臺灣博碩士論文加值系統

Unimax是一種由電渣重熔(Electro-slag Remelting, ESR)製造的鉻鉬釩合金工具鋼，具有高延展性和高硬度的出色特性，降低循環時間和延長工具壽命有助於提高整體經濟效益。氮氧化(Oxynitriding, ONC®️)是一種表面處理技術，可以讓氮氣和氧氣滲透基材，同時結合了氮化處理和氧化處理的優勢；其中最外層形成氧化物層(Fe3O4)，增強基材的耐腐蝕性，而內層為滲入較深的氮，則形成氮化物層(Fe3N)，能提高基材的硬度和表面機械性質。此外，在基材表面形成中介層，可以提高鍍膜的附著性。氮化鉻(CrN)鍍層因其低密度、高熔點、耐磨性、耐腐蝕性和高溫氧化性能等特點而廣泛應用於工具及模具等表面強化處理。此外，添加第三元素如Si或Al進入CrN形成二元化合物可以出改善其機械和摩擦性能，因此氮化鉻矽(CrSiN)塗層不僅增強了耐腐蝕性，還提高了硬度和耐磨性，進而提高了基材的效能。本研究結合氮氧化處理與CrSiN鍍層於Unimax工具鋼上進行表面複合處理，藉以延長使用壽命，以及Unimax工具鋼的各項性能。

本研究是利用物理氣相沉積(PVD)的磁控濺鍍法，將CrSiN鍍層沉積在經氮氧化處理後的Unimax工具鋼上。本實驗有三個階段，第一階段實驗改變基板溫度，分別為 200、225、250及275℃；第二階段選用第一階段最佳參數，並改變沉積時間，分別為 1.5、2、2.5及3 h；第三階段則評估CrSi/CrSiN雙層鍍層、CrSiN鍍層、氮氧化之Unimax工具鋼以及未經處理的Unimax工具鋼之差異。此外，本研究藉由磨耗試驗、奈米壓痕、極化腐蝕及附著性等實驗以評估鍍層之性質，並使用低掠角薄膜繞射、AFM、SEM、EDS與穿透式電子顯微鏡等儀器，以進行成分與結構之分析。

研究結果顯示Unimax工具鋼在經過氮氧化處理後，可以形成有效之氮氧化層，深度大約為40 μm，透過此氮氧化層可將表面硬度提升至1050 HV0.05。另一方面，經過實驗分析後，本實驗製備之CrSiN鍍層之最佳參數是預濺鍍10分鐘的CrSi/CrSiN雙層鍍層，其中Ar/N2比例45/30 sccm，基材偏壓-50 V，功率為100 W，沉積時間為2.5小時，腔體壓力1.2 Pa，溫度250℃。在此條件下製備之CrSiN鍍層，具有明顯的柱狀晶結構和最佳之耐磨耗性(荷重5 N下之體積損失量為1.49×10-4 mm3和體積損失率為5.18×10-8 mm3·m-1·N-1)，以及良好之耐腐蝕性(3.5 wt% NaCl環境下，腐蝕電流Icorr = 5.23×10-6 A·cm-2，腐蝕阻抗Rp = 782.88 Ω·cm2)。根據以上之分析結果，經過氮氧化處理以及CrSiN鍍層後之Unimax工具鋼，確實可延長其使用壽命以及有效提升各項性能表現。

Unimax is a chromium-molybdenum-vanadium alloyed tool steel remelted by Electro- slag Remelting, which features an excellent combination of high ductility and high hardness, reduces cycle times, and extends tool life to improve overall economic efficiency. Oxynitriding (ONC®️ ) is a surface treatment technology that facilitates the infiltration of nitrogen and oxygen into the substrate, thus, combining the advantages of nitriding and oxidation treatments. The outermost layer forms an oxide layer (Fe3O4 ), which enhances the corrosion resistance of the substrate, while the deeper nitrogen infiltration forms a nitride layer (Fe3N) to improve the hardness and surface mechanical properties of the substrate. Additionally, an intermediate layer is formed on the substrate surface, thus, enhancing the adhesion of thin films. Due to its characteristics of low density, high melting point, wear resistance, corrosion resistance, and high-temperature oxidation resistance, chromium nitride coating (CrN) is widely used for surface enhancement treatments in tools, molds, and other applications. The addition of a third element, such as Si or Al into the CrN binary compound, has been shown to improve its mechanical and tribological properties. As a result, the CrSiN coating enhances corrosion resistance and improves hardness and wear resistance, thus, enhancing the efficacy of the substrate. This study integrates the ONC®️ treatment with a CrSiN coating on Unimax tool steel for duplex surface treatment, which aims to prolong its lifespan and enhance the various properties of Unimax tool steel.

