CH 2. Ion-transport studies on Ba-nano ferrite dispersed PVA : (NH 4 Polymer Electrolyte

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46 Hkkjrh; oskkfud,oa vks ksfxd vuqla/kku if=kdk o"kz 22 vad 1 twu 2014 i`- 46-52 csfj;e usuks QsjkbV forfjr PVA : (NH 4 cgqyd os qr vi?kv~; esa vk;u ifjogu dk v/;;u,l,y vxzoky] ih ds 'kqdyk*] nhif'k[kk f=kikbh,oa punz izdk'k flag,l-,l-vkbz- iz;ksx'kkyk] HkkSfrdh fohkkx], ih,l fo'ofo ky;] jhok 486 003 ¼e-iz-½ *vkbz-vh-,l- vfhk;kaf=kdh egkfo ky;] xzsvj uks,mk 201308 ¼m-iz-½ lkjka'k % izlrqr dk;z esa usuks vkdkjh; csfj;e QsjkbV fefjr ikwyh fouk;y,ydksgy (PVA) vk/kkfjr usuks lfeefjr cgqyd tsyh; os qr vi?kv~; dks os qr jklk;fud ;qfdr ds vuqiz;ksx gsrq rs;kj fd;k x;ka jklk;fud vfhkfø;k }kjk usuks vkdkjh; csfj;e QsjkbV d.kksa dks PVA : (NH 4 ds tkydh; os qr vi?kv~; esa Hkfjr djds usuks lfeefjr cgqyd tsyh; os qr vi?kv~; (NCPGE) dh ijr dks la'ysf"kr fd;k x;ka Hkjd d.kksa ds,dl fdj.k foorzu ifj.kke izeq[kr% "kv~qydh; izkoflfkr usuks QsjkbV ds cuus dks n'kkzrs gasa lkfk gh,dl fdj.k foorzu v/;;u lfeefjr os qr vi?kv~; esa usuks Hkjd dh lkunzrk c<+us ls bl os qr vi?kv~; ds vukdkjh; O;ogkj esa lq/kkj dks n'kkzrk gsa izdk'kh; lw{en'khz (OM) rfkk LdSfuax bysdvªkwu lw{en'khz (SEM) }kjk bl tsyh; os qr vi?kv~; esa lfeefjr Hkjd dk fo"kekaxh forj.k ik;k x;ka pøh; fohko /kkjkfefr (CV) vf/kdre os qr jklk;fud Hkzkfedk ±1.8V ds lkfk vpnh iqu% pøh;rk dks n'kkzrk gsa izfrck/kk LisDVªen'khZ (Impedance Spectroscopy) ds ek/;e ls dh xbz os qr vi?kv~; dh vk;fud pkydrk dh x.kuk n'kkzrh gs fd usuks QsjkbV Hkj.k ls os qr pkydrk esa o`f) gksrh gsa lkfk gh ;g Hkj.k lkunzrk rfkk rki ls Hkh pkydrk es a o`f) n'kkzrk gsa vi?kv~; ijrka s dh ac pkydrk tku'pj ds?kkr fu;e dk ikyu djrh izrhr gksrh gsa Ion-transport studies on Ba-nano ferrite dispersed PVA : (NH 4 Polymer Electrolyte S L Agrawal, P K Shukla*, Deepshikha Tripathi & Chandra Prakash Singh SSI Laboratory, Department of Physics, A P S University, Rewa 486 003 (M.P.) * I.T.S Engineering College, Greater Noida 201 308 (U.P.) Abstract An attempt has been made in the present work to develop a nano sized Ba-ferrite doped PVA based nano composite polymer gel electrolyte for electrochemical device applications. Nano sized Ba-ferrite particles prepared through chemical route were dispersed in matrix electrolyte of PVA : (NH 4 to obtain NCPGE films. XRD result on a synthesised filler particle depicts formation of nano ferrite with hexaferrite as the major phase. Further XRD studies on NCPGE show improvement in amorphous character with increasing concentration of nano fillers in composite electrolytes. OM and SEM examination of NCPEs shows heterogeneous distribution of fillers. Cyclic voltammetric measurement reveals optimum electrochemical window of ±1.8V with good recyclability. Ionic conductivity of electrolyte evaluated from impedance spectroscopy technique shows enhancement in electrical conductivity upon dispersal of nano