電化學石英晶體微天平在質子交換膜燃料電池碳載體腐蝕分析及性能提升之研究

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研究生：	洪志成 Hung, Chih-Cheng
論文名稱：	電化學石英晶體微天平在質子交換膜燃料電池碳載體腐蝕分析及性能提升之研究 Studies on carbon support corrosion and performance improvement for the proton exchange membrane fuel cells by electrochemical quartz crystal microbalance
指導教授：	施漢章 Shih, Han-C. 吳志明 Wu, Jyh-Ming
口試委員:	曹春暉 Tsau, Chun-Huei 黃清安 Huang, Ching-An 王丞浩 Wang, Chen-Hao
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2017
畢業學年度：	105
語文別：	英文
論文頁數：	109
中文關鍵詞：	電化學石英晶體微天平、質子交換膜燃料電池、碳載體、碳腐蝕、火花電漿燒結
外文關鍵詞：	EQCM, PEMFC, carbon support, carbon corrosion, SPS
相關次數：	點閱：3 下載：0
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利用電化學石英天秤(EQCM)結合循環伏安法(CV)，質子交換膜燃料電池（PEMFC）中的碳載體材料電化學腐蝕劣化行為可成功地被觀察及研究。幾種常用的商業碳載體材料（Vulcan XC-72，Ketjen black ECP300，Ketjen black ECP600）以及多壁奈米碳管（MWCNT）以噴塗法製備成碳膜石英電極(C-QCE)，在298K的脫氣0.5M H2SO4溶液中，於循環伏安法（CV）的同時通過EQCM的頻率變動，可以觀察到的碳膜石英電極(C-QCE)上的質量變化。在CV正向掃描期間，表面氧化物形成並累積在碳表面上，導致碳膜石英電極的重量隨著電位上升而增加；而在較高電位區域可觀察到由於表面碳氧化物氣化成二氧化碳，所造成與碳腐蝕相關的重量減少。由實驗結果顯示，未處理商用載碳體XC-72的EQCM重量減少的發生電位為1.05V與其它碳載體腐蝕研究的結果相近；再依單位面積碳腐蝕率比較，高比表面積的商用碳載體ECP300、ECP600高於較低比表面積的XC-72，顯示較高比表面積的商用碳載體會有較大的碳腐蝕程度；另外多壁奈米碳管的EQCM重量減少的電位提高至1.62V，驗證了碳載體材料的石墨化度，可有效增強其於燃料電池環境下的抗電化學氧化性。
研究碳膜石英電極於CV期間的EQCM重量變化率以及重量減少的發生電位，可進一步討論碳載體材料的電化學碳腐蝕行為，商用碳載體材料XC-72於模擬燃料電池環境下0.5M H2SO4溶液的電化學氧化行為及其影響條件；由實驗結果證明：通入不同氣體的0.5M H2SO4溶液條件實驗，證明碳載體氧化的氧來源主要來自液體；而加入PTFE黏劑的碳膜則因表面疏水及質傳阻礙，電化學氧化程度減少。
以傳統的高溫加熱的方法可以提升質子燃料電池碳載體的石墨化程度，從而提高碳載體電化學氧化過程中的穩定性及抗腐蝕性，由實驗結果商用碳載體材料Vulcan XC-72經2200℃以上的高溫處理後，可有效的提升碳載體的石墨化度，但分析結果也顯示：碳載體本身的比表面積大幅減少，且碳載體表面的含氧官能基減少而使其表面會過於疏水，這樣的疏水表面會使得碳載體在後續的白金觸媒顆粒上漿製程中，產生不易附載及分散不均等問題；利用氧電漿處理石墨化的碳黑，可增加石墨化碳黑表面的含氧官能基，解決石墨化碳黑不易附載白金觸媒的問題，相關文獻也指出含氧官能基能使白金觸媒顆粒和碳載體間的反應及附著性更好。
以火花電漿燒結(SPS)方法增強商用碳載體材料Vulcan XC-72 的石墨化度，不僅處理時間短，對碳黑的比表面積、孔隙度及表面官能基的影響小，本研究並討論在不同的SPS實驗條件下，所得到碳材的石墨化結果；由EQCM的實驗結果顯示，經SPS法處理後和未處理的商用碳載體材料Vulcan XC-72相比，由於石墨化的提升從而使得其電化學的抗腐蝕能力增加；另外和傳統高溫加熱法比較，以SPS法處理後的碳載體XC-72表面仍可保有較好的比表面積、表面官能基及親水性，在白金觸媒的附載上也較為容易。

