pvdf-hfp/pvp supercapacitor - cheric · 2003-12-30 · 788 hwahak konghak vol. 41, no. 6, december,...
TRANSCRIPT
HWAHAK KONGHAK Vol. 41, No. 6, December, 2003, pp. 788-794
PVdF-HFP/PVP Supercapacitor
†
449-728 38-2
(2003 4 7 , 2003 9 7 )
Electrochemical Characteristics of Composite Electrodes with Polypyrrole for Supercapacitor with PVdF-HFP/PVP
Ho-Sung Oh, Kyong-Min Kim and An-Soo Kang†
Department of Chemical Engineering, Myongji University, Yongin 449-728, KoreaSan 38-2, Nam-dong, Yongin, Kyonggi 449-728, Korea(Received 7 April 2003; accepted 7 September 2003)
5-8 wt% (BP-20 YP-17) Poly (vinylidenefluoride-co-hexafluoropropylene)
(PVdF-HFP)/polyvinylpyrrolidone(PVP) n-methyl-2-pyrrolidinone(NMP) !"#.
$%& ' ·( ), *+,, AC-ESR, -./, CV impedance ) 0 1234 ) 5+!"#.
5 wt%6 +!" 7 89, :; 1<4 = >? 1234 ) @A !1
%!B CDE,F 8 wt% FG6 !A HF 4I!"#. )J, BP-20 K CDE,
F 7 wt%L 7 *+, 34.77 F/g, AC-ESR 0.65Ω, -./ 8.16 Wh/kg MN/ 1,830 W/kgO6 P2
K QR# >?!" Ragone plot PS T 7 1MU 4V W T ? XY#.
Abstract − Composite electrodes were fabricated based on activated carbons such as YP-17 and BP-20, and conducting poly-
mer of polypyrrole (pPy) prepared by chemical polymerization in our laboratory. Mixed binders of Poly (vinylidene-fluoride-
co- hexafluoropropylene) (PVdF-HFP) and polyvinylpyrrolidone (PVP) in n-methyl- 2-pyrrolidinone (NMP) were added to the
activated carbons. Electrochemical characteristics of unit cells such as charge-discharge, specific capacitance, ESR, specificenergy, cyclic voltammetry (CV) and impedance were measured. It was noted that a pPy content within 8 wt. % greatly
increased the electrochemical characteristics, mechanical strength and flexibility with the fixed 5 wt. % of mixed binder. Espe-
cially, the BP-20 electrode with 7 wt% of pPy exhibited better electrochemical characteristics than commercialized products,with 34.77 F/g of specific capacitance, 0.65Ω of AC-ESR, 8.16 Wh/kg of specific energy, and specific power of 1,830 W/kg.
Power outputs were compatible with electric vehicle applications, in due consideration of Ragone relations.
Key words: Polypyrrole, Supercapacitor, Activated Carbon, Polyvinylpyrrolidone, Poly (Vinylidene-Fluoride-Co-Hexafluoropropylene)
1.
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w" 2T, · ~ -' JD ~W<†To whom correspondence should be addressed.E-mail: [email protected]
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Ji¯"[9].
Ji] °±², ì#D í£Q Ji] rî' >?(YP-17, Kuraray
Chem.; .:;< 1,566 m2/g, æSh± 0.76 mL/g, æS 10.86 ï) % ð
ñDQ Ji] rî' >?(BP-20, Kuraray Chem.; 1929 m2/g, 0.86mL/g,
13.3 Å) Ê LMQ -'¯". @A rs >?B °±²
Ð/ sheetr ¿sQ Ji Ïо @ ÉFE
FJU -'¯". ã Ê3 @ Ñ6 ò3 Ê kó d
§ ì ôQ õL Ê Ji0 EFJQ ³ -' p PVdF-HFP
(KynarFlex® 2801, ELF Atochem) @JQ PVP(120 K, ISP Tech.)
U -'¯". ö# @÷ ÞÏÐ @A rs °±²B >?
ball millQ 12f $ @ø Ë 200µm meshQ @_ ÏÐ
@A ù.¯".
