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1. #g«#

²R Î×, ŠVF, PDA– o– ŠVÿ Zæ ††® ÿÊ ó V¾& †Ò 6&^ VÒ VÆ âkªV Vû² Z& V

² VBÊ èš6 Þ:. ʖ o– êÂ& Ö§®B ²R Vû $

– Wgš q6 Þê 6‡û ~ŽV Z g® ®îV  6Úæ Ê~ Z(LPB)Ê:. 6Úæ ZÊš ÿ®ê LPBê · ZÊ

š ÿ² †Ê® Ê~ Z(LIB)V Vê žk‡® Žr, rÆ šÿ® 6V, 6ÿª® z G® Žrfš JšÊ Z n Þê ~ŽV ZÊ:.

6Úæ ZÊ– J(&Nb {Ê2)(PEO), JšÂ²

Êr R& ®Ê k‡r Ê~ Z² k®nÆ šÿ: 6Úæ ZÊR Vâªr 6Úæ Zʲ îZ:.¹O‡†(O, S, N)Ò V 6Úæ– R"’² ‡r šÿ: 6Úæ ZÊ– š¦W 

– Ê~ ZÒ îÆ ÊÒ Ê®† Z®B š¦W è– v Zn(dielectric constant)Ò lê v† ÿ:Ò Êÿ² ÙÊ V⪠r 6Úæ ZÊÊ:.^2,3Vâªr 6Úæ ZÊ– þVr v†ÿ :V Vâr C¶š ®B 6Úæ® k‡š fâ2úÆ, 6Úæ

Ú^ /š &²®â ®Æ, B²  R® Ê~Z Bê 6Úæ O‡†–  Ê~Z® Ž çÿš fâ2r šÿ: 6Úæ ZÊ

J: ûr Ê~ ZÒ î6 Þ:. ^4-7

Vâªr 6Úæ ZÊÊ Ê~ Z® Ê&r :ÿWÎ nVÊ n zÊ · ZÊš : ¾vÊÒ ®êÆ, Ê  †W ’‡Ê

>ÓÊâ nê Žrfš V6 Þ:. ÊB² Žrfš Ê®†

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® ê ûfÊ Þ:.

N :.:&rê &>& šÂ†V Þê J(&Nb V²-co- Z²šb V²)š ¿‡®B ª¯W V¦ ÂÆÒ V zk 6Úæ ZÊš rÆ®V’Æ Ê~ Z– †W ’‡š û2ú†

Z®B îΠ†® Š† ÿZrÒ þV² zk 6Úæ ZÊš r Æ®B ZÊ® Ê~ Z– †W ’‡& V² FÂÒ nßÊ ª:. ^8-10

6Úæ ZÊ&r · Zʲr Êÿn6 Þê v† ÿ:ê n r‡ÊÆ VF‡Ê† ¢Ž&  Ê~ Z& Wÿ2 žk‡ w Ê&r Žrfš V6 Þ:. " šÒ v† ÿ:–  Rš

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¿Ž¨YÌ#§##–á#$¨#

+?Ç}»C@}‹ K}7K}‹°}¿$O}ó÷^.}¿LK^%# G@(c# ^c5c</#^.G@(c# ÄÐ5c<#

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#

D#Vwxg|#rq#wkh#Suhsdudwlrq#dqg#Fkdudfwhul}dwlrq#ri#Jho#Sro|phu#

Hohfwuro|wh#iurp#Sro|+hwk|ohqh#jo|fro,#Gldfu|odwh#lq#Lrqlf#Oltxlg#

Erud#Vklq/#Pl#Vxn#Fkr/#Gxnmrrq#Nlp/#Vdqj#Mxq#Vlp/#Ml0Khxqj#Nlp/#

Grqj#K|xq#Ohh/#Mdh0Gr#Qdp*/#dqg#\rxqjnzdq#Ohh^%# Department of Chemical Engineering,

