[보고서]금속나노입자의 전기영동 석출법에 의한 PEMFC용 다단활성층 MEA 제조법 연구

유연태

금속나노입자의 전기영동 석출법에 의한 PEMFC용 다단활성층 MEA 제조법 연구
A study on preparation method of MEA with multi active layers for PEMFC by using electrophoretical deposition method of metal nanoparticles 원문보기

보고서 정보
주관연구기관	전북대학교 Chonbuk National University
연구책임자	유연태
참여연구자	조진녕 , 김정현 , 김진우 , 이준우 , 수라쿠머 트리파티 , 아딜비쉬 강푸레
보고서유형	3단계보고서
발행국가	대한민국
언어	한국어
발행년월	2015-09
과제시작연도	2014
주관부처	미래창조과학부 Ministry of Science, ICT and Future Planning
등록번호	TRKO201700009330
과제고유번호	1711015523
사업명	기후변화대응기술개발
DB 구축일자	2017-10-28
키워드	연료전지.백금촉매전극.전기영동석출법.금속콜로이드.박막형 촉매전극.fuel cell.Pt catalyst electrode.electrophoresis deposition.metallic colloid.thin film type electrode.
DOI	https://doi.org/10.23000/TRKO201700009330

초록 ▼

본 연구는 PEM 연료전지에 사용되는 MEA (membrane electrode assembly)의 Pt 촉매 담지량을 저감화 하기 위하여, 전기영동 석출법을 이용하여 고성능 Pt/C 촉매전극의 제조 기술을 개발하는 것을 목적으로 하고 있다. 특히 2단계 연구에서 Pt/C 촉매전극 중 Pt 촉매층을 다층화하여 Pt 담지량의 이용율을 향상시켜 Pt 감량화를 달성하고자 하였고, 다음과 같은 연구결과를 얻었다. 전기영동 석출법을 이용하여 Pt/C 및 Pt-Ru/C 촉매 전극에 대하여 성공적으로 double 및 triple active catalyst layer 구조를 갖는 촉매전극을 제작하였다. 이때 사용된 Pt 및 Pt-Ru 나노 콜로이드의 입경은 모두 4-5 nm 이하를 나타내었고, 특히 Pt-Ru 복합 나노입자의 입경은 2-5 nm를 나타내었다.
또한 double 및 triple 촉매층의 각 층의 두께는 모두 2-3 ㎛ 정도인 것으로 확인되어, 박막형 다층구조 전극의 제조 가능성을 시사하였다.
본 기술의 상용화를 위한 첫 단계 기술이라고 할 수 있는 대면적 Pt/C 촉매전극 제조기술의 기본기술을 성공적으로 개발하였다. 2단계 연구에서 대면적 Pt/C 촉매전극의 크기는 25㎠이고, 전기영동석출법으로 Pt 촉매층이 매우 균일한 Pt/C 촉매전극을 제작하였다. 이 전극에 대한 CV 및 단위 셀 테스트를 통하여 signle 촉매층 보다는 double 및 triple 촉매층 전극에서 더 우수한 전기화학적 활성을 보인다는 연구결과를 도출할 수 있었다. 또한 본 기술을 이용하여 100cm2 이상의 전극면적을 갖는 Pt/C 촉매전극의 제조가 가능하다는 사실도 확인할 수 있었다.
(출처: 보고서 요약서 3p)

Abstract ▼

The polymer electrolyte membrane fuel cell (PEMFC), which can work at low temperatures, has great potential for use in stationary, transport and portable applications. One of the challenges facing PEMFC commercialization is to improve the utilization of platinum within the catalyst layer, which should ultimately reduce the platinum loading in the electrodes. Theoretically, all platinum in the catalyst layer should be active for hydrogen oxidation and oxygen reduction reactions. For this to be the case, the fuel and oxidant must react at the interfacial region between the polymer electrolyte (e.g. Nafion) and platinum catalyst, which is a three-phase reaction zone. Here, the electrode should be designed to allow rapid access of the reactants into this zone and the electrolyte/catalyst interface must enable the transfer of both protons and electrons. In the conventional method, to prepare a Pt-loaded carbon black (Pt/C) electrode, the platinum catalyst supported on carbon black should be mixed with ionomers and the resulting colloidal ink be sprayed onto a porous carbon support, such as carbon paper or cloth. In such cases, most of the platinum particles are not accessible to the reactants because they are deposited in the porous structure of the carbon support and some platinum particles are buried completely or partially in the ionomers. These problems decrease also the activity of the Pt catalyst in a direct methanol fuel cell (DMFC).
On the other hand, the electrodeposition method for preparing Pt/C is advantageous in achieving greater selectivity in the placement of platinum particles into the preformed electrode but it has also a drawback. After the initial formation of a platinum particle, further deposition continues on the same particle resulting in an increase in particle size. The mean particle size of electrodeposited platinum has been estimated to be 10-300 nm. Nevertheless, the electrodeposition method appears to be the only technique through which loadings in the microgram range can be achieved.
This research project shows a new strategy for overcoming the increase in platinum particle size during electrodeposition using electrophoresis deposition, which can maintain the size of small platinum particles loaded on an electrode during deposition and easily control the loading. To prepare a Pt/C electrode using this electrophoresis deposition, carbon paper coated with carbon black ink (without platinum) and ionomers was used as the electrode, and a Pt colloid solution with a particle size of 4-5 nm was applied as the plating bath. This study shows how a thin Pt catalyst layer is formed on a carbon black electrode and how the Pt catalyst loading can be controlled using the pulsed electrophoresis deposition technique. The change in the Pt nanoparticle (NP) loading was monitored by cyclic voltammetry and chemical analysis. The results show that the electrophoresis deposition has potential for the development of a highly active catalyst electrode for PEMFC.
