TAPCHIHOAHOC T. "52(6) 736-741 THANG 12NAM2014 DDL 1015625/0866-7144.2014-0065
K H A O S A T K H A N A N G B A O V E C H 6 N G A N M O N T H E P CLIA M A N G
PHU POLYPYRROLE TONG HOP TRONG MOI TRUONG AXIT 1 0 - C A M P H O S U N F O N I C BANG PHU'aNG PHAP DIEN HOA
Ha Manh Hiing^'', Phan Thi Bich Ng9c', Le Minh Dire', Doan Thi Yin Oanh^
Tran Vinh Dieu^, Dirdng Khanh Linh', Vii Quoc Trung'*
'Khoa Hod hgc, Trudng Bgi hgc Suphgm Hd Ngi
^Khoa Bgi hgc dgi cuong, Trudng Bgi hgc Md - Bia chdt
^Khoa Hod hgc, Truang Dgi hgc Bdch khoa, Dgi hgc Dd Ndng ''Trung tdm Nghien cuu vgt lieu polyme, Trudng Bgi hgc Bdch khoa Hd Ndi
^Nhd Xudt bdn Khoa hgc tu nhien va Cdng nghe, Vien Hdn lam Khoa hgc vd Cdng nghi Viet Nam Din Tda soan 4-9-2014; Chip nhan dang 4-12-2014
Abstract
Polypyrrole (PPy) was prepared on the mild steel CT3 by electrochemical polymerisation in a solution containing pyrrole monomer, 10-camphorsulfonic acid and molybdate dopant anions. The mild steel surface was passivated before elecfropolymerisation in a solution of sodium molybdate 0.1 M. The morphology and structure of the PPy film were studied by electron scanning microscopy (SEM). The typical cauliflower structure of PPy was observed. Raman specfroscopy showed that the obtained PPy was in oxidized state. Energy-dispersive X-ray specfroscopy (EDX) indicated that molybdate anion was doped in the PPy film. The thermal stability of PPy was investigated by TGA, showing that PPy was stable at higher than 500 °C. The corrosion behavior of mild steel (CT3) with PPy film in solution of NaCI 3 % were studied by elecfrochemical impedance specfroscopy (EIS) and other electrochemical methods. The presence of molybdate dopant anion in PPy improved the corrosion protection of mild steel.
Keywords. Polypyrrole, molybdate, conducting polymers, 10-camphorsulfonic acid, corrosion protection, elecfrochemical impedance specfroscopy.
1. DAT V A N D E khdng tan vi du nhu anion oxalat fren mang polyme dan di chuy6n ddn vj tri khuyet tat fren mang thu Sat, thep va kim loai ndi chung la nhung vat lieu dgng de tao thanh hgp chit oxalat khdng tan nen dugc su dung rat nhieu frong ddi sdng. Tuy nhien thep van dugc bao ve [4]. Trong sd cac polyme din frong dieu kien mdi trudng ndng, am chung de hi an thi ndi bat cd polyanilin (PANi) va polypyrrol (PPy) mdn nen da gay tdn that nhi6u ve kinh te. Trong cd kha nang bao ve chdng an mdn. Tuy nhien PANi thuc te cd rat nhieu each bao ve chdng an mdn cho cd nhieu uu diem nhu bao ve chong an mdn tdt fl- thep va kim lo?i. ^ 5], chi phi thip nhung nd lai cd dgc tinh cao de gay Cac polyme dan da dugc bidt la cd tac dung nhu ung thu nen polyanilin khdng dugc ung dyng nhik la mgt Idp phu de bao ve chdng lai su an mdn kim trong cdng nghiep va ddi sdng. Ngugc lai loai [1-5]. Kha nang bao ve cua polyme din cd th6 polypyrrole (PPy) la vat lieu than thi?n vdi mdi dugc giai thich: Chiing la Idp mang ehe chin khdi su ttardng, kha nang chdng an mdn rit tdt [8-10]. Mat tan cdng ciia cac tac nhan gay an mdn [6]. Mat khac khac, mang PPy dugc tdng hgp tren hh m^t kim lo^i Idp phu nay cd thedugc coi nhu la mgt anot bao ve rat mdng nhimg lai bao ve dugc kim loai mgt thdi vi mang polyme dan tdn tai d dang oxi hda lam cho gian dai [ 11 ] . . . .