@Q n-methyl-2-pyrrolidinone(NMP, Lancaster, _, England)U
-'¯ £(. 7:3 PVdF-HFP/PVP ÉFEFJU 5 wt%Q '
ù.] >?0 °±² u á¾ .Q ÉF 1<
Ú~U ' 450-500 rpm 6Q Ú~¯"[10]. ¢6 800-
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1)U ' .:;<, ÓææS(micropore, HK method) % )f-ß
&æS(meso-macropore, BJH method) m/¯, :; +Ô
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2-2.
þ 6 CD propylene carbonate(PC, Junsei,
_, Japan) ' J4_ ÿ× ) 66 CD |
«<TQ / õL ` ³ v' p tetraethylammonium-
tetrafluoroborate(Et4NBF4, Fluka, _)U £Q -' 1.0
N 6 ¶ Ji¯"[4, 11]. Ji] ¶ 66
25 oC0n 13 mS/cm!T .)3 1.195!". 1 ¶
-' supercapacitor -' (working voltage) 2.3 VôQ
@ 1.23 V D@ ¶ ¨0 50 ppm Q molecular
sieve(sodium alumino silicate, Sigma)U ' J Ë Karl-
Fischer moisture titrator(MKS-210)Q m/ ¶ ¨ D@ ª
( ¯".
2-3.
Ji Ê aluminium foil(2AL10-5/1 HX, Ùü 60-90µm, USA)
0 carbon paste(Everyohm 101S, Nippon Graphite, Japan)U '
È Ë 110oC0n 2f $ ëi Ë 0.5 cmHg j&7TQ
110oC0n 5f r ëi Ê ¨h D@ Jß
¯". D@ Jß] Ê :;0 Ê LM< 0 ¶
0.4-0.6 ml ö Ë , Nb < 0 acryl plate
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Lim., 10µHz-32 MHz, frequency resolution 0.015 ppm, accuracy 0.1%
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Arbin, USA) ' / 2.3 V, 10@f Ë /Ö 10 mA
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(CV) m/¯".
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F] °±² '0 + /wU ¸ Ji] MU
KBr @AB H 1% 6 ÉFQ H 15-20 psi 7
KBr pelletTQ Ë <´ @@ (FT-IR, model 2000,
Perkin Elmer Co.)U ' 4,000-500 cm−1 mid-IR 0n
Fourier Transform Infrared(FT-IR) b! " m/¯".
HWAHAK KONGHAK Vol. 41, No. 6, December, 2003
790
s
3.
3-1. FT-IR
°±² F % 6 Q -'] BF4− aU
n <´ @@ U -' @ EBU Fig. 10 d§¨!
". °±² -º0 # 1,536 cm−10n C=C stretching
vibration band, 1,450-1,310 cm−10n C-N, C-C vibration band, 1,210-
1,090 cm−10n C-H in plane band 960 cm−10n C-H out of
plane % # 1,030, 765 cm−10n BF4− counter ion ±½Qh
°±² F !ê ¯".
3-2.
3-2-1. ./'(
PVdF-HFP PVP 7:3 á¾.Q ÉFEFJU Ê LM
$ ᾪ( 5 wt%Q /¯[10] >?0 °±² ᾪ
( 5, 6, 7 % 8 wt%Q © Ê Ji, ÍÎ J Ë Battery
Test System ' / 2.3 V, 10@f Ë /Ö 10 mA
Q 1.0 Vä f m/¯". ¤ /'( 1 Ë Ê
á¾Q d%H ./'( W¯".
°±² ª(.0 o YP-17B BP-20 Ê · Â
 Fig. 2 Fig. 30 d§¨!". °±² ª( 7 wt%Ð ã YP-17
B BP-20 Ê0n f ÂÂ 1,546 % 1,821&Q BP-20
Ê CD /'( ' 2¾ d§(". u EB
ÉFEFJU -'¯ ã @J B Ú EF7 CD
PVP >?B °±² )* @¼ .:;< 2, Ê
V % Ñ6U ·¾ ¯T ©] °±²0 3
^< @÷U d§¨H >?B °±² -0n synergy B[8]
U ' ÕÛ ã+0 ¨hkó ò /'( Õ] ¹TQ
gÂ".
·3 °±² ª( 7 wt% C YP-17B BP-20
Ê0 © ,3 Íe ÊB © Ê ·
Fig. 40 d§¨H .Ú EB BP-20 Ê YP-17 Ê0 .
¨hkó3 .-¯Td CD¯". ¤ ÂÂ .
