鎳基合金600 (Alloy 600)與沃斯田鐵不銹鋼316L (SS 316L)為壓水式反應器(Pressurized Water Reactor, PWR)常見的結構組件材料，然而在電廠長期運轉下，結構組件腐蝕劣化問題層出不窮，如一次側冷卻水應力腐蝕龜裂(Primary Water Stress Corrosion Cracking, PWSCC)。為減緩腐蝕問題，各國電廠對於PWR進行了適當的水化學調控，如添加氫氣、控制pH值、硼酸濃度與氫氧化鋰濃度等。添加氫氣用以降低水環境因輻射分解反應而提高的氧化性，並減緩組件材料劣化，然而在目前EPRI規範的溶氫濃度25-50 cc⁄kg H2O與運轉溫度320-360℃下，仍有PWSCC發生，因此各國核電廠考慮調整溶氫濃度至5 cc/kg H2O以下，或75 cc/kg H2O以上。此外，於水迴路中添加硼酸以控制中子反應度，添加氫氧化鋰則用於平衡水環境的pH值。但隨著燃料週期的燃耗，硼濃度逐漸下降，氫氧化鋰濃度也需有所調整。藉由溶氫(dissolved hydrogen, DH)濃度與pH值的調控，可使材料避開Ni/NiO的相轉換點，進而減緩PWSCC發生。因此本研究將探討燃料週期初期(Beginning of Cycle, BOC)與末期(End of Cycle, EOC)水環境在溶氫濃度降低至5 cc/kg H2O的條件下，對於Alloy 600與SS 316L所造成的影響。
本研究透過模擬PWR一次側水環境，對於Alloy 600與SS 316L進行慢應變速率拉伸試驗(Slow Strain Rate Test, SSRT)。實驗先將Alloy 600與SS 316L試棒進行固溶退火熱處理(SA)後，再分別進行單一階段時效處理(TT)與敏化熱處理(SEN)並預長氧化膜。而後模擬燃料週期初期與末期，在320℃與溶氫濃度為5 cc/kg H2O的水環境下進行SSRT試驗，分析材料應力腐蝕龜裂(Stress Corrosion Cracking, SCC)行為，並對於試棒破斷面與表面氧化膜形貌進行觀察與分析。實驗結果顯示，對於Alloy 600而言，TT試棒在1200 ppm B + 3.5 ppm Li溶氫條件下展現最差的機械性質，但無論是除氧或溶氫環境，Alloy 600都表現出較低的SCC敏感性。而SS 316L SEN試棒在300 ppm B + 1 ppm Li溶氫條件下的最大抗拉強度(Ultimate Tensile Strength, UTS)與降伏強度(Yield Strength, YS)表現最差，然而實驗結果顯示溶氫可有效降低SEN試棒的SCC敏感性。Alloy 600表面氧化膜主要由尖晶石氧化物(spinel oxide) NiFe2O4、Cr2O3與NiO所構成，SS 316L的表面氧化膜則以α-Fe2O3、γ-Fe2O3、尖晶石氧化物NiFe2O4與Fe3O4為主。