thep d frang thai thu ddng vol thi mach hd cao [7]. Tinh chit cua mang phu PPy tdng hgp trong m6i 0 day vai trd ciia anion la rit Idn, khi tac nhan an trudng axit camphosunfonic cung da dugc nghien mdn xam nhap thdng qua cac khuyet tat tren mang cuu [12-14]. Tuy nhien, cac cdng trinh nghien cuu lam the cua thep giam, cac anion dugc giai phdng kha nang urc chi an mdn thep ciia mang PPy t6ng chiing ket hgp vdi cation kim loai tao hgp chit hgp trong mdi trudng axit camphosunfonic dugc dl
TCHH, T. 52(6), 2014
cap khdng nhilu. Trong bai bao nay chiing tdi trinh bay kit qua tong hgp mang phu PPy fren thep CT3 trong mdi tnrdng axit camphosunfonic cd va khdng cd anion pha tap molybdat va kha nang ung dung ciia mang PPy nay trong viec bao v? chong Sn mdn th^p CT3 trong mdi frudng NaCI 3 %.
2. THUC NGHIEM
2.1. Tong hop PPy tren thep CT3
Thep CT3 ciia Cdng ty Gang thep Thai Nguyen kich cd 13,5x13,5 cm (day 2 mm) dugc danh sach gi, tiy dau md bang xa phdng va dung djch kiem.
Sau dd tim thep dugc danh bdng be mat bang cac loai giiy rap vdi do min Ian lugt tir 600 din 1500 rdi dugc nj-a sach bing axeton nham tao be m^t dien cue cd do bdng cao va kha nang bam dinh tdt. Cac mau thep tren dugc tiln hanh thu ddng frong dung djch NajMoOa 0,1 M bing phuong phap phan cue the tmh d +0,5 V (Ag/AgCl) trong thdi gian 60 phiit; rua sach, lam khd, bao quan trong khi quyen nito.
Viec tdng hgp mang PPy tren thep CT3 dugc thuc hien bang phuong phap phan c^rc ddng tmh, thdi gian phan cue 50 phut va dugc thuc hi$n trong binh 3 dien cue: dien cue lam viec la tim thep CT3, dien cue ddi la tim Pt va dien circ so sanh la dien cue Ag/AgCI (KCI). Mau M l dugc tdng hgp trong dung dich chiia axit 10-camphosunfonic 0,05 M va pyrrole 0,1 M. Mau M2 dugc tdng hg^j trong dieu kien fren nhung cd them Na2Mo04 0,03 M. Sir cd m|t ciia Na2Mo04 lam cho qua trinh tdng hgp dugc thuan Igi hon do anion molybdat cd kha nang frc ehe qua frinh hoa tan Fe khi tdng hgp PPy. Mang PPy sinh ra fren thep CT3 cd dg bam dinh cao, bdng, mjn. Sau khi tdng hgp, mang polyme dugc riia, say khd frong mdi trudng nito rdi tien hanh cac thi nghiem khao sat. Cac phep do di$n hoa dugc thuc hi^n tren thilt hi Zenium (Zaehner - Due) tai Khoa Hoa hgc, Trudng Dili hgc Su pham Ha Ngi, 2.2. Cac phfroug phap nghien cihi
Hinh thai bl mat cua PPy dugc nghien ciiu bang chyp anh SEM fren may FE-SEM Hitachi S-4800 (Nh§t Ban) tai Vien Khoa hgc V^t lieu, Vien Han lam Khoa hgc va Cdng nghe Vi?t Nam. Ciu tnic hoa hgc ciia PPy dugc danh gia bang phd Raman (do d budc sdng 613 nm, nang lugng chCim tia laze 1 mW, tren may do Ramanlog 91) tai Vien Khoa hgc Vat lieu, Vien Han lam Khoa hgc va Cdng nghe Viet Nam. Phep phan tich nhi?t dugc tiln hanh phan tich fren may Shimadzu TGA-50H, tai Khoa Hda hgc, Trudng Dai hgc Su phjim Ha Ngi vdi tdc dg gia nhi?t 5 °C/phut. Tinh chit difin hda va nghien cfru
va Qudc Trung vd cgng su kha nang bao ve chdng an mdn thep CT3 ciia mang PPy dugc do fren thilt bj Zenium (Zaehner - Du:c) tai Khoa Hoa hgc, Trudng Dai hgc Su pham Ha Ngi.
