鈷、鎳以及鈷鎳合金薄膜電極材料製備及其產氫活性的研究

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研究生：	王彥貞 Yen-Chen Wang
論文名稱：	鈷、鎳以及鈷鎳合金薄膜電極材料製備及其產氫活性的研究
指導教授：	姚學麟 Shueh-Lin Yau
口試委員:
學位類別：	碩士 Master
系所名稱：	理學院 - 化學學系 Department of Chemistry
論文出版年：	2021
畢業學年度：	109
語文別：	中文
論文頁數：	186
中文關鍵詞：	鈷、鎳、鈷鎳合金、氫氣析出反應
外文關鍵詞：	cobalt, nickel, cobalt-nickel alloy, hydrogen evolution reaction
相關次數：	點閱：11 下載：0
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本研究以循環掃描電位的方式，於Au(111)或Pt(111)上沉積鈷、鎳以及不同比例的鈷鎳合金後，於鹼性溶液中(0.1M KOH)測試對氫氣析出反應(hydrogen evolution reaction,HER)之催化活性，而合金中鈷鎳的比例以角解析X射線光電子光譜(ARXPS)來分析，並藉由STM觀察這些金屬的沉積過程與表面形貌。其中CoNi6.1/Au(111)合金電極擁有較小的過電位(-223mV)以及Tafel斜率(87.7mV/dec)，對產氫(HER)活性優於純鈷、鎳以及其他比例的合金。於Pt(111)上修飾3層Ni後，其HER活性表現最突出，它有最小的過電位(-53mV)，以Tafel斜率(46.9mV/dec)推論， HER的速率決定步驟(rds)為氫氣脫附反應(Heyrovsky步驟)，其餘材料的rds皆為氫吸附的反應(Volmer步驟)，可能是由於Ni能有利於水的分解，而三層的鎳與白金之間可能有很好的電子效應，能夠提供有利於氫的吸附位點，且OHad與Ni之間的相互作用最為理想，因此大幅提升產氫活性。以STM觀察鈷鎳合金於Au(111)上成長，第一層多以針狀的方式生長為無序或整齊的moiré pattern結構。在Pt(111)上，鈷鎳離子比例為1:1時，第一層沉積膜由兩種金屬共同組成，無整齊的蜂窩狀結構，當鈷鎳比例為1:4時，第一層亦無整齊的蜂窩狀結構，而是長成樹枝狀的樣貌。也以STM觀察pH3與pH5硫酸鹽中，鎳在Au(111)和Pt(111)上的生長。

The electrodeposition of cobalt, nickel and cobalt-nickel alloys on Au(111) and Pt(111) electrodes was studied by using cyclic voltammetry (CV),scanning tunneling microscope (STM) and X-ray photoelectron spectroscopy (XPS). The electrocatalytic activities of the as-prepared filmy materials toward hydrogen evolution reaction (HER) were examined in alkaline media (0.1 M KOH). The chemical compositions of the Co-Ni alloys were analyzed with angle-resolved X-ray photoelectron spectroscopy (ARXPS).The deposition process and surface morphology of these metallic films were observed by STM. The Au(111)-supported CoNi6.1 alloy film exhibited higher HER activity than pure cobalt, nickel and the other alloys, as manifested by a smaller overpotential (-223 mV) and Tafel slope (87.7 mV/ dec). On the Pt(111) electrode the deposition of three monolayer (ML) Ni led to the most active catalyst for HER, as evaluated from the smallest overpotential (-53 mV) and Tafel slope (46.9 mV/dec). This catalyst was unique, in that the rate-determining step (rds) for HER was the hydrogen desorption reaction, as opposed to the hydrogen adsorption reaction found for others. It is assumed that as-preapred Ni films were active sites for the water splitting reaction, which facilitated dissociation of water molecule to OHad. It is assumed that Pt substrate altered the electronic configuration of the three-layer-thick nickel film, which optimized its interaction of H and OH.The first layer of the depositied Co-Ni alloys on Au(111) assumed a needle-like texture, disordered and ordered moiré patterns, which resemble those features observed with pure Ni deposit. The Co-Ni alloy films deposited on Pt(111) from a 1:1 and 1:4 Co2+/Ni2+ solutions had a disordered structure and a dendritic pattern. The latter resulted from a fractal-like growth mode. The electrodeposition of Ni on Au(111) and Pt(111) in pH 3 and pH 5 sulfate media were also examined.

