Demo
1. #g«#
ÎÖ® ZWÎ æO& ®®B kÊ ªnê Z²6Úæ(elec- troactive-polymer, EAP)ê :ç®â §ÿv n Þ² BB ÚÒ® R
¯æ, væ:Ê $ VB V6 Þê "Ê:. 6Úæ "ê
ÒO "î k¿^& Ê V#6, VKÊ Â² Z²
"²® §ÿ& VWÎ ûf V6 Þ:.1,2
Ê~6Úæ-^ã K¿"(ionic polymer-metal composite(IPMC)) ê EAP® ÒÛ², Ý 6Úæ ® ç Ê& ^ã ZOÊ Þê ÂÆÒ VÆ, ^ã ZO J ^ãÊ~ ª¯W² ®&2H k2þ:. IPMCê çZO Ê& Z« V®Ê çO(anode)
² ÂÖBêÆ, 10 V Ê®® ¦W ÎÖ Z«& ¾ f§
®Æ kçÊ Æ ÙÊ ûfÊ:. IPMCÒ Êÿ®B V#6 vF² û þ®ê ÎKRw, ʲ ²], ʲ âZ G² § ÿv n Þ:.3-6
IPMC& V² ^¢® FÂ: VÖÚ W² 3n6 Þê Þ⪠Ê~ 6Úæ , ß DuPont® Nafion, Asahi Glass®
Flemion, Asahi Chemical® Aciplex G ÿ®6 Þ:. Ê: tetra- fluoroethyleneR V® &>& vF ÊK:® Ê~
Ò V Þ⪠&&¢ÊÒ Kg¿2þ chemical structure 1 V6 Þ:.7,8
CF2 CF2
O
CF2 CF2
CF2 C F CF3
O CF2 CF2 SO3
m n
Chemical Structure 1
NFÆ Ê: 6Úæ ": VÖÚ ¦. 0.1»0.3 mm kÎ Ú k2² f:n6 ÞÆ, ÿVKÊ n ê:. Òr ÿ&
W¿² þç² k®B û OVª®ê ÙÊ Ó :.9 N :.:&rê Nafion V®B IPMCÒ rç¶ n ÞÊr ÿVKÊ Vû² 6Úæ "Ò Z² Î{ ² R, chemi- cal structure 2® fluoroalkyl methacrylate(FMA), ß DuPont® Zonyl TMR Â(AA) Kg¿®B 6Úæ² IPMCÒ rç¶
n ÞÆ, Nafion² rç² IPMC v² û V& J6
² j Þ:.10
Vrglxp#Prqwpruloorqlwhô#.Y#K Lë#LSPFÌ#.á+#U#¨à#`á#
`§ó%}ã}ÇL?#
øð(c#^c<#
+5338T#6#44¼#Q:/#5338T#9#:¼#T,#
#
Surshuwlhv#dqg#Shuirupdqfh#ri#Hohfwurdfwlyh#Dfu|olf#Frsro|phu0Sodwlqxp##
Frpsrvlwh#Prglilhg#zlwk#Vrglxp#Prqwpruloorqlwh#
Kdq#Pr#Mhrqj%/#E|xqj#Fkrrq#Nlp/#dqg#\rxqj#Vrr#Od#
Department of Chemistry, University of Ulsan, Ulslan 680-749, Korea (Received March 11, 2005;accepted June 7, 2005)
S¨Ü Sodium montmorillonite sodium montmorilloniteV Ûr macromer® Ê ®&r fluoroalkyl methacrylate
X-v â^ , Îû, nÚ·n~ G W Æ®V:. f, Ê: Êÿ®B Ê~ 6Úæ-^ K¿
"(IPMC)Ò rÆ®B n R® ÎÖ ZZ& ®² Z® ¦Ú e Z Æ/ wk² R, sodium montmorilloniteV Ê
~® Ê/ Ê®B Z® e Z® fâÒ ^î¾ V®V:
Abstract:Fluoroalkyl methacrylate and acrylic acid were bulk radical copolymerized in the presence of pure sodium montmorillonite or macromer intercalated sodium montmorillonite to get a fluorinated acrylic ionomer/sodium montmo- rillonite composite, and their physical properties, such as X-ray diffraction pattern, tensile properties, and water uptake, were examined. These composites were used to preparean ionic acrylic polymer-platinum composite (IPMC). The current and deformation responses of these IPMCs by external voltage applied across the platinum electrodes deposited on both sides of IPMC showed that the cation migration from anode to cathode was suppressed in the presence of sodium mon- tmorillonite, causing reduced current and deformation.
