Electrical and Magnetic Properties of Polyaniline-Nickel Ferrite Composites. Karnataka, INDIA.

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1 t Intrntionl Journl on Emrging Thnologis (Spil Issu on ICRIET-2016) 7(2): (2016) ISSN No. (Print) : ISSN No. (Onlin) : Eltril n Mgnti Proprtis of Polynilin-Nikl Frrit Composits Aji Kumr S Molkri *, A D Shtkr **, Rghunn B *** n Sngshtty Klyn **** * Assistnt Profssor, Dprtmnt of Physis, Guru Nnk Dv Enginring Collg, BIDAR , Krntk, INDIA. ** Assistnt Profssor, Dprtmnt of Physis, Krntk Arts, Sin n Commr Collg, BIDAR , Krntk, INDIA. *** Assistnt Profssor, Dprtmnt of Physis, Govrnmnt First Gr Collg, BIDAR , Krntk, INDIA. **** Assoit Profssor, Dprtmnt of Physis, Bhmnn Khnr Institut of Thnology, BHALKI , Krntk, INDIA. (Corrsponing Author: Sngshtty Klyn) (Riv 29 Sptmr, 2016 Apt 25 Otor, 2016) (Pulish y Rsrh Trn, Wsit: ABSTRACT: Polynilin-Nikl frrit omposits with iffrnt wight prnt of NiF 2 (10, 30 n 50 wt %) wr prpr vi intrfil polymriztion using mmonium prsulpht s n oxint, whrs NiF 2 ws synthsiz y omustion rout. Th prpr smpls wr hrtriz using som thniqus suh s FTIR, XRD n SEM. FTIR sptr rvl th formtion of som intrtions twn polynilin n NiF 2 prtils. XRD rvls th rystllin phs of omposits. Th AC onutivity is stui s funtion of frquny t room tmprtur in th frquny rng 10 Hz to 10 6 Hz. Th AC onutivity inrss s th frquny inrs. Th mgnti proprtis of th smpls wr msur t room tmprtur using virting smpl mgntomtr (VSM) in th fil rng G to G. Th omposits show frromgnti hvior. Ky Wors: Polynilin, Nikl frrit, Composits, Conutivity, Mgnti sturtion. I. INTRODUCTION Conuting polymrs hv ttrt muh intrst us of thir mny promising thnologil pplitions [1]. Among ll, polynilin is on of th most wily us onuting polymrs us of its s to synthsis, low nsity, low ost, goo prossility, xllnt nvironmntl stility, n high ltril onutivity [2-6]. Polyniln hs lso n us in mny pplitions suh s ltromgnti intrfrn (EMI) shiling, light-mitting ios, rhrgl ttry, hmil snsor, orrosion vis n mirowv sorption [7 10]. Mny kins of mtrils n us s mgnti prt of th omposit mtrils, suh s γ-f 2 O 3 [11], ZnF 2 [12, 13], CoF 2 [14], Co 3 [15] n BF 12 O 19 [16]. Among mgnti mtrils, th spinl frrits xhiitrmrkl mgnti proprtis prtiulrly in rio-frquny rgion, physil flxiility, high ltril rsistivity, mhnil hrnss n hmil stility [17]. NiF 2 is n importnt mgnti frrit whih hs n foun its xtnsiv pplitions in ivrs rs suh s prmnnt mgnts, roring mi, Frro fluis n gs snsors. In this ppr, NiF 2 prtils wr prpr y omustion rout, n Polynilin-NiF 2 omposits wr thn synthsiz vi intrfil polymriztion mtho using mmonium prsulpht s n oxiizing gnt. Th strutur n morphology of th polynilin, NiF 2 prtils n polynilin-nif 2 omposits hv n invstigt through FTIR, XRD n SEM. Th frquny pnn of AC onutivity invstigt in th frquny rng 10 Hz to 10 6 Hz. Thmgntiproprtisrmsurusingvirtingsmpl mgntomtr (VSM) t room tmprtur in th fil rng of G to G. II. EXPERIMENTAL All hmils us for synthsis r nlytil rgnt (AR) gr. Anilin n hyrohlori i hv n purhs from Alrih hmils. Anilin ws oul istill for us. Ammonium prsulpht is purhs from Quligns. Nikl frrit prtils wr synthsiz y omustion rout. Doul istill wtr ws us throughout th work.