This study utilizes the magnetron sputtering process of physical vapor deposition (PVD) to deposit CrSiN coatings onto Unimax tool steel after the nitrogen oxidation treatment. The experiment consists of three stages. In the first stage, the substrate temperature is varied at 200, 225, 250, and 275°C. In the second stage, the optimal parameters from the first stage are selected, and the deposition time is varied at 1.5, 2, 2.5, and 3 hours. The third stage evaluates the differences between CrSi/CrSiN multilayer coatings, CrSiN coatings, nitrogen-oxidized Unimax tool steel, and untreated Unimax tool steel. Additionally, the properties of the coatings are evaluated through wear tests, nanoindentation, polarization corrosion tests, and adhesion experiments. Instrumental analyses, including low-angle thin film X-ray diffraction (GIXRD), AFM, SEM, EDS, and TEM, are conducted to analyze the composition and structure.

The experimental results show that after the oxynitriding treatment, the Unimax tool steel formed an oxynitriding layer with a thickness of approximately 40 μm, while the surface hardness increased to about 1050 HV 0.05 . According to experimental analysis, the optimal parameter for the CrSiN coating prepared in
this experiment is a CrSi/CrSiN multilayer coating pre-sputtered for 10 minutes. Among them, Ar/N2 ratio of 45/30 sccm, substrate bias of -50 V, power of 100 W, deposition time of 2.5 hours, chamber pressure of 1.2 Pa, and temperature of 250°C. The CrSiN coating prepared under these conditions exhibits a distinct columnar crystal structure and optimal wear resistance (volume loss of 1.49×10-4 mm3 and volume loss rate of 5.2×10-8 mm3·m-1·N-1 under a load of 5 N), as well as good corrosion resistance (corrosion current Icorr = 3.28×10-5 A·cm-2 and corrosion resistance Rp = 793.18 Ω·cm2 in a 3.5 wt% NaCl environment). Based on the analysis results, Unimax tool steel treated with oxynitriding and coated with CrSiN can indeed prolong its service life and effectively enhance various performance characteristics.

目錄

摘要 i
ABSTRACT iii
致謝 v
目錄 vi
表目錄 ix
圖目錄 x
第一章 緒論 1
1.1 前言 1
1.2 研究目的與動機 2
1.3 研究簡介 2
2 第二章 文獻回顧 3
2.1 工具鋼(Tool steel) 3
2.1.1 碳工具鋼 3
2.1.2 合金工具鋼 3
2.1.3 高速鋼 3
2.1.4 Unimax工具鋼 4
2.2 表面處理工程(Surface Treatment Engineering) 5
2.2.1 氮化處理(Nitriding) 6
2.2.2 氧化處理(Oxidation) 7
2.2.3 氮氧化處理(Oxynitriding, ONC®) 7
2.3 物理氣相沉積法(PVD, Physical Vapor Deposition) 7
2.3.1 物理氣相沉積法之種基本原理與種類 8
2.3.2 磁控濺鍍(Magnetron Sputtering) 8
2.4 薄膜生長機制(Modes of thin-film growth) 9
2.4.1 氮化鉻矽鍍層(CrSiN, Chromium-Silicon Nitride) 10
2.4.2 CrSiN鍍層結構 10
2.4.3 CrSiN鍍層之性能特點 11
2.5 鍍層性質分析 11
2.5.1 腐蝕(Corrosion) 11
2.5.2 磨損機制(Wear mechanisms) 12
2.5.3 接觸角(Contact Angle) 14
3 第三章 研究流程與方法 16
3.1 實驗步驟與流程 16
3.1.1 試片準備及該製程參數 18
3.1.2 氮氧化(ONC®)表面處理 19
3.1.3 直流磁控濺鍍法製備CrSiN鍍層 20
3.2 鍍層性質檢測 21
3.2.1 金相顯微結構觀察 22
3.2.2 表面硬度量測 22
3.2.3 X-ray繞射分析 23
3.2.4 壓痕試驗 24
3.2.5 表面粗糙度測試 25
3.2.6 磨耗試驗 26
3.2.7 極化腐蝕試驗 27
3.2.8 水接觸角分析 28
3.2.9 顯微結構及成分分析 28
3.2.10 原子力顯微鏡分析 29
3.2.11 奈米壓痕 30
3.2.12 穿透式電子顯微鏡分析 31
4 第四章 結果與討論 33
4.1 Unimax工具鋼氮氧化處理性質分析 33
4.1.1 Unimax工具鋼氮氧化處理之XRD分析 33
4.1.2 氮氧化處理後縱深硬度分析 34
4.1.3 氮氧化處理之OM觀察 35
4.2 第一階段-不同之基板溫度對氮化鉻矽鍍層的影響 36
4.2.1 第一階段鍍層XRD分析 36
4.2.2 第一階段鍍層表面SEM與EDS分析 37
4.2.3 第一階段鍍層表面粗糙度AFM分析 39
4.2.4 第一階段鍍層水接觸角分析 41
4.2.5 第一階段鍍層橫截面FESEM分析 42
4.2.6 第一階段鍍層壓痕試驗 43
4.2.7 第一階段磨耗試驗 44
4.2.8 第一階段動態電位極化腐蝕試驗 49
4.2.9 第一階段硬度、彈性模數 50
4.2.10 第一階段小結 52
4.3 第二階段-不同之沉積時間對氮化鉻矽鍍層的影響 52
4.3.1 第二階段分析XRD分析 52
4.3.2 第二階段鍍層表面SEM分析 53
4.3.3 第二階段鍍層表面粗糙度AFM分析 55
4.3.4 第二階段鍍層水接觸角分析 56
4.3.5 第二階段鍍層橫截面分析 57
4.3.6 第二階段鍍層壓痕試驗 58
4.3.7 第二階段磨耗試驗 59
4.3.8 第二階段動態電位極化腐蝕試驗 64
4.3.9 第二階段硬度、彈性模數 65
4.3.10 第二階段小結 67
4.4 第三階段-不同表面處理之比較 67
4.4.1 第三階段硬度 68
4.4.2 第三階段磨耗試驗 68
4.4.3 第三階段動態電位極化腐蝕試驗 71
4.5 最佳參數鍍層之TEM分析 72
5 第五章 結論 75
6 參考文獻 77

