以微電鍍法製備鎳鉬合金微柱並探討其在1.0 M KOH溶液中電解產氫之性能

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程憲威(Hsien-Wei Cheng) 查詢紙本館藏

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論文名稱

以微電鍍法製備鎳鉬合金微柱並探討其在1.0 M KOH溶液中電解產氫之性能
(Fabrication of Ni-Mo Alloying micropillars by Micro-Anode Guided Electroplating and Their use in 1.0 M KOH to produce Hydrogen gas)

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摘要(中)

本研究以微陽極引導電鍍(Micro-Anode Guided Electroplating, MAGE)來析鍍鎳鉬合金微柱，隨後將這些微柱作為陰極，探討其在1.0 M KOH溶液中電解水產氫之特性。微電鍍使用含0.15 M硫酸鎳、0.008~0.064 M鉬酸鈉與0.36 M焦磷酸鈉鍍浴，微陽極與陰極之間距在40μm，電壓在4.1~5.0 V進行電鍍，過程中，以CCD監控影像，並記錄電鍍電流。析鍍產物以精密天秤秤重以計算電鍍效率。析鍍微柱以SEM觀察表面形貌、EDS檢測組成、EPMA分析橫截面之成分分布、XRD分析其晶體結構，結果顯示:若在含0.008M鉬酸鈉鍍浴中電鍍，電壓由4.1 V增至5.0 V時，所得微柱之直徑微幅縮減(由138.38 μm減至130.43 μm，縮減約5.75%)，但組成中Mo含量由28.4 增高至55.4 at. %；若在5.0 V電壓下，鉬酸鈉濃度由0.008增至0.064 M之鍍浴中電鍍，所得微柱之直徑也是微幅縮減(從130.43 μm減小至126.35 μm縮減約1.95%)，而組成中Mo含量由55.4 at.%增高至69.4 at.%。XRD圖譜顯示經本製程所得微柱均屬於非晶構造。COMSOL Multiphysics 5.2模擬電鍍時的電場分布情形，有助於理解析鍍產物的形貌、組成與結構受電鍍參數之影響。
在1.0 M KOH水溶液中，鎳鉬合金微柱之產氫反應(hydrogen evolution reaction, HER)測試，包括塔弗斜率法、循環伏安法、計時電位法等評估法。結果顯示，微柱之產氫效能受其組成影響，由塔弗斜率測試得知：當鉬含量由28.4 at.%增加至55.4 at.%，斜率由254.37 mV/dec下降至112.85 mV/dec，但鉬含量由55.4 at.%增至69.4 at.%時，斜率又回升至160.36 mV/dec，從塔弗斜率可以知道，產氫由Volmer-Tafel主導。循環伏安法之結果顯示：微柱含55.4 at.% Mo之試片，在經過100次循環後擁有最高的峰值電流密度2418 mA/cm2。在計時電位法實驗中，同時以排水集氣法收集氫氣，歷經300秒反應，微柱鉬含量在28.4~55.4 at.%時，可收集5.3~7.7 mL的氫氣，在鉬含量57.6~69.4 at.%後，氫氣體積由7.7 mL下降至7.0 mL；經由計時電位法計算電量，估計產氫之法拉第效率，微柱鉬含量在34.2~55.4 at.%時，可得到效率75.97~97.32%，在鉬含量57.6~69.4 at.%後，效率由93.56%下降至88.54%。和文獻中鎳鉬薄膜相比在電解水產氫的效果更佳，鎳鉬合金微柱的過電位更低、交換電流密度更大，因此產氫反應更容易進行。

摘要(英)

