of a typical synthesis process and surface- and process synthesis of atypical illustration ) Schematic r Grow Ref –20 min 270°C Argon lu c les th x 12h

S yringe HS –C–COO H 2 re (at 15,000r disp QD QDs separation Purificatio H ersion inH 20°C re (at 15,000r pm) and disp QDs separation –10 mLCH n Dilution with Purification ersion inCH 2 O Wa pm) and Cl te QD r- 3 soluble QDs 4 P O QD P O P –S –C P P P H modification ­modification O 2 –CO TO TO O(–) PO P , 25, 43 - - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 of citrate stabilized AuNPs was based on reduction asingle-phase of was based HAuC1 AuNPs stabilized of citrate overall volume the solution of the water.color by synthesis adding maintaining changes, while This solution. boiling solution the into The is added solution. is kept citrate at100°C sodium until Then easiest silver is using produce approach to reduction of silver (AgNO nanoparticles nitrate thermally stableNPs,andeaseofsizeadjustment[48]. ligands [47]. The mainbenefitsofthistechniquearethe facile synthesis, uniformsizedistribution, intense reducingprecursor, suchassodiumborohydride, isaddedtocreate AuNPs cappedwiththiol tetraoctylammonium bromide,andthenanorganic thiolisadded.Finally, anextra amountofan First, goldprecursorisaddedtoanorganic solvent suchastoluenewithaphasetransferagentlike thiol ligands whichcouldattachtogoldintenselybecauseofthesoftpropertiesbothSand Au. rently astheBrust-Schiffrin method[47]. This methodemployed atwo-phase synthesisthatapplied size. in about nm 20 particles produced and medium aqueous an acid (HAuC1 [45]. astabilizer and agent reduction ofa reducing citrate such chlorauric citrate sodium Sodium as following.exemplify the it in by synthesis of AuNP the [44].tion of reactions synthesis for method most common is the AuNP, method Since this we will adjust- reduc plexes and the solutions, dilute have approaches in different start to advanced and been com colloidal dispersions is reduction of of metal metal preparation the in procedure general The 3.2.3.1.1 physical reduction, biological chemical and processes, are approaches. methods most prevalent The decades. recent most in attention the attracted Ag Au,ticles has and such Pt, as of nanopar noblePreparation metal modification. surface and characterization, facile preparation, due forto requests attention biomedical significant great gold havecially nanoparticles, obtained espe noble nanoparticles, These metal properties. optoelectronic unique and shape and size their gold, like silver,Noble nanoparticles have of platinum metal and because interest received great 3.2.3.1 method, whichhasnumerousadvantages. using solutionprocedures.Synthesisofnanoparticlesdispersedinasolvent isthemostpopular nanoparticles separately. First, we will emphasize the preparation of different sorts of nanoparticles following, wewillexplain alltheseapproachesbysomeexample ofmetal,ceramic,andpolymeric which isappliedforgrowing III–VQDs.Finally, thelastgroupisgas-phase preparation[43].Inthe which can be consider nanoparticles. An important example of this method is Stranski-Krastanow, this method,diffusion ofatomsorsmallclustersonappropriatesubstratesresultinislandcreation, or ligands. tion by surfactants agglomera- against stabilized could be nanoparticles colloids, produced in results which the in This 44 ticles via sodium citrate reagent in the pH of range reagent the 5.7–11.1.ticles in citrate sodium via Reduction silver of the (Ag salt (BSA),albumin polyvinyl alcohol (PVA), cellulose. and citrate and agents such poly(vinylpyrrolidone) as byited using stabilizers some common (PVP), serum bovine [49]. of presence a surfactant the in ethanol in Aggregation prohib ofprecursor could be Ag NPs quently used technique. In this technique, HAuC1 technique, this In quently technique. used like due to the rapid reduction rate of the precursor. of However, rapid due reduction the rate the to like lower in pH value, morphology of rod- and of spherical was a mix morphology ofpH, the at higher nanoparticles that is interesting pH value. reagent high in citrate of activity It the higher pH, due the to the by increasing increased Silver nanoparticles are an additional distinguished sample of chemical reduction technique. The The reduction technique. sample of chemical distinguished additional an Silver are nanoparticles One ofthemostimportantreportsonsynthesis AuNP was publishedin1994andisknown cur The formation of monosized AuNP is achieved of formation AuNP by monosized reduction of ofThe presence gold the the in salts The second group contains techniques based on surface growth under vacuum environments. In Dong’s morphology [50] of and group size silver work the on nanopar controlling reported

Synthesis of Metal Nanoparticle ofSynthesis Metal Chemical Reduction Chemical 4 ) at 100°C was established more than 50 years ago [46] and remains the most fre ago the 50 years [46]) at100°C more than remains was established and 4 dissolves water into asufficiently form to dilute Nanocomposite Materials Nanocomposite 4 by sodium citrate in in by citrate sodium 3 ) as Ag ) as + ) was + ------

Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 Synthesis of Nanomaterials Synthesis have received the most important attention in the field of plant-based syntheses methods. Extracts field the Extracts in attention methods. haveof plant-based syntheses received most important the Silverloids, coenzymes. and (Ag) phenolic terpenoids, compounds, gold and (Au) nanoparticles several agents water-soluble reducing comprise extracted - approach. The friendly alka like plants environmentally is an plant with extracts up. preparation easily scaled It that and should noted be andpressure, temperature room in advantages ofperform suchto as easy significant reaction, fast alot has method This synthesis process. agent ions asingle-step areducing green as in of metal fabrication is using for biomolecules method plants nanoparticle from interesting extracted Another 3.2.3.1.3 glycol on the ant [53]. viscosity well solvent of as the concentration the as mixture is reli technique ethylene this with ofand AuNPs rate glycol preparation agent. reducing The the as (250–400 acontinuous uses wave technique irradiation UV This of absence agent any reducing the [52]. in precursor salt metal of the solution irradiation due laser to (SDS) dodecyl sulfate sodium surfactant of presence [51]. the the in beam tions of 0.833–4.166 work, about 3 agent. this any reducing In solution precursor without of a metallic irradiation laser using the nanoparticles ofthesis metallic was suggestion report of for of syn a new this the technique purpose agents. main any reducing The without solution aqueous of an including asurfactant asilver and irradiation laser precursor direct [51]reported usingdistribution and shape awell-defined silver with size prepare to nanoparticles microwaves, and diation, which may agents. not reducing use For example, was a new technique - irra laser irradiation, UV are nanoparticles nobleprepare to metal methods significant Some other 3.2.3.1.2 pH values. different in morphology nanoparticles of 3.6 the produced Figure illustrates or polygon was mostly triangle slownanoparticles of the because precursor. of reduction the rate C 8.3, 6.1, Chemistry 5.7. Physical of and Journal et al., The Dong X. from (Adapted 3.6 FIGURE Photochemical reduction of gold precursor has also been applied to preparation of AuNPs [53]. of AuNPs preparation to applied been reduction of also gold has Photochemical precursor aqueous the in by is explained synthesis of method formation radicals of this mechanism The

Direct Laser Irradiation Laser Direct Biological Methods Biological Transmission electron images for the silver nanoparticles synthesized under pH of values 11.1, under synthesized silver for nanoparticles the images electron Transmission (a) pH=11.1 (c) pH=6.1 mM was placed in a closed spectrophotometric cuvette and irradiated by laser cuvette irradiated and aclosed was in placed spectrophotometric mM mL of an aqueous solution aqueous of an mL of- silver concentra with nitrate 100 nm 100 nm (d (b ) pH=5.7 ) pH=8.3 nm), PVP as the stabilizer agent, nm), stabilizer the as PVP 100 nm 100 nm , 113, 6573–6576.) 2009, 45 - - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3

materials, especially oxides and oxide-based hybrids. oxides oxide-based and especially materials, hybrid organic–inorganic of and colloidal dispersions of for preparation inorganic the procedure homogenous sol–gel situations. is and awet The moderate method form pure in chemical products of to its because ability materials ceramic and glass, silica, prepare to approach was used broadly by systematic adjustmentogy nanoparticles of condition reaction [61]. For sol–gel along the time, and morphol distribution, size, size advantagesthe particle somecontrol to easy suchas significant of because particles silica pure most sol–gel to prepare is widely the The process technique used 3.2.3.2.1 [60]. tions cytotoxicitybiological in their toward applica- decreasing features physical–chemical their increase followingthe [61]. reaction 3.7 Figure in illustrated . lorthosilicate (TEOS, Si(OC (TEOS, lorthosilicate presence of mineral acid (e.g., ofpresence mineral HCl) (e.g., or base NH 3.2.3.2 [59]. time reaction and perature, pH value, the precursor, tem metal of concentration and plant extract of extract, the nature the as roseusCatharanthus ing rapidly.ing such hydroxyapatite as ceramics Nanoscale (ZrO (HA), zirconia for develop application biomedical are materials, Recently, ceramic anew of group nanomaterials, [59]. method of silver, this with utes. nanoparticles Different have prepared metals gold, other been many and min is complete reaction within The temperature. atroom a solution precursor metal of the [58]. some physicochemical of the morphology techniques than and morphology asuitable with [57]. and size any contamination yield to applied could they be without alotsynthesis approaches, because but of also nanoparticles effect physicochemical [56] many to environmental able contrary decreased not only due their to [55]algae Biological valu of have nanoparticles. are preparation to applied synthesismethods been marine and plant extracts, fruits, biomolecules plant tissue,different their such microorganisms, as employed live plantto be extracts, [54]. can plants of nanoparticles for preparation the Up now, to of have plant species adifferent effectively addition been In nanoparticles. producing in applied 46

(TiO the sol–gel procedure, which leads to the fabrication of which using (Si(OR) the to alkoxides silica silicon leads sol–gelthe procedure, This procedure includes hydrolysis procedure This (Si(OR) alkoxides condensation of and metal The general reactions of TEOS make the formation of silica particles in the sol–gel procedure as as sol–gel the procedure in formationof particles silica the make of reactions TEOS general The In this method, the production rate and properties of nanoparticles depend on some depend factors such of nanoparticles properties and production rate the method, this In Several ( such plants tea as with agent extracted is easily mixed by the plant extracts, of nanoparticles preparation In even with size nanoparticles better produce really biosynthetic approaches can that It is claimed 2 ), and alumina (Al ), alumina and

S ynthesis of Ceramic Nanoparticles ynthesis So l–Gel Method l–Gel Si ≡− have for applied biosynthesis been the of nanoparticles. Si (O 2 CH O OH 25 → 3 ) have to new produce to methods attention synthetic received great 2 −+ H Alcohol condensatio  → )H 5 42 ) Water condensatio  4 Camellia sinensis Camellia + ) or inorganic precursors such as sodium silicate (Na silicate such sodium as precursors ) or inorganic H − OS OOS −≡ Hydrolysis  n ≡ n i ≡−−≡ Si → Si −− ), ( vera, neem aloe OS i(OC 3 ) as catalyst [62–64].) as flowchart Ageneral for OS iC 25 H) ≡+ iH 32 + OH 25 HO 2 O + CH