/'( 1 EBU Fig. 50 d§¨!T, YP-17B BP-20
Ê ./'(3 ÂÂ 26.95 % 34.77 F/gTQ BP-20 Ê CD
¾ d§(".
Ê Ji °±² © >? SÊ0 ./ ö#
-U 3^<TQ @÷0TQl ¨hkó3 òå 04 k`
Sf3 Õ H Ê < ¬rÛ" -M]"[8].
u EB ðñD 11 >?B 6 N(J(VGCF)U ©
-'¯ ã 6 N(JU © ,2 ãw" ·3
< d§3 Endo K[12] EB Ða¯".
Fig. 1. FT-IR spectrum of chemically synthesized polypyrrole powder.
Fig. 2. Effect of added weight percents of polypyrrole on charge/dis-charge curves of YP-17 electrode with mixed binder.
Fig. 3. Effect of added weight percents of polypyrrole on charge/dis-charge curves of BP-20 electrode with mixed binder.
Fig. 4. Effect of addition and non-addition of 7 weight percent polypyr-role on charge/discharge curves of YP-17 and BP-20 electrodewith mixed binder.
41 6 2003 12
Supercapacitor 791
n Ê Ji 6 @#U © ã >? ö# -
U <TQ VE 66U ¬r¼ hkó3 ¦ h
@<TQ °±²0 #$ u /'((pseudo capacitance)
>?0 ) '(B F<TQ Oõ4TQl 23 ·
B ./'( d§I" ¹ D p!".
3-2-2. 2005 ·
· CD BP-20 Ê °±² ᾪ( 7 wt%
Ð ã 2005 · Fig. 60 d§¨!". 2.3 Vä /Ö 30 mA,
/ 2.3 V0n 30& $ Ë /Ö 30 mAQ 0 Vä
;n 2005 V m/ EB & 35ä 2.44% /'(
¦ 7.07% DC-ESR(IR drop0 ¨hkó) ÕU w¯Td 3
5 rh /'(B DC-ESR 6| ½ ,ê 7 D p!
". ¹3 å½8TQ Ji ÍÎ 9® sealing
,2 ã+0 ¶ %¶0 ¨hkó ÕQ D pT
, 35 r0n · cycle0 k ã+0
/ 04 k``a Ê LMQn <' " ¹ 7 D
p!". t ÍÎ 8<:F.U ' stack Î Ji;
ã /'(B ¨hkó 6|3 ' ¦ ¹ Í HX".
3-2-3. KÇ<kó
PVdF-HFP PVPU ./'( 3.2.1jB =3 ië0n ÍÎ
J Ë °±² ©(0 o KÇ<kó(AC-ESR, 1 kHz)
Fig. 70 d§¨!". 0n Ç´3 YP-17B BP-20 Í[TQ
-' C >´3 °±² © CQ © AC-ESR
?@ òåAT BP-20 C 7 wt%0n 0.65ΩTQ ` ò3 B
d§¨!". EB · % ./'( EB6 Ða
¯". ./'( ` CD °±² ᾪ( 7 wt% C
© ,3 C ÊC ±bU Nyquist plot EBU Fig. 8
0 d§¨!". tD0n d§I E = >?/Ppy F$ C
°±² -' ,3 Cw" ÊB £ 1; 1
$6 , d @# 0 Warburg ±b
_® ¦ _ ./'( Õ AC-ESR
U ¦¼ CD d§¨!". t YP-17w" BP-20
Ê AC-ESRB CD¯T ÊB 1;0n ~v6
frD å Ö /rrs0 F 6Å _
" ¹ 7 D p!".
Warburg ±b >´ )f h@0n ÷|(charge saturation)
0 1´ d§I ¹ D p!T õr3 6
@#0n Og õrTQ 6 @# °±²0
u ~v(pseudo reaction) D p!"[8, 13].
3-2-4. 0456 $756
Fig. 5. Effect of added contents and non-addition of polypyrrole on spe-cific capacitance of electrodes with mixed binder.
Fig. 6. Effect of charge/discharge curves of 200 cycles on specific capac-itance and DC-ESR of BP-20 electrode with 7 weight percent ofpolypyrrole and mixed binder.
Fig. 7. Effect of addition and non-addition of 7 weight percent polypyr-role on ESR of electrodes with mixed binder.
