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SCIENCETECHNOLOGY

r X W i -rl

rONG HOP VA NGHIEN ClJU TINH CHAT CUA COMPOZIT POLYANILIN/FEO

lYNTHESIS AND SOME PROPERTIES OF POLYANILINE/FE,0, COMPOSITE 3 4

3 4

N g u y e n N g o c T h a n h , L e T h i H o n g T h a m , V u Q u o c T r u n g

T 6 m t i l t

f^anocompozit poiianilm/Fe^O^ duoc tong hop bang phuong phap triing h ^ monome anilin va nano oxit s3t tir diing chat oxi h6a (NHJ^S^O^. Tinh chat cija vat lieu tong hop da di/gc nghien ciiu bang cac phuong phap: pho Raman, phan tich nhiet khoi luang (TGA), anh SEM, pho X-ray, phuong phap do duiing cong tir hoS. Tinh chat hap thy s6ng dien ti^ cua mang phu compozit polianilin/FejO, kha a o cho thay kha nang ling dung cQa v^t li^u n^y trong thifc te.

A b s t r a c t

Polyaniime/Fe^O, composite nanoparticles were prepared by polymerization of aniline in the presence of FSjO^ nanoparticles using (NH,)jSjOj as oxidant. Properties of the obtained polyaniline/Fe,0, composite were studied by Raman spectra, thermal gravimetric analysis (TGA), scanning electron microscopy (SEM), X-ray diffraction (XRD) and magnetization curve. The electronmagetic shielding properties of a layer formed from this material are suitable for practical applications

TS. Nguyen NgocTtianh.KS. LeThi HangTtiSm, Klioa Cong nghe Hda hoc, TrUdng E)ai hocC5ng nghiep Ha Noi PGS.TSVuQu6cTruiig

Khoa Hda hoc, Tnfdng dai h^c Su pham Ha Noi Email: ngtiianh_cdspvp@yahoo cam.vn

Ngaynhanbai: 25/06/2013 Ngay chap nhdn dang: 25/09/2013

I.OATVAND£

Ngay nay, vdi sif phat trien manh le cCia nganh khoa hgc vat li^u, cac hti khoa hpc tren the gi6i da va dang ip trung nghi§n cijfu phi/ang phap che 10 vat lieu m6i co tinh chat dac biet hSm dap Lfng nhu cau sCf dung trong jc nganh cong nghiep cong nghe cao.

ac biet, phu'Ong phap to hgp cac vat

\u oxit v6 CO v6i polime dan duoc phat ien va quan tam rong rai nham tao ra jmpozit CO tinh nang du'dc ccii thien it hcJn. Polyme dan co nhieu ufng dung jan trong nhU: chong an mon va b^o

; kim loai [1, 2], vat lieu tang hinh [3, , si^u tu dien [5,6], thiet bi dien s3c [7], it lieu cam bien sinh hgc va hoa hgc [8,

9].... Polianilin (PAni) da dugc tong hgp tLf lau, song tong hgp vat lieu compozit polianilin va nghien ctfu ilng dung cCia no trong hap thy song dien tiJ' con it dagc nghien ajfu. Trong bai bao nay, chung toi trinh bay ket qua tong hgp va nghien CLfu tinh chat cua compozit polianilin/FejO^ v6i muc dich Lfng dung loai vat lieu nay hap thu song dien tii 6 dai tan song rada quan sU.

2. THl/C NGHIEM

2.1. Tdng htfp compozit PAni/Fe^O^

Phan tan lOg Fe^O^ trong nudc cat, them vao 18,88ml isopropanol, 0,5ml anilin, khuay co hon hgp trong 1 g i d Can chinh xac 1,879g (NHJ^S^Og hoa tan trong 25ml niitifc cat, sau do nh6

tif tLf dung djch n^y vao hon hgp p h i r ijfng 6 tren, khuay manh phan tjfng trong 2 gid, phan u'ng toa nhiet manh, hon hop phan u'ng co mau xanh den, Lgc lay phan bot, say ap suat thap o 40°C trong 48 gid. San phim thu dUdc d dang bot mau xanh co f n c khong xac dinh, hieu suit phan u'ng dat 80,2%.