fillers which increases with filler concentration and temperature. Jonscher power law seems to be obeyed during ac conductivity measurement of the films. izlrkouk lu~ 1973 esa Bksl volfkk cgqyd fo qr vi?kv~; ds izfke izfrosnu vkus ds i'pkr~ Bksl volfkk os qr vi?kv~; ds bl mi{ks=k us fofhkuuk oskkfud i`"bhkwfe okys 'kks/kkffkz;ksa dk /;ku vkdf"kzr fd;k gsa fofhkuuk cgqyd os qr vi?kv~;ks a es a iz;qdr cgqydks a es a ikwyh fouk;y,ydksgy (PVA),d,slk cgqyd gs ftldk iz;ksx os qr vi?kv~;ka s es a fd;k tk jgk gs D;ks afd bles a vpns ijkos qrh; xq.k vksj o`gr rki vuqiz;ksx pksm+kbz ¼T m ls T g ijkl rd½ ds xq.k gsaa blds vfrfjdr bl foyk;d ds Qqfyr xq.k ds dkj.k ;g cgqyd tsyh; os qr vi?kv~; ds fuekz.k dk lw=k/kkj gsa ikwyh fouk;y,ydksgy

a vxzoky,oa vu; % csfj;e usuks QsjkbV forfjr PVA : (NH 4 cgqyd os qr vi?kv~; esa vk;u ifjogu dk ;;u 47 (PVA) ds vks ksfxd egro,oe~ o`gr vuqiz;ksx gksus ds ckn Hkh blesa vk;u pkydrk dk O;ogkj vhkh rd iw.kz:is.k ugha le>k tk ldk gsa dbz 'kks/kkfkhz vius iz;ksxks a }kjk fn[kk pqds gs a fd cgqyd eas _.kk;u@/kuk;u xfr'khyrk vukdkjh; volfkk esa gksrh gs vksj bldk folj.k dk rjhdk tfvy gs rfkk ftlesa PVA dh [k.mh; xfr'khyrk dh izfrhkkfxrk gksrh gs 3 A 'kq) cgqyd lajpuk esa lq/kkj djds vfkok yo.k feykdj vfkok fdlh lq?kvudkjd ds iz;ksx }kjk vfkok Hkjd d.kks a ls fu;fer isfdax dks jksddj 'kq) vkdkjh; lajpuk ls cpk tk ldrk gsa pw afd cm+ s /kuk;u vkos'k vlfkkuhdj.k dh vf/kdrk j[krs ga S] blfy, cm+s /kuk;u okys yo.k i`fkddj.k ds fy, fueu tkyd ÅtkZ dh lehkkouk n'kkzrs gsas 4]5 A blds vfrfjdr cm+s /kuk;u følvyu izfø;k esa vojks/k isnk djrs gas ftlds dkj.k vukdkjh; volfkk esa o`f) dh lehkkouk gksrh gsa ;s nksuksa rf; fudk; dh vk;fud pkydrk esa egroiw.kz o`f) ds fy, fteesnkj izrhr gksrs gsaa usuks vk;keh vdkczfud@dkczfud Hkjd tkyh; os qr vi?kv~; es a lekos'k ls u dsoy fudk; dh følvyrk es a deh djrk gs vfirq vurjki`"bh; lrg ls vk;uks a ds xeu es a o`f) djrk gs tks,d lgt ifk gks ldrk gsa bl izdkj vk;u xeu dh izo`fùk esa lq/kkj lahkkfor gss 6 A blds vfrfjdr] cgqyd tsyh; os qr vi?kv~; dks mi;qdr os qr vi?kv~; ds :i esa ns[kk tk jgk gs] D;ksafd bldh pkydrk rjy os qr vi?kv~; ds led{k izkir dh tk ldrh gss 7 A fdurq yecs le; rd j[kus ij rjy ds {kj.k ls budh vk;fud pkydrk esa deh vkrh gsa finys dqn o"kksza ls] cgqyd tsyh; os qr vi?kv~; dh bl deh dks nwj djus ds fy, lfeefjr,oa Hkjd ifj{ksfir tsyh; os qr vi?kv~; lecfu/kr 'kks/k fp=k 1 usuks vkdkjh; csfj;e QsjkbV dk,dl fdj.k foorzu fp=kke izdkf'kr gq, gsas 8 A mpp vk;fud pkydrk] vpnh ;kfu=kdh;,oa os qr jklk;fud 'kq)rk ds lkfk gky es a vxzoky,oa muds lg;ksfx;ks }kjk Al 2 vksj CNT vifefjr PVA : NH 4 SCN tsyh; os qr vi?kv~; ij 'kks/k izdkf'kr fd, x, gsa 8]9 A bl izdkj ds fudk;ksa esa] rjy dks tsyh; tkydksa esa yecs le; ds fy, j[kk tk ldrk gsa e`fùkdk (ceramic) Hkjdksa ds leqnk; esa yksg os qr QsjkbV,oa f}qyfud vkwdlkbm u;s lnl; gsa] ftudk iz;ksx usuks lfeefjr cgqyd tsyh; vi?kv~; (NCPGE) fodflr djus ds fy, lqyrkiwozd fd;k tk jgk gs 10 A bl