3. KET QUA VA T H A O LUAN 3.1. Thu dong be m | t thep CT3
De thu dugc mang PPy cd dg b ^ dinh tdt, mdng, mjn va bdng, bl mat thep CT3 dugc thy ddng bing phuong phap thi tTnh d +0,5 V (Ag/AgCI) [4].
Thdi gian thu ddng cho mdi mau thi nghiem khoang 60 phiit. Dudng bleu dien sir thay ddi ddng theo thdi gian frong qua frinh thu ddng (hinh 1).
Thdi gian, s Hinh I: Dudng thy dgng thep CT3 frong
dung dich Na2Mo04 0,1 M 3.2. Tdng hop PPy
Dudng bieu dien su thay ddi the phan eye frong qua frinh tdng hgp mang PPy khi 1 = 0,9 mA/cm dugc trinh bay frong (hinh 2). Mang PPy tdng hgp dugc cd be mat nhan min, mau den, dg day nhd va ddng deu fren toan bg be mat. Trudc khi tdng hgp bl mat thep dugc thu dgng nen sy thay ddi thi phan c\rc frong qua frinh tdng hgp mau M l va M2 khdng cd su khac nhau (hinh 2). The tdng hgp PPy vao khoang 0,75 V (Ag/AgCI).
Thdi gian, s Hinh 2: Dudng tdng hgp PPy frong
axit 10-camphosunfonic 0,05 M 3.3. Anh SEM cua PPy
Anh SEM cho thay be mat ciia PPy cd hinh dang hoa Slip lo dien hinh (hinh 3). Sir cd mat ciia anion
TCHH, T. 52(6), 2014 Khdo sdt khd ndng bao ve chdng dn mdn...
molybdat dudng nhu khdng anh hudng nhilu tdi 3.5. Phd h i p thui hong ngoai IR hinh thai cua mang.
Hinh 3: Anh SEM ciia miu Ml va M2 3.4. Pho Raman cua PPy
Dac trung phd Raman ciia PPy xuat hien trong dai phd 800-1700 cm"' (hinh 4). Tir phd Raman xac dinh dugc cac tin hieu dac frimg ciia PPy d trang thai oxi hoa trong miu Ml va M2. Pic cd cudng do m?nh d khoang 1572 din 1590 cm*' dac trung cho dao ddng hoa tri ciia nhdm C=C. Tren phd cua cac miu Ml va M2 xuit hien cac pic d khoang 1368 - 1381 cm"' ung vdi tin sd dao dgng hoa trj ciia nhdm C-N va C-C. Tin hifu dao ddng d khoang 1067-1080 cm"' ling vdi dao dgng bien dang ciia lien ket C-H.
Viing tin sd fren 900 cm"' ung vol tan sd dao dgng biln dang khong phing ciia vdng thom. Bang I quy kit cac tin hieu dac trung tren phd Raman cua Ml va M2 dugc so sanh vdi cac gia tri tinh loan ly thuylt va thuc nghi?m khac.