2.2. Nghien curu cac tinh chat cua compozit PAni/Fe^O^

Pho Raman do d bade song 633 nm, nang lUong chum tia Laser 3 mW, tren may do the he Renishaw invia Raman Microscope tai Vien Vat ly ky thuSt, Tru'dng Dai hoc Bich khoa Ha Ngi, Be mat cCia mau dugc quan sal tren kinh hien vi dien tCf quet may SEM- HITACHI-4800 tai Vien Ve sinh Djch t€

Trung ifdng. Do ben nhiet do tren ma>

ShimazuTGA-50H Bg mon Hoa Li, KhoE Hda hgc, TrUdng Dai hgc SU pham HE Noi, den 600°C vdi toe do IOC/phut Phd XRD cCia mau nghien cCfu dUdc gh tren may VNU-SIEMENS-5005 Brukei Germany tai TrUdng Oai hgc Khoa hgt Tif nhien, Dai hoc Quoc gia Ha Ndi Phep do tCf tre dUdc thuc hien tren hi do tU tre mau rung vdi do nhay 10' emu tai phdng thi nghiem Vat lieu tL va sieu dan, Vien Khoa hgc vat lieu. Qui trinh ghi s6 lieu dugc t u dgng hda qu;

viec ghep ndi cac thiet bi do vdi ma;

tinh theo dudng truyen dCf lieu IEEE 488 (GPIB), Sai so cua he do nhd hor 1%. Khi nang hap thu sdng dien t i

S o 1 8 . 2 0 1 3 • Tan rhi KHOA HOf ^ (mC, WCM

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iCONG NGHE

cua mau nghien cUu do d viing tan so 8,14-11,8GHz tai Vien Dien tCf va Vien thdng, Trung t^m Khoa hgc va Cdng nghe Quan sU.

Pho Raman, cinh SEIVI, do ben nhiet (TGA), phd XRD, dUdng cong tU hda cua cac mau nghien cUu deu do d dang bot nghien nhd. Kha nang hap thu sdng dien tU cua Fe^O^ va compozit PAni/Fe^O^thl dUOc do d dang mang phu tren tam vai.

3 . K^T Q U A V A T H A O L U A N 3 . 1 . Pho R a m a n cua m a u n g h i e n o j f u

. . !/

!

\

Hinh 1. Pho Raman cua mau PAni/Fe,0^

T r e n p h o R a m a n ( h l n h 1) c u a m a u n g h i e n cUu, d a xac n h a n d u g c s u c d m a t cLia cac v a n d a c t r U n g c h o PAni d t r a n g t h a i o x i h d a . V a n d 1587,85 cm-^

( m a n h ) la t a n sd d a o d d n g h d a trj c u a n h d m C = C , v a n d 1475,9 c m ' l a t a n so d a o d g n g c u a n h d m C = N c u a PAni, v a n d 1353,06 c m ' v a 1 2 3 6 , 1 2 c m " ' la t a n s o d a o d g n g h d a t r i c u a n h d m C - N . D a o d p n g b i e n d a n g t r o n g m a t p h a n g c u a cac l i e n k e t C-H t r o n g v d n g a n i l i n t h e h i e n b d i v a n c d t a n s o 1 1 5 7 , 1 5 c m ' . N h u v i y , PAni t r o n g m l u c o m p o z i t P A n i / Fe^O^ t o n g h d p d u o c t d n t a i d t r a n g t h a i 0X1 h d a .

3 . 2 . P h o p h a n tr'ch n h i e t k h o i i U c m g ( T G A ) c u a cac m a u n g h i e n cufu

D e t h a y r d d u g c q u a t r i n h p h a n h i i y b d i n h i e t c u a PAni v a v a t l i e u n a n o c o m p o z i t PAni/Fe^O^ t r o n g p h e p d o p h a n t i c h n h i e t c h u n g t o i t i e n h a n h d o DTG v a D I A .