izdkj ds Hkjd d.kksa ds vifej.k }kjk Mªx fmfyojh fudk;ksa] os qr pqecdh; tsls u;s vuqiz;ksxks a vkfn dks fodflr fd;k x;k gsa ikwyh fouk;y,ydksgy esa QsjkbV vifej.k ls PVA ds /kzqoh; vfhkyk{kf.kd xq.k esa o`f) lahkkfor gs] tks os qr vi?kv~; dh pkydrk esa o`f) dj ldrk gsa PVA vk/kkfjr os qr vi?kv~;kas dks QsjkbV ls Hkkfjr djus ij og fofhkuuk LFkkuks a ij flfkr jg ldrk gsa vukdkjh; vfkok vkdkjh; lhekvksa ij cgqyd J`aa[kyk esa budk izfrlfkkiu gks ldrk gs rfkk cgqyd ds vukdkjh; {ks=k esa ojh; :i esa fo eku jg ldrk gsa blds vfrfjdr] QsjkbV ds fej.k ls ;g fuf'pr gks pqdk gs fd ;g vkos'k okgdkas ds xeu ds fy, vfrfjdr Qqnd LFky fufezr djrk gs ftlds dkj.k vk;uksa dh lkunzrk esa o`f) gksrh gs rfkk ftlds QyLo:i] pkydrk esa o`f) gksrh gs 11]12 A vr% mijksdr ds ifjizs{; esa izlrqr 'kks/k esa usuks vkdkjh; csfj;e QsjkbV Hkjd dk iz;ksx dj usuks lfeefjr PVA : (NH 4 vk/kkfjr os qr vi?kv~; dks fodflr fd;k x;k gs vksj blds vfhkyk{kf.kd xq.kksa dk v/;;u fd;k x;k gsa lkexzh,oa fof/k csfj;e QsjkbV usuks Hkjd dk la'ys"k.k % iwozorhz foy;u rs;kj djus ds fy, mppk 'kq)rk ds fy, Qsfjd ukbvªsv [Fe(NO) 3 9H 2 O > 98.0%] rfkk csfj;e ukbvªsv [Ba(N ) 2 > 99.0%] vksj lkbfvªd vey [C 6 H 8 O 7.H 2 O] dk mi;ksx fd;k x;ka bu lhkh ukbvªsvkas dk f}vklfor ty esa fej.k] foy;u esa 6-7 ph eku ds e/; j[krs gq, rs;kj fd;k x;k gsa bl izdkj izkir foy;u dks tsyh; volfkk esa ifjofrzr djus gsrq pqecdh; foyksmd dh lgk;rk ls yecs le; ds fy, 80 C rkieku ij foyksfmr fd;k x;ka bl tsy dks 22?k.Vs ds fy, 150 C rkieku ij lq[kk;k x;ka 450 C ij rkih; mipkj i'pkr~ mls pwf.kzr dj NCPGE ds la'ys"k.k ds fy, csfj;e QsjkbV dk eghu pw.kz izkir fd;k x;ka

48 Hkkjrh; oskkfud,oa vks ksfxd vuqla/kku if=kdk o"kz 22 vad ¼1½ twu 2014 usuks lfeefjr cgqyd tsyh; os qr vi?kv~; dk la'ys"k.k (Synthesis of NCPGE) % usuks lfeefjr tsyh; os qr vi?kv~; dk la'ys"k.k fpj&ifjfpr foy;u fulfkkj.k rduhd }kjk djus ds fy, ikwyh foukby,ydksgy (Mw=85,000),oa yo.k (NH 4 (Mw=216) dk mi;ksx fd;k x;ka 'kq) cgqyd os qr vi?kv~; foy;u rs;kj djus gsrq mifoyk;d DMSO dk mi;ksx fd;k x;k blds i'pkr~] lkwy&tsy fof/k }kjk rs;kj csfj;e QsjkbV pw.kz dks 60 C ij PVA : (NH 4 : DMSO foy;u ds mfpr rrokuqikr esa feykdj fujarj pqecdh; foyksmd }kjk 10 ls 12?k.Vksa ds fy, foyksfmr djrs gasa vur esa isvªhfm'kksa esa izkir tsyh; foy;u dks Hkj fn;k x;ka izkir ijr dks izk;ksfxd v/;;u gsrq 30 C rkieku ij fuokzr esa lq[kk;k x;ka vfhky{k.ku % usuks Hkjd pw.kz ds lajpukred O;ogkj,oa følvyh; vkd`fr dk v/;;u,dl&fdj.k foorzu (Rikagu Miniflex-II) }kjk 150 ls 800 czsx dks.k ¼2θ½ rd fd;k x;ka QsjkbV pw.kz dh fofodr vkdkfjdh ds v/;;u gsrq LdSfuax bysdvªkwu lw{en'khz (Carl Ziess make SEM model Supra TM 40 VP),oa izdk'kh; lw{en'khz (Carl Ziess make model 482SP 22012) }kjk vfhkyf{kr fd;k x;ka os qr jklk;fud Hkzkfedk,oa vkos'kksa ds xeu dh izd`fr ds v/;;u gsrq CV vksj I-t dk ekiu os qr jklk;fud odzlvs'ku (CH Instrument model CH 608) }kjk fd;k x;ka os qr pkydrk dk v/;;u fofhkuuk rkiekuksa (283k to 363k),oa vko`fùk