Hinh 4: Phd Raman ciia M l va M2 Bdng I: Tin hieu phd Raman (cm'') ciia Ml va M2
PPy (a) 1676 1524 1307 1049 955
PPy(b) 1589 1328 1047 976
Mau MI 1590 1368 1080 933
Mau M2 1572 I38I 1067 931
Quy ket van ph6
DC-C
WC-N.UCC 5c-H
^vonE kdx
Hinh 5: Phd hdng ngoai IR ciia M l va M2 Van phd d khoang 3429 cm" cua M l va 3438 cm"' ciia M2 dac trung cho dao ddng hda tn cua lien kit N-H thom (ON-H) hoac dao dgng hda fri ciia lien kit O-H (DO-K) ciia nudc kit tinh trong miu. Cac vSn phd d vao khoang 2939 cm"', 2949 cm"' dSc frung cho dao dgng hda trj ciia nhdm C-H thom. Van a 1640 cm"' (Ml), 1531 cm"' (M2) dac frung cho dao dgng hda tri cua nhdm C^O (Uc=o). Van phi 6 khoang 1544 cm"' (Ml), 1436 cm"' (M2) d3c frung cho uc=c thom, I>C=N. Van d 1387 cni"' (Ml), 1303 cm"' (M2) dac trung cho dao ddng bien dang ciia N- H (5M.H) ho?c ciia O-H (5O.H). Van d khoang 1037 cm"' din 1047 cm"' dac trung cho dao dgng hoa trj cQa S-0 (I)S.O). Van phd d khoang tijr 776 cm"' din 889 cm"' (M2) dac trung cho dao ddng hda tn khong ddi ximg ciia nhdm (MoO^)^".
3.6. Pho tan xa tia X theo nang IfrOQg D I xac dinh sy cd mat ciia Mo trong vat lieu tao thanh, da phan tich miu bang phuong phap tan xa tia X theo nang lugng. Hinh 6 trinh bay pho EDX ciia mau Ml va M2. Thanh phan cac nguyen td chhih dugc trinh bay d bang 2.
Bdng 2: Thanh phan nguyen to ciia mau M l va M2
(PPy(a): Tin hieu Raman ciia PPy d frang th^i oxi hod theo tinh toan ly thuylt [15]; PPy(b): Tin hieu Raman cua PPy d frang thai oxi hoa frong nanocompozit PPy/Al^O]
[16]).
Mau Ml M2
Ham lirong % nguyen to C , N , 0
93,15 68,79
S 6,71
2,6 Mo
-
28,62 Ket qua EDX d hinh 6 va bang 2 cho thay, mSu M l khdng cd mat Mo nhung d miu M2 xuit hiSn ham lugng Mo la 28,62 %. Dieu nay cho thiy trong qua trinh tdng hop mau M2, su pha tap anion molybdat da xay ra.
T C H H , T 52(6), 2 0 1 4
fe IWc
lAi
Vu Quoc Trung vd cgng su da tao thanh Idp thu d d n g fren be m a t thep, ngan can kha n a n g p h a n irng ciia cac m o n o m e pyrrole, lam cho PPy tao thanh trong m a u M 2 cd phan tii khdi nhd h o n v a cd s u p h a n bd khdi l u g n g phan t u n a m trong k h o a n g hep h o n so v d i PPy trong m i u M l (hinh 7). P h i n cdn lai c u a m a u M 2 k h d n g bi p h a n b u y d rihiet dg tren 600 "C (19,31 % ) la p h i n ciia h g p chat vd c o . Dieu nay hoan toan phii h g p va chiing td mau M 2 da d u g c p h a tap anion molybdat.
Bdng 3. Ket qua phan tich nhiet mau M l , M 2
Nhiet do
%Am M l M2
<
100 ° c 89,58 90,33
100 " C - 400 °C 65,89 75,24
400 °C - 600 °C 2,017 42,37
Kh6i luong con
lai 0 19,31
Hmh 6: Phd E D X c u a M l va M 2
3.7. P h d p h a n t i c h n h i e t
M a n g PPy bj p h a n b u y t r o n g dieu kien tir nhiet do phdng den 600 "C va frong a p suat k h d n g khi vdi tdc do gia nhiet 5 °C/phiit c h o thay q u a 2 chi tieu TGA va D T A . M g t d a c diem c h u n g frong qua trinh phan hiiy ciia cac m i u P P y la d u d n g T G A cd n h i l u budc chuyin, chiing td trong m i u PPy cd nhieu thanh phan khac nhau n h u m o n o m e d u , c h i t pha tap d u va olygome (hinh 7).
