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1 2009'BAS セミナー 抄 録 電 気 化 学 の 基 礎 10th June 2009

2 プログラム 日 時 平 成 21 年 6 月 10 日 ( 水 ) 10:30~17:00 場 所 すみだ 曳 舟 文 化 センター レクリエーションホール 東 京 都 墨 田 区 京 島 TEL: :30 ~ 12:10 レクチャーコース 1 Page 電 気 化 学 計 測 の 基 礎 実 際 に 即 したCV 測 定 上 の 注 意 点 を 中 心 に 分 光 電 気 化 学 測 定 法 の 紹 介 12:10 ~ 13:10 昼 食 元 東 京 大 学 工 学 部 助 教 授 渡 辺 訓 行 ビー エー エス 株 式 会 社 戸 田 良 輔 ビー エー エス 株 式 会 社 工 学 博 士 蒋 桂 華 :10 ~ 14:45 デモコース 各 種 電 極 を 使 用 した 電 気 化 学 測 定 対 流 ボルタンメトリー 測 定 (RRDE-3) 分 光 電 気 化 学 測 定 基 礎 的 なインピーダンス 測 定 渡 辺 訓 行 先 生 による 個 別 相 談 コーナー 14:45 ~ 15:00 休 憩 15:00 ~ 17:00 レクチャーコース 2 電 気 化 学 反 応 を 利 用 した 次 世 代 画 像 表 示 技 術 千 葉 大 学 大 学 院 融 合 科 学 研 究 科 教 授 小 林 範 久 EQCM 測 定 を 利 用 したタンパク 質 の 電 子 移 動 反 応 解 析 東 京 工 業 大 学 大 学 院 生 命 理 工 学 研 究 科 講 師 朝 倉 則 行 23 31

3 1.. ; source; sink HOMO LUMO HOMO LUMO 3 LUMO HOMO LUMO HOMO e O + e R e e R O + e potentiostat R C W. 3 Cdl RctRs 1

4 Cdl Q=CdlE C dl de/dtcdl i=dq/dt= CdldE/dt R s R ct Zi Zf

5 . R f Vout = Vin R in V = R i out f in H R V out = Vin R 1 R1 R2 1 Vout=Vin.. i. + Op-1 Ref C W + Op-2 Cell 3

6 1 ei Op-1 ei 1 2 Op Op HPLC 10 E 1 R R + i 1 Ref Op-1 + C + W 1 Op-2 E 2 E W 2 R i 2 E 1 W 2 E 2 R + R E=E 2 E 1 + W 1 Ref E 1 E 1 E

7 11 1M H2SO4 40V Ag H2 2H + + 2e AgCl sat KCl aq Ag + Cl AgCl + e KCl frit 12 acl 5

8 0 RT E = E ln acl F KCl 0.197V 0.197V vs NHE Ag HgSCE KCl 0.242V 0.242V vs NHE 13. ir ir u CE Ref C dl WE R s R u R ct i 14 6

9 CV CV 15 R u 1; 0Ω 2; 100Ω 3; 200Ω 4; 500Ω 1 A + e B 100mV/s 14 Rct Cdl 50V E i() t= E exp t () Ru RuCdl V E E/R u i 0 i(0)ru 0 µ E 16 Ru Ru ir ir OK 7

10 ir op2 Rpf Eset E set R R R op1 C Ref W R f op3 E o =ir f firu Ru f R pf 16 ir f op1 Ru Eset Rpf f PC ir. JP JP M KCM HC K + H + H + K + H + 1. H + JP 8

11 JP KCl 17 α β ( t t ) RT F ln a a 1 a 1 KCl K + Cl - a 2 KCl E JP = φ φ 17. KCl JP KCl t 0.49t RT/F59.1Va1a2 1M3M 0.6V, V KCl JP NaCl 5.8 V12.2V β α = + 2. ε q1q2 q1q2 f = 2 4πε 0ε r ε0 Bu4N ClO4 BF4 PF6 9

12 35.9 THF M CV THF 0.1M [Bu4N][A] A TFAB PF6 TFABB(C6F5) 5V/s 1.5 GC ir (85) 18 M THF CV V/s CV Bu4NPF6 ir ir THF CV B(C6F5) 19 ( 8.93)(2 ) CV Bu4NPF6 Bu4N B(C6F5) PF6 19M () CV Bu4NPF6 Bu4N B(C6F5) 0.2V/s0.5Ф Pt 1) W.E. Geiger et al., Anal. Chem., 76, 6395 (2004) 2) W.E. Geiger et al., Angew. Chem. Int. Ed., 38, 248 (2000) 10