Keywords: ionic polymer-metal composite(IPMC), fluorinated acrylic ionomer, electroactive, sodium montmorillonite, composite.
†To whom correspondence should be addressed.
E-mail: hmjeong@mail.ulsan.ac.kr
C CH3
C O
O
C C F
n CH2
CH2 CH2
F F
F F 1 .
=4 n
Chemical Structure 2
IPMC® ç ZO Ê& Z« V®Ê Ê~ 6Úæ & K v ¿² 6kr ¢Ê~ Ê/¶ n î, Ê~ ¿r ^ã çÊ~ ¢O(cathode) ² nªr Úæ ¾. Ê/®â r :. Ê& Ò ¢O znâ n6, çO(anode) nënâ n² Ú k2® IPMCê çO ² Óâ r:.1,3,11 ÊB
² Â/ && ®®Ê Â/ û2ú ZÊrê Ê~ ã®
óVV ê®:. NBî N :.:&r ¿² Þ⪠Â
B Ê~ ãÒ óV2úÊ nÚ ·nÊ _ÿ®â óV®B Â/
zÞz V®®V:.10
Sodium montmorilloniteê f® silicate ¢Ê~ Ê& Na+Ê
~Ê Ê®ê Ê~ ãV R è 6ÚæÊ:.12,13 N FÂ
&rê sodium montmorilloniteÒ 6Úæ :ú& Ú2þ K¿
"Ò rÆ®Ê W k 6Úæ :ú& Úr Ê~ ã
Ò óV2 n Þ:ê f& ®B, FMA AAÒ Kg¿² Þâ ª  Ê~ 6Úæ(PFMAA) :ú& sodium montmorillonite Ò Ú2þ K¿"Ò rÆ®6, ÊÒ Êÿ®B IPMCÒ rÆ®B Â/ Æ®V:. K¿"® rÆ&ê FMA AAÒ Òj Ò Kg¿¶ ¢ sodium montmorilloniteÒ ¾. Û®B rÆ®ê ëR chemical structure 3® poly(ethylene glycol) methyl ether methacryl- ate macromerV sodium montmorillonite& Ûr K¿"Ò V
"6 14-16ÊÒ FMA, AA ¾. Kg¿2úê ë, ¦ VÒ ÿ®V:.
H2C C CH3
C
O O
n CH2 O
CH2 CH3
Chemical Structure 3
2. /#
2.1 Pdfurphu#@´÷£#g»#
ÚæÊ 562g/molÎ poly(ethylene glycol) methyl ether methacrylate macromer(PEGM, Aldrich)V sodium montmorillonite(Southern Clay Products Inc.)& Ûr K¿"(PEGMM)ê ª/acetonitrile
¿·(Ö 1/1) ã&r rÆ®V:. ß ¿· 100 mL& PEGM
3 g ÏÎ , sodium montmorillonite 7 g V² ú ~&r 2ÒZ ¦ n®V:. ® ¾Z Ú®6, ¾Z acetonitrileR ª
² WW ï² , K zf&r ~ v² 3ÒZ ÊÆ
®B :.& ÿ®V:.14-16
2.2 +ÏÛ#@´÷£#´|#Z#Ï#g»#
FMA AAÒ Kg¿² Þ⪠ Ê~ 6Úæ(PFMAA) :ú& sodium montmorilloniteÒ Ú2þ K¿"ê sodium mon- tmorillonite Z&r rƲ macromer K¿"® Ê ®&r FMA AAÒ Kg¿®B rÆ®V:. g¿ 0.3 phr® 2,2′- azobisisobutyronitrile(Aldrich) ÒjÒ r2r² ÿ®B, 60 ×,
â ® ®&r ß®V:. g¿ îâ Ön ª ã&r
¦n®ê ë² n~ ï² 60 ×&r K ÊÆ®V:. ¿
recipe, 2"Û, ¿r K¿"® Æ G Table 1& î:.