This study uses Micro-Anode Guided Electroplating (MAGE) to deposit nickel-molybdenum alloy micropillars, and then use these micropillars as cathodes to explore the characteristics of electrolyzing water in 1.0 M KOH solution to produce hydrogen. Micro electroplating uses a plating bath containing 0.15 M nickel sulfate, 0.008~0.064 M sodium molybdate and 0.36 M sodium pyrophosphate, the distance between the micro anode and the cathode is 40 μm, and the voltage is 4.1~5.0 V for electroplating. During the process, the image is monitored by CCD , And record the plating current. The electroplating product is weighed with a precision balance to calculate the electroplating efficiency. The surface morphology of the plated micropillar was observed by SEM, the composition of EDS was detected, the composition distribution of the cross section was analyzed by EPMA, and the crystal structure was analyzed by XRD. The results showed that if electroplating in a bath containing 0.008M sodium molybdate, the voltage increased by 4.1 V At 5.0 V, the diameter of the micropillars obtained is slightly reduced (from 138.38 μm to 130.43 μm, a reduction of about 5.75%), but the Mo content in the composition increases from 28.4 to 55.4 at. %; if the voltage is at 5.0 V, the molybdenum When the sodium concentration is increased from 0.008 to 0.064 M for electroplating in the plating bath, the diameter of the resulting micropillars is also slightly reduced (from 130.43 μm to 126.35 μm, a decrease of about 1.95%), and the Mo content in the composition increases from 55.4 at.% To 69.4 at.%. The XRD pattern shows that the micropillars obtained by this process are all amorphous structures. COMSOL Multiphysics 5.2 simulates the electric field distribution during electroplating, which helps to analyze the influence of electroplating parameters on the morphology, composition and structure of the plating product.
In 1.0 M KOH aqueous solution, the hydrogen evolution reaction (HER) test of nickel-molybdenum alloy micropillars includes evaluation methods such as Tarfer slope method, cyclic voltammetry, and chronopotentiometry. The results show that the hydrogen production efficiency of the microcolumn is affected by its composition. According to the Tarver slope test, when the molybdenum content increases from 28.4 at.% to 55.4 at.%, the slope decreases from 254.37 mV/dec to 112.85 mV/dec. But when the molybdenum content increases from 55.4 at.% to 69.4 at.%, the slope rises back to 160.36 mV/dec. From the Tafer slope, it can be known that the hydrogen production is dominated by Volmer-Tafel. The results of cyclic voltammetry show that the micro-column test piece with 55.4 at.% Mo has the highest peak current density of 2418 mA/cm2 after 100 cycles. In the chronopotentiometric experiment, hydrogen was collected by drainage gas collection method at the same time. After 300 seconds of reaction, when the molybdenum content of the microcolumn was 28.4~55.4 at.%, 5.3~7.7 mL of hydrogen could be collected, and the hydrogen content was 57.6~69.4 at. After .%, the volume of hydrogen decreased from 7.7 mL to 7.0 mL; the electric quantity was calculated by chronopotentiometry to estimate the Faraday efficiency of hydrogen production. When the molybdenum content of the microcolumn was 34.2~55.4 at.%, the efficiency was 75.97~97.32%. After the molybdenum content is 57.6~69.4 at.%, the efficiency drops from 93.56%to 88.54%. Compared with the nickel-molybdenum film in the literature, the effect of hydrogen production in electrolyzed water is better. The nickel-molybdenum alloy micropillars have lower overpotential and higher exchange current density, so the hydrogen production reaction is easier to proceed.

關鍵字(中)

★ 微陽極導引電鍍
★ 鎳鉬合金
★ 鎳鉬電鍍分佈
★ 產生氫反應
★ 非貴金屬觸媒

關鍵字(英)