13 CV CV CV CV CV CV CV ) No. ALS PTE Pt 23 cm RE-1B (Ag/AgCl) VC PK ) K3[Fe(CN)6] KNO3 1 ALS

14 CV 4 1 A D 1. A 1 mm 0.1M B 2 mm 0.1M C 5 mm 0.1M D 10 mm 0.1M PK µm CV 4ALS2323 ALS2323 A D CV 0.5 V0.5 V-0.1 V 0.05 V/sec

15 CV Negative A/V 2 sec +(Cathodic Positive) / V / sec CV V/sec 6 A 5 CV [Fe(CN)6] 4- [Fe(CN)6] 3- e - A D CV 7 Ipa Ipc CV Ip Ipc = n 3/2 F 3/2 A(RT) -1/2 DRed 1/2 C*Redv 1/2 Ipa = n 3/2 F 3/2 A(RT) -1/2 DOx 1/2 C*Oxv 1/2 F A R T D cm 2 /sc mol/cm 3 v A T D Ipa Ipc 6 A CV 7 A D Ipa Ipc 13

16 CV E o E o = (Epa + Epc) /2 25 n Ep Ep =Epa Epc = 57 / n RE-1B 3 M NaCl No M NaCl 8 RE-1B 8 CV 1. (2002) Joseph Wang, Analytical Electrochemistry, VCH Publishers (1994) 14

17 1. Spectroelectrochemistry, SEC) 2, 3) SEC 7) 9) 10, 11) SEC 12) 2. in situ (Thin Layer ~µ Fig. 1 Principle of TLC when using transparent and minigrid electrodes. 15

18 Cell, TLC) Fig.1 OTE(optically transparent electrode)(grid electrode) 3. (Fig.2) Fig.3 ALS2323 Fig.4 SEC2000 Fig. 3 ALS2323 Electrochemical analyzer. Fig. 2 ALS2323 Electrochemical analyzer with SEC2000. ALS bit D/A 16 bit A/D ALS2323 SEC2000 Fig. 4 Schematic diagram of SEC2000 Spectroelectrochemical system with SEC-C. 16

19 3.1 SEC-C Fig.5 SEC-C 1mm Working Electrode, WEAuPt Reference Electrode, REAg Ag/AgCl Counter Electrode, CE SEC-C Fig.2 2mM 3- Fe (CN) 6 / Fe (CN) 4-6 KNO 3 CV Fig V Fe (CN) 3-6 / Fe (CN) 4-6 Fig V 0.00 V ()() Fe(CN) e - 4- Fe(CN) 6 (Red time) (1) 4- Fe(CN) 6 Fe(CN) e - (Ox time) (2) Fig. 5 SEC-C Thin Layer Quartz Glass Spectroelectrochemical cell kit. Fig. 6. Cyclic voltammogram of 2mM K 3 [Fe(CN) 6 ]. 17

20 Fig. 7. Absorbance measurement of 2 mm K 3 [Fe(CN) 6 ]. 3.2 SEC-F Fig.8 (Spectroelectrochemistry-Flow Cell, SEC-FFig.8) Fig.9 SEC-F in siut SEC-F ITO (Indium-Tin-Oxide) Au, Pt Fig.10 ITO 350nm Au, Pt Inlet Light Source Flow cell block Outle Fig. 8 Schematic diagram of SEC-F. Outlet Inlet 1. Collimating Lens2. SEC-FT500 Teflon gasket3. Working electrode4. Reference electrode5. Probe type Optical fiber (Counter Electrode)6. Flow cell block (A)7. Flow cell Block (B)8. Dynaseal PEEK 18

21 Fig.10 Comparison of the transmittance of 0.5 mm, 1 mm quartz glass substrate with / without ITO film on. Light Source Electrochemical Analyzer SEC2000-UV/VIS Spectrometer Optical Fiber Spectroelectrochemical flow cell Fig. 9 Schematic diagram of SEC-F with spectroelectrochemical measurement system. Fig. 10 The transmittance of ITO electrode and quartz. 4. CV E 0 n 19

22 4. 1. Ru [Rubipy 3 ] 2+ UV M-1cm-1 ALS2323 CV Fig.11Fig V SEC-C 1.6 V 1.2 V Fig.11 CV measurement of 3,3'-dimethylbenzidine 1.6V Fig.12.a 450 nm 280 nm 310 nm 450nm MLCT metal to ligand charge transfer 450nm Ru Ru 280nm Ru Ru bpy 1.2V Fig.12.b 450nm Ru 1.33V 1.03V a Fig. 12 Changes of spectrum when [Rubipy 3 ] 2+ is electrically oxidized at 1.6 V(a) and 1.2 V (b). b 20

23 2+ e 2+* -e +e 3+ Ru bpy Ru()1.03 V Ru Cl - 1 mm Rubipy 3 Cl 2 Bard 21) CV Fig.13Ru 1.7 V 1.4 V Cl - Fig. 13 Cyclic voltammogram of 1 mm Ru(bipy)sCl 2 in acetonitrile at a Pt electrode with 0.2 M TBABF, supporting electrolyte.scan rate = 100 mv/sec scan from 0.0 to V. The dotted portion marks the 10-methyl-phenothia-zine oxidation wave