H Nanocomposite Materials Nanocomposite

Azadirachta indica 5 OH 2 ), (SiO silica

4 ) like tetraethy like ) 2 SiO 2 ), titania ), titania 3 ) in the the ) in ), and 4 ( ( ( ), is 3.2) 3.3) 3.1) ------Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 coprecipitation of Fe coprecipitation of Al of ethanol was prepared, then NH then was prepared, ethanol Synthesis of Nanomaterials Synthesis ganic precursor such AlCl as precursor ganic 100°C for h. 24 solution for gel agel. form to 30 was was added kept This temperature atroom work Al on producing by sol–gel the produced technique. been 3.7 FIGURE (AlCl far. thus chloride To includereported such aluminum inorganics as of group precursors ageneral [65] alcoholic medium an butoxide—in have [63,64], medium aqueous been secondary aluminum isopropylate ahydrolysis in [62], system acetonitrile nitrate—in and consisting of octanol aluminum magnetic core–shell Fe core–shell magnetic [67]. recording magnetic applications and functionalization. hydroxide reagent. precipitating by the using as ammonium tion technique coprecipita- conditions by chemical employed. the the under were prepared nanoparticles Magnetite which soluble is generally by is applied ofCoprecipitation method aprecipitate (CPT) materials, 3.2.3.2.2 values 1200°C. of and 1000°C temperature 100°C for 24 for at90°C 10slow stirring In this method, at first a solution atfirst method, of 0.1 this In Another example is usingAnother C well by biologicalIt the endured is therefore Different abiodegradable environment. material, has that implants in applied biomaterials inert as materials is one most of important the Alumina In the following, the In by coprecipitation exemplify method synthesis of we the functionalized will have field the particles in attention magnetic received of biomedical great micro-sized and Nano- by also surface of and reaction We temperature by the size changing could adjust particle the We synthesis of explain Al the 2 3 O ) and organics such as aluminum triisopropylate (C triisopropylate such aluminum organics as ) and 3 by sol–gel the method.

Coprecipitation Method Coprecipitation Flowchart of a typical sol–gel process. of atypical Flowchart h. The produced gels were calcined in a furnace for 2 afurnace gels in produced wereh. The calcined 2 + and Fe and 2 O 3 O 3 by the sol–gel technique using various precursors such as aluminum tri such aluminum as precursors using by sol–gel various the technique 4 @SiO 3 h. This gel was kept at room temperature for gel 24 wash. kept This temperature atroom 3 in the following. the in + precursor (molar solution. precursor 1:2) ratio A black precipitation alkali an in 3 9 solution (28%) agel. form to order in was It added was put under TEOS + H 2 nanoparticles [68]. Fe nanoparticles 2 21 O Colloidal silic AlO Bulk orsilic 3 by the sol–gel technique with an example an with of by inor sol–gel using the an technique Silica ge (c p H at owder 3 as a precursor, again first 0.1 first again aprecursor, as 2 alyst O +solven M AlCl * Hy * Dr * Ag l ) a drolysis andcondensation a ying andcalcin ing 3 in ethanol should be prepared. Then a28% Then NH should prepared. be ethanol in t 3 3 H O 7 atio 4 O) nanoparticles were produced by were the produced nanoparticles 3 n Al [66]Al have for used synthesis been h (heating rate 20°C/min), rate at h (heating M (C 3 H h and then dried at dried then h and h and then dried at dried then h and 7 O) 3 Al solutionAl in 47 - - 3

Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 3.2.3.3 3.8 Figure in reactor, illustrated polymerization as a and addition, generator,components: ammonia monomer particle acore an aGMA saturator, 3.2.3.2.3 24 1.0 (TEOS, silicate for at40°C 30 stirred solutiondispersion and nia this to was added will be discussed. be will of nextfor choice such the affect methods sections, preparation ofparticles In synthesis methods. consideredbe shouldto productproperties of application final as area and distribution, size particle size, of Anumber factors such polymerization. particle as emulsion, interfacial and surfactant-free fluidevaporation,technology, out, dialysis, salting supercritical miniemulsion,microemulsion, including solvent polymer produce to nanoparticles techniques various are polymers. There sized synthesis: for used (1) their are cedures of (2) monomers polymerization and dispersion of synthe Recently, have applications. numerous polymer considered in nanoparticles Two been pro main sca inorganic consisting of an nanoparticles, core–shell produce to [70]. shape spherical and structure powder mesoporous with dry to produce ability the has method gas phase this that should noted be filter. evaporate to solvent on were the the collected It nanoparticles resulting temperature high and with furnace the into directly were atomized liquidprecursors method, purity. this high and steps In [69].laser by ablation the produced of apulsed be with asolid also source can phase.gas Nanoparticles on homogeneousbased continuous nucleation, the in consequent condensation,coagulation and is purity. high with technique Generally, this material produce collection, and cheap particle simpleadvantages, production, low such fastand method, as particle fabrication green cost, conventional to the contrast many In solution has aerosol process nanoparticles. the methods, for simple is one most ofand methods synthesisof aerosol-basedmethod attractive the The vacuum in for at60°C 24 dried washed and with dence time in the reactor is about 2 reactor the in time dence formasolidto average polymervapor initiator. shell as The by addition of aerosol ammonia resi Subsequently, surface. nanoparticle inorganic polymerized monomer was chemically the coating washeterogeneous achieved condensationthe in ofvapor a supersaturation resulting on GMA the temperature, room to dropped temperature gas when saturator, the the monomer Behind at80°C. glycidylthe containing methacrylate (GMA) as organic the saturator through flow then passed was respectively, nebulization, and nitrogen gas by discharge cores spark particle-laden ganic the and continuous aerosol-based synthesis[71]. apolymer with a shell in nanoparticles of situ coating inorganic in about the article published an leaving aerosol filter. set-up, on the the Recently, directly were collected have et al. Poostforooshan nanoparticles, core–shell resulting the solvent. and avoids of Furthermore, surfactants need the and “flight” in was initiated polymerization the method, this In a continuous process. gas-phase t ultrasonic bath for bath 1 ultrasonic step, silica coated magnetic nanoparticles was synthesized, in this way, this in was synthesized, 1 nanoparticles magnetic step, coated silica EtOH. waterSubsequently, and deionized at100°C avacuum in for it was 24 dried of Fe of 48 o 80°C foro 80°C 2

In addition to the aforementioned methods, aerosol-polymerization is asimple aforementioned novel methods, addition the to and In method afew with process nanoparticles produces that aerosol-basedmethod is another Spray drying In this method, silver and silica nanoparticles were initially produced in the gas-phase as inor as gas-phase the in produced were silver initially nanoparticles method, silica and this In h . Finally, the silica coated magnetic nanoparticles were collected by a permanent magnet, then then magnet, by were apermanent collected nanoparticles magnetic . Finally, coated silica the 3 O 4

was obtained and then was constantly stirred for 1 stirred was constantly then and was obtained

S ynthesis of Polymeric Nanoparticles ynthesis A erosol Method erosol

h . The produced Fe produced . The

m

h at4 L) was added to the obtained mixture, and continuously stirred at 40°C for at 40°C continuously and stirred mixture, L) obtained to the was added 0°C was dispersed in 80 in was0°C dispersed 3

O m 4 in. The continuous experimental setup consists of four main consists of setup four main continuous experimental The in. was collected by a permanent magnet after washing with with washing after magnet by was a permanent collected

h. .

m L of methanol. Then, concentrated ammo concentrated L of Then, methanol.

h at room temperature and then heated heated then and temperature h atroom ff

old shell, polymeric in and m

Nanocomposite Materials Nanocomposite g o in. Then, tetraethylortho Then, in. f produced Fe f produced

h . in the next the . in 3 O 4 under under ------Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 FIGURE 3.9FIGURE of rate 2000 of a stirring 30°C with temperature aconstant bath at in five-neckwater thena flask the Theplaced into is flask. introduced are 4–6) range: (HLB balance hydrophilic–lipophilic amodified with dispersion stabilizer and [76,77], (4) and [78]. polymer (TVP)/PAM-c-PS synthesisof thermoviscosifying [74,75], ofthesis PAM-polystyrene nanostructure (PS) core–shell (3) synthesisof PAM/PAM-c-PS four into divided categories: (1) [72,73], synthesisof (PAM) polyacrylamide nanoparticles (2)- syn recovery oil (EOR) [72–78]. process enhanced the inverse in use to works miniemulsion are Their inverse Tablethe in emulsion is presented polymerization 3.1 3.9. shown nitrogen as gas Figure and in ping injector for for ingredients reaction recipe Atypical system, reflux heating condenser,drop and stirrer, submicron amechanical with equipped reactor a250 out in inverseThe emulsion is carried of polymer polymerization nanoparticles 3.2.3.3.1 process. aerosol-based acontinuous in shell 3.8 FIGURE Synthesis ofNanomaterials Synthesis To solvent organic PAM produce on inverse first, based emulsion NPs procedure, polymerization by in situ nanostructure S.A. have core–shell polymeric synthesized Ramazani Tamsilian and

Inorganic par

E mulsion Polymerization Method Polymerization mulsion N T Sc 2 he schematic diagram for inverse emulsion polymerization. diagram schematic he heme of the experimental setup for encapsulation of inorganic nanoparticles with a polymer a polymer with nanoparticles of inorganic for encapsulation setup experimental ofheme the inje Dropping submicron ct GMA monomer GMA Five-ne ticles or forinitiato ck fl as k Nitrogen inlet r Wa Monomer-condens

r ter inorganic par pm. After complete in dissolutionpm. After dispersion of stabilizer the bank Me chanical stirre NH ticles 3 ed Nitrogen outlet r P olymeriz . re acto ermometer ation r ermometer inorganic par Polymer-coated ticles