In the 1st research stage, we have developed a pulsed electrophoresis deposition (PED) method to avoid above mentioned disadvantage. It was shown that Pt nanoparticles in a colloidal solution could be deposited onto carbon black substrate at low pH without any change in size, and the prepared electrode had an ultra-thin Pt CL with a thickness of 2-2.5 μm. This method has the dual advantage of easy preparation and good control over Pt loading. However, previous studies were focused on a preparation of the single catalyst layer (SCL) electrode. Also, the mass-specific activity of the SCL electrode was considerably decreased with increasing deposition amount of Pt catalyst due to coagulation of Pt nanoparticles. In the 2nd research stage, we developed a novel Pt/C electrode with double catalyst layers (DCL) and triple catalyst layer (TCL) by PED method. It is aimed for improving catalyst utilization and reducing Pt loading. The catalytic activity of the Pt/C DCL and TCL electrodes were compared with that of SCL electrode. In the 3rd research stage, we developed Pt-Au/C, Pt-Pd/C, Pt/TiO2-C and Pt-Au/TiO2-C composite catalyst electrode by PED method. Moreover Pt/C electrode with 100 cm2 area was successfully prepared by PED method.
(출처: Summary 7p)

목차 Contents

표지 ... 1제출문 ... 2보고서 요약서 ... 3요약문 ... 4SUMMARY ... 7CONTENTS ... 9목차 ... 11제 1 장 연구개발과제의 개요 ... 15 제1-1절 연구개발의 배경 ... 15 제1-2절 연구개발의 필요성 ... 18 제1-3절 연구개발의 목표 ... 21제 2 장 국·내외 기술개발 현황 ... 23 제2-1절 국외 기술현황 ... 23 제2-2절 국내 기술현황 ... 23제 3 장 연구 내용 및 성과 ... 25 제3-1절 연구개발 내용의 범위 ... 25 제3-2절 이론적/실험적 접근방법 ... 26 3-2-1. 전기영동법의 원리 ... 26 3-2-2. 펄스전류법의 원리 ... 28 3-2-3. 실험적 접근방법 ... 31 제3-3절 정량적 연구성과 ... 37 3-3-1. 연구성과 요약 (2009.09.30 – 2015.09.29) ... 37 3-3-2. 논문게재 성과 ... 38 3-3-3. 특허출원 및 등록성과 ... 40 3-3-4. 기타 성과 (학술대회, 수상실적, 학위배출인력, 국외과학자교류, 언론보도) ... 41제 4 장 실험방법 및 연구 결과 ... 46 제4-1절 실험방법 ... 46 4-1-1. 시약 및 재료 ... 46 4-1-2. 금속콜로이드의 합성 (Pt, Pt-Ru) ... 47 4-1-3. 카본블랙 피복 전극 제조 ... 49 4-1-4. 전기영동법에 의한 촉매 전극 제조 (Pt/C, Pt-Ru/C) ... 51 4-1-5. 촉매 전극의 전기화학적 특성 평가 ... 52 4-1-6. 기타 특성 평가 ... 53 4-1-7. 단위 셀 테스트 ... 53 제4-2절 연구결과 ... 56 4-2-1. 전기영동 석출법에 의한 Pt/C 촉매전극 제조 ... 56 4-2-2. 전기영동법에 의한 Pt-Ru/C 촉매전극 제조 (Colloid 1) ... 83 4-2-3. 전기영동법에 의한 Pt-Ru/C 촉매전극 제조 (Colloid 2) ... 91 4-2-4. 전기영동법에 의한 백금촉매전극 제조 메카니즘 ... 102 4-2-5. 전기영동석출법에 의한 double 촉매층 GDE 제조 ... 106 4-2-6. 전기영동석출법에 의한 triple 촉매층 GDE 제조 ... 125 4-2-7. 25 cm2 대면적 Pt/C 촉매전극 제조 및 단위셀 평가 ... 132 4-2-8. 전기영동석출법에 의한 Pt/C 전극제조의 안정화 기술 ... 141 4-2-9. Multi-catalyst layer 전극 제조 및 반응 메카니즘 ... 146 4-2-10. Au-Pt 복합나노입자 합성 ... 149 4-2-11. Pd-Pt 복합나노입자 합성 ... 152 4-2-12. 전기영동석출법에 의한 Pt-Au/C 복합촉매전극 제조 및 특성 평가 ... 157 4-2-13. 전기영동석출법에 의한 Pt-Pd/C 복합촉매전극 제조 및 특성 평가 ... 169 4-2-14. 전기영동석출 Pt/C 촉매전극을 이용한 MEA 최적화 실험 ... 170 4-2-15. 25cm2 촉매전극 단위셀의 최적화 기술 개발 ... 184 4-2-16. 전기영동석출법에 의한 Pt/C계 촉매전극 제조공정 개선 ... 190 4-2-17. Pt/TiO2-C계 복합촉매전극 제조 및 장기안정성 평가 ... 202 4-2-18. 전기영동석출법 이용 Pt-Au/TiO2-C계 복합촉매전극 제조 ... 209 4-2-19. 100cm2 Pt/C 대면적 전극 제조 및 전기화학적 특성 ... 212 제4-3절 연구결과의 결론 ... 217제 5 장 목표달성도 및 관련분야에의 기여도 ... 223제 6 장 연구개발성과의 활용계획 ... 225제 7 장 참고문헌 ... 227끝페이지 ... 230

표/그림 (262)

표 The structure of fuel cell.
표 The structure of MEA.
표 Comparison of conventional and new preparation processes of MEA.
표 Conventional and new structure of MEA with Pt catalyst layer.