The carbon corrosion behavior of several carbon support materials for proton exchange membrane fuel cell (PEMFC), including commercial carbon black (Vulcan XC-72, Ketjen black ECP300, Ketjen black ECP600), graphitized carbon black and multi-wall carbon nanotubes (MWCNTs), was investigated by using the electrochemical quartz crystal microbalance (EQCM) method. The mass change during cyclic voltammetry (CV) in deaerated 0.5 M H2SO4 solution at 298 K can be observed by the frequency change of EQCM. During the positive scan, the carbon surface oxides were formed and accumulated on the carbon surface leading to an increase of the mass as the potential increasing. In the higher potential region, a drop in mass associated to carbon loss was observed which was attributed to the gasification of surface carbon oxides to carbon dioxide. Examine the mass change rate and mass drop onset potential, the behavior of electrochemical carbon corrosion was discussed.
The influence of specific surface area and graphitization of carbon supports were also investigated in this study. The results indicate that high BET surface area carbon blacks rendered less resistant to electrochemical carbon corrosion. Graphitized XC-72 and MWCNTs with higher graphitization degrees appear more intrinsically resistant to electrochemical carbon corrosion.
The commercial carbon support Vulcan XC-72 was graphitized by conventional high temperature heat treatment at various temperatures to increase the graphitization and improve the electrochemical corrosion stability of commercial carbon support Vulcan XC-72. The result shows XC-72 can be obviously increase the graphitization after 2200℃ conventional high temperature heat treatment. Meanwhile, the BET surface area and the surface functional groups of carbon support XC-72 was strongly decreased after heat treatment. After oxygen plasms treatment, the graphitized XC-72 carbon black has increased the BET surface area and the O/C ratio of surface similar to the as-received XC-72. Therefore, oxygen plasma treatment is an effective method to provide graphitized carbon blacks with surface functional groups that can act as anchoring sites to favor dispersion and deposition of platinum particles on their surface and could be helpful to prevent platinum particles agglomeration.
Comparing to conventional high temperature heat treatment, carbon support XC-72 can be graphitized rapidly by SPS method only within few minutes. Moreover, the SPS treated carbon support XC-72 do not suffer from high levels of hydrophobic character which can create problems with active phase dispersion and ink formulations. The results revealed that the SPS is an effective method to enhance the electrochemical stability and surface properties of carbon blacks for the application of PEMFC.

中文摘要    i
ABSTRACT iii
誌謝    v
CONTENTS
Chapter 1
Introduction    1
1.1    Fuel cell    1
1.1.1    The development of fuel cells    2
1.1.2    Types of Fuel Cells    4
1.2    The PEMFC    8
1.2.1    The challenges of PEMFCs    9
1.2.2    The structure of PEMFC    11
1.3    Carbon support    14
1.3.1    Carbons in PEMFC    14
1.3.2    New carbon support materials    18
1.3.3    The characteristics of carbon    19
1.3.4    Graphitization of carbon    21
1.3.5    The corrosion of carbon support for PEMFC    22
1.4    Spark plasma sintering (SPS)    26

Chapter 2
Corrosion of commercial carbon support for PEM fuel cells by EQCM...29
2.1    Introduction    29
2.2    Experimental    31
2.2.1    Carbon film quartz crystal electrodes (C-QCE) preparation    31
2.2.2    Electrochemical experiment    31
2.2.3    Physical characterization    33
2.3    Result and Discussion    34
2.3.1    EQCM measurement of XC-72    34
2.3.2    Investigation of commercial carbon blacks    43
2.3.3    Investigation of MWCNT    46
2.3.4    The influence of binder    48
2.3.5    The influence of atmosphere    51
2.4    Conclusions    53

Chapter 3
The graphitization of commercial carbon support and surface functionalization by oxygen plasma treatment for PEMFC    54
3.1    Introduction    54
3.2    Experimental    56
3.2.1    Graphitized carbon blacks preparation    56
3.2.2    Oxygen plasma treatment    56
3.2.3    Electrochemical experiment    56
3.2.4    Physical characterization    57
3.3    Result and Discussion    58
3.3.1    Investigation of graphitization for XC-72 carbon black    58
3.3.2    The investiagtion of BET surface area and pore volume    61
3.3.3    The surface chemistry and wettability of carbon blacks    63
3.3.4    Electrochemical oxidation for carbon blacks    65
3.3.5    The oxygen plasma treatment of graphitized XC-72    68
3.4    Conclusion    75