24 1 R. J. Gale Ed., Spectroelectrochemistry: Theory and Practice, Plenum Press, New York (1988) 2 D. M. Kolb; Spectroelectrochemistry (Edited by R. J Gale), p 87 (Plenum Press, 1988) 3 W. Plieth; Spectroscopic and Diffractioin Techniques in Interfacial Electrochemistry (Edited by C. Gutierrez and C. Melendres), p. 223 (Kluwer Academic Publishers, 1990) 4,, 42, 127 (1993). 5T. Sagara, M. Fukuda and N. Nakashima, J. Phys. Chem., B, 102, 521 (1998). 6T. Sagara, N. Kaba, M. Komatsu, M. Uchida and N. Nakashima, Electrochim. Acta, in press. 7P. Zanello, Inorganic electrochemistry, The Royal Society of Chemistry, (2003) 8A. J. Bard and L. R. Faulkner, Electrochemical Methods, 2 nd Ed., Wiley, New York (2001). 9 Dhawan, I. K., Shelver, D., Thorsteinsson, M. V., Roberts, G. P., and Johnson, M. K. (1999) biochemistry 39, T. P. DeAngelis and W. R. Heineman, J. Chem. Ed., 53m 594 (1976). 11. D. E. Aspnes, N. Bottka: Semiconductors and Semimetals, Edited by R. K. Willardson, C. A. Speer, Vol. 9 (1972), (Academic Press, New York). 12. W. R. Heineman, Anal. Chem., 50, 390a (1978). 13. C. H. Su, W. R. Heineman. Anal. Chem., 53, 594 (1983) (1984). 16. M. Haga, M. M. Ali, H. Maegawa, K, Nozaki, A. Yoshimura, T. Ohno, Coord.Chem. Rev., 132,99 (1994) 17Wei Zhou, Shen Ye, Masaaki Abe, Takuma Nishida, Kohei Uosaki, Masatoshi Osawa, and Yoichi Sasaki, Chem. Eur. J.,Vol. 11, No. 17, pp , A. J. Bard and L. R. Faulkner, "Electrochemical Methods", Wiley, New York, 1980, chap Hiroshi, N., Yumiko, H., Toshifumi T., The Journal of Biological Chemistry, Vol. 276m Bi, 10, Issue of March 9, pp , > > > 21. Nurhan E. Tokel, Allen J. Bard, Journal of the American Chemical Society 94:8 April 19,

25 EL (ECD) (EC) EC EC EC EC 23

26 EC 2 EC EC 1930 EC (WO 3 )EC S.K.Deb 1) B.W.Faughnan 2) WO 3 WO 3 WO 3 100msec10 7 3) EC (, ECD)25 CRT 1980 ECD EC EC EC 24

27 () WO 3 EC EC EC EC25 7 EC 4) EC WO 3 PBEC EC EC cm 2 /C 5) µc/cm 2 ECmC/cm 2 25

28 EC EC EC Zn 2+ Zn 1996Bi 6) Bi 3+ Cu 2+ 7) ITO /ITOBi 3+ Cu 2+ ph1.5ito BiBi BiEC 8) TiO 2 9) TiO 2 70% 20:13.0V 100msec ECEC EC EC EC TiO 2 26

29 (R)(G)(B(C) (M)(Y EC 4,4 -( )4 10) 1EC 11) (175 cm 2 /C) EC (TiO 2 ) 12) TiO 2 µm1000 TiO 2 TiO 2 SbSnO 2 1.2VTiO 2 TiO 2 TiO 2 20 TiO 2 13) TiO 2 NTera Ltd. 27