표 1~3단계 연구내용 요약
표 Elements of double layer relaxation processes in a colloid; (i) Interfacial transfer of exchangeable ions ; (ii) Mass transport of exchangeable ions in solution ; (iii) Space charge transport in the diffuse layers ; (iv) Lateral transport of surface ions.
표 General concepts of (a) direct current and (b) pulse current electrodeposition
표 Cyclic voltammetry 의 개략도
표 (a) 순환전압전류법에서의 전위주사의 형태, (b) 이에 의해 얻어지는 순환전류곡선
표 Cyclic voltammogram의 각 점에서의 전극 표면 근방에서의 O와 R의 농도분포
표 (a) CV 주사속도에 따른 전형적인 가역계의 CV 곡선, (b) 비가역적 CV 곡선.
표 A typical cyclic voltammogram of Pt-C/GC electrode in 1 M H2SO4 and 1 M CH3OH(scan rate = 50 mVs-1).
표 Chemical reaction at the peak of a, b and c.
표 Specs of carbon black (Vulcan XC-72R).
표 Specs of carbon paper (TGP-H-series).
표 Process for preparation of Pt colloid synthesis
표 Process for preparation of carbon black coated carbon paper
표 Process for preparation of pretreated carbon black
표 Schematic of electrophoretic deposition.
표 Schematic of the three-electrodes cell
표 Press for preparing MEA.
표 Prepared MEA with gasket.
표 Single cell test system.
표 Various setting points at monitor for running single cell test system.
표 Pt colloid solution and TEM image (Pt size ; 4-5 nm)
표 Zeta potential ( ζ ) of Pt colloid as a function of pH.
표 UV-Vis spectra and photographs of Pt colloid with different Pt content.
표 FESEM images of the Pt nanoparticles loaded on a carbon black electrode by electrophoresis deposition at various pHs: (a) pH 5, (b) pH 4, (c) pH 3, (d) pH 2.
표 CVs of Pt-loaded carbon black by using electrophoresis method at various Pt colloid pH
표 CV scan results of Pt/C catalysts electrode obtained at pH=2 colloid solution with different duty cycles.
표 Current density change of Pt/C electrode obtained at pH=2 colloid solution with different duty cycles.
표 FESEM image Pt/C electrode obtained at pH=2 colloid solution with different duty cycles. (a) 5% (b) 10% (c) 25% (d) 50%
표 Cyclic voltagrams of Pt-loaded on carbon black electrode by using electrophoresis method at different stirring speeds with various deposition times. (a)100rpm, (b) 200rpm, (c) 300rpm
표 CVs of Pt loaded carbon black electrodes in 1 M H2SO4 and 1 MCH3OH for different deposition times: (a) current density vs. potential, (b) mass-specific current density vs. potential.
표 Pt NP loading and change in current density of Pt loaded carbon black electrode depending on the deposition times.
표 TEM images of Pt nanoparticles loaded on a carbon black electrode by electrophoresis deposition at different depths in a carbon black layer.
표 Cyclic voltagrams of Pt-loaded carbon black electrode prepared with TGP-H-060 and TGP-H-090 by using electrophoresis method at different deposition time.
표 CVs of Pt-loaded on carbon black electrode with different wet-proofing carbon papers by using electropho resis method.
표 Carbon black coated electrode with size of 5 cm × 5 cm.
표 CVs of Pt-loaded carbon black electrode prepared by using electrophoresis method at different load current.
표 Potential change curve of Pt-loading carbon black electrode prepared by electrophoresis method at various load current; (a) 30mA/cm2, (b) 60mA/cm2, (c) 90mA/cm2.
표 SEM images of Pt-loaded carbon black electrode prepared by electrophoresis method at 90mA load current with various deposition times; (a) 5min, (b) 10min, (c) 15min, (d) 20min.
표 CVs of Pt-loaded carbon black electrode prepared by electrophoresis method at 90mA/cm2 current density with various deposition times
표 Carbon black coated electrode with size of 2.5 cm × 2.5 cm.
표 FESEM images of Pt/C electrode prepared depending upon loading current density; (a) 30 mA/cm2, (b) 60 mA/cm2, (c) 90 mA/cm2 (pH=2, deposition time; 10min).
표 CVs of Pt/C electrode prepared depending upon load current density; (a) 30 mA/cm2, (b) 60 mA/cm2, (c) 90 mA/cm2 (pH=2, deposition time; 10min).
표 FESEM images of Pt/C electrode prepared depending upon deposition time; (a) 10 min, (b) 20 min, (c) 30 min (pH=2, Ion= 60 mA/cm2).
표 ICP results and Pt loading amount of Pt/C catalyst electrode prepared according to deposition time (pH=2, Ion= 60 mA).
표 CVs of Pt/C electrode prepared depending upon deposition time (pH=2, Ion= 60 mA/cm2).
표 CVs of Pt/C electrode prepared depending upon deposition time (pH=2, Ion= 60 mA/cm2).
표 ICP results and Pt loading amount of Pt/C catalyst electrode prepared according to deposition time (pH=2, Ion= 60 mA).
표 I-V curves of Pt/C electrode prepared depending upon deposition time
표 Current densities at 0.6V and Pt loading amount of Pt/C catalyst electrode prepared according to deposition time (pH=2, Ion= 60 mA).
표 The electrode of MEAs and reaction mechanism models; (a) conventional method, (b) electrophoresis method.
표 UV-Vis. spectra of RuCl3 solution and Ru colloid.
표 TEM image of Ru colloid.
표 Zeta potential of Ru colloid.
표 UV-Vis. spectra of Pt-Ru alloy colloid.
표 Zeta potential of Pt-Ru colloid.
표 TEM image of 50Pt-50Ru alloy nanoparticle
표 EDX result of 50Pt-50Ru alloy nanoparticle.
표 XRD patterns of Pt-Ru NPs with different Ru content.
