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研究生： 謝宜寰
Hsieh, Yi-Huan
論文名稱： 經高溫氧化之添加鎢元素鉻薄膜磨潤性能研究
Tribological performance of chromium films with tungsten doping after high temperature oxidation treatment
指導教授： 蘇演良
Su, Yan-liang
學位類別： 碩士
Master
系所名稱： 工學院 - 機械工程學系
Department of Mechanical Engineering
論文出版年： 2007
畢業學年度： 95
語文別： 中文
論文頁數： 117
中文關鍵詞： 機械性質 、氧化鎢 、氧化鉻 、非平衡磁控濺鍍
外文關鍵詞： Cr-O, mechanical properties, W-O, closed field unbalanced magnetron sputtering
相關次數： 點閱：91  下載：2 
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    • 本研究使用非平衡磁控濺鍍系統，濺鍍Cr-W鍍膜於高速鋼、矽晶片、微鑽針及捨棄式刀具。主要目的為探討添加鎢元素之鉻薄膜於高溫氧化前後之機械性質、磨潤性質及切削性能。實驗主要分為三部分：第一部分探討鎢元素含量對於Cr-W鍍層機械性質的影響；第二部分探討600 ℃ 1小時氧化處理對Cr-W鍍層機械性質的影響；第三部分探討不同溫度及時間氧化處理對Cr-W鍍層機械性質的影響；最後選用較佳鍍層進行乾車削及微鑽孔試驗，以瞭解鍍膜披覆刀具之實際工作效能。
    由實驗結果可知，Cr-W鍍層於鎢靶電流為2.0 A時，鍍層擁有最高硬度值HK25g 1650及最佳耐磨耗性。Cr-W(2.0 A)鍍層經600 ℃ 1小時氧化處理後，硬度可提升至HK25g 1820以上，且耐磨耗性及附著性亦有顯著提升，此外氧化過後鍍層之摩擦係數有明顯的下降。而在不同溫度及時間之氧化處理，則以600 ℃2小時氧化之Cr-W(2.0 A)鍍層擁有最佳之耐磨耗性及附著性。由實際切削、鑽削實驗的結果得知，高溫氧化處理之Cr-W(2.0 A)鍍層能有效降低車刀及鑽針磨耗量，可降低車刀刀腹磨耗量71 %及微鑽針刀角磨耗量63 %。

    In this study, Cr-W coatings were deposited on JIS SKH51 disks, silicon wafers, micro-drills and indexable inserts by closed field unbalanced magnetron system. The main purpose of this study is to research the mechanical and tribological properties and cutting performance of the Cr-W coatings before and after high temperature oxidation. The experiment is divided into three stages. In first stage, the effect of tungsten content on the mechanical properties of the Cr-W coatings was investigated. In second stage, the effect of one hour oxidation treatment at 600 ℃ on the mechanical properties of the Cr-W coatings was investigated. In third stage, the effect of oxidation treatment at different temperature and duration on the mechanical properties of Cr-W coatings was investigated. Finally, the actual cutting performances of the optimal coatings were understood in the turning and micro-drilling tests.
    The results reveal that the highest hardness of HK25g 1650 and the best wear resistance were performed by the Cr-W coatings with the tungsten target current of 2.0 A. The hardness of Cr-W(2.0 A) coatings after 600 ℃ and one hour oxidation treatment increased to HK25g 1820. The wear resistance and adhesion performance of the Cr-W coatings improve apparently after oxidation. The coefficient of friction of Cr-W coatings after oxidation declines obviously. The best wear resistance and adhesion were performed for Cr-W(2.0 A) coatings after 600 ℃ and two hours oxidation treatment.
    In actually turning and micro-drilling tests, the wear on Cr-W(2.0 A) coatings deposited on inserts and drills with high temperature oxidation treatment can be reduced about 71 % and 63 %, respectively.