Fig. 8. Effect of addition and non-addition of 7 weight percent polypyr-role on Nyquist plot of electrodes with mixed binder.
HWAHAK KONGHAK Vol. 41, No. 6, December, 2003
792
°±² ª( 5, 6, 7 % 8 wt%Q Ê Ji Ë 0456
$756U Table 10 d§¨!". ./'( ` CD >
?0 © °±² ᾪ( 7 wt%Ð ã YP-17B BP-20Ê
0456 ÂÂ 6.33 % 8.16 Wh/kg! $756 ÂÂ 567
% 1,830 W/kgTQ ® BP-20 Ê CD¯".
u EB ðñD 11 >?B 6 N(JQ VGCFU
© Ê Ji¯ã ESR 0.8Ω, 0456 5.87 Wh/kg
d§3 Endo K[12] EBw" CD d§G". õLä
w] VW -H0n supercapacitor 0456 2-7 Wh/kg
à VW0n °±² ª( 7 wt%Ð ã 0456 8.16 Wh/kgTQ
0456w" 23 EBU ¸! 1,830 W/kg 23 $75
6 Conway[4] Ragone plotr0n &´r0 a ¹TQ wå
n r' #$06 @® <' D p" Í]".
3-2-5. SEM @
|«< ` CD BP-20 Ê °±² ª( 7 wt%
Ð ã ÍÐEFJ ÉFEFJ Ê :; 1,000: & SEM
Fig. 90 d§¨!". Ji] Ê :;Wi Ñ6 % ¶ ª
Ì +Ô EB ÂÂ Ê :;3 "S WiU D p
!T Ê Ñ6 CD ¶ @® ªÌâ D pê 7
D p!". tud PVdF-HFP ÍÐEFJU -' Ê(A)w" ÉF
EFJU -' Ê :;(B) :;Wi ' ÏÐ NSJ
B Ú EF7 CD PVP0 >?B °±² )* @
¼ .:;< 2, Ê V % Ñ6U ·¾ ¯T ©
] °±²0 3^< @÷U d§¨H >?B °
±² -0n synergy BU ' ÕÛ ã+0 |«<
CD¯"[8].
3-2-6. CV
Fig. 10 % 113 ÂÂ >? YP-17 % BP-200 °±² 7 wt% ©
C -6U 5, 10, 20 % 50 mV/sQ CV0n m/
Ö56U - 6Q d%H 0 & ./'( d§3 EB
". BP-20 Ê YP-17 Êw" CD ./'( d§¨
! -60 r+ ÉFEFJU -' °±² ª( 7
wt%U ©; ã '(- >´ ;< Õ CD ./
'( d§¨!". EB Ê .:;< ½ °±²0
66 Õ #$ u /'( >? .u
/'(B F<TQ Oõ H ./'( Õ¯ ã+,
ÊB 1; 1 $6 Õ¯ frD å
Ö /r rs0 F 6Å D pTôQ CV>´ (plateau)
h@ d§I" Yoon K[14] EB Ða¯ ß r# ¿s
Q /'( 2¾ d§(". tud Ü0n I¾ » ¹
3 J E = °±² |, ^~v0 u '(
Table 1. Effect of polypyrrole weight percents on energy density and power density of YP-17 and BP-20 electrodes with mixed binder
Polypyrrole[wt%]
YP-17 BP-20
Energy density [W·hr/kg] Power density [W/kg] Energy density [W·hr/kg] Power density [W/kg]
5 4.30 261 5.85 4206 5.05 313 6.53 6417 6.33 567 8.16 1,8308 5.63 396 7.49 764
Fig. 9. SEM micrograph of BP-20 electrodes with 7 weight percent poly-pyrrole with (a) PVdF-HFP binder, and (b) PVdF-HFP+PVP mixedbinder.
Fig. 10. Effect of scan rate on specific capacitance of YP-17 electrodewith 7 weight percent polypyrrole and mixed binder.
41 6 2003 12
Supercapacitor 793
ã+"[4].