*Department of Polymer Science & Engineering, Sungkyunkwan University, Suwon 440-746, Korea (Received February 25, 2005;accepted March 17, 2005)

imidazolium bis((trifluoromethyl) sulfonyl) amide(BuMeIm⁺Tf2N^-)² ‡r ZÊ ÿ·š ¾v®ê z k2® 6Úæ ZÊš rÆ®V:. Ê~‡ ·V 6Úæ ZÊ® Ê~ Z& N®ê Wûš Æ®V’Æ, †Ê® v†

ÿ:Ò y– 6Úæ ZÊJ: è– Ê~ Z(ca. 10^-3 S/cm)– Z† ª¯W žk‡š îš ¢ n Þ:.G

Abstract:A new type of polymer gel electrolyte was prepared from poly(ethylene glycol) diacrylate(PEGDA) and 1- butyl-3-methylimidazolium bis((trifluoromethyl) sulfonyl) amide(BuMeIm⁺Tf2N^-) ionic liquid. The effect of the ionic liquid on ionic conductivity of the gel polymer electrolyte was investigated. It was observed that the gel polymer electrolyte having the ionic liquid exhibited higher ionic conductivity (ca. 10^-3 S/cm) as well as electrochemical stability than that using organic solvent.

Keywords: polymer gel electrolyte, PEGDA, ionic liquid.

†To whom correspondence should be addressed. E-mail: yklee@skku.edu

G

ÿ®B rƲ 6Úæ ZÊ® Ê~ Zê ²V Þ:. Ê

~ Z® ûš ZÊ  R® ¾š èÊÊ, æ Ê® ¾

&rê 6Úæ® vZÊ ~V ®â n Ê~ ZV fâ®â r:.^11-14 ÊB² Žrfš Ê®† ZÊrê JW, Z†

ª¯W’² žk®Êr  Ê~® Ê/š J: þ~W’² ó V2r Z n Þê ² k2® VârÒ Û®ê ÙÊ šê®:.

®ê Ê~‡ Rš ®N®Æ N g ~&r ·² Ê®ê Ù

š ~ Ê~‡ ·(room temperature ionic liquid, RTIL)Ò ²:. Ê~

ê j¢ÊN:ξ, ¢’jÚ, 4_ ªþÚ, 4_ BúBÚ GÊ Þ’Æ ¢Ê~’²ê NO^3-, BF4

-, PF6 -, AlCl4

-, Al2Cl7

-, AcO^-, TfO^-, CF2SO2)2N^-, CH3CH(OH)CO2-GÊ Þ:. Ê~‡ ·ê k ÿ:² r šnr‡, Š‡, šVF‡ÊÆ n² JW žk‡, è– Ê~

Z, i– ZZ“ Gš V6 Þ:.^15,16 ÊB² ‡ ¢Ž& Ê

~‡ ·ê _:– v† ¿‡ 2 ÿ:²r ÿnÆ ·-· Ú¹⁷ N6 Z† ª¯ ÚÒ G®^18-20:ç² ÚÒ&r Êÿn6 Þ:. Ê

~‡ ·V l6 Þê è– ZÊ ‡R šB, Òn v† ÿ:

–ê :Êâ – 󆫖 †Ê ZV l6 Þê žk‡ ŽrÒ Ê¶ n ޚ ْ² †Vn:.

N :.&rê Ê~‡ ·² 1-butyl-3-methyl imidazolium bis(trifluo- romethyl sulfonyl) amide(BuMeIm⁺Tf2N^-)Ò ¿‡®B²¹è– Ê~ Z

Ò VÊr n² Z† ª¯W žk‡š Vê zk 6Úæ ZÊ® rÆ& Êÿ®V:.

2. /#

2.1 'È

BuMeIm⁺Tf2N^-Ò rÆ®† ZÊr ªNÊN:Î(99%, Aldrich), b

²þÖ(99%, Aldrich), ʲ²&(Aldrich),  šúb²

²ªN zB&šN2(97%, Aldrich)– jʲ²ª(Junsei)š ÿ

®V:.

z 2® 6Úæ ZÊš rÆ®† ZÊ PEGDA(Mn ca. 700, Aldrich ), úÆÒ Ò³Ê2(BPO, Aldrich),  b²²ªz BzÊ(Li⁺TfO^-,Aldrich), Z²šbÊJzÊ(PC, Aldrich), &Nb ÊJzÊ(EC, Aldrich)Ò ÿ®V:.