    授權書………………………………………………………………… Ⅰ 口試合格證明書……………………………………………………… Ⅱ 摘要…………………………………………………………………… Ⅲ Abstract……………………………………………………………… Ⅳ 誌謝…………………………………………………………………… Ⅴ 總目錄 ………………………………………………………………Ⅵ 表目錄 ………………………………………………………………Ⅹ 圖目錄 ………………………………………………………………ⅩⅡ 第一章 緒論…………………………………………………………1 1-1前言…………………………………………………… 1 1-2研究動機……………………………………………… 3 第二章 理論探討與文獻回顧………………………………………4 2-1薄膜成形……………………………………………… 4 2-1-1薄膜成形技術…………………………………… 4 2-1-2薄膜成形技術的用途…………………………… 4 2-1-3薄膜成形技術的種類…………………………… 5 2-2濺鍍理論…………….…………………………………7 2-2-1直流濺鍍原理…………………………………… 7 2-2-2磁控濺鍍………………………………………… 9 2-3磨耗機構原理………………………………………… 10 2-4氧化鉻、鎢及氧化鎢鍍膜介紹……………………… 13 2-4-1氧化鉻……………………………………………… 13 2-4-2鎢及氧鎢…………………………………………… 14 第三章 實驗方法與步驟……………………………………………16 3-1實驗目的……………………………………………… 16 3-2實驗流程……………………………………………… 16 3-3實驗方法與規劃……………………………………… 17 3-3-1 濺鍍參數與鍍膜安排……………………………17 3-3-2 實驗材料…………………………………………17 3-3-3 成分分析…………………………………………18 3-3-4 結構分析…………………………………………19 3-3-5 硬度試驗…………………………………………19 3-3-6 附著性試驗………………………………………19 3-3-7 磨耗實驗…………………………………………20 3-3-8 高溫氧化實驗……………………………………21 3-3-9 車削實驗…………………………………………21 3-3-10 鑽削實驗……………………………………… 22 3-3-11 表面、斷面和磨耗型態分析………………… 23 3-4 實驗設備…………………………………………… 23 第四章 Cr-W、Cr-W-O鍍膜實驗結果與討論………………………26 4-1 Cr-W鍍膜-鎢靶電流變化對鍍膜的影響…………… 26 4-1-1鍍膜基本性質…………………………………… 26 4-1-1-1鍍膜微結構…………………………………26 4-1-1-2鍍膜表面及斷面SEM觀察………………… 26 4-1-1-3鍍膜表面之粗糙度分析……………………27 4-1-1-4鍍膜膜厚及成分分析………………………27 4-1-1-5鍍膜硬度……………………………………27 4-1-1-6基材效應對於微硬度實驗影響探討………27 4-1-2鍍膜附著性……………………………………… 28 4-1-2-1壓痕試驗……………………………………28 4-1-2-2刮痕試驗……………………………………28 4-1-3鍍膜磨潤性質…………………………………… 29 4-1-3-1 Cr-W鍍膜與AISI 1045中碳鋼圓柱對磨…29 4-1-3-2 Cr-W鍍膜與AISI 52100鉻鋼球對磨…… 29 4-1-3-3磨耗機構……………………………………30 4-1-4小結……………………………………………… 30 4-2 600 ℃持溫1小時氧化對Cr-W鍍層的影響………… 31 4-2-1鍍膜基本性質…………………………………… 31 4-2-1-1鍍膜微結構…………………………………31 4-2-1-2鍍膜之表面及斷面SEM觀察……………… 31 4-2-1-3鍍膜之表面粗糙度分析……………………32 4-2-1-4鍍膜之顏色變化及成分分析………………32 4-2-1-5鍍膜硬度……………………………………33 4-2-1-6基材效應對於微硬度實驗影響探討………33 4-2-2鍍膜附著性……………………………………… 33 4-2-2-1壓痕試驗……………………………………33 4-2-2-2刮痕試驗……………………………………33 4-2-3鍍膜磨潤性質…………………………………… 34 4-2-3-1 600 ℃持溫1小時氧化Cr-W鍍層與 AISI 1045中碳鋼圓柱對磨……………… 34 4-2-3-2 600 ℃持溫1小時氧化Cr-W鍍層與 AISI 52100鉻鋼球對磨……………………35 4-2-4小結……………………………………………… 35 4-3不同溫度氧化W20鍍膜之實驗結果與討論(I)……… 35 4-3-1鍍膜基本性質…………………………………… 36 4-3-1-1鍍膜微結構…………………………………36 4-3-1-2鍍膜之表面及斷面SEM觀察……………… 36 4-3-1-3鍍膜之顏色變化及附著情形………………36 4-3-1-4鍍膜之表面粗糙度分析……………………37 