¿² K¿"ê 165 ×&r «ë k®B ¦. 0.16 mm® Ú k2² ": IPMC® rÆ& ÿ®V:.
2.3 LSPF£#g»
Ú çÊ& ^ ZO k2þ Þ⪠ Ê~ 6Ú æ-^ K¿"(ionic acrylic copolymer-platinum composite, IPMC) ê ª¯ ®&ë² rÆ®V:.11,17 «ëk² Ú Ê~ r Ʋ ^rnÒ ÿ®B n~ ï®6, ~® ^rn& 2ÒZ J  z2þ ú, Ó 10-2M ã² tetraammine platinum(II) chloride hydrate, Pt(NH3)4Cl2áxH2O (Aldrich)Ò ^rn& ÏÎ 50 × nÿ·&
32Z J ÊK:® H+Ê~ ^ Ê~² ¦®®V:.
¦®r ^ Ê~ NaBH4(Aldrich)Ò 5 wt%² ÏÎ nÿ·² 40 ×&r ®&2H ^Ê Ú ²Ê& sòr IPMCÒ rÆ®V :. ^ Ê~ ¦®R ®& Æç 4~ nK®B ÿÚ² ¦.®
^Ê ²Ê& sòn³ ®VÊ, 3, 4ÞN® ®& 2&ê ~Ò 60 ×¢ èV:.
2.4#l`#
KÛÚs(1H-NMR) Varian Plus 300 MHz NMR² ~&r ®V :. 6Úæê trifluoroacetic acid& ÏB wk®V:.
K¿" g® sodium montmorillonite ¾ JgÚsë² ß
®V:. ß, TA Instrument® Jg Ús(TGA 951)² K ÚZ
&r 10 ×/min ã² 700 ×¢ VJ² ê®ç wk®B 2
" g sodium montmorillonite® ¾ ®V:.
Table 1. Acrylic Copolymer Composites Used in This Study
Feed composition (weight ratio) Polymer composition (weight ratio)
FMA AA Sodium montmorillonite PEGM FMA AA Sodium montmorillonite PEGM
ZAN0 70.00 30.00 - - 82.00 18.00 - -
ZAN3 70.00 30.00 3.00 - 79.89 20.11 3.96 -
ZAN7 70.00 30.00 7.00 - 86.05 13.95 8.66 -
ZAP3 70.00 30.00 2.46 0.54 88.83 11.17 2.35 0.67
ZAP7 70.00 30.00 5.73 1.27 79.75 20.25 4.97 1.14
X-v â^Ús X-ray diffractometer(X'PERT, Philips)² Cu K;(
1.54 Å) v ÿ®B, â^W 1.21²Ö 1.2 °/min² óV2 úÊr ß®V:.
«ëk² Ú® Îû Ú 25 × ^rn& 2ÒZ J Þ z2þ Îû2.(Instron 4411)Ò ÿ®B wk®V:. V
² 10 mm, Ê 30 mm, ¦. 0.16 mmÎ 2 ÿ®B, Îûã
10 mm/min² wk®V:.