論文目次

摘要 i
ABSTRACT iii
致謝 vi
目錄 viii
表目錄 xi
圖目錄 xii
第一章、序論 1
1-1 前言 1
1-2 研究動機 2
1-3 研究目的 3
第二章、理論背景與文獻回顧 4
2-1 電化學原理(電鍍與產氫電化學) 4
2-1-1 鎳鉬合金薄膜之電鍍 4
2-1-2 微電鍍技術之發展 5
2-1-3 鎳鉬合金微柱之電鍍 9
2-1-4 奈米壓痕量測 13
2-1-5 電場模擬軟體COMSOL 14
2-1-5 陰極極化曲線 16
2-1-6 電化學交流阻抗(Electrochemical Impedance Spectroscopy，EIS) 16
2-2 鎳鉬合金之鹼性電解產氫 17
2-2-1 水之電解產氫 17
2-2-2 析氫火山圖 19
2-2-3 鎳基合金之鹼性電解產氫 19
2-2-4 鎳鉬合金之鹼性電解產氫 21
2-2-5 電解產氫電化學測試 22
2-2-5-1 產氫之陰極極化曲線與塔弗斜率 22
2-2-5-2 循環伏安法(Cyclic Voltammetry) 23
2-2-5-3 計時電位法(Chronopotentiometry) 25
2-3 法拉第效率 25
第三章、實驗設備與研究方法 27
3-1 實驗流程 27
3-1-1 實驗設備 27
3-1-2 微陽極影像引導電鍍法 30
3-2 微電鍍製備鎳鉬合金微柱 30
3-2-2 陰陽極製備 30
3-2-3 鍍浴配置 30
3-3 樣品觀察與分析 31
3-3-1 SEM與EDS 31
3-3-2 EPMA 31
3-3-3 XRD 31
3-3-4 電鍍電流量測與電鍍效率計算 32
3-3-5 奈米壓痕 32
3-4 鎳鉬合金微柱之熱處理 32
3-5 電場模擬軟體COMSOL 33
3-6 動態電位陰極極化曲線之設備、電極與步驟 34
3-7 定電位EIS之設備、電極與步驟 34
3-8 氫氣收集及效率計算 35
3-9 產氫電化學測試 35
3-9-1 陰極極化曲線 35
3-9-2 循環伏安法 36
3-9-3 計時電位法 36
第四章、結果 37
A. 微柱的析鍍與特性分析 37
4-1 鍍浴中鉬酸鈉濃度對所得微柱之形貌、成分、電場分布之影響 37
4-1-1 微柱形貌(SEM)之改變 37
4-1-2 微柱之成分分析(EDS) 37
4-1-3 柱徑之變化 38
4-1-4 析鍍電流量測與析鍍電流效率之計算 38
4-1-5 COMSOL模擬所得電場分布情形 41
4-2 析鍍偏壓對微柱之形貌、成分、電場分布之影響 42
4-2-1 微柱形貌(SEM)之改變 42
4-2-2 微柱之成分分析(EDS) 42
4-2-3 柱徑之變化 43
4-2-4 析鍍電流量測與析鍍電流效率之計算 43
4-2-5 COMSOL模擬所得電場分布情形 46
4-3 微柱之機械性質(奈米壓痕測試)之改變 47
4-4 微柱之結構(XRD)之改變 49
4-5 微柱之成分分布(EPMA) 50
4-6 動態電位陰極極化曲線、定電位EIS探討 51
4-6-1 動態電位陰極極化曲線探討 51
4-6-2 定電位EIS探討 52
B. 不同組成之微柱在鹼性水溶液中之電解產氫性能探討 53
4-7 微柱中電解產氫電化學測試結果 53
4-7-1 產氫反應之極化曲線 53
4-7-2 循環伏安法(Cyclic Voltammetry) 56
4-7-3 計時電位法(Chronopotentiometry) 56
第五章、討論 60
A. 微柱的析鍍與特性分析 60
5-1 影響微柱形貌、成分、結構、性質之電鍍因素 60
5-1-1 鉬酸鈉濃度、析鍍偏壓對COMSOL電場分布之影響 60
5-1-2 鉬酸鈉濃度、析鍍偏壓對鎳鉬合金微柱組成之影響 60
5-1-3 鉬含量對鎳鉬合金微柱XRD圖譜之影響 61
5-1-4 鎳鉬合金中鉬含量對微柱機械性質之影響 62
5-1-5 電場強度對鎳鉬合金微柱柱徑之影響 63
5-1-6 熱處理和微柱組成對鎳鉬合金微柱之EPMA之影響 63
5-1-7 鍍液中鉬酸鈉濃度對動態電位陰極極化曲線之影響 64
5-1-8 鍍液中鉬酸鈉濃度對定電位EIS圖譜之影響 65
B. 不同組成之微柱在鹼性水溶液中之電解產氫性能探討 66
5-2 微柱特性對鹼性水電解產氫性能之影響 66
5-2-1 微柱組成對產氫陰極極化之影響 66
5-2-2 微柱組成對循環伏安法之影響 67
5-2-3 微柱組成對計時電位法之影響 67
5-2-4 本論文之產氫效能與其他研究結果之比較 68
第六章、結論與未來展望 70
6-1 結論 70
6-2 未來展望 73
參考文獻 74

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指導教授

林景崎(Jing-Chie Lin)

審核日期

2022-9-16

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