4-3-1-5鍍膜成分分析………………………………38 4-3-1-6鍍膜硬度……………………………………38 4-3-2鍍膜附著性……………………………………… 38 4-3-2-1壓痕試驗……………………………………38 4-3-2-2刮痕試驗……………………………………39 4-3-3鍍膜磨潤性質…………………………………… 39 4-3-3-1不同溫度氧化W20鍍膜與 AISI 1045中碳鋼圓柱對磨…………………39 4-3-3-2不同溫度氧化W20鍍膜 與AISI 52100鉻鋼球對磨………………… 40 4-3-4小結……………………………………………… 40 4-4不同溫度氧化W20鍍膜之實驗結果與討論(II)………40 4-4-1鍍膜基本性質…………………………………… 41 4-4-1-1鍍膜微結構…………………………………41 4-4-1-2鍍膜之表面及斷面SEM觀察……………… 41 4-4-1-3鍍膜之顏色變化及附著情形………………41 4-4-1-4鍍膜之表面粗糙度分析……………………42 4-4-1-5鍍膜成分分析………………………………42 4-4-1-6鍍膜硬度……………………………………43 4-4-2鍍膜附著性……………………………………… 43 4-4-2-1壓痕試驗……………………………………43 4-4-2-2刮痕試驗……………………………………43 4-4-3鍍膜磨潤性質…………………………………… 44 4-4-3-1不同溫度氧化W20鍍膜與 AISI 1045中碳鋼圓柱對磨……………… 44 4-4-3-2不同溫度氧化W20鍍膜 與AISI 52100鉻鋼球對磨………………… 44 4-4-4小結……………………………………………… 45 4-5乾車削實驗…………………………………………… 46 4-6 PCB微鑽削實驗……………………………………… 47 第五章 結論與未來展望……………………………………………48 5-1結論…………………………………………………… 48 5-2未來展望……………………………………………… 49 第六章 參考文獻……………………………………………………50 作者簡歷………………………………………………………………116 著作權聲明……………………………………………………………117 表目錄 Table 3-1 Deposition parameters of Cr-W coatings…………54 Table 3-2 Chemical composition (wt. %) of AISI 1045 cylinder, JIS SKH51 disk and AISI 52100 ball…54 Table 3-3 SRV wear test parameters……………………………55 Table 3-4 Oxidation experimental detail for Cr-W coatings I………………………………………………55 Table 3-5 Oxidation experimental detail for Cr-W coatings II…………………………………………… 55 Table 3-6 Oxidation experimental detail for Cr-W coatings III……………………………………………56 Table 4-1 The elemental composition of Cr-W coatings……56 Table 4-2 The effects of indentation depth on the Knoop micro-hardness of the Cr-W coatings (JIS SKH51 disk)………………………………………56 Table 4-3 Indentation fracture level of Cr-W coatings… 57 Table 4-4 Scratch test results of Cr-W coatings………… 57 Table 4-5 Estimated Cr-W coatings adhesion properties by scratch test……………………………………………57 Table 4-6 The elemental composition of Cr-W coatings after oxidation treatment (600 ℃ 60 min)…… 58 Table 4-7 The effects of indentation depth on the Knoop micro-hardness of the Cr-W coatings after oxidation treatment (600 ℃ 60 min) (JIS SKH51 disk)…………………58 Table 4-8 Indentation fracture level of Cr-W coatings (after oxidation treatment 600 ℃ 60 min)…… 58 Table 4-9 Scratch test results about Cr-W coatings (after oxidation treatment 600℃ 60 min)………59 Table 4-10 Estimated Cr-W coatings