«ëk² ÚR IPMC® nÚ·n :¢ 3(1) Êÿ®B
®V:. Ê 3&r Wwetê 2"Ò 25 × ^rn& 2ÒZ JÞ
z2þ ú® âÊ6, Wdryê z² 2"Ò :2 80 × Kzf
&r 2ÒZ ÊƲ ® âÊ:.5
Water uptake (g-water/100 g-dry sample) 100
dry dry
wet− ×
W W W
(1)
IPMC® >ÊR ²Ê® þJ²ê ÊƲ 2&r 2"& ^
sputtering² ú RZæZN(SEM, Jeol JSM 820)² V®V:.
>Ê ·â² W² ú b² 2"® >Ê V®V:.
Figure 1& î û®Ò ÿ®B ² û² 4 V® ZZÒ V
®Æî 1 Hz² 2V, 2VÒ Þ^VÊr IPMC& ÖV®ê
Z® Ê7 k kÒ wk®V:.3,5 IPMCê C 6 mm® N þ ç² îÒ ² ³ û®& 6k®B Z« V®6 :Î ³
Z«& ®Ê Ⲡʳ ®B Êê kÒ ^ÊV² wk®V:. Â/®ê N® Êê 25 mm² ®V6, ³&r 5 mm
f&r ^ÊV² ZÒ wk®V:. 2"ê Ý ~ ^ Â/
² ú f§ h: wk®B wkh® Z èV:.
3. ûG Z ë«
3.1 [0k#×S#Ïh#
Figure 2(a) (b)& WW sodium montmorillonite sodium mont- morillonite& PEGMÊ Ûr K¿"(PEGMM)® X-v ÚsR Ò î:. Sodium montmorilloniteê rÆÎ Southern Clay®
v æ" ®â 2 θ7.8°&r ÂÒ VêÆ Ê, PEGMM
2 θ6.3°&r ÂÒ V& R n Þ:. Ê Rê macromerÎ PEGM® Û² ήB sodium montmorillonite® Z ZÿÊ â
¢¢ JBV:.14-16 P. Aranda G® F R& ®®Ê sodium montmorillonite® Ê&ê poly(ethylene oxide)V Ó 0.26 g/g-mont- morillonite¢ Ûv n ÞÆ, Ò> Ûr poly(ethylene oxide)ê ÿ:& ®Ê n ê Ù² J6r j Þ:.15N FÂ&r rƲ PEGMM g PEGM macromer® ¾ Table 1&r 0.22 g- PEGM/g-sodium montmorillonite² rn² poly(ethylene oxide)J: Ó Z Wâ Û~ R n Þ:. Êê PEGM&ê poly(ethylene oxide) Wr:. ², Figure 2(e) (f)&r PEGMM FMA, AA Kg¿2 H rƲ ZAP3R ZAP7 PEGMMR ² Z®&r X-v â^
montmorilloniteê VÖÚ poly(ethylene oxide) VV Ûr ÂÆÒ v¾ JBV:. Ê& nÊ FMA AAÒ Kg¿¶ ¢ sodium mont- morillonite æÒ Û®B rƲ ZAN3R ZAN7 2 θ5»8° ê Z& ÚB®ê ¦W i X-v â^ ÂÒ V& R n Þ:
(Figure 2(c)
ê ê 6Úæ :ú g& sodium montmorilloniteV BB V
:ç² k2² Ún Þ¢ JBV:.
3.2 ?Ϭ?#
r¶&r v² j oÊ IPMC® Â/&ê Úæ® C¶Ê gꮲ N :.& ÿ² 6Úæ K¿"Ò «ëk² Ú R ÊÒ ÿ®B rƲ IPMC® nÚ·n wk®B Table 2&
î:. Ú® , ZAN3 ZAP3 sodium montmorilloniteV B¾n ZAN0& Ê nÚ·nÊ WÆ Êê Nylon 6/mont- morillonite nanocomposite&r Vr j oÊ f® silicateV nÚ® Ú Ö²® « Ê® ¢² 3Wr:.18 NB î ZAN7R ZAP7 ZAN0J: nÚ·nÊ zÞz $Æ, Êê sodium montmorillonite æV ²nʲ sodium montmorillonite
® çÊ $ ê " Z& ²n WCÊ óVnê þRV 20mm
5mm
6mm Laser displacement
sensor
Potentiostat Waveform generator
displacement cathode anode
20mm
5mm
6mm Laser displacement
sensor
Potentiostat Waveform generator
displacement cathode anode
Figure 1. A schematic of displacement measuring system.