ijkl 40Hz vksj 100kHz ds e/; fg;ksdh QeZ }kjk fufezr,y lh vkj ;a=k (model 3520) }kjk fd;k x;ka ifj.kke,oa foospuk,dl fdj.k foorzu dk v/;;u la'ysf"kr usuksfefjr cgqyd tsyh; os qr vi?kv~; (NCPGE) vksj bles a iz;qdr csfj;e QsjkbV d.kks a dh izkolfkk vfhkfu/kkzj.k,oa vkdkj fu/kkzj.k gsrq mudk,dl fdj.k foorzu }kjk lajpukred vfhky{k.k fd;k x;k gsa fp=ke 1 esa lksy&tsy fof/k }kjk fufezr csfj;e QsjkbV dk,dl fdj.k foorzu (XRD) fp=k esa n'kkz;k x;k gsa ;s fp=k vusd følvyh; J`axksa ds vflrro dks n'kkzrs gsa tks QsjkbV pw.kz dh følvyh; vkdkfjdh dks izdv djrk gsa,dl fdj.k foorzu ls izkir vkdm+ksa rfkk JSPDS ls izkir vkdm+ksa dk rqyukred v/;;u csfj;e gsdlk QsjkbV (BaFe 12 O 13 ) (2θ=30.3, 35.6, 37 and 63 ),oa csfj;e,do.khz volfkk QsjkbV (BaFe 2 O 4 ) (2θ=27.6, 43.4, 46.8 and 49.2 ) ds fej.k dh miflfkfr iznf'kzr djrk gsa 33.3 ds fudv miflfkr LdU/k J`ax U;wu ek=kk esa BaC ds fuekz.k ls lg&lecfu/kr fd;k tk ldrk gsa blh izdkj] yxhkx 30, 53.7 vksj 63.3 ds fudv dbz NksVs J`ax α Fe 2 dh miflfkfr v'kqf) ds :i esa QsjkbV ikmmj esa miflfkfr n'kkzkrs gasa BaC vksj α-fe 2 dh miflfkfr lehkor% tsy pw.kz ds de rki ij fulrkiu ds QyLo:i gs 13 A,Dl fdj.k foorzu ls BaFe 12 O 19, BaFe 12 O 4, α-fe 2 vksj BaC dh miflfkfr dk irk pyrk gs] fdurq mlesa eq[;?kvd gsdlk QsjkbV gsa la'ysf"kr d.kks a ds følvyh; vkdkj dk fu/kkzj.k gsdlk QsjkbV (2θ=35.6 ),oa,do.khz QsjkbV (2θ=43.4 ) ds eq[; J`ax ds fy, fmckbz 'ksjj lecu/k dk mi;ksx dj fd;k x;k 14 A bl laca/k ds vuqlkj] d = 0.9λ βcos θ (1) tgk β Jàx dh jsfm;e esa lokszppk Jàx dh v/kz Å pkbz ij Jàx dh iw.kz pksm+kbz] d d.k dk følvyh; vkdkj] λ,dl fdj.k iq at dk rjax ns/;z,oa θ J`ax ds fy, czsx dks.k gsa bl ifjdyu ls vkslr d.kksa dk vkdkj 15.36 nm izkir gqvk tks QsjkbV Hkjd ds usuks vkd`fr dh iqf"v djrk gsa cgqyd tsyh; os qr vi?kv~; DMSO : (NH 4 : PVA csfj;e QsjkbV Hkjd ikmmj ds fcuk vksj mlds fefjr ru=k dh,dl fdj.k foorzu (XRD) vkd`fr dks fp=k 2 esa iznf'kzr fd;k x;k gsa lhkh,dl fdj.k foorzu fp=ke] usuks vkdkjh; Hkjd dks fefjr djus ij cgqyd tsyh; fp=k 2 0-8 eksy NH 4 ( esa fofhkuu csfj;e QsjkbV lkunzrk (a) 0.0 (b) 0.5 (c) 0.9,oa (d) 1.1 wt % ls fufezr usuks lfeekfjr tsyh; cgqyd vi?kv; ds,dl fdj.k foorzu fp=kke

vxzoky,oa vu; % csfj;e usuks QsjkbV forfjr PVA : (NH 4 cgqyd os qr vi?kv~; esa vk;u ifjogu dk ;;u 49 os qr vi?kv~; dh izeq[k J`ax dh pksm+kbz esa o`f) dks n'kkzrs gsaa iwoz esa] DMSO esa fufezr PVA dh tsyh; irz ds v/;;u esa,d lkis{kh; rh{.k J`ax 2θ = 19.6 vksj,d LdU/k J`ax yxhkx 2θ = 9 ij flfkr ik;k x;k gs 7 A Jàx dh pksm+kbz vksj 2θ dk eku 0.5wt% ek=kk esa csfj;e QsjkbV usuks Hkjd dks vifefjr djus ij mppk 2θ dks.k dh rjq fn[krk gs tks QsjkbV ds tsyh; vko;wg esa lafuos'ku ds QyLo:i gsa fp=ke (b) esa nks NksVs Lda/k J`ax 2θ=36.1 vksj 2θ=43.7 ij fn[kkbz im+rs gasa ;g NksVh Ja`xas lehkor% csfj;e gsdlk QsjkbV dh J`axas (2θ=35.94 vksj 43.3 ) gas] tks QsjkbV ds cgqyd rfkk yo.k dh ijlij fø;k ds dkj.k LFkkukUrfjr gks x;h gsaa,dl fdj.k foorzu fp=ke esa csfj;e QsjkbV ¼fp=k 1½ ls lacaf/kr dksbz vu; Jàx izkir u gksus dk rkri;z ;g gs fd Hkjd d.kks a vksj tkydh; os qr vi?kv~; ds e/; etcwr ikjlifjd fø;k gks jgh gsa Hkjd dh vuqikr ek=kk 0.9wt% rd c<+kus ij 2θ=36.1 vksj 47.74 ij flfkr J`ax ¼foorZu fp=k½ ds xk;c gksus ds lkfk eq[; J`axkas dh rhozrk esa deh,oa pksm+kbz esa o`f) gksrh gs] tks csfj;e QsjkbV ds d.kks a ds tkydh; os qr vi?kv~; esa leiw.kz vo'kks"k.k dks n'kkzrk gsa csfj;e QsjkbV dh lkunzrk vksj c<+kus (1.1 wt%) ij usuks Hkjd ds vfhky{kf.kd ijkorzu iqu% fola;kstu ds dkj.k izdv gksrs gsa ¼fp=k 2½A,Dl fdj.k foorzu v/;;u ls ;g fu"d"kz fudyrk gs fd csfj;e QsjkbV usuks Hkjd dk cgqyd os qr vi?kv~; esa vf/kdre vo'kks"k.k 0.9wt% gsa lkfk gh] ;g csfj;e QsjkbV cgqyd yo.k dh ijlifjd fø;k vukdkjh; izd`fr ds lkfk n'kkzrk gsa vkdkj,oa vkd`fr esa d.k,df=kr gsaa bl izdkj dh tkudkjh Vksiky,oa muds lg;ksfx;ks a 15 vksj lkstjh,oa lg;ksfx;ks a16 }kjk Hkh nh xbz gsa LdSfuax bysdvªkwu lw{en'khz ls izkir izfrfcec es a lw{e v/ ;;u ls dqn xksyh; d.k Hkh fn[kkbz nsrs gsa tks,do.khz QsjkbV dh miflfkfr dks Hkh crkrs ga S ftldk lk{; gedks fp=k 1 es a,dl&fdj.k foorzu ds v/;;u ls Hkh izkir gqvk gsa estcku ikwyh fouk;y,ydksgy cgqyd lw{e lju/kz:ih <k pk j[krk gsa yo.k ds vifej.k ds ckn nzo; fnnzks a es a ik'ku (trapping) ds ckn vksj PVA ds lkfk vur% fø;k ds QyLo:i lju/kz fnnzksa dk vkdkj?kvus yxrk gsa bl izdkj] 'kq) os qr vi?kv~; fudk; vukdkjh; lajpuk viukrk gs tks fp=k 2 ¼c½ esa iznf'kzr gsa [PVA : (NH 4 ] : xwt% csfj;e QsjkbV ¼tgk x=0.7 vksj 0.9 wt%½ dk izdk'kh; izfrfcec 3¼l&n½ esa fn[kk;k x;k gsa Hkjd ds y?kq lkunzrk gksus ij d.kks a dk vlekaxh forj.k fn[kkbz im+rk gsa Hkjd dh lkunzrk c<+kus ij PVA os qr vi?kv~; dh lajpuk vius vkjafhkd vkdkj ls cnyrh fn[kkbz nsrh gsa fp=kksa 3¼l&n½ ds rqyukred v/;;u ls irk pyrk gs fd tgk d.kksa ds leku :i ls forj.k esa o`f) vksj nwljh vksj izkjafhkd lajpuk esa cnyko ds dkj.k LihuksMy vi?kvu izdkj dh lajpuk fn[krh gs] tks PEO : NH 4 SCN : AlZn QsjkbV fudk; ds fy, Hkh crkbz xbz gs 17 A izdk'kh; vksj LdSfuax bysdvªku lw{en'khz }kjk v/;;u fp=k 3 es a KBr fefjr la'ysf"kr usuks QsjkbV pw.kz 'kq) os qr i?kv~;,oa fofhkuuk Hkjd lkunzrk okys NCPGE dk izdk'kh; izfrfcec iznf'kzr gsa fp=k 3¼v½ esa nf'kzr izdk'kh; izfrfcec esa NM+ :ih vkdkj 'kq) csfj;e QsjkbV ds vleku forj.k ds lkfk fn[krk gsa NM+:ih d.k dk vkslr vkdkj yxhkx 150-200nm ik;k x;ka lkwy&tsy fof/k ls izkir QsjkbV d.kksa dk SEM izfrfcec Hkh [khapk x;k gs ¼fp=k bz rfkk ;½ gok eas 450 C ij 3?k.Vs rd fulrkfir mrikn dk izfrfcec d.kksa ds vleku forj.k ds lkfk "kvqydh; ifv~vdk dks iznf'kzr djrk gsa blds vfrfjdr] fofhkuuk fp=k 3 'kq) csfj;e QsjkbV d.kksa dk LdSfuax bysdvªku lw{en'khz izfrfcec ¼v,oa c½,oa 'kq) csfj;e QsjkbV ¼l½ 0.0 wt % ¼n½ 0.7 wt % ¼b½ 0.9 wt % ¼Q½ csfj;e QsjkbV usuks vkdkjh; d.kksa ls fufezr usuks lfeejr os qr vi?kv~;ksa dk izdk'kh; izfrfcec

