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系統識別號 U0026-1708202011022600
論文名稱(中文) 奈米結構的鎳鐵磷合金:電合成及其在中性下產氫反應的應用
論文名稱(英文) Nanostructured nickel-iron-phosphorus alloy:electrosynthesis and application for hydrogen evolution reaction at neutral pH
校院名稱 成功大學
系所名稱(中) 化學工程學系
系所名稱(英) Department of Chemical Engineering
學年度 108
學期 2
出版年 109
研究生(中文) 張舜閔
研究生(英文) Shun-Min Zhang
學號 N36071235
學位類別 碩士
語文別 中文
論文頁數 65頁
口試委員 指導教授-林家裕
口試委員-陳嘉勻
口試委員-林仕鑫
口試委員-賴怡璇
口試委員-龔仲偉
中文關鍵字 產氫反應  中性條件  鎳鐵磷合金  電沉積 
英文關鍵字 Electrodeposition  Hydrogen evolution reaction  Neutral condition  Nickel-iron-phosphorus alloy 
學科別分類
中文摘要 在本研究中,我們利用電化學沉積法合成具奈米結構的鎳鐵磷合金,並將其應用在中性環境下產氫反應。此電觸媒的物化特性是透過掃描式電子顯微鏡、拉曼光譜儀、感應耦合電漿原子發射光譜儀、X光光電子能譜儀、線性掃描伏安法、循環伏安法和計時電位法來進行分析。結果發現電鍍電流密度和電鍍液的組成對所製備的鎳鐵磷合金電觸媒的表面型態以及化學組成具有極大的影響。例如,在高電流密度(geq -2 mA cm-2)、低Ni/Fe莫爾數(le 2)比和不含磷的濃度(0 M)之條件下,可製備出具奈米立方體結構之鎳鐵磷合金,而在低電流密度、低鐵濃度和含有不同磷濃度之條件下,則可製備出具奈米球形結構之鎳鐵磷合金。此外,在最佳的合成條件下所製備之鎳鐵磷合金電觸媒表現出優良的產氫活性,在中性環境下分別需要260.5±0.01 和200 mV之過電位去達到10 mA cm-2的電流密度以及37.29±5.81的轉換頻率。
英文摘要 In this study, nanostructured nickel-iron-phosphorus alloys (nanoNiFePx) were synthesized by electrochemical deposition and their applications as the electrocatalysts for the hydrogen evolution reaction (HER) were investigated. The physicochemical properties of the prepared nanoNiFePx were characterized using scanning electron microscopy, Raman spectroscopy, inductively coupled plasma mass spectrometry, and X-ray photoelectron spectroscopy, linear sweep voltammetry, cyclic voltammetry, and chronopotentiometry. It was found that deposition current density and composition of plating solution used for the electrosynthesis of nanoNiFePx had great influences on the surface morphology and chemical composition of the prepared nanoNiFePx. For example, electrodeposition with high deposition current density (geq -2 mA cm-2), low Ni/Fe molar ratio (le 1), or phosphorus-free content (0 M) resulted in the formation of NiFePx nanocubes, whereas electrodeposition with low deposition current density, low iron content, or any amount of phosphorus favored the formation of NiFePx nanospheres. In addition, nanoNiFePx prepared with optimal synthetic conditions exhibited the best HER activity, requiring overpotentials of 260.5±0.01 and 200 mV to achieve a current density of 10 mA cm-2 and turnover frequency of 37.29±5.81 h-1 at neutral pH, respectively.