Figure 2. X-ray diffraction patterns of (a) sodium montmorillonite, (b) PEGMM, (c) ZAN3, (d) ZAN7, (e) ZAP3, and (f) ZAP7.
Intensity
5# 7# 9# ;# 43#
2 θ
OP OP OP OP O P OP
OP OP OP OP O P OP
vW² çÿ® ¢² 3Wr:. «ëk² Ú ÿ
®B ª¯W ®&ë² IPMCÒ rÆ®ê Rk&r ÚÊ Ââ
z~ V¶ n ÞêÆ, Êê -COOHV OÊ Æ -COO- Na+² Ên6 Na+Ê~& Ê nª~& Î Ù² 3Wr:.19,20 Table 2&r IPMCV ÚJ: > $ nÚ·n V& « ζ n Þ:. IPMC® ê V² sodium montmorilloniteV ÓZ
® nÚ·n ZAN0& Ê óV2úê þRV Þî, ¾&
Î ªê ò® ¢ Table 2&r R n Þ:.
3.3 ÃðW|#
6Úæ K¿"Ò «ë k² Ú 25 × ã& 2ÒZ J Þ z2þ ú wk² stress-strain 7v Figure 3&, ʲÖ
ê kWÎ Îû Table 3& î:. ZAN0 F² 6Ú æ® Vî, ÒnWÎ K¿"&rîR21-26 ZAN3R ZAP3
sodium montmorillonite® JkþR& ®Ê ZAN0& Ê þB úV óV~ ¢ n Þ:. NBî ZAN7 ZAN3J: ZAP7 ZAP3 J: þBúV fâ¾ R n ÞêÆ, Êê nÚ·n® óV&
®² z(Table 2 Æ)² ÚæZ Î{Ê fâ¾& ®² ÙÊ ² &
β 3Wr:.
3.4 ó?§#
Figure 4& SEM² V² IPMC® >Ê e ²Ê® þJ²Ò î:. Figure 4(a)® >Ê k&r Ó 2 2 ¦.® ^Ê s òr ZO Ê kn Þ¢ V¶ n Þ:. Figure 4(b)® ²Ê k&rê Ó 20 2 ® WC:Ê þæÊ k2² ʾ
V¶ n ÞêÆ, Êê IPMC rÆ2 zn® ²Ê® ^ Ê SEM V ZÊ Êƶ ¢ nënÊr ²ÊÊ îâ Ön&
& ήê Ù² 3Wr:.1 3.5 OO#£§#·#
Figure 5& IPMC& 4 V® ® ZZÒ V² Z® Z®
ª 2®VêÆ, Z®ê _ÿ®â óV®V:V fâ®ê Æ /, Zê rrÞ óV®ê Æ/ R n Þ:. Ê oÊ Z®
Z Ê& ÓZ® 2Z FÊ Þê Êvê çÊ~& nªr Ö §{& ®Ê ZV 3ê ÙÊ r~W² Ê> ¢
² 3Wr:. f, çÊ~® Ê/& ®Ê vrnê «& ®Êr ÒÖ Ê ¢O ² êV² B Z& B®ê Ù ² &
// /
(a) (b)
Figure 4. Scanning electron micrographs of (a) the cross-section (b) the surface of IPMC from ZAN0.
Figure 5. Initial current and displacement responses of IPMC by the applied voltage of 4V ; () ZAN0, (-- . -- . -- ) ZAN3, (-- . . -- . . --) ZAN7, ( - - - - -) ZAP3, (...) ZAP7.