:.& ÿ² þ6 2Ó:– ® krRk Ê ÿ®V:.

2.2 s#¿s|#¬ÿ/#ExPhLp^.Wi5Q⁰£#´|##

BuMeIm⁺Tf2N^-ê P. Bonhote– o– 뒲 ¿‡®V:.²¹¿‡r BuMeIm⁺Tf2N^-® ÂÆê ¹H-NMR– ¹⁹F-NMR² «Î®V:. ¹H-NMR /706SSPV+W+W+(t, 2H), 4.07(s, 3H), 2.00~1.90(m, 2H), 1.39(sext, 2H), 0.95(t, 3H).

2. 3 o '£ +ÏÛ O¿£ g»

z 2® 6Úæ ZÊ(polymer gel electrolyte, PGE)– EC– PC Ò 1V 4® ֒ š² ’¿®B "6 ’¿ ÿ:& 0.5 mol Li⁺TfO^-š

Rk f& ֖ :¢ V_®B 80 ×® zf& y J ª2þ:

[PGE(EC/PC+Li)].⁸ Z– o– ÆÊ&r EC– PC ’¿ ÿ: V6&

¿‡² Ê~‡ ·Î BuMeIm⁺Tf2N^-Ò ÿ:² ®B :Î Û®®

6Úæ ZÊš "6:[PGE(BuMeIm⁺Tf2N^-+ Li)].

B² Ê~‡ ·"’² ZÊš rÆ®B [PGE(BuMeIm⁺Tf2N^-)]

 RÊ :Z 6Úæ ZÊR® ‡š š¦®V:

PEGDA– · ZÊ® š~–  š² 1V 3Ê6, r2rê 6Úæ Vš 1 wt%Ê:. ʲ¾  6Úæ ZÊ šÚ– 200

m® ¦.Ò VÆ vF² z 2Ê:. N :.– šÊ: Vú ÚZ† ®® 2ÒÊ kú &r ß®V:.

2.4 l` Z Ïh

2.4.1 ⁴K0QPUG#^4<I0QPU#Ïh##

:.š Ê – Ê~‡ ·Î BuMeIm⁺Tf2N^-® ÂÆÒ «Î®

† Z®B Varian® Varian 500 NB ††Ò ÿ®B ¹H-NMRR

19F-NMRš wk®V:.

2.4.2 GVF#Ïh

DSCÒ Êÿ®B BuMeIm⁺Tf2N^-– 6Úæ ZÊ® JW ‡

š Ús®V:. wk ††² Seiko® Exstar 6000(DSC 6100) r ޚ ÿ®V:.

BuMeIm⁺Tf2N^-® &ê -50»6 ×® ~ êZ&r 5 ×/min®

~ ã² ⠆® ®& wk®V:.

PGE(EC/PC+Li)R PGE(BuMeIm⁺Tf2N^-+Li)® vZÊ ~® Æ/

š ¢šJ† ZÊ -80»40 ×® ~ êZ&r 5 ×/min® ~ ã

² ⠆® ®& wk®V:.

2.4.3 WJD#Ïh##

BuMeIm⁺Tf2N^-– EC/PC ÿ·® JW žk‡š š¦ Ús®† Z

®B TGAÒ wk®V:. wk ††²ê Perkin-Elmer® TGA-6š

ÿ®V’Æ 25»500 ×® ~ êZ&r 10 ×/min® ~ ã

² ⠆® ®& 2ß®V:.

2.4.4 ¿s O£ l`

rƲ Ž Û®® 6Úæ ZÊ® Ê~ Zê ¦®Ò ®zR Æ Ú’®úÒ wk¾’²¾ ®V:. wk& ÿr ûšê Solar- tron® SI 1260 Impedance/Gain phase analyzerÊ:. ¦® Z«® C

– 5 mVrmsÊ6 Rbnê 10 mHz»100 kHz² ª2†:. Ê~ Z

ê ú¢Îú úN ZOš ÿ² š²‡ ZO –š ‡²

 21 ×&r 84× ~ êZ&r 30ÚZ v²  wk®V:.