50 Hkkjrh; oskkfud,oa vks ksfxd vuqla/kku if=kdk o"kz 22 vad ¼1½ twu 2014 fohko /kkjkfefr v/;;u fp=k 4 es a 'kq) vksj usuks csfj;e QsjkbV Hkfjr lfeefjr os qr vi?kv~; ds Øfed fohko /kkjkfefr fp=ke dks fn[kk;k x;k gs A dbz pø rd iz;ksx djus ij lhkh lfeefjr os qr vi?kv~;ksa esa NksVs dsfkksfmd,oa,uksfmd J`ax yxhkx ±1.3 V ij fn[kkbz nsrs gsaa ;s J` ax eq[;r% cgqyd lfeefjr os qr vi?kv~; es a foyk;d (DMSO) ds vkwdlhdj.k vip;u ds dkj.k fn[kkbz nsrs gsa ftldk lk{; foyk;d DMSO dh IR vksj CV v/;;u }kjk Hkh izkir gksrk gsa,d NksVh vkwdlhd`r Ja`x 0.5V ij izkir gksrh gs tks NH 4+ /H + vk;u ls lecfu/kr gsa ;g lfeefjr os qr vi?kv~; esa izksvkwuh pkydrk dks n'kkzrk gs9]18 A csfj;e QsjkbV usuks Hkjd dks 0.5 ωt% rd cgqyd tsyh; os qr vi?kv~; esa lfeefjr djus ij os qr jklk;fud flfkjrk es a (1.8V) o`f) fn[krh gsa blls vf/kd csfj;e QsjkbV usuks Hkjd dh ek=kk c<+kus ij (0.9 ωt%) os qr jklk;fud flfkjrk?kvrh gs tgka bldh os qr jklk;fud Hkwfedk -1.4 V ls +1.4 V gsa blds ckn iqu% 1.1 ωt% rd vfhkfej.k ls os qr jklk;fud flfkjrk c<+rh gsa lfeefjr os qr vi?kv~; ds fy, vf/kdre os qr jklk;fud fohko dh Hkzfedk csfj;e usuks Hkjd ds 0.5 ωt% vuqikr ij (±1.8V) izkir gqbz gsa os qr jklk;fud fohko dk vf/kdre eku (± 1.8V) n'kkzrk gs fd bldk mi;ksx vk;fud midj.kks a [kklrksj ij Bksl volfkk csvjh ds fy, gks ldrk gsa os qr vi?kv~; fudk; dh mrøe.kh;rk dk v/;;u nl pøksa ds fy, fd;k x;k gsa fp=k 4 ¼b½ esa nl pø ds nksjku os qr jklk;fud fohko dh Hkzfedk esa folfkkiu ns[kus dks feyrk gs] fdurq bldh n{krk esa fxjkov dkqh de ns[kus dks feyrh gsa vk;u&ifjogu dk v/;;u lfeefjr tsyh; os qr vi?kv~; dh leiw.kz vk;u ifjogu la[;k] osxuj /kzqo.k rduhd }kjk vk;uh&vkos'kksa ds ifjogu dks izekf.kr djus gsrq Kkr fd;k x;ka [PVA : (NH 4 ] os qr vi?kv~; fudk; ij iwoz ds v/;;u ds vk/kkj ij [PVA : (NH 4 : x t% csfj;e QsjkbV [tgka x=0.5,0.7,0.9,oa 1-1ωt%] cgqyd os qr vi?kv~; fudk; Hkh xfreku vkos'k okgdks a dh izd`fr izksvkwuh lahkkfor gsa 0.5 V es a fd;k fohko iz;qdr djus ij /kkjk dk le; ds lkfk ifjorzu fp=k 5 esa iznf'kzr fd;k x;k gsa leiw.kz vk;u ifjogu dh x.kuk fueu lw=k }kjk dh xbz gs % fp=k 5 PVA : 0.8 M NH 4 ( COO)2 0.5 Wt % csfj;e QsjkbV usuks Hkjd lfeekfjr cgqyd os qr vi?kv; dk /kkjk /kqzo.k fp=kke t ion tinitial t final = ¼2½ t initial lfeefjr os qr vi?kv~; fudk; ds tion dk vf/kdre eku 0-98 csfj;e QsjkbV ds 0.5 ωt% vuqikr ij izkir gqvk gsa bl vk;u ifjogu dk mppre eku] fudk; esa vkos'k ifjogu izdkj vk;fud gksus dks izekf.kr djrk gsa fp=k 4 DMSO eas fufezr PVA : 0.8 M NH 4 ( tsyh; ijrksa (a) 0.5 wt % csfj;e QsjkbV Hkjd ds lkfk lfeekfjr os qr vi?kv; (b) fohko /kkjkfefr fp=kke fo qr pkydrk O;ogkj fp=k 6 esa csfj;e QsjkbV forfjr NCPGE dh lfe"v fo qr pkydrk dk O;ogkj Hkjd dh lkunzrk ds lkis{k iznf'kzr fd;k x;k gsa 'kq: esa csfj;e QsjkbV Hkjd dk vuqikr 0-5 ωt% rd c<+kus