표 Lattice distance changes of Pt (111) plane according ot different Ru contents.
표 FESEM image of Pt-Ru catalyst electrode prepared by conventional electrodeposition method.
표 EDX result of Pt-Ru catalyst electrode prepared by conventional electrodeposition method.
표 FESEM images of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at different pHs; (a, b) pH=2, (c) pH=3, (d) pH=4.
표 CVs of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at different pHs.
표 CVs of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at different deposition times.
표 TEM images of Pt-Ru alloy nanoparticles prepared with different contents of tri-sodium citrate solution; (a) 34 mM, (b) 68 mM.
표 EDX result of Pt-Ru alloy nanoparticle prepared with 68 mM tri-sodium citrate.
표 XRD profiles of pure Pt nanoparticle and Pt-Ru alloy nanoparticle prepared with 68 mM tri-sodium citrate.
표 FESEM images of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at different pHs; (a) pH=2, (b) pH=3, (c) pH=4, (d) pH=5
표 CVs of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at different pHs; (a) pH=2, (b) pH=3, (c) pH=4, (d) pH=5
표 FESEM images of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at different pHs; (a) pH=2, (b) pH=3, (c) pH=4, (d) pH=5
표 EDX result of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at pH 2
표 EDX and ICP results of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at different pHs; (a) pH=2, (b) pH=3, (c) pH=4, (d) pH=5
표 CVs of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at different pHs; (a) pH=2, (b) pH=3, (c) pH=4, (d) pH=5
표 FESEM images of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at pH=2 for different deposition times
표 EDX result of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at pH=2 for 10 min deposition time.
표 EDX results of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at pH=2 for different deposition times
표 CVs of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at pH=2 for different deposition times (using Pt-Ru colloid 2, 68 mM 3Na citrate).
표 FESEM images of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at pH=3 for different deposition times ; (a) 10 min, (b) 20 min, (c) 30 min
표 EDX result of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at pH=3 for 10 min deposition time.
표 EDX results of Pt-Ru alloy catalyst electrode prepared by electrophoresis method at pH=3 for different deposition times.
표 Schematic illustration of double layer and electro charge of surface in a colloid.
표 Schematic illustration of electrophoresis method.
표 Stern model of electrical double layer.
표 Zeta potential of Pt colloid and model of surface charge models.
표 Repulsive model of charged Pt nanoparticles.
표 Schematic representation of Pt/C catalyst electrodes prepared by PED method.
표 FESEM images of the (a) carbon black electrode and the Pt nanoparticles deposited on the carbon black electrode by PED, at various deposition times: (b) 30 sec, and (c) 60 sec.
표 SEM cross-sectional images and EDX depth profile of Pt/C double catalyst layer: a) cross-sectional view of entire electrode; b) cross-sectional view of Pt double catalyst layer; and c) EDX depth profile for carbon and platinum.
표 CVs of the Pt/C double catalyst layer electrodes in 0.5 M H2SO4 containing 1 M CH3OH at various deposition times: (a) current density vs. potential; (b) mass-specific current density vs. potential.
표 CVs of the Pt/C single catalyst layer electrodes in 0.5 M H2SO4 solution containing 1 M CH3OH at various deposition times: current density vs. potential.
표 Comparison of the current density for SCL and DCL electrodes toward methanol oxidation at 0.65 V.
표 CVs of the Pt/C double catalyst layer electrodes in 0.5 M H2SO4 at various deposition times: (A) current density vs. potential; (B) mass-specific current density vs. potential.
표 TEM images of Pt-Ru colloid with various molar ratio of Pt and Ru.
표 FE-SEM images of Pt-Ru loaded carbon blacks prepared at different condition. (Ioff = 0 ㎃/㎠, toff = 0.75s, Ion = 30 ㎃/㎠, ton = 0.25s, 25℃, 10min)
표 ICP results of Pt-Ru alloy catalyst electrodes prepared by electrophoresis method at different deposition condition.
표 EDX results of Pt-Ru alloy catalyst electrodes prepared by electrophoresis method at different deposition condition.
표 SEM cross section images of Pt-Ru/C electrodes with mono catalyst layer (MCL) and double catalyst layer (DCL).
표 CV of Pt-Ru/C mono catalyst electrode and double catalyst electrode with composition of Pt:Ru = 5:5. (0.5 M H2SO4 and 1M CH3OH was used as an electrolyte)
표 CO-tolerance test of Pt/C and Pt-Ru/C alloy catalyst electrode prepared by electrophoresis method (0.5 M H2SO4 solution was used as an electrolyte).
표 Potential change for CO oxidation at according to onset point.
표 SEM cross-section images of Pt-Ru/C electrodes with different positions of double catalyst layer prepared by different spray ratios of carbon black slurry at 1st and 2nd step; (a)3:2, (b) 4:1.
표 CVs of Pt-Ru/C electrodes with different positions of double catalyst layer prepared by different spray ratios of carbon black slurry at 1st and 2nd step; (a) 3:2, (b) 4:1.
표 FESEM images of Pt-Ru/C electrodes prepared by electrophoresis and electrodeposition according to depositon time; (a) 5 min, (b) 10 min, (c) 20 min.
표 Deposition time for preparing Pt-Ru catalyst layer with mono and double catalyst layers (Pt layer; electrophoresis, Ru layer; electrodeposition).
표 SEM cross-section images of Pt-Ru/C electrodes with mono and double catalyst layers prepared by electrophoresis and electrodeposition; (a) mono Pt-Ru catalyst layer, (b) double Pt-Ru catalyst layer electrode.
표 CVs of Pt-Ru/C electrodes with mono and double catalyst layers prepared by electrophoresis and electrodeposition according to deposition time of Ru; a) mono Pt-Ru catalyst layer, (b) double Pt-Ru catalyst layer electrode.