2.4.5 O{ Ÿ¤L Ïh

6Úæ ZÊ šÚ® Z† ª¯W žk‡š ¢šJ† Z®B r

® Z« Z®ë(cyclic voltammetry, CV)š wk®V:. wk ††² Ametek® PARSTAT 2263 Potentiostat/GalvanostatÒ ÿ®V:. Ê¢

cell– SS//6Úæ ZÊ//Li//SS² ":, çZO’²ê ú¢Î

^ú úN ZOš ÿ®6 †V ZO e V ZO’²ê  Z

N

N CH₃

Bromobutane

o o F₃ C-S-N-

-S-CF₃ o o Li⁺

phase separation

+ H₂O N

N CH₃

C4H9

N N CH3

C₄H₉ Br^-

o o F₃ C-S-N-

-S-CF₃ o o

BuMeIm⁺Br^-

BuMeIm⁺Tf₂N^-

G

Scheme 1. Synthesis of BuMeIm⁺Tf2N^-.

G

Oš ÿ®B -5»10 V ZZ ÂZ&r 100 Mv sec® ã² r

®®B wk®V:. Z« ª& †Î Z® ª²Ö† Z†ª¯

W žk ZZ êZÒ Â®V:.

3. ûG Z ë«

3.1 ExPhLp^.Wi5Q⁰‹#+ÏÛ#O¿£#?L#|

Figure 1– BuMeIm⁺Tf2N^-® DSC thermogram’² JW Æ/š î

:. Figure 1² BuMeIm⁺Tf2N^-® ÏêfÊ -13.4 × Úš V†®

V’Æ ~&r ·Úš «Î¶ n Þ:.

Figure 2ê 6Úæ ZÊ® DSC thermogram’², ÊÒ Ê PGE (BuMeIm⁺Tf2N^-+Li)Ê PGE(EC/PC+Li)J: – vZÊ ~Ò V

&š «Î®V:.

6Úæ ZÊÊ è– Ê~ Z‡š l† ZÊrê – v

ZÊ ~Ò VŽ 6Úæ ® Ú^ /Ê &²ÊÒ ²:. šî 6 Úæ ZÊ® DSC R²Ö† PGE(BuMeIm⁺Tf2N^-Li)Ê PGE(EC/

PCLi)J: 6Úæ ® vF‡Ê ᢚ «Î¶ n Þ:.

Ê~‡ ·ê v† ÿ:– B JW žk‡Ê n®:6 ¢z

Ž Þ:.²¹Êê EC– PC® ’¿ ÿ:– BuMeIm⁺Tf2N^-® TGA N îZÒ Ê «Î¶ n Þ:. Figure 3š JÊ EC– PC® ’¿ ÿ :ê Ó 170 ×&r _ÿ² Šâ fâÒ JÊê nÊ& BuMeIm⁺Tf2N^- ê 450 × Ê&r Šâ fâÒ JV:. ÊÒ Ê BuMeIm⁺Tf2N^- V v† ÿ:J: >‚ i– ~ êZ&r JW’² žk¾š « Î ¶ n Þ:.

3.2 +ÏÛ O¿£ ¿s O

Figure 4ê Ž Û®® 6Úæ ZÊ® ~& V² Ê~ Z

Ò š¦² ْ² Z ~ êZ&r PGE(BuMeIm⁺Tf2N^-+Li)Ê Vû è– Ê~ ZÒ JBV:.

Ê~‡ ·"’² "6 6Úæ ZÊ®  ~&r 1.7Ý10^-4 S/cm® Ê~ ZÒ îÆ ~V èš&& †Ò Ê~ Z

 óV®B 84 ×&rê 1.3Ý10^-3 S/cm® Ê~ ZÒ î

:. PGE(BuMeIm⁺Tf2N^-)– :Î ¦ Û®® ZÊ& šÊ – Z

Ò Vî  R® ÖVWÎ þV Ê Ê~‡ ·"’²

š¦W è– ZÒ V:ê f&r Rÿ¶ "®:6 3Wr:.