vxzoky,oa vu; % csfj;e usuks QsjkbV forfjr PVA : (NH 4 cgqyd os qr vi?kv~; esa vk;u ifjogu dk ;;u 51 ij usuks lfeefjr cgqyd tsyh; os qr vi?kv~; dh pkydrk c<+rh gs] fqj 0.7 ωt% lkunzrk rd?kvrh gsa os qr vi?kv~; vfudk; es a Hkjd dh ek=kk FkksM+h vksj c<+kus ij FkksM+h cgqr o`f) gksrh gs fdurq rri'pkr rsth ls?kvrh gsa ;g,d izfr:ih lfeefjr os qr vi?kv~; ds O;ogkj dks n'kkzrk gs 7]8]19 A de lkunzrk (0.5 ωt% ls de) ij tkydh; os qr vi?kv~; esa Hkjd d.kksa dk vlekaxh forj.k cgqyd yo.k Hkjd dh vur% fø;k ds dkj.k vk;u ifjogu ds fy, u;s Qqnd LFky izlrqr djrk gs] ftlds QyLo:i ifjogu djus okys vk;uksa dh lkunzrk esa o`f) gksrh gsa lkfk gh Hkjd d.kksa ds feykus ij vukdkjh; O;ogkj esa o`f) izdk'kh; fp=k.k esa fn[kkbz xbz gsa vr% ;g nksuksa rf; lesfdr :i ls vk;fud pkydrk esa egroiw.kz o`f) fueu lw=k dss ifjizs{; esa n'kkzrsa gsaa ωt%) Hkjd d.k bdv~bs gks tkrs gsa tks vk;u ifjogu ds fy, dqfvy ifk dk fuekz.k djrs ga S vksj bl dkj.k pkydrk es a egroiw.kz deh izkir gksrh gsa fp=k 7 esa os qr vi?kv~; ds lkfk usuks lfeefjr cgqyd tsyh; os qr vi?kv~; dh pkydrk dh rki fuhkzjrk O;ogkj dks n'kkz;k x;k gsa Hkjd dh vuqiflfkfr es a pkydrk O;ogkj dks eq[; :i ls VTF rfkk vkjgsfu;l O;ogkj dks lekfgr djrs gq, fueu lecu/k n~okjk n'kkz;k tk ldrk gsa fp=k 7 csfj;e QsjkbV Hkjd ds fofhkuu vuqikr ( ) 0.0 Wt %, ( ) 0.2 Wt % ( ) 0.1 Wt % ( ) 0.5 Wt %, ( ) 0.7 Wt %, ( ) 0.9 Wt %,,oa ( ) 1.1 Wt % ds fy, cgqyd usuks lfeekfjr tsyh; os qr vi?kv;ksa dk rki fuhkzj os qr pkydrk O;ogkj fp=k 6 csfj;e QsjkbV Hkjd lkunzrk ds lkfk usuks lfeekfjr cgqyd os qr vi?kv; dh pkydrk dk lerkih; ifjorzu σ = neµ ¼3½ tc Hkjd ek=kk dks 0.5wt% ls vkxs c<+k;k tkrk gs rc czhfnax psu ekwmy }kjk of.kzr vk;u lgpj.k izhkko ns[kus dks feyrk gs tks vpkyh; vk;u ;qxeksa dh miflfkfr n'kkzrk gsa blfy, xeu ds fy, eqdr vk;uksa dh lkunzrk esa deh ds dkj.k pkydrk esa deh vkrh gsa iqu% tc Hkjd dh ek=kk 0.7 ωt% rd c<+k;h tkrh gs rc pkydrk esa FkksM+h ek=kk esa o`f) fudk; dh vkdkfjdh vk;uh pkydrk dks?kvrh okgd la[;k n ds Åij izhkkoh gksus ds dkj.k fn[krh gsa vurr% mpp lkunzrk ij (>1.1 σ = σ 0 exp (-Ea/KT) (4) σ = σ 0 T 1/2 exp (-Ea/KT) (5) tgka σ 0 izh pj?krkadh Xkq.kkad] Ea mriz sj.k ÅtkZ] K oksyvt+kesu fu;rkad,oa T 0 (= Tg-60 C) Doklh lke; Xykl laøe.k rkieku gsa Hkjd dh ek=kk c<+kus ij tsls gh vukdkjh; {ks=k esa o`f) gksrh gs] osls gh cgqyd J`a[kyk dh vkurfjd xfr vksj cu/kksa ds pø.k es a rhozrk vkrh gs tks l[k.mh; xfr es a o`f) djrk gsa fp=k 7 )kjk Kkr gksrk gs fd Hkjd dh ek=kk c<+kus ij usuks fefjr cgqyd tsyh; os qr vi?kv~; dh pkydrk es a folrkj,d?kkrkad es a lhfer gsa lkfk gh] mpp Hkjd vuqikr ij] VTF O;ogkj] vkjghfu;l O;ogkj esa ifjofrzr gks tkrk gs] ftldh leiw.kz O;k[;k lw=k ¼4½ }kjk dh tk ldrh gsa

52 Hkkjrh; oskkfud,oa vks ksfxd vuqla/kku if=kdk o"kz 22 vad ¼1½ twu 2014 fu"d"kz bl v/;;u esa usuks vkdkj ds csfj;e QsjkbV dk cuuk,dl&fdj.k foorzu,oa LdSfuax bysdvªkwu lw{en'khz n~okjk lqfuf'pr fd;k x;k gsa csfj;e QsjkbV ds følvyh; Ja`x],do.khZ,oa "kv~qydh; csfj;e QsjkbV ds fuekz.k dh iqf"v djrs gsaa d.kksa ds vkdkj dh x.kuk 'ksjj lw=k }kjk dh xbz gs tks 15.25nm izkir gqbz gsa LdSfuax bysdvªkwu lw{en'khz ds fp=k ls Hkh,do.khZ,oa "kv~qydh; csfj;e QsjkbV dh miflfkfr dk fu/kkzj.k gqvk gsa izdk'kh; lw{en'khz ds fp=k ls fliuksmy vi?kvu (spinodal decomposition) lajpuk Li"V gksrh