표 CO stripping voltammetries of Pt-Ru/C electrodes with mono and double catalyst layers prepared by electrophoresis and electrodeposition according to deposition time of Ru; a) mono Pt-Ru catalyst layer, (b) double Pt-Ru catalyst layer electrode.
표 Onset point changes of Pt-Ru/C electrodes with mono and double catalyst layers prepared by electrophoresis and electrodeposition according to deposition time of Ru.
표 Single cell test system.
표 I-V curves of Pt/C electrode prepared by electrodeposition with mono and double catalyst layer (electrode area; 5㎠).
표 I-V curves of Pt/C electrode prepared by electrodeposition with mono and double catalyst layer (electrode area; 5㎠).
표 Change of current and power densities in I-V courves for Pt/C electrode with double catalyst layers depending upon depostion time (Pt loading amount).
표 I-V curves of Pt-Ru/C electrode prepared by electrodeposition with mono and double catalyst layer (electrode area; 5㎠).
표 SEM images of Pt/C catalyst electrodes with triple Pt catalyst layers.
표 SEM image and EDX result of Pt/C catalyst electrodes with triple Pt catalyst layers.
표 SEM images of the surface of 1st Pt catalyst layer on TCL Pt/C electrode. (a)(b) deposition time ; 30 sec, (c)(d) deposition time ; 3 min.
표 Deposition conditions of carbon black support loading and Pt catalyst loading for SCL, DCL and TCL electrodes, and EASA values for each electrode.
표 Cyclic voltammograms of SCL, DCL and TCL Pt/C electrodes prepared by PED in 0.5 mol/L H2SO4 solution.
표 Cyclic voltammograms of SCL, DCL and TCL Pt/C electrodes prepared by PED in 0.5 mol/L H2SO4 and 1 mol/L CH3OH solution.
표 The changes of peak current density and current density at 650 mV for SCL, DCL and TCL electrodes.
표 SEM image and EDX result of Pt-Ru/C catalyst electrodes with triple Pt catalyst layers.
표 Cyclic voltammograms of SCL, DCL and TCL Pt-Ru/C electrodes prepared by PED in 0.5 mol/L H2SO4 and 1 mol/L CH3OH solution.
표 The changes of peak current density and current density at 650 mV for SCL, DCL and TCL electrodes.
표 Schematic diagrams of electric contact area between carbon black electrode and metal clip; (a) just clip contact, (b) clip and Cu foil contact.
표 Photographs of (a) carbon black electrode (5cm×5cm) contacted with Cu foil and (b) contact part protected by Teflon sealing tape.
표 Photographs of carbon black electrode and Pt count electrode set up in Pt colloid bath.
표 Large size carbon black electrode (5cm×5cm) with Pt catalyst layer prepared by electrophoresis deposition method.
표 Photographs of large size Pt-loaded carbon black electrodes (5cm×5cm) prepared on different GDLs by electrophoresis deposition method; (a) self-prepared GDL, (b) commercial GDL.
표 Properties of commercial GDL (GDL 370, CeTech Co. Ltd)
표 Cross-sectional SEM image of commercial GDL.
표 Cross-sectional SEM image and EDX result of Pt-loaded commercial GDL electrode by electrophoresis deposition method.
표 Photographs of large size Pt-loaded carbon black electrodes (5cm×5cm) prepared for different deposition times by electrophoresis deposition method; (a) 5 min, (b) 10 min, (c ) 20 min.
표 Pt loading amount on Pt/C electrode with 25 ㎠ area according to deposition time.
표 Histogram of relationship between Pt loading and deposition time in large size GDL electrode with area of 25 cm2.
표 Pt loaded carbon papers (GDLs) with 5 cm×5 cm size; (a) Pt/C electrode prepared by spray deposition method as a anode, (b) Pt/C electrode prepared by electrophoresis deposition method as a cathode.
표 MEA with Pt/C electrode of 5 cm × 5 cm.
표 Photograph of unit cell for MEA with Pt/C electrode of 5 cm × 5 cm.
표 Monitering screen of unit cell test for Pt/C electrode of 5cm×5cm.
표 I-V curve for MEA with Pt/C electrode of 5 cm × 5 cm prepared at 20 min deposition time.
표 Change of current and power densities in I-V courves for Pt/C electrode with double catalyst layers depending upon depostion time (Pt loading amount).
표 SEM cross-section images of Pt/C electrodes with double catalyst layers prepared by electrophoresis method without and with press treatment before 2nd Pt loading; (a) without press, (b) with press.
표 CVs of Pt/C electrodes prepared by pulsed electrophoresis deposition at various cycle times (a) in 0.5 M H2SO4 solution and (b) in 0.5 M H2SO4 containing 1 M CH3OH solution.
표 Electrocatalytic activities of Pt/C electrodes on methanol and hydrogen oxidation at various cycle times.
표 Effect of toff time on Pt loading at constant ton time.
표 Pt loading amount change according to current off time at 5 ms of current on time.
표 CVs of Pt/C catalyst electrode prepared by electrophoresis method at different Nafion condition. (0.5 M H2SO4 and 1M CH3OH was used as an electrolyte).
표 CVs of Pt-Ru/C catalyst electrode prepared by electrophoresis method at different Nafion condition. (0.5 M H2SO4 and 1M CH3OH was used as an electrolyte).
표 Zeta potential of Pt colloid and model of surface charge models.
표 Repulsive model of charged Pt nanoparticles
표 Comparison of (a) conventional method (spray method) and (b) electrophoresis deposition method.
표 Structure of half electrode of MEAs prepared by (a) conventional method, (b) and (c) electrophoresis method.