Chapter 4
A rapid method to improve the performance of carbon support for PEM fuel cell by SPS    76
4.1    Introduction    76
4.2    Experimental    78
4.2.1    The preparation of carbon blacks    78
4.2.2    Electrochemical experiment    79
4.2.3    Physical characterization    80
4.2.4    Preparation of carbon-supported Pt catalysts    80
4.3    Result and Discussion    81
4.3.1    The heating temperature of SPS treatment    81
4.3.2    Investigation for three carbons    83
4.3.3    TEM measurement of carbons    85
4.3.4    The BET specific surface area    87
4.3.5    The surface chemistry and wettability of carbon blacks    89
4.3.6    The electrochemical corrosion resistant    91
4.3.7    Electrical conductivity    93
4.3.8    Thermal stability    94
4.3.9    Deposition of Pt catalytic particles on carbon blacks    95
4.4    Conclusion    99

Chapter 5
Summary    100

LIST OF FIGURES
Fig. 1.1  Schematic of an individual fuel cell.    2
Fig. 1.2  Sir William Grove and the scheme of his gas voltaic battery     3
Fig. 1.3  (A) the maximum operating temperature of fuel cells vs. output power (B) the electric efficiencies and combined heat and power (CHP) efficiencies of various fuel cells    6
Fig. 1.4  Fuel Cell Today data from 2009-2013 for a) shipments by application  b) shipments by fuel cell type    7
Fig. 1.5  Modeled cost of an 80-kWnet PEMFC system based on projection to high-volume manufacturing (500,000 units/year)    9
Fig. 1.6  Waterfall chart for projection of automotive fuel cell system cost down to DOE 2020 target $40/kWnet, and DOE ultimate target $30/kWnet    10
Fig. 1.7  The basic structure of proton exchange membrane fuel cell (PEMFC)    11
Fig. 1.8  Chemical structure of Nafion monomer     13
Fig. 1.9  The physicochemical properties of carbon black    17
Fig. 1.10  The structure of graphite    20
Fig. 1.11  Structural model for the process of graphitization    21
Fig. 1.12  A schematic illustration of reactions in four distinct regions when an air/fuel boundary is formed at the anode. Cathode catalyst layer thickness was reduced to about 1/3 of its original value after 80 cycles, while the anode thickness did not show much change    23
Fig. 1.13  Schematic representation of degradation of carbon catalyst support during operation in the absence of fuel    24
Fig. 1.14  Comparison of CO2 mass-spectra profiles for MEAs with non-graphitized support N-Pt/C and graphitized support G-Pt/C at 1.4 V    25
Fig. 1.15  The schematic of the SPS system    26
Fig. 1.16  Energy dissipation in the microscopic scale during the SPS process    27
Fig. 1.17  The mechanism of speak plasma sintering    28
Fig. 2.1  Schematic of the EQCM system and carbon film quartz crystal electrodes    33
Fig. 2.2  The EQCM mass change responses for the bare Au quartz crystal electrode (Au-QCE) recorded simultaneously with the CV in deaerated 0.5 M H2SO4, at a scan rate of 10 mV s-1 and a temperature of 298 K    34
Fig. 2.3  The EQCM mass change responses for the Vulcan XC-72 carbon film quartz crystal electrode (C-QCE) recorded simultaneously with the CV in deaerated 0.5 M H2SO4 at a scan rate of 10 mV s-1 and a temperature of 298 K    36
Fig. 2.4  Schematic diagram of the mass change of C-QCE during the positive scan of CV by EQCM    37
Fig. 2.5   (a) CV and (b) EQCM data for Vulcan XC-72 C-QCE  at a scan rate of 10 mV s-1 in deaerated 0.5 M H2SO4 at 298 K after holding at a constant potential of 1.2 V for 0, 3 and 15 h.    39
Fig. 2.6  EQCM mass change (positive CV scan) for 1000 cycles    40
Fig. 2.7  Maximum mass gain and mass drop onset potential vs. CV cycles    41
Fig. 2.8  EQCM mass change versus time for the XC 72 carbon support as a function of specific potentials in deaerated 0.5 M H2SO4 at a scan rate of 10 mV s-1 and a temperature of 298 K.    42
Fig. 2.9  EQCM mass change (positive CV scan) of (a) the original, and (b) normalized by the BET surface area for XC-72 , ECP300 and ECP 600 in deaerated 0.5 M H2SO4 at a scan rate of 10 mV s-1 and a temperature of 298 K.    45
Fig. 2.10  EQCM mass change (positive CV scan) for MWCNTs in deaerated 0.5 M H2SO4 at a scan rate of 10 mV s-1 and a temperature of 298 K.    47
Fig. 2.11  EQCM mass change of XC-72 with and without PTFE in deaerated 0.5 M H2SO4 at a scan rate of 10 mV s-1 and a temperature of 298 K.    49
Fig. 2.12  EQCM mass change of XC-72 in N2 purged and O2 purged 0.5M H2SO4 at a scan rate of 10 mV s-1 and a temperature of 298 K.    52
Fig. 3.1  The XRD patterns of carbon black XC-72 after various temperature treatments    58
Fig. 3.2  The plots of the interlayer spacing d(002), crystalline width (La) and the crystalline height (Lc) as a function of heating-treatment temperature    60
Fig. 3.3  XPS spectra of XC-72 before and after heat treatment    63
Fig. 3.4  The test of wettability for as-received XC-72 and graphitized XC-72    64
Fig. 3.5  EQCM mass change (positive CV scan) of the original, in deaerated 0.5 M H2SO4 at a scan rate of 10 mV s-1 and a temperature of 298 K    66
Fig. 3.6  EQCM mass change (positive CV scan) of normalized by the BET surface area for XC-72 and graphitized XC-72 in deaerated 0.5 M H2SO4 at a scan rate of 10 mV s-1 and a temperature of 298 K    66
Fig. 3.7  The Raman spectrum of the graphitized XC-72 after oxygen plasma treatment for 0, 10, 20 and 30 seconds    69
Fig. 3.8  The general XPS spectra of graphitized XC-72 under different oxygen plasma treatment times    70
Fig. 3.9  The peak fitting of the C1s XPS spectra of XC-72 carbon blacks under different oxygen plasma treatment times    73
Fig. 3.10  The percentage of each component of XC-72 carbon supports under different oxygen plasma treatment times    74
Fig. 4.1  SPS-511S spark plasma sintering system (Sumitomo Coal Mining) [102]    79
Fig. 4.2  Plot the X-ray diffraction patterns of three carbon supports, AR XC-72, SPS XC-72 and HT XC-72    83
Fig. 4.3  The TEM image of Vulcan XC-72 and the cutaway model of a carbon-black particle with concentric layers    85
Fig. 4.4  The TEM images for three carbon supports, (a) AR XC-72, (b) SPS XC-72 and (c)HT XC-72    86
Fig. 4.5  XPS spectra for different carbons, AR XC-72, SPS XC-72 and HT XC-72    90
Fig. 4.6  Dispersion of different carbon blacks HT XC-72, SPS XC-72 and as-received XC-72 in water    90
Fig. 4.7  EQCM mass change (positive CV scan) of normalized by the BET surface area for AR XC-72 , SPS XC-72 and HT XC-72 in deaerated 0.5 M H2SO4 at a scan rate of 10 mV s-1 and a temperature of 298 K    92
Fig. 4.8  Through-plane electrical conductivity of different carbon blacks.    93
Fig. 4.9  TGA curves of different carbon blacks.    94
Fig. 4.10  TEM images of Pt catalytic particles deposited on (a) AR XC-72,    98