Ê~‡ ·ê †Ê v† ÿ:–ê B Ê~® k2² Ê®ê ÿ:ʆ ¢Ž& ÖVWÎ Ê~® þV Ê Ê~ ZÒ V

 n Þ¢š «Î¶ n Þ:. MacFarlaneR N® /":® FÂ

&r Z– v² RÒ R n Þ:.²²N® FÂ&rê N F – v² ۮΠEtMeIm⁺Tf2N^- Ê~‡ ·& PMMA– P(VP-co- VA)Ò Êÿ®B 6Úæ ZÊš rÆ®B Ê~ ZÒ wk®

VêÆ N hÊ 10^-3 S/cmÒ â²:. B² Fuller® &ê P(VdF- HFP)R Ê~‡ ·Î EtMeIm triflate² zk 6Úæ ZÊš rÆ

®V6, ~&r® Ê~ Zê »10^-3 S/cmÊ:.²³

v† ÿ:Ò ¾v®ê PGE(EC/PC+Li)® , ~&r 6.3Ý10^-4 S/cm® ZÒ JV’î ~V óV¾& †Ò óV®B 84.14 ×

&rê 1.47Ý10^-3 S/cm Ê~ ZÒ î:. Ê~‡ ·Ò ¾v

®ê PGE(BuMeIm⁺Tf2N^-Li)® &ê :Î ¦ Û®® 6Úæ Z ÊJ: þ6 ~ êZ&r n² Ê~ ZÒ JVêÆ ~

&r 1.01Ý10^-3 S/cm, 84.14 ×&rê 2.8Ý10^-3 S/cm® ZÒ î Figure 1. DSC thermogram of BuMeIm⁺Tf2N^-.

G

# 073# 063# 053# 043# 3# 43# Temperature(×)

Endo ←

Figure 2. DSC thermogram of PGE(EC/PC+Li) and PGE(BuMeIm

+ Tf2N^-+Li).

G

073# 053# 3# 53# 73#

Temperature(×)

Endo ←

Figure 3. TGA traces of BuMeIm⁺Tf2N^-and EC/PC under nitrogen atmosphere.

G

433#

;3#

93#

73#

53#

3#

Weight %

3# 433# 533# 633# 733# 833# 933# Temperature(×)

Figure 4. Arrhenius plots of ionic conductivity of polymer gel electrolytes with EC/PC and BuMeIm⁺Tf2N^-.

G

0517 051:

0613 0616 0619 061<

log ionic conductivity(S/cm)

51;# 51<# 613# 614# 615# 616# 617# 1000/T(K^-1)

T(×)

;7147# :41;6# 93166# 7<18;# 6<18# 63136#54145

:.

Z® Rê v† ÿ:Ò ¾v®ê PGE(EC/PC+Li) ZÊ 2ú

²J: Ê~‡ ·Ò ¾v®ê PGE(BuMeIm⁺Tf2N^-+Li)&r Êr

 Ê~® nV $6  Ê~® ÚÊ ²r®† ¢ŽÊÒ 6 6zr:. BuMeIm⁺Tf2N^-ê EC/PC& š®B O‡Ê Æ ÿ:ÊÆ ÒnW’² O‡Ê Æ ÿ:ê vZ~ B² è– Ù’² ¢zŽ Þ :.  R– è– vZnÒ V ÿ:& ®Ê Ê~ªnê Æ Ê~‡ ·Ò ÿ¾’²¾ ª $–  Ê~š š n Þ6 ʲ ÎÊ ª $– Ê~(charge carrier)Ê Z Rk& ŽB®â v

ÙÊ:.^24-26 RaiendranR N® /":® FÂ&r Z– v² R

Ò «Î¶ n Þ:.²⁷

6Úæ ZÊ&r  Ê~– 6Úæ R® Ú^ /’² ÎÊ Î:. NBî 6Úæ R& Ê®ê O‡ &¢Ê†®

k² Zæ R⠇–  Ê~Ê æv²Ê ÊêÆ Ê ê â² çÿ¶ n Þ:. PGE(BuMeIm⁺Tf2N^-+Li)® , Ê~R 6Úæ

® O‡ &¢Ê†Z® Ž çÿÊ ª þ~W’² fân 

Ê~Ê ª æv²Ê Ò n Þ:. ÚæZ® Î{š þ~W’² f â2 n Þê ÿ:® ‡– vZ nÎÆ, š BuMeIm⁺Tf2N^- +Li® vZ nV EC/PC+Li J: èš Ù’² ^nÆ †ÒrÊ