30 SbSnO 2 EC 14) EC EC 15) 1000 EC 3 16 EC EC 17) 18) EC TiO 2 28

31 EC µw/cm 2 14) 1) S. K. Deb : Philos. Mag., 27, (1973). 2) B. W. Faughnan, R. S. Crandall and M. A. Lampert : Appl. Phys. Lett., 27, (1975). 3) C. G. Granqvist, Handbook of Inorganic Electrochromic Materials, Elsevier (1995) 4) N. Kobayashi, R. Hirohashi, H. Ohno and E. Tsuchida, Solid State Ionics, 40/41, (1990). 5) S. A. Roberts, D. R. Bloomquist, R. D. Willett and H. W. Dodgen, J. Am. Chem. Soc., 103, (1981). 6) Polyvision Inc., 2 nd International Meeting on Electrochromism, San Diego (1996). 7) J.P.Ziegler, Sol. Energy Mater. Sol. Cells, 56, (1999). 8) 100, 73 (2007). 9) K.Shinozaki, SID 02 Digest, (2002). 10) P.M.S.Monk, The Viologens, Wiley, (1998). 11) F.J.Green, The Sigma-Aldrich Handbook of Stains, Dyes and Indicators, Aldrich Chem. (1990). 12) A. Hagfeldt, N. Vlachopoulos, and M. Grätzel,., J.Electrochem.Soc., 141, L82-L84 (1994). 13) M.Ryan, NTera Ltd., private communication; 14) H. Pettersson, T. Druszecki, L-H. Johansson, A. Norberg, M.O.M. Edwards and A. Hagfeldt, SID-02 Digest, (2002). 15H. Urano, S. Sunohara, H. Ohtomo and N. Kobayashi, J. Mater. Chem., 14, (2004). 16) 44, (2005). 17) Y. Watanabe and N. Kobayashi, Pan-Pacific Imaging Conference 2008, Proceeding 18) Y. Goh, S. Sunohara, M. Nishimura and N. Kobayashi, Proceedings of IDW/AD 05, (2005). 29

32 30

33 EQCM EQCM ATP NADH III b K b T c 1 c IV EQCM(Electrochemical Quartz Crystal Microbalance) EQCM 31

34 EQCM ph 1-5 EQCM 1 QCM 6 EQCM vs. 15 mm vs. EQCM EQCM 32

35 EQCM MHz Hz.4 ng EQCM ng 100 ng 7,8 EQCM EQCM EQCM EQCM EQCM 0.01 Hz EQCM 1,1 --4,4 -MV 2+ (a) 3(b) 1 33

36 EQCM (b) 2 Hz b) CH 3 + N N + CH (a) 0 (b) Current / µa 0 Frequency / Hz Potential / V (vs. Ag/AgCl) Potential / V (vs.ag/agcl) (a)(b) 3 mm 100 mm (ph7.4) 25 o C 100 mvs -1 (b) 34

37 EQCM 9 (b) EQCM EQCM EQCM c 3 c 3 4 I II III c 3 IV 35

38 EQCM c 3 H 2 2H + + 2e - 2 c 3 c EQCM c 3 c 3 c 3 c 3 c 3 c 3 c 3 36

39 EQCM -0.6 V vs. Ag/AgCl e V vs. Ag/AgCl EQCM c 3 c 3 c 3 (a) x10-11 mol cm -2 (b) c 3 c 3 c x10-13 mol cm -2 c A c 3 c 3 37

40 EQCM (a) (b) S N 4 x mol cm -2 2 S N + (C + N N + 6 H 12 ) CH 3 S S S N N N + (C 6 H 12 ) + N N + CH 3 Fe Fe Fe Fe 1.3 x mol cm x mol cm -2 Current / µa 0 2 c Potential / V (vs. Ag/AgCl) 5(c) c 3 4 x mol cm -2 c 3 4 c 3 EQCM V -0.6Vvs.Ag/AgCl -0.3 V -0.6V 38

41 EQCM -0.3 V -0.6 V -0.3 V sec -0.5 Hz 0-0.3V -0.6V c 3 c 3 0.5s c V -0.3V c 3 c 3 39

42 EQCM -0.6V c 3 c 3 6 c 3 20 c s s 100 s -1 EQCM EQCM EQCM 1 K.Chen, J.Hirst, R.Camba, C.A.Bonagura, C.D.Stout, B.K.Burgess, F.A.Armstrong, Nature (2000) 2 D. M, Murgida, P. Hidebrant, J. Pys. Chem. B, 105, 1578 (2001) 3 A.Avila, B.W.Gregory, K.Niki, T. M. Cotton, J. Phys. Chem. B 104, 2759 (2000) 4 D.E.Khoshtariya, J.Wei, H.Liu, H.Yue, D.H.Waldeck,J. Am. Chem. Soc (2003) 5 I.Gomes, R.E.Di Palolo, P.M. Pereira, I.A.C. Pereira, L.M.Saraiva, S.Penades, R. 40

43 EQCM Franco, Langmuir, (2006) 6 D. A.Buttry, ;D. M. Ward, Chem. Rev. 92, (1992) 7 T.Tasuma, Y.Yokoyama, D.A.Buttry, N.Oyama J. Phys. Chem. B 101, (1997) 8 M. R.Deakin, O.Melroy J. Electroanal. Chem. 239, 321 (1988) 9 D. Johannsmann, Macromol. Chem. Phys. 200, (1999) 10 N. Asakrua, T.Kamachi, I. Okura, J. J Biol Inorg Chem, 9, (2004) 41

44 MEMO 42

45 会 場 アクセス 毎 年 2 回 ビー エー エス セミナーを 開 催 しています ビー エー エス メールニュース 好 評 配 信 中

46 主 催 :ビー エー エス 株 式 会 社

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