Hinh 2, Gian do phan tich nhiet cua mau PAni/FejO, Tren g i a n d o h i n h 2, k h i t a n g n h i e t d d t i f n h i e t d o p h o n g d e n k h o a n g 100°C, k h d i I U d n g m a u g i a m 9 , 8 6 1 % d o sU b a y h o i cCia n u d c a m . d k h o a n g n h i e t d d t U 100°C d e n e O C C , d o c d sU p h a n h u y c u a cac m o n o m e c o n d U c d t r o n g san p h a m , d i m e , t r i m e , o l i g o m e , p o l y m e t a o t h a n h t r o n g q u a t r i n h p h a n U n g l a m k h o i l U d n g m a u g i a m 9,072%, n h U v a y l u g n g Fe^O^

c d n lai t r o n g m a u la 8 1 , 0 6 7 5 % . 3 . 3 . A n h S E M cCia m a u n g h i e n cufu

s^B^fiB^KfSi m

Hinh 3, Anh SEM cua mau PAni/FejO, Anh SEM cua mau compozit PAni/

Fe^O^ dugc the hien trong hinh 3. Mau PAni/Fe^O^ cd dang bdt vdi hat hinh cau kha dong deu, kich thUdc hat khoang 14-=-17nm (Idn hon kich thudc cUa hat Fep^8,4^2nm).

3.4. Ket qua do nhieu xa tia X cua cac m i u nghien cihi

Kj\J^,^'^

phii hdp vdi vi tri cac dinh cua Fe^O, (hinh 4a) ddng thdi khdng xuat hien pha la, do ban rdng cua cac dinh trong cac trudng hop tuong ddi dong deu, do vay kich thudc hat khdng thay doi. Nhu vay, tU pho nhieu xa tia X ta thay kich thudc hat nanocompozit che tao duac kha nhd, mau tao thanh ia dOn pha, viec bgc Idp vd polyme vao vat lieu khdng Snh hudng den cau true tinh the.

3 . 5 . K e t quci n g h i e n cuTu tJnh chat tCTcua c a c m a u n g h i e n CIJ:U

De nghien cdu nhCfng Snh hudng cua PAni tdi tif tinh cCia vat lieu chiing tdi dua vao dudng cong tU hda ctia FejO^ va nanocompozit ciia PAni/Fe 0 trong hlnh 5.

Gia tri momen t d bao hoa M (emu/g) ciia Fe^O^ la 66,05 va cua PAni/

Fe^O^ la 60,46. DUdng cong XU hda ciia cac mau deu la dudng thuSn nghjch, gia trj H^ ciia cac mau rat nh6 nen chung deu the hien tinh sieu thuan tu. Momen t d bao hda cua PAni/FejO, cd gia t n tif do bao hda nhd hOn ciia nano sat tU nhung dang dudng cong t d hda gidng nhau chUng td cac m3u nanocompozit tong hop duoc cung c6 tinh chat t d gidng nhu nano sat tU.

Hinh 4. Pho XRD cua mau Fe^O, (a) va PAni/FejO,(b) H l n h 4 t h e h i e n p h o X R D c u a Fe^O^

v a PAni/Fe^O^. H i n h 4 b c h o t h a y v j t r i cac d i n h c u a m a u PAni/Fe^O^ t U o n g d o i

f

(b) He (Oe) Hlnh 5. eirimg cong tir hoa cOa mau Fe,0, (a)»

5 2 T a p d i i K H O A H O C & C O N G N G H E . S o 1 8 . 2 0 1 3

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SClENCETECHNOLOGYl

3 . 6 . P h o h a p t h u s o n g d i e n tf^ cOa m a u n g h i e n c i h i

.('v'"'

( • ' • , , L^n

'\ '\\

(b) " . . . Hinh 6, Pho hap thu song ffien tif ciia Fe^O^ (a) vaPAni/Fe,OJb)

Cac mau nghien cdu Fe^O^ va PAni/

Fe^O^ dugc quet len Vcii, K h i nang che chin dugc d i n h gia qua cdng thUc;

SE = 1 0 . l o g ^ P,

Trong dd SE la do hap thu (dB); p^ - cong suat sdng tdi (W), p, - cong suit song di qua

Hlnh 6a the hien k h i n i n g hap thu song dien t d ciia vat lieu oxit sat tU. Gia tn SE dat cue dai tai tan sd 1 l,35GHz, SE --0,29dB:

^ = 0,9350

Su che c h i n dat dUdc la 6,50%.

Hinh 6b the hien kha n i n g hap thu sdng dien tU ciia mau PAn\/Fep^. Gia tn SE cue dai tai tan sd 10,87GHz, SE - -4,49dB:

^ = 0,3556 PI

Suche c h i n dat dugc la 64,44%.