m L five-neck 49 - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 via polymerization using the surfmer as the hydrophobic the as monomer surfmer shell. of using Consequently, the the polymerization via the emulsifier, the the as shell is obtained whereas surfmer of using cores polymeric the polymerization involves one first The inverse described. system are Twoemulsion smart the prepare to procedures (surfmer). surfactant or inverse chemically polymerized hydrophobicshort grafted blocks are that nanolayering (surfactant properties) such PAM-b-PS as up copolymer of made long and hydrophilic such PAM, as polymerhydrophilic nanoparticle HPAM, TVP, a hydrophilic–hydrophobic and coat system, up of including made a acore of asmart preparation is design section object and ofThe this S.A. coworkers. and work of Ramazani future is the nanoparticle of core–shell type This properties. weight) its is 10 size and nanometers. its shell is and ananolayer nanometers, is 80 Daltonsize (molecular of polystyrene 40,000 with Dalton of 10 (molecular with polyacrylamide its nanocore weight) that million itsstructure and agglomeration. powders Finally, synthesized nano have the nanostructure core–shell core–shell consideredbe preventmustto purification Further is terminated. process reaction the time, this (about 30 way, is prevented. this process forchain In polymerization asecond time short by the considering propagation extra of and a polymer nanolayer time aspecial must done in be chain of the transfer continuously. is propagated chain this and The of polystyrene fprm, achain to causes nanoparticle polymer of the monomer surface simultaneously,organic on the must injected be initiator the and the and steps second of the initiator conditions. the out point to that It is interesting temperature ananolayer low for in injected making monomer are styrene and redox initiator the process, of the monomer and of nanolayerinitiator hydrophobicity with steps second Therefore, the in properties. second inject to the time the are and weight molecular produced high with polyacrylamide are of nanoparticles time, this After condition for mixing. 3or 4daysperature without mechanical under mentioned conditionsunder for 30 remains reactor the that selected is polymerization of period time reactor. first the into The rial (5:2 is injected persulfate, potassium condition − ratio) temperature in system initiator (redox), the phases, organic water and mixing and the including sulfate ferrous After amicroinjection. via reactor the in phase organic mixed the to water is injected phase the 20 and ofmer acrylamide 2000 around speed with mixer mechanical by those using a mixing after and necks, three with areactor in mixed are surfactant span80 50 rpm [72,73]. rpm of 400 speed stirrer and 60°C for 150 is performed reaction polymerization The mixture. reaction the into charged is then 400 and at 60°C set are speed inverse(W/O) to time in form fied oil and water stirrer emulsion.temperature Then, aspeci injector by within reactor dropping submicron the into solved water is dripped deionized in solventthe for 1 As mentioned before, a third category is due to synthesize core–shell nanostructure with binary binary with nanostructure core–shell is due category synthesize to mentionedAs before, athird 60 To PAM-PS nanostructure, synthesize core–shell min), the thin layer of polystyrene is made on nanoparticles of polyacrylamide and after layer after of and min), polyacrylamide of thin polystyrene on the nanoparticles is made h under nitrogen bubbling, gas h under monomer hydrophilic - dis such polyacrylamide as rpm, respectively, solutionrpm, (AIBN) initiator hexane in azobisisobutyronitrile and AIBN initiator Span80 surfactant Hexane solvent Water Acrylamide monomer Ingredients Polymerization of Polyacrylamide Typical Inverse Recipe Emulsion for the 3.1 TABLE mL of deionized water, is dispersed to the previous water, the to of solution. deionized mL is dispersed Then, min and after that immediately is moved low very immediately the to that tem after and min rpm, the water including phase, the 5 rpm, mL of hexane solventmL 0.0035 and Weight% 45 35 15 0.0068 5 15°C mate this by entering Nanocomposite Materials Nanocomposite g hydrophilic monog hydrophilic min at min mL of mL ------Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 The International Conference on Nanotechnology: Fundamentals and Applications (ICNFA 2013) ­ philic (ICNFA 2013) Applications and Fundamentals Nanotechnology: on Conference S.A., International The Y. (Adaptedfrom Ramazani A. Tamsilian, nanostructure. core–shell polymer–surfmer FIGURE 3.11FIGURE aprotective as not layercopolymer only acts and nanocomposites for water soluble polymer from 3.11). (Figure monolayer the produce to end open chains hydrophilic of the with block copolymers grafted are agents. Hydrophobic without propagated any termination which monomers are chains live radical using other polymerization via shell is obtained the whereas terminated, and polymerized are that inverse via emulsion using some monomers obtained hydrophilic polymerization polymer are cores 3.10). doublethe surfactant-monomer (Figure function application of the demonstrate to shell is proposed of core–surfmer hydrophilic nanostructure term 3.10FIGURE Synthesis of Nanomaterials Synthesis H Ab H ydrophilic monomer ydrophilic monomer sorption ofh This core–shell system consists of polymer-surfmer core–shell hydrophilic polymer-block or hydrophilic This core-block hydrophilic of copolymer the shell. The one relates second ananostructure to The + surfactant polymer-block copolymer core–shell nanostructure. (Adapted from Y. Tamsilian, A. Ramazani S.A., Y. from (Adapted Ramazani A. Tamsilian, nanostructure. polymer-block core–shell copolymer monomers H Su ydrophilic monomer

ydrophilic rfmer polymeriza ( ( See color insert. See See color insert. See R adical p and in Sec ond p H verse emulsionmeth olymeriz ydrophilic initiator Coupling agen olymeriz tion ) The schematic diagram for inverse emulsion polymerization of hydrophilic of hydrophilic for inverse emulsion polymerization diagram schematic ) The ) The schematic diagram for inverse emulsion polymerization of hydro for inverse emulsion polymerization diagram schematic ) The ation me R adical p ation and in t chanism H verse emulsionmeth olymeriz od ydrophilic initiato ation me Nanost chanism Ab r Organic solven od ru ev sorption ofsurfmer Re ct ap ure of disp oratio Mono some openend erse hy n disp drophilic core–surfmershel t erse , Canada, 2013.), Canada, core-blo Nanost s hy hy drophilic p ru drophilic chains ck cop ct ure of , Canada, 2013.), Canada, olymer shel olymer hy drophilic l + l 51 - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 A starch solution by dissolution is prepared A starch of 0.5 [78].materials respectively, properties, EOR finally prepared the (3)study and by thermo-thickening and smart als nanomateri synthesized of the (2) characterization rheology investigate to and studies structure the including phases, (1) nanoshell, three study is into divided nanocore-organic This synthesis of TVP layer. interface water the viscosity in increasing which phase, oil dramatically could resultin in dissolution of nanolayer after organic oil–water interface in releases TVP intelligent nanostructure This degradations. thermal or bacterial, oftations classical suchas mechanical, polymer flooding overcome limi and and reservoirs oil intelligently to weakness in ratio control mobility prepared is designed and a nanolayerprotection as for material core material tive the organic an polymer and active an thermosensi as of TVP study by mentioned group, anovel the nanostructure core–shell reservoir,oil may overcome deficiencies the of most solublewater In last EOR. polymers during the in ratio mobility optimize to salinity and temperature on increasing whose viscosity increases polymers (TVPs) thermoviscosifying could be tion. So, selection best the for material core the elevation previous by the temperature works- due in PAM to decrease degrada chain nanomaterial pitfalls.However,ing viscosity of polymer aqueous solution including PAM core as nanoparticles remove and EOR process exist the the considerably idea can optimize nanostructure core–shell the 21takes 3.12b). days (Figure a nanolayer from condition of polystyreneacrylamide dissolveto similar water under phase the in 3.12a), 6days (Figure takes 90–100°C oftemperature poly release of nanoparticles total but the Dalton (molecular dissolution weight) the 6million with polyacrylamide that of pure the under show results is investigated variable viscometer. obtained dilute wettability via with The reservoirs underground its water in of nanolayer phase from the effects on rheological and properties coating behavior the addition, of release In polyacrylamide environment. reaction the monomers in of virgin is no effect there done and is successfully nanoscale of polymer hydrophilic coating nanoparticles the that UV, seen done SEM, EDX, be by It DSC, can are IR, AES. NMR, and XPS, properties ticle nanopar core–shell of the investigation The recovery oil process. characterization and enhanced some applications approach in such delivery the as is another targeting but also degradations 52 States, 2015.) States, US20150148269,process, U.S. Patent, flooding polymer S.A., Smart Y. from Ramazani A. United Tamsilian, 3.12FIGURE solution of concentration with 0.5 (a)

0.5 Kinematic viscosity1.5 (cSt) 2.5 Another example of polymer NP synthesis by emulsion mechanism is starch nanoparticles. example nanoparticles. of synthesis byAnother polymer is emulsion starch NP mechanism show results S.A., that obtained the by Ramazani Tamsilian and experiments initial the to Due 0 1 2 04 y =1E–08x

Viscosity of (a) PAM-PS and (b) pure polyacrylamide in water phase versus time. (Adapted ofViscosity (a) versus time. phase water in PAM-PS (b) polyacrylamide and pure 08 4 – 4E–06x T ime (h) R 2 3 0 = 0.9974 + 0.0004x 3 M. The mixture is heated to 80°C for 80°C to 1 is heated mixture M. The – 0.001x+0.7334 120 160 (b g native powder sago 50 starch in Kinematic viscosity (cSt) ) 1.2 1.4 1.6 1.8 0.2 0.4 0.6 0.8 1 0 0 y =3E–05x 36 4 – 0.0017x Nanocomposite Materials Nanocomposite h under magnetic stirring stirring magnetic h under T 9 ime (d R 3 2 + 0.0236x = 0.9986 ay 12 ) 2 – 0.0437x+0.7896 15 mL of NaOHmL 18 21 ------Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 by adjusting the FR by FR adjusting the dimensions, respectively, deep and 5 also and 1174–1178.) 2014, 900 at rate (c)and stirring with 3.13FIGURE mately 55 device. approxi microfluidic of size PLGAfabricated nanoparticles, on the Small (FRs) based forat 80°C 2 is baked dish Petri the device in placed the then and interconnection tubing this protect to is placed 3.14b). hole the into (Figure aplastic tube inserting PDMS layer Another on topPDMS of the chip before end tube of the the is adhesive smearing is An made. sealant surface dish the and channel micro embedded the between contact and dish PDMS down aPetri The is chip pressed in inlet. a 0.5 holediameter make withto is used aflat-tipped needle a blade, then and for 80°C to mold 2 heated the into and 3.14a 50 (Figure and is 300 channel ). semicircular the To nanoparticles, the prepare 4.5 of pressure a upto keep can structure This equipment.(PDMS) devices microfluidic with external polydimethylsiloxane irreversibly to shows section technique interconnect tubing This afantastic 3.2.3.3.2 [80]. nanoparticles smaller homogeneous of dispersion mobility and nucleated uniform, causes to be species enhanced rates, stirring higher solution; and the agglomerate to particles leading through uniformly not dispersed 3.13c). synthesis (Figure the during using mixing nucleation the rates, are At species low mixing 3.13b) have (Figure and distribution aggregate to size wider particle nanoparticles to compared as morphology of the starch affect can rate mixing nique is suitable formation. The for nanoparticle - solution tech nanoprecipitation the reprecipitation starch of Thus, ethanol. also the into tion and have solu by nativeaqueous into dissolution nanoparticles starch converted into prepared of the 20–40 around size of range adiameter the in surface smooth [79]. ratios oil sunflowerand oleic oil, acetone),and acid), propanol, butanol, (methanol, cosurfactants and water/ oil, olein (hexane, phases ratios, oil palm surfactant’s the oil-co-surfactant concentrations, varying at900 mixing of under surfactant) amount certain (e.g., phase organic an to drop-wise is added perature 15 solution cooled tem room to of starch after ahomogeneous solution. starch obtain to milliliter One Synthesis ofNanomaterials Synthesis size difference is because of diffusion mixing against convective convective against The mixing. mixing mixing of diffusion is because difference size results. DLS Table and TEM 3.2 polydispersity shows and size (PDI). effects on particle This FR (a) Poly(lactic-co-glycolic flowrations rate varying with acid) (PLGA) is synthesized nanoparticles dimensions with 50 channel a straight has microfluidic chip the tests, leakage During 3.13a, onBased Figure with shape mostly of are large, oval native particles granular sago starch

MPa by experimental and theoretical investigations theoretical [81]. and byMPa experimental 10 kv