~R 6Úæ® O‡ &¢Ê†Z® Ž çÿÊ ª þ~W’² fâ n  Ê~Ê ª æv²Ê Ò n Þ:. NBî Z¢

Ê~‡ ·® vZn hš J6² ^ê ”š n :. B² 6 Úæ ® Ú^ /Ê &²¾– – vZÊ ~Ò Vê ْ² ¢ n Þ:. Êê 6Úæ ZÊ® DSC R(Figure 2)&r

 «Î¶ n Þ:.

ÊB² Êv:² ήB PGE(BuMeIm⁺Tf2N^-Li)® Ê~ Z

V PGE(EC/PC+Li)J: è:6 "r:.

3.3 +ÏÛ O¿£ O{Ÿ¤L “`|

6Úæ ZÊš  2~ Z& §ÿ®† ZÊrê ÿ®ê

šÒ ²:. ÒnW’² 4 V Ê® è– ZZÒ lê çO® òZ

’² ήB Ê& Ö§¶ n Þê ZÊ– è– ZZ ÂZ&r Z

† ª¯W’² žkÊÒ ²:. ÊÒ ZÊ r® ZZ-Z®ëš Êÿ

®B 6Úæ ZÊ® Z† ª¯WÎ žk‡š ¢šJ®:.

Figure 5ê PGE(EC/PC+Li)® ZZ-Z® ‡ 7v’²r, 2»5 V êZ&r Z† ª¯W’² žk² ْ² JB :. Figure 6– PGE (BuMeIm⁺Tf2N^-Li)® ZZ-Z® ‡ 7v’² -4»4.5 V® êZ&

r Z† ª¯W’² žk² ٚ ¢ n Þ:. ʲֆ PGE(BuMeIm⁺

Tf2N^-+Li)Ê PGE(EC/PC+Li)J: ª i– êZ&r Z† ª¯W’²

žk®:ê ٚ ¢ n Þ:.

4. û«

PEGDA& Ê~‡ ·, BuMeIm⁺Tf2NÒ Êÿ®B ² Û®®

zk 6Úæ ZÊš rÆ®V:. Ê rÆr 6Úæ ZÊ– † Ê® v† ÿ:Ò Vâr² Êÿ®B "6 6Úæ ZÊJ: è–

Ê~ Z– Z† ª¯W žk‡š JBV:. BuMeIm⁺Tf2N^-Ò Ê ÿ®B ~&r 2.29Ý10^-3 S/cm® è– Ê~ ZÒ VÆ 4.5 V

¢ Z† ª¯W’² žk² 6Úæ ZÊš š n Þ:. Ê

~‡ ·ê 6Úæ ZÊ® Ê~ Z e Z† ª¯W žk‡

š û2š ¢ n Þ:.

[÷£ KÜN FÂê ¯v » >® gfFÂâ & (R rގ KRF 2004-005-D00063)& ®®B nßn’Æ Ê& f2

:.

ƒ+S

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Figure 5. Cyclic voltammogram of gel polymer electrolytes with EC/PC.

G

3 2 1 0 1 2

At room temp.

Voltage range : -5 ~ 10 V Scan rate : 100 mV/sec

5 4 3 04 05 06 Current(mA/cm2 )

#09# 07# 05# 3# 5# 7# 9# ;# 43# Applied voltage(V)

Figure 6. Cyclic voltammogram of gel polymer electrolytes with BuMeIm⁺Tf2N^-.

G

2 1 0 1 2 3 4 5

At room temp.

Voltage range : -5 ~ 10 V Scan rate : 100 mV/s

3138#

3137#

3136#

3135#

3134#

3133#

03134#

03135#

Current(mA/cm2 )

09# 07# 05# 3# 5# 7# 9# ;# 43# Applied voltage(V)

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