0 1 2 3 4 5 0 0 0 0
3# 5# 7# 9# ;# 43#
Time(sec) 73
63 53 43
8 7 6
5 4 3
Displacement(mm) Current(mA)
Table 3. Tensile Properties of Wet Acrylic Copolymer Films
Sample
Tensile modulus (MPa)
Tensile strength at break
(MPa)
Elongation at break
(%)
ZAN 0 0.43 2.23 68
ZAN 3 1.20 3.37 78
ZAN 7 0.61 2.03 33
ZAP 3 1.02 3.63 46
ZAP 7 0.61 2.37 34
Figure 3. Stress-strain curve of wet acrylic copolymer film ; (a) ZAN0, (b)ZAN3, (c)ZAN7, (d) ZAP3, and (e)ZAP7.
8#
7#
6#
5#
4#
3#
Stress(MPa)
# 3# 53# 73# 93# ;3# 433
Strain(%)
0 1 2 3 4 5
(a) (b)
(c) (d)
(e)
Table 2. Water Uptake of Film and IPMC
Water uptake (g-water/100 g-dry sample) Sample
film IPMC
ZAN0 22.3 67.2
ZAN3 14.7 78.0
ZAN7 25.0 68.7
ZAP3 21.2 76.1
ZAP7 35.7 66.1
(d)
(b)
(c) (a) (e)
β 3Wr:.1,3,11 Figure 5&r sodium montmorillonite² r² ZAN3, ZAN7, ZAP3, ZAP7® Z® Z h þ¦V ZAN0& Ê çâ îþ R n ÞÆ, sodium montmorillonite® ¾& Î ò² ª û V¶ n :. Êê sodium montmorilloniteV IPMC ® Ê~ ãÒ óV2úê ®", ÎÖZZ& ®Ê PFMAA
® -COO-Na+& Ör Na+ Ê~Ê R ¾. Ê/®ê Ù Ê®ê çÿÊ Þ¢ JBV:.
Figure 6&ê 1^ Zÿ² +2 V, -2 VÒ Þ^ IPMC& ÖV²
Z® Z® ª 2®V:. Figure 5&r oÊ ^R®
â ¾ f§®ê Z® ÊJ: æâ f§®ê ZV îþ
R n ÞÆ, sodium montmorillonite² r² ZZ& ®² Z
® Z® f§Ê fâ¾ V¶ n Þ:.
4. û«
X-v â^ Ús Rê sodium montmorillonite æ macromerV
Ûr sodium montmorillonite® Ê ®&r FMA AAÒ ÒjÒ Kg¿®ê sodium montmorillonite& PFMAAV Ûr K¿
"Ò þ~W² rƶ n Þ¢ JBR:. ZAN0R ÊÒ sodium montmorillonite² r² K¿"Ò Êÿ®B IPMCÒ rÆ®6, V Ê Z«& ®Ê vr Z® Z h wk² R: sodium montmorilloniteV IPMC g& Ê~® ãê óV2úî Ê~® Ê / Ê®B Z® Z h® fâÒ V JBR:.
[÷£# KÜN FÂê JÊKÖ JÊ®"v»® &
& ®®B Ê> ÙÚ(RrÞ: 02-PJ3-PG10- 31402-0001).
S+S
G
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Figure 6. Current and displacement responses of IPMC by 1 Hz·2 V step, voltage repeatedly applided ; (--- ) ZAN0, (-- . -- . --) ZAN3, (-- . . -- . . --) ZAN7, ( - - - ) ZAP3, (...) ZAP7.
# 4# 5# 6# 7# 8#
Time(sec) 5
4 3 04 05
483 433 83 3 083 0433 0483 413 318 313 0318
Displacement(mm) Current(mA) Voltage(V)
5 0 5 0 0 0 0 0 0 0 0 -2 -1 0 1 2