표 CVs of Pt/C with (a) mono and (b) double catalyst layer electrodes in 0.5 M H2SO4 containing 1 M CH3OH at various deposition times.
표 UV-Vis. spectra of Au colloids with (a) 5-8 nm and (b) 15-20 nm diameter.
표 TEM images of Au colloids with (a) 5-8 nm and (b) 15-20 nm diameter.
표 TEM images of Au-Pt core-shell colloids with core-size 5-8 nm prepared depending upon adding the amount of Pt stock solution (a) 0.5 mL, (b) 1.0 mL, (c) 2.0 mL.
표 TEM images of Au-Pt core-shell colloids with core-size 15-20 nm prepared depending upon adding the amount of Pt stock solution (a) 0.5 mL, (b) 1.0mL, (c) 2.0 mL.
표 TEM images of Au-Pt core-shell colloids with core-size 5-8 nm prepared depending upon adding the amount of Pt stock solution (a) 0.5 mL, (b) 1.0 mL, (c) 2.0mL (after 12,000rpm centrifuge).
표 TEM images of Au-Pt core-shell colloids with core-size 15-20 nm prepared depending upon adding the amount of Pt stock solution after 12,000rpm centrifuge (a) 0.5 mL, (b) 1.0 mL, (c) 2.0 mL (after 12,000rpm centrifuge).
표 Preparation process and TEM image of Pd nanoparticle.
표 Preparation process and TEM image of Pd nanoparticle.
표 Experimental condition for synthesis of Pd-Pt core-shell NPs.
표 TEM images of Pd-Pt core-shell NPs with different volumes of Pt precursor when the volume of Pd precousor is 5 mL and the mole of Pt precursor is 10 mM. (a) 1 mL, (b) 2 mL, (c) 3 mL.
표 TEM images of Pd-Pt core-shell NPs with different volumes of Pt precursor when the volume of Pd precousor is 2 mL and the mole of Pt precursor is 5 mM. (a) 1mL, (b) 2 mL.
표 TEM images of Pd-Pt core-shell NPs with different volumes of Pt precursor when the volume of Pd precousor is 2 mL and the mole of Pt precursor is 10 mM. (a)1 mL, (b-d) 2 mL (different magnifications).
표 High resolution TEM image (a, b) of Pd-Pt core-shell NPs and line scan images (b) for Pd (green line) and Pt (red line) elements.
표 FESEM images of Au/C electrodes prepared by electrophoresis method at different pH, (a) pH = 2, (b) pH = 4, (c) pH = 5.5.
표 FESEM images of Au/C electrodes prepared by electrophoresis method at different deposition time (Au size: 5-8 nm) (a) 1 min, (b) 3 min, (c) 5 min, (d) 10 min.
표 FESEM images of Au/C electrodes prepared by electrophoresis method at different deposition time (Au size: 15-20 nm) (a) 1 min, (b) 3 min, (c) 5 min, (d) 10 min.
표 The contents of carbon black slurry for spraying on carbon sheet with different amount of Nafion.
표 Resistance change of carbon black electrode with different Nafion contents
표 FESEM images of Au/C electrodes prepared by electrophoresis method at different Nafion contents (Au size: 15-20 nm) (a) 5 wt%, (b) 10 wt%, (c) 20 wt%, (d) 33wt%, (e) 40 wt%.
표 The loading amount of Au NPs on carbon black electrode with different Nafion contents analyzed by EDX.
표 Schematic of 2 step loading method for preparing Au-Pt/C catalyst electrode by electrophoresis.
표 TEM image of Pt nanoparticle prepared by reduction method form HAuCl4 solution
표 FESEM images of Au-Pt/C electrodes prepared by electrophoresis method at different deposition times of Au NPs (a) 1 min, (b) 3 min, (c) 5 min, (d) 10 min (Pt deposition time; 10 min, Nafion content; 5 wt%).
표 FESEM images of Au-Pt/C electrodes prepared by electrophoresis method at different deposition times of Au NPs (a) 1 min, (b) 3 min, (c) 5 min, (d) 10 min (Pt deposition time; 10 min, Nafion content; 10 wt%).
표 FESEM images of Au-Pt/C electrodes prepared by electrophoresis method at different deposition times of Au NPs (a) 1 min, (b) 3 min, (c) 5 min, (d) 10 min (Pt deposition time; 10 min, Nafion content; 33 wt%).
표 The loading amount of Au & Pt NPs on carbon black electrode with different Nafion contents analyzed by EDX.
표 CV curves of Au-Pt/C electrodes prepared by electrophoresis method at different deposition times of Au NPs (a) 1 min, (b) 3 min, (c) 5 min, (d) 10 min (Pt deposition time; 10 min, Nafion content; 10 wt%) (0.5 M H2SO4 + 1 M methanol solution).
표 CV curves of Au-Pt/C electrodes prepared by electrophoresis method at different deposition times of Au NPs (a) 1 min, (b) 3 min, (c) 5 min, (d) 10 min (Pt deposition time; 10 min, Nafion content; 33 wt%) (0.5 M H2SO4 + 1 M methanol solution).
표 FESEM images of Au-Ptcore-shell/C electrodes prepared by electrophoresis method at different deposition time (Au core size: 5-8 nm) (a) 10 min, (b) 20 min.
표 FESEM images of Au-Ptcore-shell/C electrodes prepared by electrophoresis method at different deposition time (Au core size: 15-20 nm) (a, b) 10 min, (c, d) 20 min. (a, c; ×50,000, b, d; ×200,000)
표 CV curves of Au-Ptcore-shell/C electrodes prepared by electrophoresis method at different deposition time (0.5 M H2SO4 + 1 M methanol solution) (Au core size: 5-8 nm).
표 CV curves of Au-Ptcore-shell/C electrodes prepared by electrophoresis method at different deposition time (0.5 M H2SO4 + 1 M methanol solution) (Au core size: 15-20 nm).