×500

n Mi m, is synthesized at a high flow rate. The sizes of the nanoparticles show flow a the nanoparticles atahigh The variation of sizes rate. is synthesized m,

h. 50 crofluidic Method crofluidic S EM micrographs of (a) native sago starch; starch nanoparticles prepared (b) without stirring; (b) stirring; without prepared of (a) nanoparticles micrographs starch EM native sago starch; μ m1 0000 (Figure 3.15(Figure 12 30SEI

r Scientia Iranica F Iranica S.A., Scientia Y. (Adapted from pm. Ramazani A. Tamsilian, ) and a good dispersion of PLGA nanoparticles are presented by presented a good dispersionare of) and PLGA nanoparticles (b) 10 kv

h ×20,000 . The PDMS. The slab is removedby substrate silicon the from

cm f

μ m

r or the total length. Degassed PDMS Degassed length. is injected total or the 0000 pm for 1 11 30SE

m L of cyclohexane, 5

µ 10kv I h m . The same procedure is repeated by is repeated procedure same . The . The microsizes of starch granules granules of starch microsizes . The (c) 2,0 1 ×20,000

m

m L of ethanol, and a and L of ethanol, μ 0000 m m in the channel channel the m in

×

μ 50 m f 11 30SE

×

or wide 50 I

μ , 21, m 53 - - - - 3

Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 Lab on Chip on Lab et al., from J. (Adapted fabrication. Wang interconnection tubing view the of (b)devices. fluidic cross-sectional A 54 on Chip on J. (Adaptedfrom Wang (d) Lab 20, versus FR. et al., 10, (e) FR: and of PLGA nanoparticles distribution size 3.15FIGURE 37.2°C. in (LCST) solutioncal temperature overincreased 37.2°C, below absorbance the whereas 37.2°C showing low constant, is steadily criti 3.17 Figure in results of is abruptly poly(NIPAM-co-AA) absorbance that nanoparticles demonstrate Ultraviolet (UV)-visible temperature. atroom opaque, it whereas transparent changes become to solution the represent that results of at37.2°C poly(NIPAM-co-AA) obtained nanoparticles The is poly(NIPAM-co-AA) synthesize to at80°C nanoparticles. initiator (KPS) is subsequently and onto conjugated AA persulfate potassium with NIPAM monomer is grafted onto route [82] thermosensitive byas polymer grafting is synthesized ( poly(NIPAM-co-AA) acid produce to of acrylic N-isopropylacrylamide nanoparticles and Grafting 3.2.3.3.3 flowviceand high rate versa. distribution by size narrow a prepare to distribution size particle the influence directly flow can rate Moreover, deposition PLGA provide size nanoparticles. can of arapid small interfacial choice of the 3.14FIGURE The solution of poly(NIPAM-co-AA) nanoparticles is significantly affected by temperatures. solution temperatures. The by affected of is significantly poly(NIPAM-co-AA) nanoparticles (a) (c) (a) Pl SU-8 asma bonding togl bonding asma Silicon , 14, 2014, 1673–1677.) PDMS FR:20 FR:40

G

rafting Method rafting ( ( S S ee color insert. ee ee color insert. ee , 14, 2014, 1673–1677.) as sA (b) (d) Punched hole Punched FR:10 FR:30 PDMS mould ) TEM images of PLGA nanoparticles with (a) with (b) 30, (c) 40, of FR: FR: PLGA nanoparticles images ) TEM FR: ) (a) Schematics of fabricating a tubing interconnection for PDMS micro interconnection ) (a) atubing of fabricating Schematics ssembled de ssembled vi ce (e)

Size (nm) Glue Pe 100 200 300 tri dish 0 Un cover Pl a cu stic tube 10 re ed d PDMS withglue 20 (b ) Nanocomposite Materials Nanocomposite Figure 3.16Figure FR Tu Hole SU-8 be 30 ). In this way,). this In Bulk Low flowrate High flowrate Glue Silicon PDMS Gl PDMS PDMS as 40 s - - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 Synthesis of Nanomaterials Synthesis B.G. Journal BioChip Chung, 3.17FIGURE 3.16 FIGURE composites [87–89]. improve for production active of clay highly polyethylene catalyst produce to structure clay nano of clay. exfoliatedwith structure To to method achieve have goal, they acid treatment an this used polyethylene/claysynthesized clay by Ziegler-Natta mineral from nanocomposites catalyst system S.A. coworkers and have [83–86]. Ramazani stability solvent and environmental and resistance, flammability properties, show nanocomposites barrier and These improvements mechanical to of polymer nanoparticles. of properties applications effective different due the to optimization have Most polymer/clay researchers to attention good industrial and research in nanocomposites 3.2.3.3.4 N-Isopropylacr Absorbance H 3 0.00 0.02 0.04 0.06 0.08 0.10 0.12 0.14 0.16 0.18 0.20 C H 300 2 HN (NIP C CH

AM In-Situ Polymerization Method Polymerization In-Situ

CH ) ylamide C CH 400 Synthesis of poly(NIPAM-co-AA) nanoparticles using KPS initiator at 80°C. at initiator KPS using nanoparticles of poly(NIPAM-co-AA) Synthesis UV–visible analysis of poly(NIPAM-co-AA) nanoparticles. (Adapted from B. Seo, H. Ku, from (Adapted UV–visible nanoparticles. of poly(NIPAM-co-AA) analysis 3 Microfluidics Microfluidic Lowand (High FlowRates) of PLGA Precipitated Using Comparison Nanoparticles 3.2 TABLE Microfluidics Source: O Wa 500 + veleng Adapted fromJ. Wang et al.,LabonChip,14,2014,1673–1677. , 8, 2014,, 8, 8–14.) th (nm) 600 H Ac 2 C ry Total Flow Rate(mL/h) lic acid(A 700 C CH OOH 41–44 410 A) 800 80°C Absorbance KPS 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 Minimum Size(nm) 15 110 55 20 H * 3 C 25 HN Te H C CH 2 mp Po PDI erature 0.2 0.1 ly(NIP CH 30 HH C CC 3 37.2°C AM ( ° 35 -c O C) H o- 2 AA ) 40 CO C OH 55 45 * - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 3.2.3.3.5 nanocomposites. of the process preparation the of clay. amount small However, and/or during exfoliated clay the intercalated must significantly be considerably are nanocomposites of improved the a by properties introducing thermomechanical show results the that obtained The investigated techniques. are by awide of range characteristic vacuum oven at70°C for 24 ina dried tively. and filtered, polymerseveral the times, step, withis ethanol final washed the In - agent, donor, transfer respec chain external DMCHS, hydrogen and cocatalyst, as and used are of point hexane. boiling To (TIBA), and of 4bars sure reactor, the inject triisobutylaluminum into Buchi (1 the in procedure polymerization by slurry hexane is synthesized 4 lowing ( steps respectively. or atetramer, formatrimer to cation dimer PANIradical fol polymer with is formed cationhaving monomerthe with two and possible radical the with reaction including reactions the itsform. cation resonant and radical the formationbetween dimer next substituent The stepis the inductive its effect its hindrance. to absenceof and important steric level 2senergy the from electron the nitrogen of atom. the by transferring is formed cation, whichseveraland forms has resonant radical aniline formationof the step is the first cases: the both in following The proceeds mechanism of aniline. mechanism polymerization [93].requirements these all of satisfies medium such low as volatility, ionic no strength, although should controlled noncorrosive be and properties To time. and oxidant, desirable of some results, concentration the factors of medium, obtain ture as are follows:- product tempera and final of the type nature on the and reaction of the course on the of intensity oncoloration. the major effective effective The the parameters oxidant are parameters which probably of concentration the the soluble is due and the to medium of the oligomers. type The colorvantages. By the oxidative black to of the progressing solution condensation of turns aniline, which is one intractable, of- essentially its disad are that excessan materials to oxidantleads of the conjugated to monomersis, polymer the is converted directly by acondensation However, process. offor peroxydisulfate for acid, synthe example, and example, type ammonium hydrochloric. this In glass. (ITO) oxide for electrode, tin example, or conducting indium metallic Pt inert on an and current and tial [91,92]. dopants different polymer solvents, due common its to insolubility in improvedobtained be it although by can using of processibility the poor is the method of this more feasible is the limitation The method. aniline oxidation of chemical production, the For salt. bulk emeraldine an polymer is called synthesized The acid media. aqueous the in (PANI) is widely polyaniline polymerization synthesize to used [90]. polymerization or electrochemical initiated Chemical photochemically and catalyzed someoxidation ones less such synthesis, and enzyme- monomers, common of as chemical the To including of electrochemical anumber methods are conducting polymers, there synthesize under mixing conditions. In the next conditions. the step, In TiCl mixing under Mg(OEt) 56 heated to 115°C. to heated TiCl with toluene fresh treated with productis washed several and The times

h at115°C. The final properties of produced nanocomposite such as mechanics, morphology, nanocomposite such as mechanics, produced of dispersionand properties final The To polyethylene/clay prepare by nanocomposites Figure 3.19, shown as Figure in Then, with dimer by the is formed oxidizing cation dimer anew radical 3.18 shown forms Figure in resonance different the Among , form(c) more reactive is the one due or chemical electrochemical the in is aclose there similarity mechanism, polymerization the In oxidant, synthesis, monomer solution aqueous chemical (aniline) in In containing is synthesized poten by oxidation constant acidic media synthesis,in PANI electrochemical is synthesized In To remove layers, silicate on OH the groups clay the for 6 is dehumidified 2

and toluene are added to the clay the to toluene added atcontinuous flow. argon and 80°C to are is heated The slurry S ynthesis of Conductive Polymer Nanoparticles Figure 3.20Figure ).

h. 4 and electron donor are added to the slurry and and slurry the to added donor electron are and polymerization method, propylene method, polymerization in situ in Nanocomposite Materials Nanocomposite

L - atapres reactor ) type

h at4 00°C. Then Then 00°C. 4 for for - - - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 Synthesis of Nanomaterials Synthesis from I. Harada, Y. Metals F. Synthetic Ueda, Furukawa, I.Harada, from 3.18FIGURE Synthetic MetalsF. Ueda, Synthetic 3.20 FIGURE Y. Furukawa, Metals F. Synthetic Ueda, 3.19FIGURE