表目錄
表3.1 第一階直流磁控濺鍍法製程參數 17
表3.2 第二階直流磁控濺鍍法製程參數 18
表3.3 第三階段直流磁控濺鍍法製程參數 18
表3.3 Unimax工具鋼組成成分(wt%) 19
表4.1 不同基板溫度之CrSiN鍍層元素含量(含氮原子, at%) 39
表4.2 不同基板溫度之CrSiN鍍層元素含量(不含氮原子, at%) 39
表4.3 不同基板溫度之CrSiN鍍層低荷重(3 N)磨耗測試總表 48
表4.4 不同基板溫度之CrSiN鍍層高荷重(5 N)磨耗測試總表 49
表4.5 不同基板溫度之CrSiN鍍層極化腐蝕電流密度、電位及阻抗 50
表4.6 不同基板溫度之CrSiN鍍層硬度、彈性模數、H/E及H3/E2數據 51
表4.7 不同沉積時間之CrSiN鍍層低荷重(3 N)磨耗測試總表 64
表4.8 不同沉積時間之CrSiN鍍層高荷重(5 N)磨耗測試總表 64
表4.9 不同沉積時間之CrSiN鍍層極化腐蝕電流密度、電位及阻抗 65
表4.10 不同沉積時間之CrSiN鍍層硬度、彈性模數、H/E及H3/E2數據 66
表4.11不同表面處理之CrSiN鍍層高荷重(5 N)磨耗測試總表 70
表4.12 不同表面處理之CrSiN鍍層極化腐蝕電流密度、電位及阻抗 72
圖目錄
圖2.1 Fe-Cr相圖[5] 4
圖2.2 Fe-Mo相圖[6] 5
圖2.3 Fe-V相圖[7] 5
圖2.4薄膜生長機制的三種模式[16] 10
圖2.5 液滴接觸角之示意圖[23] 14
圖3.1 實驗流程圖 17
圖3.2 Unimax工具鋼試片示意圖 19
圖3.3 Nitrex公司氣體氮化爐 19
圖3.4 Unimax工具鋼氮氧化處理升溫曲線圖 20
圖3.5 LT-PVD400機台 21
圖3.6 LT-PVD400機台示意圖 21
圖3.7 Nikon-ECLIPSE-LV150N光學顯微鏡 22
圖3.8 硬度量測方法示意圖 23
圖3.9 MATSUZAWA MMT-X微小維氏硬度機 23
圖3.10 BRUKER D8A25 XRD分析儀 24
圖3.11 壓痕試驗之附著力分級標準[26] 25
圖3.12 INDENTEC洛氏硬度機 25
圖3.13 KOSAKA SE300精密型表面粗度儀 26
圖3.14 POD-FM800-25NT磨耗試驗機 27
圖3.15 磨耗試驗示意圖 27
圖3.16 動態電位極化腐蝕儀器 28
圖3.17 Sindatek Model 100SB接觸角量測儀 28
圖3.18 JEOL-JSM6510-LV電子顯微鏡 29
圖3.19 Park XE-100 AFM機台 30
圖3.20 Bruker INNOVA SPM機台 30
圖3.21 TI-950奈米壓痕試驗機 31
圖3.22 FEI Tecnai G2 F20 TEM機台 32
圖4.1 Unimax工具鋼經氮氧化處理後之XRD分析 34
圖4.2 Unimax工具鋼經氮氧化處理後之縱深硬度圖 35
圖4.3 Unimax工具鋼經氮氧化處理後之橫截面OM圖(500X) 36
圖4.4 不同基板溫度之CrSiN鍍層的XRD分析 37
圖4.5 不同基板溫度之CrSiN鍍層表面SEM圖(1000X) 38
圖4.6 不同基板溫度之CrSiN鍍層表面SEM圖(5000X) 38