Ni-based Alloy 600 and 316L austenitic stainless steel are major structural component material of pressurized water reactors (PWRs). However, as the pressurized water reactors (PWRs) age, incidents of Primary Water Stress Corrosion Cracking (PWSCC) are more likely seen in the structural components. To mitigate the risk of material degradation, the water chemistry modifications of PWR including dissolved hydrogen (DH), the pH at high temperature and the concentration of boric acid and lithium hydroxide are necessary. Hydrogen is added into the primary water to maintain the reducing condition and minimize the corrosion of material. Nevertheless, the dissolved hydrogen existed in proximity to the metallic Ni to nickel oxide (NiO) phase transition would have a negative influence on the Ni-based alloy surface oxide film stability and cause stress corrosion cracking (SCC). Therefore, an alteration of dissolved hydrogen to >75 cc/kg H2O or to <5 cc/kg H2O may be beneficial. In addition, boric acid is added in the PWR primary water to control the reactivity and lithium hydroxide is used to control pH of the water environment. To avoid the Ni/NiO phase transition boundary and PWSCC, the modification of DH and pH can be adopted.
The aim of this study is to investigate the effect of lower dissolved hydrogen and B/Li concentrations on PWSCC response of Alloy 600 and SS 316L at 320 ℃ in a simulated PWR primary water environment. The SCC initiation and propagation behavior were studied via slow strain rate tensile (SSRT) tests. The detailed characterization on the morphologies and microstructure of the samples were observed by scanning electron microscopy (SEM) and Laser Raman spectrophotometer. According to the test results, the Alloy 600 TT sample tested at 1200 ppm B + 3.5 ppm Li with DH of 5 cc/kg H2O showed the worst mechanical property among the Alloy 600 tested samples. The SS 316L SEN sample tested at 300 ppm B + 1 ppm Li with DH of 5 cc/kg H2O condition showed the lower ultimate tensile strength (UTS) and yield strength (YS) among the SS 316L SEN tested samples. In addition, the mechanical performance of Alloy 600 samples was better than that of 316L samples. The oxide films of Alloy 600 samples in different conditions exhibited similar structures and were consisted of spinel oxide NiFe2O4, Cr2O3 and NiO. The oxide films of 316L SS samples in different conditions were composed of α-Fe2O3, γ-Fe2O3, spinel oxide NiFe2O4 and Fe3O4.

摘要 i
Abstract iii
目錄 v
表目錄 viii
圖目錄 x
第一章 緒論 1
1.1 前言 1
1.2 研究動機 2
第二章 文獻回顧 6
2.1 壓水式反應器結構組件材料 6
2.1.1 鎳基合金600 7
2.1.2 316L不銹鋼 8
2.2 應力腐蝕龜裂 10
2.2.1 形成要素 10
2.2.2 應力腐蝕龜裂之過程 11
2.2.3 應力腐蝕龜裂機制 13
2.2.3.1 保護膜破裂機制(Film-rupture Mechanism) 13
2.2.3.2 吸附誘發破裂相關機制 13
2.2.3.3 表面遷移機制(Surface-Mobility Mechanism) 15
2.2.3.4 膜誘發劈裂機制(Film-induced cleavage) 15
2.2.3.5 氫致破裂相關機制 16
2.2.5 應力腐蝕龜裂的影響要素 18
2.2.5.1 硼酸與氫氧化鋰濃度 18
2.2.5.2 溶氫濃度 23
2.2.5.3 合金元素 28
2.3 慢應變速率拉伸試驗 40
2.4 鎳基合金與不銹鋼的氧化膜型態 41
2.4.1 Alloy 600在高溫水環境下的氧化膜型態 41
2.4.2 SS 316L在高溫水環境下的氧化膜型態 46
2.5 拉曼散射光譜分析 52
第三章 研究方法與實驗步驟 60
3.1 實驗流程 60
3.2 試片製備 61
3.3 金相試驗 63
3.4 敏化程度測試 64
3.5 高溫高壓水循環系統 66
3.6 慢應變速率拉伸實驗 68
3.7 表面分析 69
3.7.1 掃描式電子顯微鏡(SEM) 69
3.7.2 能量散佈X光分析儀(EDS) 71
3.7.3 共軛聚焦顯微拉曼光譜儀 72
第四章 結果與討論 74
4.1 材料金相觀察 74
4.2 敏化程度測試結果 75
4.3 慢應變速率拉伸試驗結果 77
4.3.1 Alloy 600拉伸試驗結果 77
4.3.1.1燃料週期初期除氧水環境 77
4.3.1.2燃料週期初期溶氫水環境 81
4.3.1.3燃料週期末期溶氫水環境 86
4.3.1.4 Alloy 600拉伸試驗結果整理 90
4.3.2 SS 316L拉伸試驗結果 94
4.3.2.1 燃料週期初期除氧水環境 94
4.3.2.2 燃料週期初期溶氫水環境 97
4.3.2.3 燃料週期末期溶氫水環境 100
4.3.2.4 SS 316L拉伸試驗結果整理 103
4.4 表面氧化層結構與形貌觀察 107
4.4.1 Alloy 600的表面氧化層 107
4.4.2 SS 316L的表面氧化層 111
第五章 結論 115
第六章 未來工作 117
參考文獻 118

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