3.8. B a o v e c h o n g a n m d n t h e p C T 3
„ 3.8.1. Bo thi mgch hd (OCP) theo thdi gian K h a n a n g bao v e c h d n g an m d n thep C T 3 ciia m a n g Ppy tren mau M l , M 2 ciing vdi thep C T 3 da d u g c thu d d n g trong N a 2 M o 0 4 0,1 M d u g c ngam trong d u n g dich N a C I 3 % the hien d t h i mach h d t h e o thdi gian cho tdi khi the ciia cac mau b i n g v d i the an m d n c u a t h e p C T 3 trong d u n g dich NaCI 3 % . Hinh 8 cho t h i y ca hai mau M l , M 2 d i u cd t h i mach h d Idn h o n the an m d n ciia t h e p C T 3 k h d n g d u g c phu PPy. NghTa la t h e p C T 3 d m i u M l va M 2 da d u g c bao ve. T u y nhi6n, m a u M 2 ( d u g c pha t a p anion m o l y b d a t ) cd thdi gian bao v e dai h o n . Hinh 8 c u n g cho thay, tir 25 den 70 gid, the mach h d dao d d n g quanh gia trj the -0,33 V / ( A g / A g C I ) va duy fri trong k h o a n g thdi gian n a y t r u d c khi giam den t h e an m d n . D i e u nay cho thay su cd m a t anion m o l y b d a t da t h e hi?n k h a n a n g t u bao v e cita m a n g .
Hinh 7: Phd p h a n tich nhiet ciia M l 1: DTA; 2. TGA
Giam khdi l u g n g frong k h o a n g nhiet d o tir 2 0 - 100 °C la sy m i t n o d e cd m a t t r o n g m a u . G i a m khdi lirgng frong k h o a n g nhiet d o 100-400 °C la d o s u phan buy c u a c a c o l y g o m e v a thanh p h a n p h a tap camphosunfunic cd frong mau. K h o a n g p h a n h u y ciia PPy n i m trong viing 4 0 0 - 6 0 0 °C ( b a n g 3). 6 m i u M l , k h o a n g p h a n buy m^nh n h i t ciia P P y d 453 °C, c d n d m i u M 2 la d 500 °C. S u khac biet nay d u g c giai thich la d o sir cd m a t c u a anion m o l y b d a t
Thdi gian, h
Hinh 8: T h e m a c h h d c u a m a u C T 3 , M l va M 2 3.8.2. Do dudng cong phdn cue Tafel
M a u d u g c phan c u e t r o n g k h o a n g -0,5 V d e n + 0 , 5 V ( A g / A g C I ) , t r o n g d u n g djch N a C i 3 % . D u d n g c o n g Tafel c u a c a c m a u d u g c t h i hien fren
TCHH, T 52(6), 2014 Khdo sdt khd ndng bdo ve chdng an mdn...
hinh 9. Tir day, ddng va the an mdn dugc xac dinh len (hinh 10c va lOd). Khi dd gdc pha xuat hien r5 (bang 4). ret d viing tin sd nay thi hien mang chuyin din sang trang thai ban din (trgng thai khOr ciia PPy). Tdng trd cua mau M2 (hinh lOd) cao hon M l (hinh 10c) dugc giai thich la do sy xuit hien mgt hgp chat kho tan sinh ra trong qua trinh polyme hda d mau M2 nhieu hon trong mau M l [17]. Kit qua nay phii hgp vdi ket qua do TGA (bang 3).