2 Molkri, Shtkr, Rghunn n Klyn 165 As prpr nikl frrit ws us for prprtion of polynilin omposits. Th smpls so otin r rush finly in th prsn of ton mium in gt mortr n pross into irulr pllts of 10 mm imtr n thiknss vrying from 1 to 2 mm y pplying prssur of 90 MP using hyruli prss. For onutivity msurmnts, th pllts r ot with silvr pst on ithr si of th surfs to provi ttr ltril ontts. Synthsis of Polynilin. Th synthsis of polynilin ws s on mixing quous solution of nilin, hyrohlori n mmonium prsulpht t room tmprtur, follow y th sprtion of polynilin hyrohlori pripitt y filtrtion n rying. Anilin hyrohlori (quimolr volums of nilin n hyrohlori i) is issolv in oul istill wtr in volumtri flsk to 100 ml of solution. Ammonium prsulpht (0.25M) ws issolv in wtr lso to 100 ml solution n thn kpt for 1 hour t room tmprtur (25 o C), thn mix in kr, stirr mhnilly n lft t rst for omplt polymriztion. Aftr 24 hours th polynilin pripitt is ollt on filtr, wsh with 0.2M HCl n similrly with ton. Finlly, th rsultnt polynilin hyrohlori powr is ri in ir n thn vuum t 60 o C to hiv onstnt mss. Synthsis of NiF 2 prtils (Comustion rout). Nikl frrit prtils wr prpr y, known quntity of nikl slt n iron slt ws mix thoroughly n is groun wll with polyvinyl lohol in 1:5 in pstl n mortr. Th rtion mss ws trnsfrr in to ruil initilly urnt in n ltril ovn for omplt volution of th fums. Ni slt Mtl slts mixtur F slt (1:5) Rtion mixtur Complt omustion Crystllin prout NiF 2 prtils (rown olor) PVA (Ful) Fig. 1. Flow hrt: Synthsis of NiF 2 Prtils. Th rsultnt rsiu ws ht ontinuously for omplt omustion. Th rtion ws omplt within 30 minuts to form rown olor rystllin NiF 2 is form. On ooling to room tmprtur ron impuritis in th frrit smpl is rmov y trting with ton. Th ron flowts on th ton is nt n vport th ton. Th vrious stps involv in hmil synthsis of NiF 2 prtil is shown in flow hrt (figur 1). Synthsis of Polynilin-NiF 2 omposits. Th Polynilin-NiF 2 omposits wr prpr vi intrfil polymriztion mtho with iffrnt wight prntg of NiF 2 (10, 30 n 50 wt %). On grm of nilin ws issolv in 40 ml of CHCl M mmonium prsulpht ws issolv in 1M HCl n th NiF 2 prtils r to th ov mixtur of quous n orgni phs. Aftr 5 minuts rk grn pripitt form slowly t th intrf n thn grully iffus into quous phs. Aftr 24 hours, th ntir quous phs ws fill homognously with rk grn olor film, orgni lyr osrv shows orng olor u to th formtion of nilin oligomrs. Th quous phs ws thn ollt n wsh with thnol n wtr to rmov th unrt nilin. Th rsiu of polymr thus otin is purifi n ri in vuum ovn t 40 o C for 36 hours. Th ri polymr omposit smpl ws us for struturl hrtriztion n furthr us to stuy th ltril n mgnti proprtis. III. CHARACTERIZATION Th ov synthsiz smpls wr struturlly n morphologilly hrtriz y using iffrnt thniqus lik FTIR, XRD n SEM. Th FTIR sptr of smpls wr ror on ThrmoNiolt, Avtr 370 sptromtr in KBr mium t room tmprtur. Th X-ry iffrtion pttrns of th prpr smpls wr otin y mploying Brukr AXS D8 vn X-ry iffrtomtr using CuK α rition (λ=1.5418a o ) in th 2θ rng 20 o to 80 o. Th surf morphplogy ofpolynilin, NiF 2 prtils n polynilin-nif 2 omposits wr stui y using Jol mol JSM-6390 LV snning ltron mirosop (SEM). To msur th AC onutivity, th pllts of th prpr smpls wr ot with silvr pst on ithr si ws hl twn two nominlly spring lo oppr plts n th AC prmtrs wr msur using N4L-PSM 1735 NumtriQ progrmml LCR mtr in frquny rng 10 to 10 6 Hz. Th mgntiztion msurmnts wr rri out t room tmprtur using virting smpl mgntomtr (VSM) Lkshor VSM-7410 with mximum fil of G to G. IV. RESULTS AND DISCUSSION A.Infrr sptr Th IR sptr of NiF 2 prtils, polynilin n polynilin-nif 2 (10, 30 n 50 wt %) omposits r shown in figur2.