NH NH + The formation of the aniline radical cation and its different resonant structures. (Adapted structures. resonant its different and cation radical aniline of the formation The Formation of the dimer and its corresponding radical cation. (Adapted from I. Harada, I.Harada, from (Adapted cation. radical its corresponding and dimer of the Formation One possible way of PANI polymer formation. (Adapted from I. Harada, Y. possible Furukawa, I.Harada, wayOne (Adaptedfrom of PANI formation. polymer •• 2 – e Dimer , 29, 1989, 303–312.) NH NH NH + – • –e P 2 NH + olymer – + 2 (a) + • • • NH + 2 , 29, 1989, 303–312.) NH NH + • 2 2 + NH NH + Rearrangemen 2 2 Rearrangemen (b) –e –2 H – NH + , 29, 1989, 303–312.) 2 + t t NH + (c) •• H N NH + + NH + N H N H 2 NH • + –H • Te 2 –H • tramer + –2 e + NH + • – H N (d) NH + NH + NH NH + NH NH + + 2 • 2 2 2 2 NH + • NH 2 2 57 Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 necked round bottom flask, then 0.745 flask, bottom round necked PANI. single-doped produce to polymerization PANI (2) doped and ventional emulsion binary homogeneous produce to polymerization solution 3.22Figure [85]. of ones. nondoped that than conductivity is about 9–10 the method of greater PANI that is known this times with when doped 3.21. shown as acids Figure protonic aqueous in with base emeraldine bydoping process treating It [93]. doping method by regime this of form base PANI this did conducting metallic They highly to converted emeraldine time for first the Angelopoulos polymer ofelectrons unchanged. the et al. conductive produce ofto number of the with doping polymer. process is akind transfer Charge 58 Synthetic Metals Synthetic 3.22 FIGURE Metals 3.21 FIGURE avacuum oven in salt PANI were dried cakes at50°C emeraldine for binary-doped obtained The oligomers, initiators. and aniline materials, water remove to acetone, and methanol, with unreacted for solution the 20 that, was centrifuged tion. After - system of reac stopping the the and balance PANI hydrophilic–lipophilic powder the by disrupting PANI doped dispersion precipitate to binary SDS–HCl the into were of methanol added amounts were 2.5, kept respectively. 0.5 and SDS and aniline to Excess aniline to of ratios molar APS the experiments, colored without PANI the any precipitation.green In dispersions were obtained without for agitation 24 proceeded polymerization as nounced 20–40 100 into drop-wise HCl (1 solution aqueous M) 0.923 with nitrogen for atmosphere under 30 temperature at room vigorouswith stirring In aconventionalIn emulsion system 5.768 Here PANI by oxidation (emeraldine ES) two salt, methods: (1) is synthesized chemical con show studies of formation shown cation astable as the Earlier polysemiquinone in radical for of used PANI state be doping nonredox process can emeraldine only the It that is known , 29, 1989, 303–312.) min, the homogeneous recipes were turned into a bluish tint and the coloration the abluish was into and pro tint homogeneous the were recipes turned min,

, 29, 1989, 303–312.) Protonic acid doping of PANIs. (Adapted from I. Harada, Y. F. Synthetic Ueda, Furukawa, I.Harada, of PANIs. doping acid from (Adapted Protonic A stable polysemiquinone radical cation. (Adapted from I. Harada, Y. F. Ueda, Furukawa, I.Harada, from (Adapted cation. radical polysemiquinone A stable 20–30 during of mixtures reaction mL N H N H + Cl N H – g aniline in 10 in g aniline mL ammonium persulfate (APS) oxidant were persulfate an added as ammonium mL 40 g of in SDS was dispersed

N Cl N H N H

+ – 2n HCl at8000 min mL HCl (1 M) was introduced to the mixture mixture HCl (1 the to mL was introduced M) min. After the purging period of about period purging the After min. + N H Cl

N Cl N H + –

h at room temperature. Finally, dark temperature. h atroom – rpm. The precipitation was washed The rpm. Nanocomposite Materials Nanocomposite N H mL HCl (1mL N H N H n n n min. Then, 10 Then, min. M) in atwo- in M) mL mL - - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 Synthesis ofNanomaterials Synthesis (Adapted from I. Harada, Y. F. Metals Synthetic Ueda, Furukawa, I.Harada, (Adapted from 3.24 FIGURE 100 PANI-ES with acontrol (EB) by base as prepared suspending PANI was prepared Emeraldine also avacuum in oven PANI) salt product(single-dopedwas dried at50°C for emeraldine 48 obtained for 24 stirred monomer 3.23 with . Figure shows schematically oxidation of aniline what during happens acidic media. in APS 48 F. Ueda, Metals Synthetic 3.23 FIGURE 0.7, 1 and were of 0, amounts 0.1, PANI/graphene graphene preparation nanocomposite. The 0.2, 0.3, 0.4, 0.5, sion for was emulsion used solution both and 3.25 Figure shows polymerization. the schematically 1 in persed were of- graphene dis amounts prescribed that difference the with for aniline described method asimilar with were PANI/graphene prepared such The nanoparticles graphene. as nanoparticles (emeraldine base), 3.24. shown Figure in

The solution polymerization prepared with the same molar ratio of ratio molar monomer oxidantto same was the with solutionThe prepared polymerization To increase electrical conductivity of polyaniline nanoparticles, one can add highly conductive highly add one can To nanoparticles, conductivity of polyaniline electrical increase h

m L of NH

wt% according to the monomer the to net weight according wt% [95].

M H

h atr 4 P O OH (24%) solution convert to PANI the hydrochloride (emeraldine salt) PANI to Cl solution of aniline monomer with sonication and the monomer-graphene monomer the sonication solution with and Cl disper of aniline ANI emeraldine salt is deprotonated in the alkaline medium to PANI emeraldine base. base. PANI to emeraldine medium alkaline the in deprotonated is salt emeraldine ANI xidation of aniline hydrochloride with APS. (Adapted from I. Harada, Y. Furukawa, I. Harada, (Adapted from APS. with hydrochloride of aniline xidation + Cl NH oom temperature under N2 purging, to obtain PANI by the same procedure. The The PANI procedure. by same N2 obtain to under the purging, oom temperature – NN , 29, 1989, 303–312.) NH 4n Aniline hy Polyaniline Polyaniline Cl NH + 2nHCl5H + drochloride – NH + Cl NH Polyaniline (emeraldinebase) – 2 hy ·HCI hy drochloride (emeraldinesalt) drochloride (emeraldinesalt) 2 SO + NH NH NH 4 +5n(NH Ammonium per H Cl –2n H Deprotonation 5n (NH + 4 , 29, 1989, 303–312.) ) 2 SO – 4 ) + Cl 4 2 NH S 2 – NH NH O ox 8 ydisulfate n n n

59 h - . Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 from I. Harada, Y. Metals F. Synthetic Ueda, Furukawa, I.Harada, from large alignment torque to direct the nanotube parallel to the electric field.advantages electric the One the to of of parallel nanotube the torque direct to alignment large of SWNTs by fieldsZhang’s directions electric growth the controlled has [102], group a produced 3.3.1.2 posts. silicon by the Waals der and van self-orientated forces are nanotubes between nanotubes arrayed the case, FIGURE 3.25 FIGURE 60 square regions (700°C; carbon source, C regions source, (700°C;square carbon in particles iron with patterned substrates silicon and onsilicon porous (MWNTs) growth by CVD sites catalytic [98].specific from of locations nanotubes for growth arrayed positioning the catalyst in structures, nanotube Today, of nanotubes. growth the have approaches growth developed organized patterned obtain to nucleate to seeds considered as [97]. are for reactor catalyst aperiod particles tube The the through flowing materials) and gas a hydrocarbon such alumina as materials area surface on high ported sup typically involves synthesis by (metal CVD nanoparticles CNT acatalyst material heating 3.3.1.1 site selective.controllable are locations that atarrays grow nanotube substrates patterned field on catalytic electric and methods using CVD ablation. laser and by last two and Tangleddischarge, methods the produced could be nanotubes arc- CNTs produce to growth, field including methods CVD, electric several nanotube main are relations [96]. There structure–property and structures in enrichment and extreme versatility the CNTs representing have configuration, simplest composition bonding the atomic chemical and s 3.3.1 3.3 method on the substrates (900°C; carbon source, CH source, (900°C; substrates carbon on the method by CVD formed the are orientations nanotube desired SWNTs networks the with ordered with works. of results as these synthesis stage of atthe nanotubes formed networks were and arrays nanotube ordered The of orientation nanotubes. the control manipulate to including self-assembly single-walledfor multiwalled and nanotubes, both active field and electric displays.panel massivearrays defined derived spatially simple the by toapplyroutes fieldemitter in flat chemical exhibit field electron excellent in nanotubes emissioncreate to arrayed tions. characteristics The - Waals der by van grown interac closely binding due strong to intratube catalyst particles spaced nanotubes from resulting surface, substrate the to perpendicular direction along the well aligned are The earlier work has presented the ordered arrays of CNT consisting of multiwalled nanotubes consisting of multiwalled of nanotubes CNT arrays ordered work the presented earlier has The Contact printing technique is used to transfer catalyst materials onto the tops of pillars, and and tops of onto pillars, the catalyst materials transfer to is used technique printing Contact growth University atStanford patterned Dai out [99] arrayed have colleagues his with carried

ONE-DIMENSIONAL NANOMATERIALS ONE-DIMENSIONAL Chemical VaporChemical Deposition Electric Field-Directed Nanotube Growth Nanotube Field-Directed Electric y n thesis

( See color insert. See

of N a n otubes Aniline monomer ) Schematic process of preparing PANI/graphene nanocomposites. (Adapted nanocomposites. PANI/graphene of preparing process ) Schematic Graphene sheet 2 H 4 ; alumina-supported iron catalyst) iron [99]. nanotubes ; alumina-supported The , 29, 1989, 303–312.) 4 ; supported iron catalyst) iron [100,101].; supported this In Polyaniline/graphene nanocomposite(PAG) Nanocomposite Materials Nanocomposite - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 Synthesis of Nanomaterials Synthesis by the researchers in the Nature the in by researchers the CNTs The is self-assembled represented molecules surface on aplatinum by precursor organic 3.3.1.3 synthesis. nanotube during interested by applied fieldsbe varying can on flat substrates fabric structures tube complex and However, wires nano molecular procedure. suspended of studies both growth further the during alignment and the gas flow of stability is fluctuations thermal fieldusing electric against Nature J.R. elongation. Sanchez-Valencia (Adaptedfrom epitaxial bonds; green: et al., S1; new C–C lines: dashed red seed of the segment blue: CNT and short elongation Orange (EE). epitaxial (P1) via (2) growth and nanotube C cyclodehydrogenation via (6,6) formation (CDH) polycyclic as precursor SWCNT seed hydrocarbon 3.26 FIGURE SWCNTs shows(SHIM) produced nm. the 300 that than have greater lengths helium ion 3.26). microscope decomposition (Figure of ethylene Scanning surface platinum on the catalytic the from originate and end attach SWCNTing cap. atoms by is formed More this carbon for nanotube’s is folded the outparameter grow flat oflid molecule.the the The structure, atomic of defined the germ, bonds. The split to reaction off hydrogen form new and atoms carbon–carbon using acatalytic surface on ahot platinum germling, as named object is transferred, dimensional , 512, 2014, 61–64.) Molecular Seeds Self Assembly Self Seeds Molecular CD 1 H

(6,6) SW ( See color insert. See s eed (S1) CN T ) Two of SWCNTs: synthesis bottom-up step (1) ultrashort singly capped journal [103]. In this research, starting molecule [103]. a three- into journal starting research, this In 2E C Pr 96 ec H E ursor 54 (P1) (6,6) SW Singly capp CN ed T 96 H 61 54 - -

Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 ticles N under using amicrowaveMWCNTs synthesized are oven polystyrene nickel with calcinate to nanopar 3.3.1.4 62 2, 2014,2, 2773–2780.) 2, (DNi), (a) 10, (b) (c) 20, (d) 50, and 90 3.27 FIGURE mixtures of components through arc-vaporization of two carbon rods placed end placed endto with rods of arc-vaporization two ofcarbon components through mixtures produce to easiest method and most common is the discharge arc carbon The 3.3.1.6 target. the carbon near fluid the dynamics and pressure, temperature, type, gas inert of power laser catalysts, wavelength, type and and such amount as on several synthesis parameters distribution between 1.0 between distribution 1.6 and diameter flow of produce walls the to SWNTstube with a condense on the vapors bon and varied self-assemble will car from nanotubes The a cooled downstream. into chamber temperature high argon the under furnace tube SWNTs [105,106].ate process quartz a1200°C in placed targets, is focused laser onto carbon The produce to temperature high at target agraphite from carbon power ahigh ablation laser vaporize to is used method, the laser In 3.3.1.5 respectively. 15 700°C, 10 min, and min D function, by alinear is correlated nickel of nanoparticles catalytic diameter the and nanotubes carbon of the show results outer diameter arelationship the between that tometer. obtained The - x-ray awide-angle 3.27), spectrophotometer, and (Figure by aRaman diffrac TEM characterized CNT =1.01D Arc Discharge Method Arc Discharge Microwave Heating Method Laser Ablation Method Laser (c) (a)

Ni 2 nm and D +14.79 and nm TEM images of CNTs for calcination at 700°C for 15 700°C at of CNTs for images calcination TEM purging at 700 or 800°C for 15 or 800°C at700 or 10 purging as particles SWNTs and using MWNTs metal both atmosphere (~500atmosphere torr) [107]. the vapors from the carries gas Argon quality and quantity The nm. CNT Journal of Materials Chemistry A Chemistry Materials of Journal et al., Ohta K. from (Adapted nm. =1.12D Ni + 7.80 (b) (d) nm for the calcination condition of 800°C, condition for of calcination nm 800°C, the min [104].min MWCNTs synthesized are The min using different nano Ni diameters Ni diameters nano different using min nanotubes carbon of these Nanocomposite Materials Nanocomposite CNTs or complex to catalysts depend depend gener - - - , Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 C-plane sapphire substrate plate (5 substrate C-plane sapphire study, asolution of cycloparaphenylenes (0.5 of 50–100 current drive to adirect applied 3.3.1.7 [107,108]. parameters two deposit most of of important the the are temperature the and electrode.To plasma ofdeposit arc other the yield on the high CNTs, uniformity obtain the rod-shaped asmall forms and electrodes, of one carbon of surface the the vaporize to two electrodes Synthesis ofNanomaterials Synthesis TiO the patch with graphene It the was interface. found contacting atthe that or toward graphene the 3.30 Figure graphene. with excitation shows interface movement atthe the of away electrons from, phene [110].- gra maximized with active materials It would photocatalytically amenable synthesize to be percentage of the CNTs ofpercentage the was 1.7 between 1.3 and conclude to high regime size the that consistent It by is observed also this with TEM. diameters 3.28f different with Figure of in number nanotubes was the derived from histogram distribution molecules( ethanol with seed these heating spectroscopy. Raman and by TEM lowed for at500°C by15 heating follows: as methods current the with compared chirality several advantages synthesisapproach control to for CNT are organic the CNTs pitches. helical different with There well as chiral to as CNTs diameters, different with chair arm zigzag and both produce to method attractive template approach is an reactions. This ization macrocyclic (2) templates and development longer templates CNTs obtain ofto these by polymer Two considered for synthesisof bottom-up CNTs: the are of research (1) basic areas using aromatic the from removeto metals purification catalytic approximately a1 ing graphene and TiO and graphene ing 1.3–1.7 range diameter the in distributed CNTs the were that indicate results spectroscopy mode. Raman breathing of frequency radial and (d) regions a relationship mode diameter and between 3.28dFigure breathing shows radial the 3.28d e, Figure cycloparaphenylenes residual result and in was not found plate. reaction on the previously spectroscopy the CNTs under synthesized mentioned Raman conditions. the Regarding TiO shows case top oxygen the to this graphene clearly in from measurement transfer charge layer of removal the addition of of and electrons the denote respectively. electrons, substrates, CDD The negativeand density (CDD), difference charge of the two of the interaction the density charge in mately 0.017 e TiO Omachi et al. initiated well-defined carbon nanorings to grow carbon nanotubes nanotubes grow[109].to carbon nanorings this In well-defined carbon initiated et al. Omachi • • After extensiveAfter investigations, it was found CNTs CPPs by that from grown could be simply • In addition, Mogilevsky and his coworkers succeeded to prepare a hybrid nanostructure includ- ahybrid nanostructure coworkers Mogilevsky addition, prepare to his In and succeeded Special advantage of (e.g., aphotoactiveSpecial material TiO

2 2 2 which were also confirmed the TiOfor which were confirmed also oxygen the to graphene from electrons transfer to top causes layer molecules the in surface of , to produce positive, to produce negative and graphene TiO organic synthesisapproach. organic L techniques. closer for current 1000°C to the temperatures with compared S reactions. well-understood F − TiO irst, the process is easier to troubleshoot and optimize because of its mechanistically of its because mechanistically is easier troubleshoot to optimize process and the irst, econd, the synthesis condition for organics is typically at temperatures below 200°C synthesiscondition attemperatures for the econd, is typically organics

ast, it is possible to produce CNTs with incorporation of nitrogen, boron, or sulfur by it the ast, is possible of or sulfur nitrogen, boron, CNTs produce to incorporation with B 2 ottom-Up Chemical Synthesis interface (see 3.29 interface Figure − per carbon atom. carbon per

m m gap, in a chamber filled with inert gas at low pressure. It requires further further at gas lowinert pressure. with requires It filled m gap, achamber in 2 by a bottom-up synthetic approach of alizarin and titanium isopropoxide titanium and by approach of synthetic a bottom-up alizarin

m

m in under ethanol gas purging. The CNTs formed were analyzed CNTs were The purging. gas formed analyzed ethanol under in m ).

×

n 5 m, very close very m, of CPP (1.7 that to

A m 2 Figure 3.28aFigure -sandwiched graphene and graphene ribbons. Positive ribbons. graphene and -sandwiched graphene , following a high temperature discharge between the the between discharge , following temperature ahigh m). chamber, fol the plate reaction was in placed The

m

M in toluene)M in at4000 was spin-coated p nm in diameter. in nm roduced CNTs. A potential difference of CNTs. 20 difference roduced Apotential 2 , which the total charge transfer is approxi transfer charge total , which the 2 ) is the charge transfer degree after photo after degree transfer charge ) is the ). Figure 3.28b and c are TEM images of images ). TEM 3.28b Figure care and

n m). diameter Also,the

r pm on a

V i 63 s - - - - - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 ylenediamine-70 64 imple Hydrothermalimple Method vents (water, H and ethanol, synthesis solid Ni (salen) (120–180°C), complexes temperatures atdifferent (6–24 times to interest Using hydro/solvothermal is of of nickel with ligand particular salen treatment nitrate 3.3.2.1 s 3.3.2 Nature et al., (e Chemistry g). Omachi H. and (Adaptedfrom given in are CPP for CNTs from grown data and given (d in f) are CPP for and CNTs from Data grown grams. histo CPP, distribution from of (f CNTs,of g) CNTs and diameter (d synthesized and spectra e) and Raman 3.28 FIGURE ( with distilled water and ethanol. The product obtained after 6 after productobtained The ethanol. water and distilled with washed several and times is collected color material precipitated red-orange The treatment. mal steel autoclave. astainless into hydrother autoclave The after is cooled down temperature room to of Ni(NO of (b Figure 3.31aFigure 13, to b). and time reaction 18, synthesis after out point to that It is and interesting (c) ) (a) 10 nm 10 nm

[12]CPP 3 S y ) 2 n

⋅ thesis

6H ( S 2

ee color insert. ee m O dissolved 30 in

of L of H N a n 2 O as aqueous solution, aqueous O as followed for 15 by mixing oro 2 O, C O, Et ) (a) Schematic presentation of growth experiments, (b and c) TEM images c) images and (b TEM experiments, ) (a) of growth presentation Schematic d hanol ga s 2 (e (d H s

) m ) 100 0 5 0 5 0 350 300 250 200 150 100 5

OH, and acetonitrile) [111].OH, and synthesis, 0.75 atypical In Intensity (a.u.) Intensity (a.u.) L of H . . . . .50.75 0.85 1.0 1.2 1.5 2.0 . . . 1.0 1.2 1.5 2.0 Diameter of Diameter of 5 0 5 0 350 300 250 200 150 Raman shift (c shift Raman Raman shift (c shift Raman Sa Ex pphire wafer(C 2 O is added to 0.75 to O is added 500°C, 15min 500°C, pe Chamber rimental setting [12]CPP CN CN T (nm) m m T (nm) .50.75 0.85 488 nm 633 nm 488 nm 633 nm -p , 5, 2013, 572–576.) –1 –1 lane) ) )

m h c Pump mol of N,N (g onsisted of separated nanorods nanorods onsisted of separated (f)

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m in and transferred transferred and in Carbon nanotub Carbon CN CN

h T (nm) T (nm) ), sol and

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Under hydrothermal conditions, the soluble conditions,Under the hydrothermal Ni 3.32Figure Ni(salen) shows of ananorod formationmechanism the complex two- asequential as h p slowsdownchargere phot (3) Graphenepatchaccept thermallycon (2) Ali isoprop (1) Ali and/or < > and/or Ti hy 4 is added under magnetic mixing for 2 mixing magnetic under is added

O brid str za za 2 oe comp S rin– rin andtitanium(I eed-Mediated and Seedless Methods xc oxide formali

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m V) L of 0.2

isoprop m M of HAuCl

m m UV oxide 2

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M o 2 SO 4 M of AgNO , 10

m Ti Ti O L deionized water is L deionized

O m 2 2 4 . Then, 0.006 . Then, Calcination 3 2 , and , and O to O to

65 M - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 started by adding 0.01 by adding started 66 . After 12 . After 30 &Interfaces Materials ACSet al., Applied from G. Mogilevsky figure. side(Adapted of the right onthe graph of the y-axis the and cell unit of the z-axis 3.30 FIGURE (0.1–0.15 film, and QD growth without any catalyst. High purity product and easy fabrications of nanorod andeasy fabrications productof nanorod anywithoutHigh purity growth and catalyst. QD film, thin for vapor used nanorods, deposition ZnO chemical been also (MOCVD) has Metal–organic ( phase growth complete primary the hydratechloride (BDAC). BDAC to ratios aspect higher with nanorods into shape the helps direct benzyldimethylhexadecylammonium solution utilizing growth through primary removing the in except identical procedure, for by KBr an solution the was prepared experiments of for the all volumereaction 100 from gold solution nanorods uniform [114]. by primary the nanorods is possible the This increase to agents.reducing the as of paradioxybenzene ascorbic acid and a mixture and acid, gallic paradioxybenzene, acid, 3.3.2.3 uct yield began to decrease byuct yield reductiongold of the decrease to began ions 0.3 to concentration water. in is redispersed precipitate 36 geneous. After whereas the width of rods still was 13.4 still of width rods the whereas tate is redispersed in water. in is redispersed tate of HAuCl

The seeded or secondary growth method is manageable to scale up larger amounts of gold up isamounts manageable larger scale to method growth or secondary seeded The The gold ions concentration also was tried to downregulate the width ( width the downregulate goldto The was ions tried also concentration In the seedless route [113], seedless the In 0.15 by mixing prepared gold are nanorods s

M 4 M M of AgNO , 100 ) would be favored to form rods with higher aspect ratio using ascorbic acid, tartaric ) would using ratio ascorbictartaric favored acid, be aspect higher with formrods to etal–Organic Chemical Vapor Method Chemical Deposition etal–Organic

h M , the reaction is stopped by centrifugation with 10,000 with by is stopped reaction centrifugation , the

m odel cell alongside with the planar averaged charge difference. d(Å) difference. position averaged onthe charge the is planar the alongside with cell odel

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M o

f NaBH m L to 1 L to 3 f paradioxybenzene, and 1.19 and f paradioxybenzene, , 0.05 4 solution. Finally, for solution 30 the is stirred

L Figure 3.34Figure

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n m. High concentrations of concentrations Ag High m.