표 FESEM images of Pd-Ptcore-shell/C electrodes prepared by electrophoresis method at different deposition time (Pd core size: 3-5 nm) (a) 5 min, (b) 10 min, (c) 15min, (d) 20 min.
표 CV curves of Pd-Ptcore-shell/C electrodes prepared by electrophoresis method at different deposition time (0.5 M H2SO4 + 1 M methanol solution) (Pd core size: 3-5 nm).
표 Properties of commercial GDLs and self-made GDL.
표 FESEM images of the surface of GDL-A before Pt deposition.
표 FESEM images of Pt/C electrodes prepared by electrophoresis method for 10 min deposition time on GDL-A.
표 FESEM images of the surface of GDL-B before Pt deposition.
표 FESEM images of Pt/C electrodes prepared by electrophoresis method for 10 min deposition time on GDL-B.
표 FESEM images of the surface of GDL-C before Pt deposition.
표 FESEM images of Pt/C electrodes prepared by electrophoresis method for 10 min deposition time on GDL-C.
표 CV curves of Pt/C electrodes prepared by electrophoresis method for 10 min deposition time on different GDLs in (a) 0.5 M H2SO4 solution and (b) 0.5 M H2SO4 + 1 M methanol solution.
표 Catalytic activities of Pt/C electrode prepared on different GDLs.
표 Schematics of Pt/C electrodes with different thickness of carbon black layer, (a) 17 ㎛, (b) 40 ㎛, (c) 58 ㎛.
표 Thickness changes of carbon black layer according to carbon black loading amount
표 FESEM images of Pt/C electrodes prepared by electrophoresis method for 10 min deposition time on carbon paper without carbon black layer.
표 FESEM images of Pt/C electrodes prepared by electrophoresis method for 10 min deposition time on carbon paper with 17 ㎛ carbon black layer.
표 FESEM images of Pt/C electrodes prepared by electrophoresis method for 10 min deposition time on carbon paper with 40 ㎛ carbon black layer.
표 FESEM images of Pt/C electrodes prepared by electrophoresis method for 10 min deposition time on carbon paper with 58 ㎛ carbon black layer.
표 FESEM images of Pt/C electrodes prepared by electrophoresis method for 10 min deposition time on carbon paper with different thickness of carbon black layer (a) 0 ㎛, (b) 17 ㎛, (c) 40 ㎛, (d) 58 ㎛.
표 EDX analysis for surface of Pt/C electrode with different thickness of carbon black layer prepared by electrophoresis method for 10 min deposition time.
표 CV curves of Pt/C electrodes with different thickness of carbon black layer prepared by electrophoresis method for 10 min deposition time ( 0.5 M H2SO4 + 1 M methanol solution).
표 Schematics of Pt/C double catalyst layers electrodes with different distance between both Pt catalyst layers, (a) 8 ㎛, (b) 100 ㎛, (c) 20 ㎛.
표 SEM cross-sectional images of Pt/C double catalyst layers electrodes with different distance between both Pt catalyst layers, (a) 8 ㎛, (b) 100 ㎛, (c) 20 ㎛.
표 CV curves of Pt/C double catalyst layers electrodes with 8 ㎛ distance between both Pt catalyst layers depending upon deposition time.
표 CV curves of Pt/C double catalyst layers electrodes with 100 ㎛ distance between both Pt catalyst layers depending upon deposition time.
표 CV curves of Pt/C double catalyst layers electrodes with 20 ㎛ distance between both Pt catalyst layers depending upon deposition time.
표 Catalytic activities of Pt/C double catalyst layers electrodes with different distance between catalyst layers obtained from CV curves.
표 Structure and photograph of MEA used in single cell test.
표 Combining process of single cell unit.
표 Experimental conditions for single cell test.
표 I-V curve for MEAs with different GDLs for cathode.
표 Unit cell properties for MEAs with different GDLs for cathode.
표 I-V curve for MEAs with different GDLs for cathode, the electrode structure of GDL-A and C electrodes, and FESEM images of GDL-B and C electrodes.
표 I-V curve for MEAs with GDL-C for cathode according to combining torque of end plate in single cell unit.
표 I-V curve for MEAs with GDL-C for cathode with and without hot press process when preparing MEA.
표 FESEM images of Pt/C electrodes with 5 wt% Nafion prepared by electrophoresis method depending upon deposition time (magnification ×100.0k).
표 FESEM images of Pt/C electrodes with 10 wt% Nafion prepared by electrophoresis method depending upon deposition time (magnification ×100.0k).
표 FESEM images of Pt/C electrodes with 20 wt% Nafion prepared by electrophoresis method depending upon deposition time (magnification ×100.0k).
표 FESEM images of Pt/C electrodes with 30 wt% Nafion prepared by electrophoresis method depending upon deposition time (magnification ×100.0k).
표 EDX results for Pt/C electrodes with 20 wt% Nafion prepared by electrophoresis method depending upon deposition time.
표 Summary of EDX results for Pt/C electrodes with various Nafion content tent
표 Electrical resistance change of carbon black electrodes with various Nafion content.
표 CV curves of Pt/C electrodes with different Nafion content prepared by electrophoresis method for 10 min deposition time in (a) 0.5 M H2SO4 solution and (b) 0.5 M H2SO4 containing 1 M methanol solution (scan rate of 50 mV/s).
표 Catalytic activities in 0.5 M H2SO4 solution of Pt/C electrodes with different Nafion content prepared by EPD for 10 min deposition time.
표 Catalytic activities in 0.5 M H2SO4 containing 1 M methanol solution of Pt/C electrodes with different Nafion content prepared by EPD for 10 min deposition time.