論文目次 摘要 I
Extended Abstract II
致謝 IX
總目錄 XI
表目錄 XIII
圖目錄 XIV
第一章 緒論 1
1.1 研究背景 1
1.2 產氫之觸媒介紹 3
1.2.1 純金屬之產氫觸媒 3
1.2.2 金屬合金之產氫觸媒 5
1.2.3 金屬混非金屬之產氫觸媒 5
1.2.3.1 製備方法 6
1.2.3.2 磷對產氫活性的影響 8
1.3 中性下之產氫機制 9
1.3.1 中性下之產氫觸媒 10
1.4 研究動機 12
第二章 原理與文獻回顧 13
2.1 電沉積法 13
2.1.1 直流電沉積 13
2.1.2 脈衝電流電沉積 14
2.1.3 脈衝反向電沉積 14
2.2 評估產氫活性參數 16
第三章 實驗步驟與研究方法 18
3.1 實驗材料 18
3.2 實驗儀器 20
3.3 電極製備方法 21
3.3.1 以不同電流密度合成鎳鐵磷電觸媒 22
3.3.2 以不同成分電鍍液合成鎳鐵磷電觸媒 22
3.4 物性分析方法 23
3.4.1 感應耦合電漿原子發射光譜儀(Inductively Couple Plasma Optical Emission Spectrometer, ICP-OES) 23
3.4.2 X-ray光電子能譜儀(X-ray photoelectron spectroscopy, XPS) 23
3.4.3 拉曼光譜儀(Raman spectrometer) 24
3.5 電化學分析方法 25
第四章 結果與討論 27
4.1 成長機制 27
4.1.1 電流效應 27
4.1.2 不同金屬比例效應 33
4.1.3 磷的效應 36
4-2 電化學分析 39
4.2.1 電流效應 39
4.2.2 不同金屬比例效應 44
4.2.3 磷的效應 48
第五章 結論與未來展望 54
5-1 結論 54
5-2 建議與未來展望 55
第六章 參考文獻 56
附錄 61
個人簡歷 65



表目錄
表 1-1 各種合成金屬磷化物之方法 7
表 1-2 中性環境下之產氫觸媒的電化學參數整理。 11
表 3-1 本研究所使用之化學藥品清單。 18
表 3-2 本研究所使用之儀器清單。 20
表 4-1 不同電流密度合成之鎳鐵磷電觸媒中各成分元素所占百分比、真實之鎳鐵元素總量。 29
表 4-2 不同金屬比例合成之鎳鐵磷電觸媒中各成分元素所占百分比、真實之鎳鐵元素總量。 34
表 4-3 不同磷濃度合成之鎳鐵磷電觸媒中各成分元素所占百分比、真實之鎳鐵元素總量。 37
表 4-4 不同電流密度合成之鎳鐵磷電觸媒的重要參數整理表。 43
表 4-5 不同金屬比例合成之鎳鐵磷電觸媒的重要參數整理表。 47
表 4-6 不同磷濃度合成之鎳鐵磷電觸媒的重要參數整理表。 52
表 A-1 不同磷濃度合成之鎳鐵磷電觸媒中各成分元素所占百分比、真實之鎳鐵元素總量。 61
表 A-2 不同磷濃度合成之鎳鐵磷電觸媒的重要參數整理表。 64










圖目錄
圖 1-1 交換電流與金屬和氫離子鍵結強度關係之火山圖[4]。 4
圖 2-1 不同的恆電流電鍍之方法:(a) 直流電沉積、(b) 脈衝電流電沉積、(c) 脈衝反向電沉積。 13
圖 2-2 PRC電鍍鎳鐵相比於DC之內應力對電流密度之關係圖[54]。 15
圖 3-1 製備SPCE電極示意圖。(a)全新之SPCE基材 (b)製備後之SPCE電極。 21
圖 3-2 三極式電化學分析系統裝置架設。 25
圖 4-1 不同電流密度合成之鎳鐵磷電觸媒SEM圖:(a) -200 mA cm-2、(b) -20 mA cm-2、(c) -2 mA cm-2、(d) -0.2 mA cm-2、(e) -0.025 mA cm-2、(f) -0.0125 mA cm-2。各電流之總電荷數:0.54 C cm-2。比例尺:500 nm。 28
圖 4-2 不同電流密度合成鎳鐵磷電觸媒之電鍍圖:(a) -200 mA cm-2、(b) -20 mA cm-2、(c) -2 mA cm-2、(d) -0.2 mA cm-2、(e) -0.025 mA cm-2、(f) -0.0125 mA cm-2。各電流之總電荷數:0.54 C cm-2。 30
圖 4-3 不同電流密度合成鎳鐵磷電觸媒之XPS圖:etching 120s。(a)(b) Ni 2p、(c)(d) Fe 2p。(i) -200 mA cm-2、(ii) -20 mA cm-2、(iii) -2 mA cm-2、(iv) -0.2 mA cm-2、(v) -0.025 mA cm-2、(vi) -0.0125 mA cm-2。 31
圖 4-4 不同電流密度合成鎳鐵磷電觸媒之XPS圖:etching 120s。(a)(b) P 2p、(c)(d) O 1s。(i) -200 mA cm-2、(ii) -20 mA cm-2、(iii) -2 mA cm-2、(iv) -0.2 mA cm-2、(v) -0.025 mA cm-2、(vi) -0.0125 mA cm-2。 32
圖 4-5 不同金屬比例之鎳鐵磷電觸媒SEM圖:(a) FeP、(b) r = 0.5、(c) r = 1、(d) r = 2、(e) r = 9、(f) NiP。比例尺:500 nm。 33
