本研究的目的是討論中空陰極離子鍍著(HCD-IP)系統和非平衡磁控濺鍍(UBMS)系統鍍著之氮化鋯薄膜對於抵抗充氫的能力。首先，使用兩種鍍膜系統鍍著氮化鋯薄膜於與鋯四合金上，接著分別將鍍膜樣品與作為對照組的無鍍膜樣品在65℃的1 M的硫酸水溶液中施以-120 mA/cm2電流進行陰極充氫法48小時，在此期間氫氣會擴散進去與鋯四合金反應生成氫化鋯，由X光繞射圖顯示，無鍍膜與UBMS系統鍍著氮化鋯的鋯四樣品均有ZrH1.66相產生，但HCD-IP系統鍍著氮化鋯的鋯四樣品仍只有α-Zr相。使用氫化鋯選擇性蝕刻液對樣品橫截面蝕刻後，觀察到對照組與UBMS系統鍍著氮化鋯的鋯四樣品均有產生表面氫化鋯層被蝕刻後的形貌，氫化鋯層厚度分別為有9 μm和6 μm ，而HCD-IP系統鍍著氮化鋯的鋯四樣品僅有觀察到氫化鋯條零星分佈，接著對充氫完畢的樣品進行均質化熱處理，獲得氫化鋯均勻分布基材內部的鋯四樣品，以氫分析儀分析後得到對照組、UBMS系統鍍著氮化鋯的鋯四樣品和HCD-IP系統鍍著氮化鋯的鋯四樣品氫含量分別為271 ± 19 ppm、212 ± 17 ppm 和 36 ± 5 ppm；從此結果了解到兩系統鍍膜樣品針對氫進入阻隔能力有明顯的差異，造成該差異的主要原因推測是兩系統在鍍著氮化鋯薄膜時離化率的不同，產生的離子轟擊效應造成氮化鋯薄膜層有不同的點缺陷密度，而點缺陷作為氫陷阱捕捉的氫含量不同造成的。

The purpose of this study is to discuss the ability to resist hydrogen charging of zirconium nitride films plated by the hollow cathode ion plating (HCD-IP) system and the unbalanced magnetron sputtering (UBMS) system. First, zirconium nitride films were deposited on Zircaloy-4 substrate using hollow cathode ion plating (HCD-IP) system and unbalanced magnetron sputtering (UBMS) system, and then the coated samples and the uncoated sample as a control group were subjected to cathodic hydrogen charging in 1 M sulfuric acid solution, solution temperature 65°C with a current of -120 mA/cm2 for 48 hours. Hydrogen diffused in and react with the Zircaloy-4 to precipitate zirconium hydride. The X-ray diffraction pattern shows that the uncoated samples and zirconium nitride coated sample by UBMS system all have ZrH1.66 phase, but the coated sample by HCD-IP system didn't and it still only has α-Zr phase. After etching the cross-section of the samples with the selective zirconium etching solution, it was observed that both the control group and the coated samples by UBMS system has a morphology of etched zirconium hydride layer, and the thickness of the zirconium hydride layer was 9 μm and 6 μm, respectively. The coated samples by HCD-IP system were only observed to have scattered zirconium hydride strips. Then the sample is homogenized by heat treatment after hydrogen charging. The zirconium tetra samples with uniform distribution of zirconium nitride inside the substrate were obtained. The hydrogen content analysis of the control group, the coated sample by UBMS and HCD-IP systems were 271 ± 19 ppm, 212 ± 17 ppm and 36 ± 5 ppm, respectively. From this result, it is understood that the coating samples of the two systems have obvious differences in the barrier ability of hydrogen entry. The main reason for this difference is presumed to be the difference in the ionization rate of the two systems when they are coated with zirconium nitride films. The ion peening effect causes the zirconium nitride film layer to have different point defect densities. The point defects are caused by the difference in the amount of hydrogen captured by the hydrogen traps.

致謝 i
摘要 ii
Abstract iii
目錄 v
圖目錄 ix
表目錄 xi
Chapter 1 緒論 1
Chapter 2 文獻回顧 3
2.1 鋯的晶體結構 3
2.2 氫對鋯合金的影響 3
2.2.1 氫化鋯的特性 3
2.2.2 氫化物對於鋯合金機械性質影響 5
2.3 充氫技術 6
2.3.1 陰極充氫法 7
2.3.2 均質化熱處理 9
2.4 鍍膜技術以及氮化鋯薄膜性質 10
2.4.1 非平衡磁控濺鍍系統 (UBMS) 10
2.4.2 中空陰極離子鍍著系統 (HCD-IP) 11
2.4.3 氮化鋯薄膜 12
Chapter 3 實驗原理與方法 14
3.1 樣品製備 14
3.2 鍍膜程序 15
3.3 鋯四合金充氫 19
3.3.1 充氫樣品製備 19
3.3.2 陰極充氫法 20
3.3.3 均質化熱處理 21
3.4 充氫處理前後鋯四合金的極圖 23
3.5 特性 23
3.5.1 X光繞射儀(XRD) 23
3.5.2 場發射型掃描式電子顯微鏡 (FEG-SEM) 24
3.5.3 X光光電子能譜儀 (XPS) 24
3.5.4 聚焦離子束顯微鏡 (FIB) 25
3.6 性質 25
3.6.1 電阻率 25
3.6.2 硬度與楊氏膜數 26
3.6.3 殘餘應力 26
3.7 充氫樣品氫量測與表面形貌 27
3.7.1 氫分析儀 27
3.7.2 氫化鋯微結構觀察 27
Chapter 4 結果 29
4.1 預充氫樣品的結構 29
4.2 結構與成分 33
4.2.1 X光繞射與低掠角X光繞射 35
4.2.2 掃描式電子顯微鏡與聚焦離子束顯微鏡 38
4.2.3 X光光電子能譜儀 39
4.3 性質 40
4.3.1 電阻率 40
4.3.2 硬度和楊氏膜數 40
4.3.3 殘餘應力 41
4.4 充氫試片氫含量分析 42
4.4.1 氫化鋯層厚度 42
4.4.2 氫化鋯表面形貌 43
4.4.3 氫分析 46
Chapter 5 討論 48
5.1 預鍍著的ZrN薄膜性質 48
5.1.1 HCD-IP系統與UBMS系統薄膜性質差異 48
5.2 陰極充氫法對鋯合金樣品的影響 48
5.2.1 未鍍膜對照樣品 48
5.2.2 HCD-IP系統製備氮化鋯薄膜ZBxx 和ZCxx 系列樣品 49
5.2.3 UBMS系統製備氮化鋯薄膜樣品ZUH0 系列樣品 51
5.2.4 薄膜抵抗充氫機制 54
5.3 含氫量預測 56
Chapter 6 結論 58
References 59
附錄一 各氫含量對應的氫化表面形貌 65
附錄二 二次離子質譜分析儀(SIMS)縱深成分分析 68
附錄三 熱處理時間 70
附錄四 預充氫含量對於鋯四合金在室溫硫酸與鹽水環境中之腐蝕行為影響 73

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