3 Molkri, Shtkr, Rghunn n Klyn 166 Figur 2() shows IR sptr of polynilin.th hrtristi pks of polynilin our t 1564, 1478, 1301, 1244, 1137, 808 n 702 m -1. Th pks t 1564 n m -1 r ttriut to th hrtristi C-C strthing of th quinoi n nznoirings, th pks t 1301 n 1244 m -1 r ssign to C-N strthing of th nznoi ring, th ro pk t 1137 m -1 whih is sri s ltroni-lik n is ssoit with virtion mo [18] n th pk t 808 n 702 m -1 r ttriut to th out of ning of N-H n C-H on in romti rings rsptivly. Th IR sptr of NiF 2 prtils (Fig. 2), th min pk t 546 m -1 is u to intrinsi strthing virtions of mtl t ttrhrl sit nth pk t 468 m -1 is u to othrl-mtl strthing virtions. Th IR sptr of polynilin-nif 2 (10, 30 n 50 wt %) omposits (fig.2 -) shows th pks of th omposits shift to highr frqunis. This inits tht thr is som intrtion twn NiF 2 prtils n polynilin kon. (4 4 4) rystl plns. All th pks mth with th hrtristi rfltion of NiF 2 (JCPDS Cr No ). Th XRD pttrns of polynilin- NiF 2 omposits (Fig. 3-3) xhiit oth th hrtristi pks of NiF 2 n th ro iffrtion of polynilin. Ths rsults onfirm th formtion of polynilin-nif 2 omposits. In t n s ity o u n ts T r n s m itt n ( % ) Fig. 3. XRD pttrns of () Polynilin () NiF 2 n (-) polynilin-nif 2 omposits. C. SEM nlysis Th surf morphology of polynilin-nif 2 (10, 30 n 50 wt %) omposits ws invstigt y mns of SEM θ in grs Wv numr (m -1 ) Fig. 2. FTIR sptr of () Polynilin, () NiF 2 prtils n (-) polynilin-nif 2 omposits. B.X-ry iffrtion Th XRD pttrn of polynilin (Fig. 3) shows two ro pks ntr t 2θ=20.7 o n o, whih r sri to th prioiity prlll n prpniulr to th polymr hins, rsptivly [19-21]. Th XRD pttrn of NiF 2 prtils (Fig 3), th prominnt pks t 2θ= o, o, o, o, o, o, o n o orrspons to (2 2 0), (3 1 1), (4 0 0), (4 2 2), (5 1 1), (4 4 0), (6 2 2) n Fig. 4. SEM mirogrphs of polynilin-nif 2 (10, 30 n 50 wt %) omposits

4 Molkri, Shtkr, Rghunn n Klyn 167 Figur 4(-) givs th SEM mirogrphs of polynilin-nif 2 omposits, suggsting tht th polynilin is posit on th surf of NiF 2 prtils. V. ELECTRICAL PROPERTIES Figur 5( n ) shows th vrition of AC onutivity s funtion of frquny for th polynilin n polynilin-nif 2 (10, 30 n 50 wt %) omposits. From th fig 5() it is sn tht th onutivity of polynilin rmins onstnt up to 10 4 Hz ftr tht thr is inrs in onutivity t highr frqunis. Figur 5() shows th onutivity of polynilin-nif 2 omposits, it is sn tht th onutivity inrss grully for ll th omposits. Inrs onutivity my u to inrs hrg polriztion [22]. Among th omposits, 30 wt% shows th highr onutivity. VI. MAGNETIC PROPERTIES Figur 6 (-) shows room tmprtur mgntiztion urvs for Polynilin, NiF 2 n Polynilin- NiF 2 omposits. It hs n foun tht polynilin show imgnti hvior whrs NiF 2 prtils n polynilin-nif 2 omposits show frromgnti hvior. Th sturtion mgntiztion (M S ) of polynilin-nif 2 (10, 30 n 50 wt %) omposits inrs in frrit % in th polymr mtrix. Among th omposits, 30 wt% show low sturtion mgntiztion vlu of 0.97 mu g -1. Th sturtion mgntiztion (M S ), Rmnnt mgntiztion (M R ) with Coriv fil (H C ) for th smpls r list in tl1. 10 σ in S m x x x x x10-2 Polynilin Momnt/Mss ( mu g -1 ) AC onutivity ( S m -1 ) 1.0x Frquny in Hz Fig. 5. Vrition of AC onutivity with frquny for Polynilin. 3.2x x x x x x x x x x x x x x x x x10-6 polynilin - NiF 2 (10 wt%) omposit polynilin - NiF 2 (30 wt%) omposit polynilin - NiF 2 (50 wt%) omposit Frquny (Hz) Fig. 5. Vrition of AC onutivity with frquny forpolynilin-nif 2 omposits. Momnt/Mss ( mu g -1 ) Appli Fil (G) polynilin NiF 2 prtils polynilin - NiF 2 (10 wt%) omposit polynilin - NiF 2 (30 wt%) omposit polynilin - NiF 2 (50 wt%) omposit Appli Fil (G) Fig. 6. Mgntiztion urvs for () Polynilin, () NiF 2 n (-) Polynilin-NiF 2 omposits.