Qua ket q u i phan tich tren cho thay vat lieu nanocompozit PAni/Fe^O^

cd k h i nang hap thu sdng dien t d k h i tot d viing 8,14-1 l,80GHz (Ung vdi d i i song rada quan sU). Tuy nhien, sU hap

thu sdng dien tU nay la khdng dong d^u va hap thu manh nhat d tan sd 10,87GHz vdi SE= - 4,49dB, tUc sU che chan dat 64,44%, cao hOn xap xi 10 lan so vdi dp che chan cue dai cua Fep^

rieng re, chi dat 6,50% tai 1 l,35GHz.

4. K^T LUAN

Trong cdng trinh nay, chung tdi da tdng hop dugc nanocompozit PAni/

FCjO^ true tiep trong dung mdi. Tinh chat cua vat lieu da dugc nghien cdu b i n g cle phUdng phap pho Raman, phan tich nhiet, SEM, phd XRD, do dudng cong tU hda va phd hap thy sdng dien tU.

Cic ket qua nghien cdu da ch! ra r i n g PAni cdtrong mau dtrang thai oxi hda, eo do ben nhiet cao, cd do dong d^u cao, kich thUdc hat Fe^O^ khdng ddi (9,8nm), Mang phu che tao tU nanoeopozit PAni/FejO^ tren nen vai cd k h i nang hapthu manh sdng dien t U d d i i rada quan sUva d t a n sd 10,87GHz do hap thu dat dUOC SE - -4,49dB, tUc SLf che chan dat den 64,44%.

Phan bien khoa hoc: PGS.TS Le Xuan Que

TAILI^UTHAMKHAO

[1|, T, Schauer, A Joos, L Dulog, C D, Eisenbach.

Protechon of imn against corrosion with polyaniline primers. Progress in Organic Coatings, 33(1), 20-27 (1998).

[2]. S. Sathiyanarayanan, S. Syed Azim, G.

Venkatachari. Corrosion protection of galvanized iron by polyaniline containing wash primer coating.

Progress in Organic Coatings, 65(1), 152-157 (2009).

[3]. B. fi, Kim, H. K. Lee, S. H. Park, H K Kim, Electromagneticinterferenceshieldingcharactenstics and shielding effectiveness of polyaniline-coated films, Thin Solid Films,519(11),3492-3496 (2011),

[4]. B, R. Kim, H K, Lee, Eunmi Kim, Suck-Hyun Lee, Intrinsic electromagnetic radiation shielding/

absorbing characteristics of polyaniime-coated

transparentthm films. Synthetic Metals, 160(17-18), 1838-1842(2010).

[5], Kongyu lull, Xiaogang Zhang, Sudong Yang, Xiangguo Ye, Jianming Luo. Polyaniline nanofibers as the electrode material for supercapacitors. Materials Chemistry and Physics, 112(1), 127-131 (2008).

[6]. Limin Li, Enhui Liu, Jian Li, Yanjing Yang, Haijie Shen, Zhengzheng Huang, Xiaoxia Xiang, Wen Li. A doped activated carbon prepared from polyaniline for high performance supercapacitors, JoumalofPowerSources, 195(5), 1516-1521 (2010)

[7]. Suman PahaL M. Deepa, Shweta Bhandari, K. N. Sood, A. K, Srivastava. Eiectrachromism and redox switching of cobalt hexacyanoferrate- polyaniline hybrid films in a hydrophobic ionic liquid.

Solar Energy Materials and Solar Cells, 94(6), 1064- 1075(2010).

[8]. Arkady A, Karyakin, Oksana A Bobrova, Lyiia V, Lukachova, Elena E, Karyakina. Potentiometric biosensors based on polyaniline semiconductor films.

Sensors and Actuators B: Chemical, 33(1-3), 34-38 (1996).

[9]. Vu Quoc Trung, floan Thi PhUflng Lmh, Thai Doan Tinh, Pham Van Hoan, Che tao va nghien Cliu tinh chat cQa mang phu compozit polyanilin/

polyacrylic. Tap chi hoa hoc, T,47 (4A), Tr.742-747, (2009).

^ n 1 R '7ni7.T:inrhikMnAiinr;irf)Mr,Mr,Mf ^ -

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