gsa lfeefjr os qr vi?kv~; dk izdk'kh; lw{en'khz v/;;u vukdkjh; lajpuk Li"V djrk gsa lokszùke os qr jlk;u dh flfkjrk lfeefjr os qr vi?kv~; esa csfj;e QsjkbV Hkjd pw.kz dh ek=kk 0.5 ωt% gksus ij V izkir gqbz gsa os qr vi?kv~; ijrsa eq[;r% vk;uks a dh xfr'khyrk dks n'kkzrh gsa pkydrk O;ogkj dk v/;;u pkydrk esa,d vuqøe dh o`f) QsjkbV Hkj.k djus ij n'kkzrk gsa rki vkfjr pkydrk ds v/;;u es a VTF,oa vkjghfu;l O;ogkj la;qdr :i ls fn[krk gsa vkhkkj es a Jh vt; /kj,oa Jh Mh-ds- fejk] inkfkz fokku vfhk;kaf=kdh fohkkx] lh,lvkbzvkj - jk"vªh; HkkSfrdh iz;ksx'kkyk] ubz fnyyh Hkkjr] dk vkhkkj O;Dr djrk gw ftuds rduhdh lg;ksx ls vi?kv~; uewuksa dk,dl fdj.k foorzu,oa LdSfuax bysdvªku lw{en'khz fp=kke izkir gks ldka lunhkz 1- vksosu ts vkj] QkLV vk;u damfdvax ikwyhej bu lqij vk;fud lkwfym,.m lkwfym bysdvªksykbv~l fjlsuv VªsUM~l ¼bMh,l½,-,yyLdj],l punzk],dsmfed izsl] U;w;kdZ] ¼1989½ 111-2- vxzoky vkj lh,oa ik.ms; th ih] tuzy vkwq fqftdl Mh&,IykbM fqftdl] 41¼2008½ 223001 3- vxzoky,l,y,oa vof/k;k,] cqysfvu vkwq fevsfj;yl lkbul] 27 ¼2004½ 523-4- vjksjk,u,oa 'ks[ku,l,l] bu vk;u d.mfdvax fevsfj;yl F;ksjh,.M,Iyhds'ku ¼bZ Mh,l½, vkj dqyd.khz,oa ih xksikyu] ujkslk ifcyf'kax gkml] ubz fnyyh ¼2001½ 88-5- tsbzdqysdw vks bz ;kax ts] csyh vkj MCY;w],jhxj,l bz] isfuxavu MCY;w Vh,oa MslekjVsM Mh Mh] lkwfym LVsV vk;fudl] 148 ¼2002½ 173-6-,iSfVph th ch] tksu Mh,oa løkslvh ch] tuzy vkwq bysdvªksdsfedy lkslk;vh] 151¼2004½ 1369-7- vof/k;k,-] LVMht vkwu vk;u dumfdvax ikwfyej tsy bysdvªksykbv] ih,p-mh- ffkfll],-ih-,l- ;wuhoflzvh] jhok ¼e-iz-½ ¼2006½- 8- vxzoky,l,y] jk;,u] uvjktu Vh,l,oa pun,u] vk;fudl] 19 ¼2013½- 9- vxzoky,l,y] jk;,u,oa pun,u] buvjus'kuy tuzy vkwq ikwfyej fevsfj;y] 62 ¼2013½- 10- ik.ms; ds] f}osnh,e,e] flag,e,oa vxzoky,l,y] Qst+ VªkfUt'kUl] 84 ¼2011½ 343-11- ik.ms; ds] f}osnh,e,e] flag,e,oa vxzoky,l,y] tuzy vkwq ikwfyej fjlpz] 17 ¼2010½ 127-12- v ;j vkj] ns'kkbz vkj,oa mik/;k; vkj ;w] cqysfvu vkwq fevsfj;y lkbal] 32 ¼2009½ 141-13- uqjgnh,l] ckyw;ks] vyekftn] vcnqy,] egewn,,oa lksfyeku],mokul fevsfj;y fjlpz] 463 ¼2012½ 1468-14- dqyvh ch Mh],yhesUV vkwq,dl&js fmýsd'ku&ii ¼bZMh,u½],UMjlu os'ys yunu] ¼1978½ 281-15- xqirk,e,oa ;qxus MCY;w,y] bu % ekbøoso,.m esvyl] tkwu okbys,oa lul izkbosv fyfevsm] ¼2007½- 16- gqvkax ts] tqgqvkax,p,oa fy MCY;w] tuzy vkwq fevsfj;y fjlpz cqysfvu] 98 ¼2003½ 149-17- ik.ms; ds] f}osnh,e,e] flag,e,oa vxzoky,l,y] bu izksflfmax vkwq bysdvªks,fdvo ikwfyej % fevsfj;yl,.m fmokbl ¼b- Mh-,l-½,l-,- gkleh] vferk punzk,oa vejh'k punzk % esdfeyu ifcy'kj] ubz fnyyh] 3 ¼2009½ 184-18- pun,u] jk;,u] vxzoky,l,y,oa ivsy,l ds] cqysfvu vkwq fevsfj;y lkbul] 34 ¼2011½ 1297-19- ik.ms; ds] flag,e] vlfkkuk fuf/k] f}osnh,e,e,oa vxzoky,l,y] buvjus'kuy tuzy vkwq fevsfj;y lkbul] 1 ¼2010½ 9-20- vxzoky,l,y] 'kqdyk ih ds] vof/k;k,] ivsy vkj ch,oa ivsy,l ds] bu izkslsfmax vkwq bysdvªks,fdvo ikwfyej % fevsfj;yl,.m fmokbl ¼bZ-Mh-,l-½,l-,- gkleh vferk punzk,oa vejh'k punzk % esdfeyu ifcy'kj ubz fnyyh] 3 ¼2009½ 205-