adhesion properties by scratch test (after oxidation treatment 600 ℃ 60 min)……59 Table 4-11 EDS analysis result of Cr-W coatings after oxidation treatment (different temperature and duration) (JIS SKH51 disk)…………………………………… 60 Table 4-12 The effects of indentation depth on the Knoop micro-hardness test of the Cr-W coatings after oxidation treatment (different temperature and duration) (JIS SKH51 disk)…………………………………… 60 Table 4-13 Indentation fracture level of Cr-W coatings after oxidation treatment (different temperature and duration)………… 60 Table 4-14 Scratch test results of Cr-W coatings on JIS SKH51 disk after oxidation treatment (different temperature and duration)………… 61 Table 4-15 Estimated Cr-W coatings adhesion properties by scratch test Cr-W coated on JIS SKH51 disk after oxidation treatment (different temperature and duration)………… 61 Table 4-16 Color of Cr-W coatings after oxidation treatment (different temperature) (JIS SKH51 disk)…………………………………… 61 Table 4-17 EDS analysis result of Cr-W coatings after oxidation treatment (different temperature) (JIS SKH51 disk)…………………………………… 62 Table 4-18 The effects of indentation depth on the Knoop micro-hardness of the Cr-W coatings after oxidation treatment (different temperature) (JIS SKH51 disk)…… 62 Table 4-19 Indentation fracture level of Cr-W coatings after oxidation treatment (different temperature)……………………………62 Table 4-20 Scratch test results of Cr-W coatings after oxidation treatment (different temperature)…63 Table 4-21 Estimated Cr-W coatings adhesion properties by scratch test Cr-W coated on JIS SKH51 disk after oxidation treatment (different temperature)……………………………63 圖目錄 圖2-1 薄膜形成技術種類……………………………………………64 圖2-2 典型直流鍍膜系統構造示意圖… 65 圖2-3 輝光放電示意圖...………………………………………… 65 圖2-4 傳統磁控與非平衡磁控濺鍍示意圖…………………………66 圖2-5 由硬顆粒或突出強行在固體表面移動所致的磨粒磨耗 (Abrasion)示意圖……………………………………………66 圖2-6 由於固體被磨面受到流動或沖激液漿的機械作用造成材料 的沖蝕磨耗(Erosion)示意圖……………………………… 67 圖2-7 由於固體被磨材與對磨材之間相對運動產生局部鍵結 (Local Bonding)所致的黏著磨耗(Adhesion)示意圖…… 67 圖2-8 起因於周期性滾動或滑動產生的表面疲勞 (Surface Fatigue)示意圖………………………………… 67 圖2-9 Cr-O溫度與壓力關係圖………………………………………68 圖3-1 實驗流程………………………………………………………69 圖3-2 KD-550U封閉式非平衡磁控濺鍍系統(主腔體)…………… 70 圖3-3 KD-550U封閉式非平衡磁控濺鍍系統(控制系統)………… 70 圖3-4 KD-550U封閉式非平衡磁控濺鍍系統 (腔體內部構造示意圖)……………………………………… 71 圖3-5 壓痕破裂型態示意圖…………………………………………71 圖3-6 刮痕測試機台示意圖…………………………………………72 圖3-7 (a) SRV磨耗測試機 (b) 上試件夾具 (c) 下試件磨痕類型…………………………………………73 圖3-8 車刀磨耗型態及切削性能評估準則示意圖…………………74 圖3-9 PWB微鑽孔實驗示意圖 (a) 實驗架構示意圖 (b) 實驗參數……………………… 75 圖3-10 FR-4雙面板之單層疊構圖………………………………… 76 圖3-11 微鑽針磨耗評估準則……………………………………… 76 圖4-1 Cr-W鍍膜之XRD繞射圖……………………………………… 77 圖4-2 Cr-W鍍膜之表面與斷面SEM圖……………………………… 78 圖4-3 Cr-W鍍膜之表面粗糙度比較圖………………………………80 圖4-4 Cr-W鍍膜之元素含量與厚度圖 (EDS分析)…………………80 圖4-5 鎢含量與Cr-W鍍膜硬度的關係 (JIS SKH51基材)…………81 圖4-6 Cr-W鍍膜之刮痕深度及摩擦係數圖(40處)…………………81 圖4-7 Cr-W鍍膜之SRV線磨耗試驗結果 (12分鐘) (a) 50 N, (b) 100 N……………………………………… 82 圖4-8 Cr-W鍍膜之SRV點磨耗試驗結果 (2分鐘) (Load =10 N)…83 圖4-9 W20鍍膜表面磨痕形貌(與AISI 1045對磨-線磨) (時間：12 min ; Stroke：0.5 mm；Load：100 N)………84 圖4-10 AISI 1045圓柱表面磨痕形貌(與W20對磨-線磨) (時間：12 min ; Stroke：0.5 mm；Load：100 N)………85 圖4-11 600 ℃ 1小時氧化Cr-W鍍膜XRD繞射結果…………………86 圖4-12 600 ℃ 1小時氧化Cr-W鍍膜表面及斷面SEM圖……………87 圖4-13 原材及600 ℃ 1小時氧化Cr-W鍍膜之表面粗糙度比較圖 89 圖4-14 600 ℃ 1小時氧化Cr-W鍍膜之表面顏色觀察…………… 89 圖4-15 利用GDS分析不同鎢含量鍍膜之氧化深度(600 ℃ 1小時)90 圖4-16 原材及600 ℃ 1小時氧化Cr-W鍍膜硬度值……………… 90 圖4-17 原材及600 ℃ 1小時氧化Cr-W鍍膜之 刮痕摩擦係數圖(40 N)…………………………………… 91 圖4-18 600 ℃ 1小時氧化Cr-W鍍層SRV線磨耗試驗結果 (12分鐘) (a) 50 N, (b) 100 N………………………………………92 圖4-19 600 ℃ 1小時氧化Cr-W鍍層SRV點磨耗試驗結果(10N) (時間：2 min ; Stroke：0.2 mm)……………………… 93 圖4-20 600 ℃ 1小時氧化Cr-W鍍層SRV點磨耗試驗結果(10N) (時間：6 min ; Stroke：0.5 mm)……………………… 93 圖4-21 不同溫度氧化W20鍍膜之XRD繞射結果-I………………… 94 圖4-22 不同溫度氧化W20鍍膜之SEM圖-I………………………… 95 圖4-23 不同溫度氧化W20鍍膜之表面顏色觀察-I…………………97 圖4-24 不同溫度氧化W20鍍膜之表面粗糙度比較圖-I……………98 圖4-25 利用GDS分析不同溫度氧化W20鍍層之氧化深度-I……… 98 圖4-26 不同溫度氧化W20鍍膜之硬度值-I…………………………99 圖4-27 不同溫度氧化W20鍍膜之刮痕摩擦係數圖-I (40N處)……99 圖4-28 不同溫度氧化W20鍍膜之SRV線磨耗結果-I (12分鐘) (Load=100 N)..…………………………………………… 100 圖4-29 不同溫度氧化W20鍍膜之SRV點磨耗結果-I (10 N) (時間：6 min ; Stroke：0.5 mm)……………………… 100 圖4-30 不同溫度氧化W20鍍膜之XRD繞射結果-II…………………101 圖4-31 不同溫度氧化W20鍍膜之SEM圖-II…………………………102 圖4-32 不同溫度氧化W20鍍膜之表面顏色觀察-II……………… 104 圖4-33 不同溫度氧化W20鍍膜之表面粗糙度比較圖-II………… 105 圖4-34 利用GDS分析不同溫度氧化W20鍍膜之氧化深度-II………105 圖4-35 不同溫度氧化W20鍍膜之硬度值-II……………………… 106 圖4-36 不同溫度氧化W20鍍膜之刮痕摩擦係數圖-II (40 N處)…106 圖4-37 不同溫度氧化W20鍍膜之SRV線磨耗結果-II (12分鐘) (Load=100 N)…..………………………………………… 107 圖4-38 不同溫度氧化W20鍍膜之SRV點磨耗結果-II (10 N) (時間：6 min ; Stroke：0.5 mm)……………………… 107 圖4-39 車削實驗結果……………………………………………… 108 圖4-40 車刀刀腹磨耗圖(利用光學顯微鏡觀察)………………… 109 圖4-41 HT6-2鍍膜披覆於車刀之刀腹磨耗SEM圖………………… 111 圖4-42 鑽削實驗結果……………………………………………… 112 圖4-43 鑽針刀角及刀腹磨耗SEM圖…………………………………113 圖4-44 HT6-2鍍膜披覆於微鑽針之磨耗SEM圖…………………… 115

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