5 Molkri, Shtkr, Rghunn n Klyn 168 Tl 1: Mgnti prmtrs of Polynilin, NiF 2 prtils n polynilin-nif 2 omposits. Smpls M S in M R inmu H C in mu g -1 g -1 G Polynilin x NiF 2 prtils Polynilin-NiF (10 wt%) omposit Polynilin-NiF (30 wt%) omposit Polynilin-NiF 2 (50 wt%) omposit VII. CONCLUSIONS In summry, NiF 2 prtils n polynilin-nif 2 omposits hv n sussfully synthsiz y omustion rout n n intrfil polymriztion rsptivly. FTIR n XRD nlysis shows thr is som intrtion twn polynilin n NiF 2 prtils. Th AC onutivity inrs with inrs frquny, th omposits with 30 wt% of NiF 2 in polynilin show high onutivity. Th mgnti prmtrs suh s sturtion mgntiztion n orivity of omposits wr foun to pn on th wt % of NiF 2 prtils in polynilin. Th omposits showfrromgnti ntur. REFERENCES [1] T.A. Skothim, R.L. Elsnumr, J.R. Rynols, Hnookof Conuting Polymrs, son., Mrl Dkkr,Nw York, [2] Gospoinov N n Trlmzyn L, Prog. Polym. Si,23,1443, [3]. A.G,MDirmi, Currnt Appli Physis,Vol.1,pp-269, [4] L. Li, J. Jing, F. Xu, Mtrils Lttrs, Vol. 61, pp , [5]. R. Mthur, D. R. Shrm, S. R. Vr, N. Kumr, At mtr, Vol.49, pp , [6]. A.G. MDirmi, A.J. Epstin, Synthti Mtls, Vol. 69, pp-86-92, [7] T. Mkl, S. Pinim, T. Tk, S. Jussil, n H. Isotlo, Synthti Mtls,85, 1335, [8] S. Kuwt, S. Msui, H. Yonym, Eltrohim. At, 44, 4593, [9] J.Q. Kn, X.H. Pn, C. Chn, Biosns. Bioltron.19, 1635, [10] N. Ahm, A.G. MDirmi, Synthti Mtls,78,103, [11] Sy Khsim, S C Rghvnr, M Rvnsipp n M V N Amik Prs, Bull. Mtr.Si,Vol34, No 7, pp , [12] Aji Kumr S Molkri n SngshttyKlyn, IJRISET, Vol. 4, Issu 7, [13] Rmsh Ptil, Ashis S. Roy, Kopplkr R. Anilkumr, SrikntEkhlikr, Journl of Appli Polymr Sin, Vol. 121, , [14] G. D. Prsnn, H.S.Jynn, A.R. Lmni n S. Dsh, Synthti Mtls,161, , [15] BhrtiNnpur, SuhshKonwr, Mhsh Slunkh n ArtiNnpur, Journl of Composit Mtrils,0(0), 1-9, [16] P. Xu, X. J. Hn, J. J. Jing, X. H. Wng, X. D. Li, n A. H. Wn, J. Phys. Chm,111, 12603, [17] Hung X n Chn Z,Mtr. Rs. Bull.40, 105, [18] Quillr S, Lourn G, Lfrnt S n MDirmi A G, Phys. Rv. B50, 12496, [19] Moon Y B, Co Y, Smith P n Hgr A J, Polym. Commun,30, 196, [20] Fng W, Sun E, Fujii A, Wu H C, Niihr K n Yoshino K, Bull. Chm. So. Jpn,73, 2627, [21] Pougt J P, Jozfowiz, Epstin A J, Tng X n MDirmi A G, Mromoluls,24, 779, [22] Rjshkr B, Vishnuvrhn T K, Shshihr N, Stishkumr K B, Bsvrj C n Chnrshkhr M, IJREAS,5, 36, 2015.