CV>´0n plateau h@3 -6 5 mV/s0n BP-20 Ê
YP-17 Êw" ' OÅ] ¹ D p!". tud -6
£DK rounding (sloping) õr Õ CV>´ h
@ H '( d§¨ - r#¿ CV
H ¹TQ wå '( ß$ ½¾ k ¹TQ Í
D p!"[4, 14]. Fig. 10 % 110n 7 D pL -6 òDK
-'( >´ ·åA ã+0 1-6 YP-17B BP-20
Ê0n 5 mV/sQ d§(". ® 1-6 5 mV/s r0n
ÍÎ ¨hkó3 ' ¾ 04 k` w"
@ !"[4]. CV>´ plateau h@, 1-6U .Ú ã YP-17
Êw" BP-20 Ê0n $6 Õ frD
' å ./'( CD" ¹ 7 D p!". EB<TQ
Ë ¡3 5 mV/s -6Q ¯".
-6 5 mV/s C YP-17 % BP-20 Ê0n °±² ª(
6|0 o ./'( Fig. 12 % 130 d§¨!". °±² ª
( 7 wt% C ./'( ` ·2". EB 0456,
ESR % ±b ¬ MNÌ D p! ·0n m/ .
/'(B6 Ða¯". °±² © C © ,3
C ./'( Fig. 140 d§¨!". tD0n 7 D pL j
EB Ða¯ BP-200 7 wt% °±² © C Ê
` CD¯".
3-2-7. Ê .:;<
ÉFEFJU 5 wt%Q / °±² ª(0 o BP-20 Ê
æS @÷U Fig. 150 d§ !". Fig. 15(a) micropore mesopore
æSh±(HK method)U d§3 ¹ (b) mesopore macropore
æSh±(BJH method)U d§3 ¹". ©] °±² ª
( 7 wt%Ð ã BP-20 Ê BET m/O0 .:;<3 ÍÐ
EFJÐ ã 884 m2/g, ÉFEFJÐ ã 1,632 m2/g, HK m/O0
Ï æS ½ 15.8 Å0n 5P] ¿r d§¨!". eD >
? C0n .:;<(2,015 m2/g)w" °±²B ÉFEFJU
©ªTQl Ê .:;<3 r&<TQ ¦¯". Ê .:
;< QDK, frD DK ./'(B 0456 Õ
ª 7 D p!".
5.
Coconut shell1 YP-17 % ðñD1 BP-20 rî' >?0 #
$ Ji °±²B PVdF/PVP ÉFEFJU -' Ê Ji
Ë ÍÎ J · , ./'(, ESR, .:;<, 0
Fig. 11. Effect of scan rate on specific capacitance of BP-20 electrodewith 7 weight percent polypyrrole and mixed binder.
Fig. 12. Effect of polypyrrole weight percents on specific capacitance ofYP-17 electrode with mixed binder, 5 mV/s scan rate.
Fig. 13. Effect of polypyrrole weight percents on specific capacitance ofBP-20 electrode with mixed binder, 5 mV/s scan rate.
Fig. 14. Effect of addition and non-addition of 7 weight percent poly-pyrrole on specific capacitance of electrodes with mixed binder;scan rate=5 mV/s.
HWAHAK KONGHAK Vol. 41, No. 6, December, 2003
794
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=3 ER ¸!".
(1) °±² ©¯ C Ó© w" |«<
¯, ÍÐEFJw" ÉFEFJU -'; ã .:;< Õ
¯ YP-17w" BP-20 Ê |«< CD¯".
(2) ÉFEFJU 5 wt%Q / BP-20 % YP-17 >?0 °
±² @A ©; ã |«< CD Ê Ji D
p °±² ᾪ(3 8 wt% ¨ <S¯".
(3) >? BP-200 °±² 7 wt% © Ê .:;< 1,632
m2/g, ./'( 34.77 F/g, AC-ESR 0.65Ω, 0456 8.16 Wh/kg
% $756 1,830 W/kgTQ r'|] w" CD¯
Ragone plot r0n ã #$0 <' D p" Í]".
(4) 7 wt% °±² ©¯ ã '(- >´(CV) plateau
h@, -6U .Ú ã YP-17w" BP-20 Ê0n $6
Õ frD ' å ./'( ' ¹ 7 D
p! õr3 |·^0 h@< u /'( >
?0 .u /'(B F<TQ d§d ¹ D
p!T, 1-6 5 mV/sQ Í !".
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Fig. 15. Pore volume distribution vs. (a) micro- and meso-pore and (b)meso- and macro-pore at various polypyrrole contents of BP-20electrodes with 5 wt% mixed binder.
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