표 (a) IV curves and (b) power density curves of Pt/C electrodes with different Nafion content prepared by pulsed EPD.
표 Summary of single cell performance for Pt/C electrodes with different Nafion content prepared by pulsed EPD.
표 Mass-specific (a) IV curves and (b) power density curves of Pt/C electrodes with different Nafion content prepared by pulsed EPD.
표 Summary of mass-specific single cell performance for Pt/C electrodes with different Nafion content prepared by pulsed EPD.
표 Sputtering system for pre-deposition of Pt catalyst.
표 FESEM images of carbon black electrode with Pt pre-sputtered layer according to sputtering time; (a) 5 sec, (b) 1 min and (c) 2 min.
표 CV curves of Pt/C electrodes with only pre-sputtered Pt layer formed at different sputtering times; in (a) 0.5 M H2SO4 solution and (b) 0.5 M H2SO4 containing 1M methanol solution.
표 Summary of catalytic activities for Pt/C electrodes with only pre-sputtered Pt layer formed at different sputtering times.
표 CV curves of Pt/C electrodes which Pt pre-sputtered layer was formed for different sputtering times and then main Pt catalyst layer was prepared by EPD for 5min deposition time without IPA dipping; in (a) 0.5 M H2SO4 solution and (b) 0.5 M H2SO4 containing 1 M methanol solution.
표 Summary of catalytic activities for Pt/C electrodes with only pre-sputtered Pt layer formed at different sputtering times.
표 CV curves of Pt/C electrodes which Pt pre-sputtered layer was formed for different sputtering times and then main Pt catalyst layer was prepared by EPD for 5min deposition time with IPA dipping; in (a) 0.5 M H2SO4 solution and (b) 0.5 M H2SO4 containing 1 M methanol solution.
표 Summary of catalytic activities for Pt/C electrodes with only pre-sputtered Pt layer formed at different sputtering times.
표 FESEM images of carbon black electrodes with different content of TiO2; (a, b) 2.5 wt%, (c, d) 5 wt% and (e, f) 10 wt% (magnification, a, c, e; ×50.0k, b, d, f; ×100.0k).
표 EDX resutls of carbon black electrodes with different content of TiO2; (a) 5 wt% and (b) 10 wt%.
표 FESEM images of Pt/TiO2-C electrodes prepared by EPD on carbon black eletrode with 5 wt% of TiO2 according to deposition time; (a) 30 sec, (b) 1 min, (c) 5min, (d) 10 min, (e) 15 min and (f) 20 min (magnification ×100.0k).
표 FESEM images of Pt/TiO2-C electrodes prepared by EPD on carbon black electrode with 10 wt% of TiO2 according to deposition time; (a) 30 sec, (b) 1 min, (c) 5min, (d) 10 min, (e) 15 min and (f) 20 min (magnification ×100.0k).
표 CV curves in 0.5 M H2SO4 solution for Pt/TiO2-C electrodes with different TiO2 contents prepared by EPD for 10 min deposition time.
표 Summary of catalytic activities for Pt/TiO2-C electrodes with different TiO2 contents prepared by EPD for 10 min deposition time.
표 Long term changes of CV curve in 0.5 M H2SO4 solution for Pt/TiO2-C electrodes with different TiO2 contents prepared by EPD for 10 min deposition time; (a) 0 wt% TiO2, (b) 5 wt% TiO2 and (c) 10 wt% TiO2.
표 Summary of long term catalytic activity changes for Pt/TiO2-C electrodes with different TiO2 contents prepared by EPD for 10 min of deposition time.
표 Pt active surface area of CV curve in 0.5 M H2SO4 solution for Pt/TiO2-C electrodes with different TiO2 contents prepared by EPD for 10 min deposition time; (a) 0 wt% TiO2, (b) 5 wt% TiO2 and (c) 10 wt% TiO2.
표 Pt active surface area of CV curve in 0.5 M H2SO4 solution for Pt/TiO2-C electrodes with 10 wt% TiO2 contents prepared by EPD for 10 min and 20 min of deposition time.
표 (a) Au colloid bath for EPD, (b) TEM image and (c) UV-Visible spectrum of Au colloid.
표 FESEM images of Au/C electrodes prepared by EPD on carbon black eletrode with 5 wt% of TiO2 according to deposition time; (a, b) 1 min, (c, d) 2 min, (e, f) 5 min, (g, h) 10 min (a, c, e, g; ×10.0k, b, d, f, h; ×50.0k).
표 FESEM images of Pt-Au/TiO2-C electrodes prepared by EPD on carbon black electrode with 5 wt% of TiO2 during 5 min of deposition time; (a; ×50.0k, b; ×100.0k).
표 Small and large contact between clip and carbon electrode.
표 100 cm2 carbon black electrode with large contact area prepared by using Cu foil.
표 Photographs of carbon black electrode (working electrode) and Pt mesh electrode (counter electrode) (a) before and (b) after set up in electrophoresis deposition bath with 3 liter volume.
표 (a) voltage-current-time profile and (b) voltage-time profile during electrophoresis deposition of Pt on carbon black electrode with 100 cm2 area
표 (a) large size carbon black electrode before EPD and (b) large size Pt/C

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금속나노입자의 전기영동 석출법에 의한 PEMFC용 다단활성층 MEA 제조법 연구
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금속나노입자의 전기영동 석출법에 의한 PEMFC용 다단활성층 MEA 제조법 연구 A study on preparation method of MEA with multi active layers for PEMFC by using electrophoretical deposition method of metal nanoparticles 원문보기

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금속나노입자의 전기영동 석출법에 의한 PEMFC용 다단활성층 MEA 제조법 연구
A study on preparation method of MEA with multi active layers for PEMFC by using electrophoretical deposition method of metal nanoparticles 원문보기

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