). d (Å) 25 30 10 15 20 0 5 –0.5 03–. . 0.3 0.1 –0.1 –0.3 Charge difference(e

r + pm for 10 0.5 (0.12

Nanocomposite Materials Nanocomposite M o

Figure 3.33Figure

r M o pm for 10 f HCl. The reaction is reaction f HCl. The

–

m –

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m M - - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 FIGURE 3.31 FIGURE Synthesis of Nanomaterials Synthesis 16, 2014, 8020–8026.) 6 h, (ch, d) 13 and (e) (g) (c) (a) 26 KV 26 KV 26 KV 26 KV

20.0 KX 40.0 KX 20.0 KX 20.0 KX SEM images of H Ni(salen) in images SEM prepared nanocomplexes h, (e and f) 18 (eh, f) and 1 μm 1 μm 1 μm 1 μm h, and (g and h) and (g 24 and h, KYKY-EM3200 KYKY-EM3200 KYKY-EM3200 KYKY-EM3200 SN:0539 SN:0539 SN:0539 SN:0539 h. (Adapted from M. Mohammadikish, CrystEngComm M. Mohammadikish, (Adaptedfrom h. (h) (d) (f) (b) 26 KV 26 KV 26 KV 26 KV 40.0 KX 20.0 KX 20.0 KX 40.0 KX 2 O at 140°C and various times: (a and b) times: 140°CO at various and 1 μm 1 μm 1 μm 1 μm KYKY-EM3200 KYKY-EM3200 KYKY-EM3200 KYKY-EM3200 SN:0539 SN:0539 SN:0539 SN:0539 67 , Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 Journal of Materials Chemistry A Chemistry Materials of Journal 68 of Materials of (c) using nanorods 0.25 gold final and of (b) primary images the TEM and of CTAB: amount (a) spectra absorbance standard optical 3.34 FIGURE 3.33 FIGURE 3.32 FIGURE (b) 0.5 (a) (a) 100 nm Absorbance 65.4 ±6.0*21.52.2nm 2.0 0.0 0.5 1.0 1.5 H 0.6 mM 400 mM, (c)mM, 0.4 ydrothermal condition AR =3.0 Ni(N H , 25, 2013, 4537–4544.) 2 –S

1.5× BDAC 1.0× BDAC 0.5× BDAC 0.25× BDAC NRS1, 0.0×KBr 500 O alen Schematic illustration of a proposed mechanism for the formation of the Ni(salen) of the formation for the nanorods. mechanism of aproposed illustration Schematic TEM images of gold nanorods synthesized with different Au different with synthesized of gold images nanorods TEM Secondary growth of the primary and final gold nanorods with with BDAC the goldto nanorods addition final in and primary of the growth Secondary 3 ) mM, and (d) and 0.3mM, 3 (b) 100 nm 600 × Wavelength (nm) 72.4 ±6.7*20.02.6nm , (d), 0.5 Nucl 0.5 mM AR =3.6 700 ea × tion , (e) 1.0 , 2, 2013, 3528–3535.) 2013, 2, , mM. (e) Corresponding UV–vis–NIR spectra. (Adapted from X. Xu X. et al., from (Adapted spectra. (e) UV–vis–NIR mM. Corresponding 800 × (c) 100 nm , and (f) 1.5 (f) , and 68.8 ±7.0*16.32.1nm

900 (0 1 0) 1 (0 0.4 mM AR =4.2

(1 0 0) × BDAC. Chemistry Kozek et al., K.A. from (Adapted at Oriente Grow tac hmen 88 ×22nm (e) 10× 82 ×24nm (c) 0.25× Au th (0 01) (d) 100 nm d 3+ (0 01) t 60.5 ±6.8*13.41.6nm concentration – 0.3 mM AR =4.5 100 nm 59 ×16nm (b) NRS1

(1 0 0)– (0 1 0) 1 (0 Nanocomposite Materials Nanocomposite 3

+ – concentration (a) concentration 0.6 (e) Agg Absorbance (a.u.) 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 87 ×23nm (d) 0.5× 91 ×22nm (f) 1.5× 400 regation 500 Wavelength (nm) 600 700 800 900 0.3 mM 0.4 mM 0.5 mM 0.6 mM 1000 mM, mM, Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 several methods (includingseveral reaction), gaseous methods evaporation, and reduction, chemical subsequently is probably by nanowires generated and vapor synthesis where vapor phase are nanorods, species most extensivelyThe including whiskers, explored of formation 1D the approach to nanostructure 3.3.2.4 flow, gas nanostructures. turbulent flow laminar the inducing between by high-speed is tips obtained just gases on nanorod reactant of fresh adsorption addition, In growth. anisotropic for reason main is the ZnO of energy wurtzite surface anisotropic out that pointed be it can gated, investi thoroughly not been has of nanorods ZnO mechanism catalyst-free growth the Although major (see case the advantages for 3.35). are Figure this heterostructures and structures quantum W.I. Letters (Adaptedfrom Physics et al., nanorods. Park ZnO grown Applied MOCVD of (c) images (e) FE-SEM (d) MOCVD, (b) and and and catalyst-free (f) catalyst-free and process VLS-grown 3.35 FIGURE Synthesis of Nanomaterials Synthesis (a) (c) (e) Vapor Synthesis Phase

Schematic diagrams illustrating the growth of ZnO nanorods (nanowires) (a) from nanorods of ZnO VLS growth the the illustrating diagrams Schematic VLS process 1 μm 100 nm catalyst Metal (b) (d) (f) Catalyst freeMOCVD , 80, 2002, 4232–4234.) 2002, , 80, 69 - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 attachment of colloidal Cu attachment on long NWs ZnO by electrostatic manufactured the successfully are seeds CuO procedure, this by ratios electrophoresis-assistedaspect electroless deposition of onto NWs CuO ZnO [118]. During of high ZnO/CuO with arrays (NW) nanowire is synthesis of core–shell structure attractive Another 3.3.3.2 (e), direction (f). polarization scanning for the and from circular 90° tion (d), polarization atlinear - direc 45° scanning the polarization from for linear patterns of dependence nanowire polarization of 60 diameters with nanowires produce to method alternative is an radiation scattered surface Using of and interposition incident radiation laser the 3.3.3.1 growth. for NW is positioned downstream the catalysts with atthe precoated asubstrate and downstream, the into material evaporated source the forwarding to gas hydrogen acarrier as is used while powder of CVD. furnace, Source atwo-zone tube upstream is put atthe metal–organic and systems feigned such other to growth MBE as no entanglement compared of toxic precursors, gas III–V NWs ofvarious its because relatively importantly, and, low procedures, simple cost, growth solid powder (solid-source source widely CVD) been of has explored for growth years recent the in and conventional the furnace tube utilizing method growth aCVD (MBE).epitaxy all, Among vapor including deposition chemical growth, (CVD), beam ablation, molecular laser and pulsed have NWsSpecifically, produce to techniques applied the vapor-phasebeen for precursors various rates. growth yield also epitaxial and high materials precursor for the trapping interface energy provide can low- particles The nanoclusters exist solid VSS, as particles. in metal the mechanism, NWs.VLS the Unlike grow crystalline into congregate to and starts semiconductor material the droplets, on which of catalytic super saturation to the leads precursors ofContinuous the feeding alloy. metal–semiconductor of liquiddroplets system, in the resulting metal–semiconductor the of point eutectic the than should higher be that attemperatures introduced are precursors phase vapor- growth, aVLS In mechanisms. growth (VSS) (VLS) solid–solid vapor–liquid–solid and vapor– via catalysts nanoclusters as Generally, by metal semiconductor NWs synthesized be can s 3.3.3 nanowires. and of nanorods ZnO methods investigated activities, and physical works, research the focusing chemical nanorods and on current [116] For quantities. large example, in Yi et al. obtained be have areview on ZnO paper written control Withover proper can super-saturation factor, material. the source the 1D nanostructure lower of that atemperature with than onto condensed asolid surface and substrate transported 70 single (a), double (b), (c) nanowires triple and of width with 60 substrate. for the heating enough sufficientintensity produce to spot must focal of narrow be the peak intensity the because is a single This nanowire. point to forming zoneof plates is a critical the aperture numerical high for incident ofdevice radiation the fabrication. the tion direction - (i.e.,erties orientation), polariza and length, byand intensity diameter, controlled the be which can [117]. prop controlled with substrate on adielectric produced are Also,multiplenanowires parallel resolution for high vapor the deposition is needed chemical heating which periodical nanowires, deposition mechanism. modelingresultsarepresented tovalidate thesupposed dielectrophoresis-assisted electroless namic thermody conventional observationstions and in electroless experimental deposition The method. - limita diffusion solution deposition the inherent in the prevail to by kinetic-limited fabricated are Figure 3.36 Figure in show radiation laser polarized horizontally from grown ofSEM images nanowires control, which the for diameter interference nanowire silicon 3.32 radiation Figure the illustrates

Sub y El n ectrophoresis-Assisted Electroless Deposition Electroless ectrophoresis-Assisted thesis diffraction Laser Synthesisdiffraction Laser

of N a n 2 owires O NPs under thermal oxidation. The core–shell ZnO/CuO nanowires nanowires ZnO/CuO core–shell oxidation. The thermal under O NPs

n m. This condition causes spatially confined confined condition spatially causes This m.