摘要    I
Abstract    II
誌謝    III
目錄    IV
圖目錄    VIII
表目錄    XVIII
第一章、緒論    1
1-1 電化學分解水製氫    1
1-1-1 簡介    1
1-1-2 火山曲線圖(Volcano plot)    4
1-1-3 過電位(Overpotential)    6
1-1-4 塔弗斜率(Tafel slope)與反應機制    7
1-1-5 穩定性(Stability)    10
1-1-6 質量活性與特定活性(Mass and specific activities)10
1-1-7 轉換頻率(Turnover frequency, TOF)與法拉第效率(Faradaic Efficiency, FE)        11
1-1-8 電催化劑    13
1-2 鎳與鈷鎳合金之概論    16
1-2-1 鎳的沉積    16
1-2-2 鎳的應用    17
1-2-3 鈷鎳合金的沉積    26
1-2-4 鈷鎳合金的應用    28
1-3 研究動機    35
第二章、實驗部分    36
2-1 藥品部分    36
2-1-1 實驗用藥品    36
2-1-2 鈷鎳之電鍍液    36
2-2 實驗用氣體    37
2-3 金屬線材    37
2-4 實驗用儀器    37
2-4-1 循環伏安儀（Cyclic Voltammetry , CV）    37
2-4-2 掃描式穿隧電子顯微鏡（Scanning Tunneling Microscope ,             STM）    37
2-4-3 點焊機(D.C. Spot Welder)：    38
2-4-4 研磨拋光機（Grinder and Polisher）    38
2-4-5 超音波震盪器（Ultrasonic Cleaner）    39
2-4-6 X射線光電子能譜（X-ray photoelectron spectroscopy , XPS）    39
2-5 實驗步驟    43
2-5-1 金(111)和鉑(111)單晶CV用的電極製備    43
2-5-2 金(111)和鉑(111)單晶STM用的電極製備    43
2-5-3 STM探針製備    43
2-5-4 循環伏安法(CV)的實驗步驟    44
2-5-5 電化學掃描式穿隧電子顯微鏡(EC-STM)的實驗步驟    45
2-5-6 角解析XPS(ARXPS)的樣品製備    45
第三章、Au(111)上修飾鈷鎳合金對於氫氣析出反應的電化學活性49
3-1 Au(111)上修飾鈷於pH3硫酸鉀溶液中之電沉積探討    49
3-1-1 鈷於Au(111)電極上之循環伏安圖    49
3-1-2 鈷於Au(111)上之STM圖    53
3-2 Au(111)上修飾鎳於pH3硫酸鉀溶液中之電沉積探討    57
3-2-1 鎳於Au(111)電極上之循環伏安圖    57
3-2-2 鎳於Au(111)上之STM圖    60
3-3 Au(111)上修飾鈷鎳合金於pH3硫酸鉀溶液中之電沉積探討63
3-3-1 鈷鎳合金於Au(111)電極上之循環伏安圖    63
3-3-2 鈷鎳合金於Au(111)電極上之元素比例分析    69
3-3-3 鈷鎳合金於Au(111)上之STM圖(Co2+:Ni2+=1:1)    75
3-3-4 鈷鎳合金於Au(111)上之STM圖(Co2+:Ni2+=1:4)    81
3-4 Au(111)上修飾鈷、鎳以及鈷鎳合金氫氧化物對產氫催化活性之探討    84
3-4-1 Au(111)上修飾鈷、鎳以及鈷鎳合金於鹼液中進行HER的測試84
3-4-2 Au(111)上修飾鈷、鎳以及鈷鎳合金氫氧化物於鹼液中進行HER後之電化學特性    90
3-5 Au(111)上修飾鎳於pH5硫酸鉀溶液中對氫氣析出反應之變化93
3-5-1鎳於Au(111)上之STM圖(1mM Ni2+)    93
3-5-2鎳於Au(111)上之STM圖(0.1mM Ni2+)    101
3-6 結論    108
第四章、Pt(111)上修飾鈷鎳合金對於氫氣析出反應的電化學活性109
4-1 Pt(111)上修飾鈷和鎳於pH3硫酸鹽中之電沉積探討    109
4-2 Pt(111)電極上修飾鈷鎳合金於pH3硫酸鹽中之電沉積探討112
4-2-1 鈷鎳合金於Pt(111)電極上之循環伏安圖    112
4-2-2 鈷鎳合金於Pt(111)電極上之STM圖(Co2+:Ni2+=1:1)118
4-2-3 鈷鎳合金於Pt(111)電極上之STM圖(Co2+:Ni2+=1:4)127
4-3 Pt(111)上修飾鈷、鎳以及鈷鎳合金對產氫催化活性之探討133
4-3-1 Pt(111)上修飾鈷、鎳以及鈷鎳合金於鹼液中進行HER之測試133
4-3-2 Pt(111)上修飾鈷、鎳以及鈷鎳合金氫氧化物於鹼液中進行HER後之電化學特性    141
4-3-3 Pt(111)上修飾鎳於鹼性環境中之STM圖    145
4-4 Pt(111)上修飾鎳於pH5硫酸鉀溶液中對氫氣析出反應之變化149
4-5 結論    157
第五章、參考文獻    158


                                

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