圖4.7 不同基板溫度之CrSiN鍍層表面AFM觀察 40
圖4.8 不同基板溫度之CrSiN鍍層表面AFM分析 40
圖4.9 不同基板溫度之CrSiN鍍層的水接觸角分析 41
圖4.10 不同基板溫度之CrSiN鍍層橫截面FESEM圖(10000X) 42
圖4.11 不同基板溫度之CrSiN鍍層壓痕試驗後的SEM觀察(100X) 43
圖4.12 不同基板溫度之CrSiN鍍層的磨耗數據比較圖 44
圖4.13 不同基板溫度之CrSiN鍍層低荷重(3 N)磨耗試驗後之SEM觀察(100X) 45
圖4.14 不同基板溫度之CrSiN鍍層低荷重(3 N)磨耗試驗後之SEM觀察(500X) 46
圖4.15 不同基板溫度之CrSiN鍍層高荷重(5 N)磨耗試驗後之SEM觀察(100X) 47
圖4.16 不同基板溫度之CrSiN鍍層高荷重(5 N)磨耗試驗後之SEM觀察(500X) 47
圖4.17 不同基板溫度之CrSiN鍍層經磨耗試驗後之摩擦係數比較圖 48
圖4.18 不同基板溫度之CrSiN鍍層極化腐蝕曲線圖 50
圖4.19 不同基板溫度之CrSiN鍍層硬度(H)及彈性模數(E) 51
圖4.20 不同沉積時間之CrSiN鍍層的XRD分析 53
圖4.21 不同沉積時間之CrSiN鍍層表面形貌SEM觀察(1000X) 54
圖4.22 不同沉積時間之CrSiN鍍層表面形貌SEM觀察(5000X) 54
圖4.23 不同沉積時間之CrSiN鍍層表面AFM觀察 55
圖4.24 不同沉積時間之CrSiN鍍層表面AFM分析 56
圖4.25 不同沉積時間之CrSiN鍍層的水接觸角分析 56
圖4.26 不同沉積時間之CrSiN鍍層橫截面之FESEM圖(10000X) 57
圖4.27 不同沉積時間之CrSiN鍍層壓痕試驗後之SEM觀察(100X) 58
圖4.28 不同沉積時間之CrSiN鍍層的磨耗數據比較圖 59
圖4.29 不同沉積時間之CrSiN鍍層低荷重(3 N)磨耗試驗後之SEM觀察(100X) 60
圖4.30 不同沉積時間之CrSiN鍍層低荷重(3 N)磨耗試驗後之SEM觀察(500X) 61
圖4.31 不同沉積時間之CrSiN鍍層高荷重(5 N)磨耗試驗後之SEM觀察(100X) 62
圖4.32 不同沉積時間之CrSiN鍍層高荷重(5 N)磨耗試驗後之SEM觀察(500X) 62
圖4.33 不同沉積時間之CrSiN鍍層經磨耗試驗後之摩擦係數比較圖 63
圖4.34 不同沉積時間之CrSiN鍍層極化腐蝕曲線圖 65
圖4.35 不同沉積時間之CrSiN鍍層硬度(H)及彈性模數(E) 66
圖4.36 不同表面處理之Unimax工具鋼硬度比較圖 68
圖4.37 不同表面處理之Unimax工具鋼高荷重(5 N)磨耗數據比較圖 69
圖4.38 不同表面處理之Unimax工具鋼高荷重(5 N)磨耗試驗後之摩擦係數比較圖 70
圖4.39 不同表面處理之Unimax工具鋼極化腐蝕試驗曲線圖 71
圖4.40 最佳參數之CrSiN鍍層橫截面之Bright Field與SAED圖 72
圖4.41 最佳參數之CrSiN鍍層HR-TEM圖 73
圖4.42 最佳參數之CrSiN鍍層HR-TEM圖 74 

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