n m. Also, these images show images Also,these m. the Nanocomposite Materials Nanocomposite - - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 initial reagents and precipitator, reagents and respectively,initial CeO the synthesize to at sufficiently ( lowtemperatures powders given of the compositions dispersion (fromoxide ahigh with nanocrystalline 100 1to ionic-molecular level; reagents obtain to atthe initial subsequentlythe gives this opportunity an of mixing most because general is the method This product. obtained of the treatment quent thermal precipitation with subsevia conducted is chemical oxide films synthesis of nanostructured The 3.4.1.1 s 3.4.1 3.4 10 alength with duced μ it Also, were time. was nanowires pro found ZnO growth with that linearly increases nanowires of show length results the the that obtained The environment. air an in DIwith water, dried and solution, growth is brought substrate the out followed from the reaction, by several washing times for 0.5–5.0 is performed process heating The solutionsolution of process. the solution surface the keep to on the experimental volume the during followed by two Teflon injection the into third The thetubes.Teflon used is pumping tube extra for solution amicrowave with aqueous heated and methylenetetramine oven 2.45 frequency with hexa hexahydrate and - nitrate including zinc abeaker into is dipped deposited substrate ZnO the (PLD). deposition tin glass substrate by pulsed-laser oxide technique Then, doped onited fluorine equilibrium. dynamic in concentration reactants the retain avoid and which can timeout growth the [119]et al. amicrowave of proposed long arrays, control to growth nanowire method ZnO heating conductive oxide on atransparent substrate. Recently, arrays nanowire ZnO Liu aligned vertically for synthesis of long the arapid procedure is obtain to method this challenge in main The method. extensively devices are optical and for by hydrothermal nanowires electrical ZnO the synthesized 3.3.3.3 Nature Reports, Scientific J.I. Mitchell et al., 3.36 FIGURE Synthesis of Nanomaterials Synthesis cipitation, gel the including precipitates, Ce(OH) The solutions of cerium and zirconium nitrates and aqueous ammonia solution are used as the the solution as used are ammonia aqueous and nitrates solutions zirconium The and of cerium layer initially, microwave- is thin depos aZnO method, growth nanoseed-mediated heating In

TWO-DIMENSIONAL NANOMATERIALS TWO-DIMENSIONAL Chemical Precipitation with Subsequent Thermal Treatment Thermal Subsequent with Precipitation Chemical y Microwave Method Heating Growth n thesis

Schematic of radiation interference for silicon nanowire diameter control. (Adapted from (Adaptedfrom control. diameter nanowire for silicon interference of radiation Schematic (d (a)

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3.4.1.3 72 control the film thickness at the nanometer scale. the nanometer at thickness film control the sition films [123]. (MLD) formed-polyimide easilyto The cycle a parameter are good numbers the pyrolysisby are synthesized layerof molecular nanofilms depo carbon uniform Continuous and at–25°C fastto freezing for 24 Nature Reports, J.I.Scientific al., et (Adaptedfrom Mitchell polarization. for, and circular (f) direction, scanning the from degrees 90 (e) at polarization direction, linear scanning the from 45 degrees for, polarization (d) patterns linear of nanowire dependence polarization the onstrate dem images SEM nanometers. of 60 awidth has (b) wire single (c) double, the and and nanowires, triple 3.37 FIGURE ing to the layer the to ing follows: as formationmay represented be - lead reactions chemical remove to used The reaction. been the bubble gas has the formationduring TX-100 Nonionic reaction. surfactant chemical the bubbles through bath have the in formed been with pale have the yellow,substrate to films been Many adherence andfound. gas good uniform of 343 temperature bath condition constant ing and previousfor the to solution. 15 water is added solution stirred distilled The been has solution (25%). ammonia drop-wise add to beaker glass asolution Thereafter, of TX-100 double and 3.4.1.2 [122] 3.38 (Figure ). hydroxides amorphous of the crystallohydrates gels the coprecipitated of in the by freezing the (the 360°C and removal of hydroxyl groups). 3.37b Figure shows reductionwater of content the 165°C in recorded water) effects are (theendothermic crystallization removal and of adsorption by DTAstudied 3.37). (Figure 3.37a Figure In gels two precipitated of without the freezing, solution aqueous homogeneousclear an of solution. all, 0.01 After nanofilms of CdS, an aqueous solutionan CdS, of nanofilms of 0.02 have Depositiondeposited on ofbeen nanofilms CdS glass substrates. depositionFor well cleaned of

C M hemical Bath Techniquehemical olecular Layerolecular Deposition

[( (d) (a) Cd S EM images of nanowires grown from horizontally polarized laser radiation show: (a) radiation laser single, polarized horizontally from grown of nanowires images EM NH 3n )] 60 nm 2 [) +− Cd(N CS(N ++ CS(N Hn

H) h 3 . Thermolysis of the synthesized powders on. Thermolysis CeO synthesized of based the 22 H) 22 ], (b) (e) +→ 22 ++ 2O … 2O HC Cd −− HC

M ca →+ +

HN K a dmium chloride anhydrous has been taken in a in taken been has anhydrous chloride dmium nN 22 ds Hn nd pH solution of the at11.60. resulted The film 3 + 2H = CN 12 (c) 2 (f) ,, OS 22 Hn +

36 , 4, 3908–3912.) 4, , M t , ++ 2 hiourea is added under mix under is added hiourea

Nanocomposite Materials Nanocomposite NH

32 HO 2H

m

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N Hydrothermal Method Combined with aMild Ultrasonic with Combined Hydrothermal Method Graphene-Based Nanocoatings Graphene-Based a n o 2 DTA and TG curves of coprecipitated powders in ZrO powders in of coprecipitated DTA curves TG and c /Fe oati 3 O n 4 nanocomposite with good stability and photocatalytic efficiency degrade to photocatalytic and stability good with nanocomposite gs 2 /Ar gas flow at normal pressure to produce continuous and uniform carbon carbon uniform and continuous/Ar produce to pressure flow gas at normal , 111, 2012, 043519-6.) (b (a) ) DT DT TG TG A A h under protecting H protecting h under 165°C 2 nanosheet-coated Fe nanosheet-coated 360°C 2 /Fe 3 O 540°C 4 2 nanocomposite have nanocomposite verified mag by been /Ar gas, and then immersed into 1MNaOH into /Ar immersed then gas, and 570°C 3 O 4 2 nanocomposite [124]. nanocomposite method This –CeO 2 system (a) the freezing without nm pore diameter, the the diameter, pore nm 2 O 73 - - 3 2

Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 and then graphene oxide is later reduced by a strong reducing agent known as hydrazine hydrate. by oxide agent hydrazine astrong reducing graphene reduced as is later known then and permanganate, potassium hydrochloric acid, and acid, of presence sulfuric oxide the graphene into in are oxidized flakes graphite method, oxide. graphene this oxide In synthesis of reduced graphene and graphene. 1100°C. to uum production of quality is mass high method advantages of of One the this atlow heated and vac- afurnace into placed are substrates the method, this catalysts. In as used are Si coverage. large showson the substrate and excellent quality the crystal grown graphene themselves layers. graphene into epitaxial The rearrange to substrate the from mate subli atoms silicon time, this vacuum In graphene. under produce to temperatures athigh heated 2004 [125].in time for isolate to first very graphene method the this used Novoselov of and scale production. Geim small very is Its due disadvantage sheets. the to graphene 74 [131].of is described zeolite a Teflon-linedtypically autoclave. preparation the In following,for procedure hydrothermal ausual container, reaction is asealed put in precursor appropriate an as silicoaluminate technique, this synthesis conditions [129].adjusted controlling with be morphology can their also and zeolites; purity for higher with example, produced be can they nectivity. have zeolites natural to synthetic It that some should comparison noted advantages be in con and sizes pore distinguished with zeolites forming to lead by templates that various produced 10 5to from ranging typically sizes pore with or silicates nosilicates alumi crystalline microporous, are Zeolites imaging. fieldanddelivery the in drug interest of great materials. porous following, the in thus, book; brieflyof nano we this preparation the some about will explain facts such clay as oxide. multilayered graphene and materials intercalated extremely and nanocomposites, nanoporous, contain nanomaterials examples of three-dimensional most important The close matrix. in the with contact are that of nanomaterials of any kind types beyond dimensions have 100 three materials dimension. These any in nanoscale the to not limited are that materials are nanomaterials or bulk Three-dimensional 3.5 The last method is a chemical method (Hummer’s for method method the is achemical last method), method main whichThe is the vapor depositions is chemical method (CVD) or nickel copper like which third substrates in The (SiC). carbide SiC silicon from method, is growth this In epitaxial is the method second The The most significant method for preparation of zeolites is the hydrothermal technique technique [130].the is zeolites hydrothermal of method mostpreparation In for significant The have mesoporous silica, and such zeolites obtained as mesoporous materials, and Microporous • • • groupsIUPAC: by three classifiedinto are Nanoporous materials of parts other in detail in discussed are Synthesis multilayered of and nanocomposite particles 2. 4. 3. 1.

amount of zeolite crystals and could be obtained by purification, washing, and drying. and bywashing, purification, obtained could be and of crystals zeolite amount dissolved solution the in precursors convertFinally, identical anearly amorphous to all is observed. crystals zeolites first the producing onset temperature passing the for after along and amorphous time, remain reactants The oven. apreheated or in reactor solution aqueous asealed in The is heated pH values. high essential obtain to applied agents, are ion hydroxides, well mineralizing as which known are alkali dissolved Usually, abasic are in medium. alumina of and silica precursors Amorphous nm 50–1000 materials: Macroporous 2–50 nm Mesoporous materials: 0.2–2 nm materials: Microporous THREE-DIMENSIONAL MATERIALS THREE-DIMENSIONAL nm, but one or more may comprise nm, Å [128]. could be material This Nanocomposite Materials Nanocomposite - - - - Downloaded By: 10.3.98.104 At: 01:06 28 Sep 2021; For: 9781315372310, chapter3, 10.1201/9781315372310-3 Synthesis of Nanomaterials Synthesis mechanism is very useful. is very mechanism [132–134]. procedure total of the by kinetics negligible.is controlled generally the of is mainly Therefore, zeolite preparation of zeolite preparation enthalpy change bonds). for total thermal (Si–O–Al the lite reason, For this bonds) zeo produced oxides and Al–O (Si–O and precursor in bond type dueobserved asimilar to no considerable method, enthalpy change is this In produced. could be bonds, Si–O–Al comprise units. smaller form to of chains depolymerization causes mixture the Heating precursors. of the ratio, purity solution and of pHsilicon/aluminum value, reactants, nature factors such on various depend as which phase, features precrystalline the as is known exist. This oligomer silicate and chains aluminate which both in gel make would obtained be aprecursor silicate, to aluminate By adding precursors. as used are aluminate sodium well water as glass—and known REFERENCES future. the near in attention more find will terials - nanoma respectively.groups, three-dimensional and Nevertheless, two- that it anticipated could be priority are nanomaterials one-dimensional and concluded so on.be zero- nique, It and that can - tech bath chemical method, discharge arc ablation laser method, method, microfluidic method, microwave-assisted emulsion synthesis, sol–gel aerosol method, synthesis, sonochemical method, have considered; however, been nanomaterials such emphasis was as mostly methods on chemical different of preparation methods for synthesis specific and General two-, three-dimensional. and four including into one-, groups, zero-, have categorized been few past nanomaterials the The years. worldwide wide attention gained has in that area research interdisciplinary Nanotechnology is an 3.6

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