LIST OF TABLES
Table 1 1  The summary of characteristics and applications for major fuel cells    5
Table 1 2  List of characteristics of carbon blacks as catalyst supports for PEMFCs    15
Table 1 3  The requirements for a suitable carbon support and data of XC-72     16
Table 1 4  The main characteristics of different carbon support materials     18
Table 2 1  The BET data and EQCM results of XC-72, ECP300 and ECP600.    44
Table 2 2  A comparison of carbon corrosion measurement approaches    50
Table 3 1  The interlayer spacing d(002), the crystalline width (La) and the crystalline height (Lc) at various heating-treatment temperature    59
Table 3 2  BET specific surface area and pore volume data of as received XC-72 and graphitized carbon blacks    62
Table 3 3  The BET and EQCM data for as received and graphitized XC-72    65
Table 3 4  The O/C ratio of graphitized carbon XC-72 under different oxygen plasma treatment times    71
Table 3 5  The ID/IG ratio, BET surface are and O/C ratio of graphitized carbon XC-72 under different oxygen plasma treatment times    72
Table 4 1  The 2θ(002) , interlayer spacing d(002) and BET surface area (S) at various SPS heating temperatures and times    81
Table 4 2  The interlayer spacing d(002), the crystalline width (La) and the crystalline thickness (Lc) for three carbons    84
Table 4 3  BET specific surface area and pore volume data of as received XC-72 and treated carbon blacks    88
Table 4 4  The O/C ratio of three carbons, AR XC-72, SPS XC-72 and HT XC-72    89
Table 4 5  The BET and EQCM data for AR XC-72, SPS XC-72 and HT XC-72    92

                                

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