The Sn mdn, V
Hinh 9: Dudng cong phan eye I/E ciia mau CT3, Ml va MZ trong dung dich NaCI 3 % Bdng 4: Thi an mdn (Ecor) va ddng an mdn (Icor) cua
CT3, Ml va M2 trong dung djch NaCI 3 % I„,(A/cm')
E„(V/AgCI) CT3 8,9x10-*
-0,654 Ml 1,1x10""
-0,206 M2 9,7x10"'
0,098 Sd lieu thu dugc tren hinh 9 va bang 4 cho thay, cac miu M l va M2 cd Ecor duong hon E^, cua thep CT3. Chiing td miu thep CT3 cd phii PPy cd pha tap cac anion dac biet la anion molybdat cd kha nang uc chi bao ve an mdn. TiJr sd lieu ddng an mdn cho thiy Icor cua Ml va M2 cao hon ciia CT3, dieu nay cd the Iy giai la trong giai doan nay mang PPy cd vai frd nhu mgt anot bao ve.
3.8.3. Phd tdng trd
Hinh 10 trinh bay pho tdng trd dien hoa (EIS) cua mang Ml va M2 frudc va sau khi do OCP. Phd tdng trd thu dugc chia lam 3 viing:
- Viing 1 (viing tin sd fren 1 kHz) the hien dac tinh cua dung dich dien li. Viing nay gdc pha gin bing khdng va dien trd ciia dung dich dien li khoang 50 Q.
- Viing 2 (viing tin sd frung binh) the hien dac tinh cua mang polyme.
- Viing 3 (viing tin sd thip) the hien dac tinh ciia vung tiep giap giua mang PPy va dien cue. Cd mgt ty dien do Idp dien tich kep va dien frd chuyen dien tich xuat hien [17].
Ket qua nghien cihi cho thiy mang PPy trudc khi do OCP d frang thai dan nen cd gia tri nhd (hinh 1 Oa va j Ob), frong dd miu M2 (hinh 1 Ob) cd trd Idn hon miu Ml (hinh 10a). Diiu nay giai thich su cd mat ciia anion molybdat lam tang kha nang phan iing vdi cation Fe^"^ de tao ra hgp chit khd tan va lam tang di§n frd ciia mang. Kit qua nghien cuu nay phii hgp vdi nghien cuu tdng trd ciia mang PPy do trong dung djch H2SO4 [17]. Sau khi do OCP, mang PPy chuyen sang frang thai khii, do dd frd ciia mang tang
:K, ^ "
"'^^r^
(a) (b) EIS Ml (a) vi M2 (b) ban dau
...--
\
».
g ^
\
\
1. 1»
(c) (d) EIS Ml (c) v^ M2 (d) sau khi do OCP
Hinh 10: Phd tdng trd mau M l va M2 khi bit diu va kit thiic do OCP frong dung dich NaCI 3 % 4. KET LUAN
Mang polypyrrole (PPy) dugc tdng hgp tren bl mat thep CT3 da thy dgng trong dung djch nafri molybdat 0,1 M bing phuang phap dien hda trong dung dich chua monome pyrrole, chit pha tap molybdat va 10-camphosunfonat. Hinh thai hi mat ciia man§ PPy (SEM) cd hinh dang hoa xiip lo diln hinh. Phd Raman cho thay PPy tdng hgp dugc d frang thai oxi hda. Phd tan xa tia X theo nang lugng (EDX) cho thay so xuit hien ion molybdat frong mang PPy. Ket qua phan tich nhiet cung cho thiy sy xuat hien ciia hgp chit vd co chiia Mo khd bj phan huy (gan 20 % khdi lugng miu). Kha nang \SQ chi chdng an mdn thep CT3 frong dung dich NaCI 3 % cua mang PPy theo do thd mach hd (OCP), do dudng cong phan cue Tafel va do phd tdng trd. Cac ket qua cho thiy, mang PPy cd pha tap ion molybdat dugc cai thien dang ke so vdi mang PPy khong c6 ion nay.
Loi cam on. Cdng trinh nghien cuu ndy dugc tdi trg bdi Bi tdi Cdp ca sd ciia Trudng Bgi hgc Mo -
T C H H . T 52(6), 2 0 1 4
Bia chdt vd Quy phdt triin khoa hoc vd cdng nghe qudc gia (NAFOSTED), di tdi md sd 104.02-
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