圖 4-6 不同金屬比例合成鎳鐵磷電觸媒之拉曼分析:(a) FeP、(b) r = 0.5、(c) r = 1、(d) r = 2、(e) r = 9、(f) NiP。 35
圖 4-7 (a) 不同電鍍液之LSV:(i) Ni2+ + Fe2+ + H2PO2-、(ii) Ni2+ + Fe2+、(iii) Fe2+、(iv) H2PO2-、(v) Ni2+、(vi) NH4Cl。(b) 不同金屬比例合成鎳鐵磷電觸媒之電鍍圖:(i) FeP、(ii) r = 0.5、(iii) r = 1、(iv) r = 2、(v) r = 9、(vi) NiP。 35
圖 4-8 不同磷濃度之鎳鐵磷電觸媒SEM圖:(a) 1 M、(b) 0.2 M、(c) 0.04 M、(d) 0.02 M、(e) 0 M。比例尺:500 nm。 36
圖 4-9 (a) 含磷與不含磷的電鍍液LSV:(i) FeP、(ii) r = 0.5、(iii) r = 1、(iv) r = 2、(v) r = 9、(vi) NiP、(i') Fe、(ii') r = 0.5(NiFe)、(iii') r = 1(NiFe)、(iv') r = 2(NiFe)、(v') r = 9(NiFe)、(vi') Ni。(b) 不同磷濃度之LSV:(i) 1 M、(ii) 0.2 M、(iii) 0.04 M、(iv) 0.02 M、(v) 0 M。 38
圖 4-10 (a) 不同電流密度合成鎳鐵磷電觸媒之產氫反應極化曲線。(b) 不同電流密度合成鎳鐵磷電觸媒之產氫反應穩定性。(i) -200 mA cm-2、(ii) -20 mA cm-2、(iii) -2 mA cm-2、(iv) -0.2 mA cm-2、(v) -0.025 mA cm-2、(vi) -0.0125 mA cm-2。 39
圖 4-11 在開環電位pm50 mV之電位窗範圍,以掃描速率80, 100, 200, 400, 600 mV s-1進行循環伏安法量測電雙層電容。(a) -200 mA cm-2、(b) -20 mA cm-2、(c) -2 mA cm-2、(d) -0.2 mA cm-2、(e) -0.025 mA cm-2、(f) -0.0125 mA cm-2、(g) 各電流密度條件下之電流密度差值與掃描速率關係疊圖。 41
圖 4-12 為不同電流密度合成之鎳鐵磷電觸媒Tafel plot疊圖。(a) -200 mA cm-2、(b) -20 mA cm-2、(c) -2 mA cm-2、(d) -0.2 mA cm-2、(e) -0.025 mA cm-2、(f) -0.0125 mA cm-2。 42
圖 4-13 (a) 不同金屬比例合成鎳鐵磷電觸媒之產氫反應極化曲線。(b) 不同金屬比例合成鎳鐵磷電觸媒之產氫反應穩定性。(i) FeP、(ii) r = 0.5、(iii) r = 1、(iv) r = 2、(v) r = 9、(vi) NiP。 44
圖 4-14 在開環電位pm50 mV之電位窗範圍,以掃描速率80, 100, 200, 400, 600 mV s-1進行循環伏安法量測電雙層電容。(a) FeP、(b) r = 0.5、(c) r = 1、(d) r = 2、(e) r = 9、(f) NiP、(g) 各金屬比例條件之電流密度差值與掃描速率關係疊圖。 45
圖 4-15 為不同金屬比例合成之鎳鐵磷電觸媒Tafel plot疊圖。(a) FeP、(b) r = 0.5、(c) r = 1、(d) r = 2、(e) r = 9、(f) NiP。 46
圖 4-16 (a)不同磷濃度合成鎳鐵磷電觸媒之產氫反應極化曲線。(b) 不同磷濃度合成鎳鐵磷電觸媒之產氫反應穩定性。(i) 1 M、(ii) 0.2 M、(iii) 0.04 M、(iv) 0.02 M、(v) 0 M 48
圖 4-17 在開環電位pm50 mV之電位窗範圍,以掃描速率80, 100, 200, 400, 600 mV s-1進行循環伏安法量測電雙層電容。(a) 1 M、(b) 0.2 M、(c) 0.04 M、(d) 0.02 M、(e) 0 M、(f) 各磷濃度條件之電流密度差值與掃描速率關係疊圖。 50
圖 4-18 為不同磷濃度合成之鎳鐵磷電觸媒Tafel plot疊圖。(a) 1 M、(b) 0.2 M、(c) 0.04 M、(d) 0.02 M、(e) 0 M。 51
圖 4-19 產氫活性最好條件之鎳鐵磷電觸媒XRD圖。 53
圖 A-1 不同磷濃度之鎳鐵磷電觸媒SEM圖:(a) 2 M、(b) 1 M、(c) 0.2 M、(d) 0.04 M、(e) 0.02 M、(f) 0 M。比例尺:500 nm。 61
圖 A-2 (a)不同磷濃度合成鎳鐵磷電觸媒之產氫反應極化曲線。(b) 不同磷濃度合成鎳鐵磷電觸媒之產氫反應穩定性。(i) 2 M、(ii) 1 M、(iii) 0.2 M、(iv) 0.04 M、(v) 0.02 M、(vi) 0 M M。 62
圖 A-3 在開環電位pm50 mV之電位窗範圍,以掃描速率80, 100, 200, 400, 600 mV s-1進行循環伏安法量測電雙層電容。(a) 2 M、(b) 1 M、(c) 0.2 M、(d) 0.04 M、(e) 0.02 M、(f) 0 M、(g) 各磷濃度條件之電流密度差值與掃描速率關係疊圖。 63


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