反應式射頻磁控濺鍍法製備 AlCrNbSiTi 高熵氮化物薄膜及其性質之研究

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研究生：	王孟琪 Wang, Meng-Chi
論文名稱：	反應式射頻磁控濺鍍法製備 AlCrNbSiTi 高熵氮化物薄膜及其性質之研究 High-entropy Nitride Films of AlCrNbSiTi Alloy by RF Reactive Magnetron Sputtering
指導教授：	林樹均 Lin, Su-Jien
口試委員:	洪建龍陳盈潔李勝隆
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2019
畢業學年度：	107
語文別：	中文
論文頁數：	238
中文關鍵詞：	反應式射頻磁控濺鍍法、AlCrNbSiTi 、高熵、氮化物、薄膜
外文關鍵詞：	High-entropy, Nitride Films, AlCrNbSiTi, RF Reactive Magnetron Sputtering, Reactive Magnetron Sputtering
相關次數：	點閱：2 下載：0
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本研究將以往實驗室製備之最佳合金成分 AlCrSiTi 增添耐火元素 Nb，利用真空電弧熔煉製備非等莫耳AlCrSiTiNb 多元合金靶材，以反應式射頻磁控濺鍍法鍍製高熵氮化物薄膜。藉由硬度、楊氏模數及氧化層厚度計算出薄膜之綜合性質(H^3/(x^2×E^2 )) 值，以此綜合性質作為薄膜性質之評估。在氮氣流率、基板偏壓及基板溫度變量下，得到兩種最佳製程參數N40 及N50，前者硬度為21 GPa，在1000 ˚C 持溫2 小時爐冷的氧化層厚度為90 nm，空冷的氧化層厚度為 99 nm ; 後者硬度為20 GPa，在1000 ˚C 持溫2 小時爐冷的氧化層厚度僅82 nm，空冷的氧化層厚度也僅有97 nm。在附著性及磨耗測試中加入三種不同中間層，分別為自身合金中間層、純Cr 中間層及純Ti 中間層，皆對薄膜性質有不同程度的提升。在銑削試驗中以 N40 加入純Cr 中間層的最大刀腹磨耗表現最為出色，在低速切削試驗中，最大刀腹磨耗僅有100 μm，平均刀腹磨耗為74 μm；在高速切削試驗中，最大刀腹磨耗僅有99 μm，平均刀腹磨耗為76 μm；表現皆優於商用TiN、TiAlN 及TiAlCrN 薄膜，顯示本實驗之AlCrSiTiNb 高熵氮化膜極具工業發展潛力。

A refractory element, Nb, was firstly added into the AlCrSiTi alloy,
the best alloy designed by our lab and then the non-isomolar AlCrSiTiNb multi-element alloy targets were prepared by vacuum arc melting. The multi-element nitride films were deposited by reactive radio frequency (RF) magnetron sputtering. Evaluated by the integrate property (H3/(x2·E2)) with different nitrogen flow ratio, substrate bias and substrate temperature, we got two best parameters. One is the N40 film with a hardness of 21 GPa and an oxide thickness of 90 nm at 1000 C, 2 h oxidation by cooling in a furnace. The other is the N50 film with a hardness of 20 GPa and an oxide thickness of only 82 nm at 1000 C, 2 h oxidation by cooling in a furnace. Even by cooling in air, the oxide thickness of the N40 film was 99 nm and
the oxide thickness of the N40 film was only 97 nm. In the adhesion test and the wear test, the properties of the nitride films could be improved in vary degrees due to the addition of different intermediate layer, such as the self-alloy intermediate layer, the pure Cr intermediate layer, and the pure Ti intermediate layer. In the cutting test, the N40 film with the pure Cr intermediate layer presented the lowest value of the maximum flank wear. In the condition of low revolutions per minute, the maximum flank wear of this film was only 100 μm, and the average flank wear of this film was 74 μm. In the condition of high revolutions per minute, the maximum flank wear was only 99 μm as well, and the average flank wear was 76 μm. The performance of the N40 film was much better than the cutting tools deposited with TiN, TiAlN and TiAlCrN. The AlCrSiTiNb high-entropy nitride shows a great potential to be an protective hard coating on the cutting tools.

致謝............................................................................................................. I
摘要...........................................................................................................III
Abstract ......................................................................................................V
目錄.........................................................................................................VII
圖目錄....................................................................................................XIII
表目錄.................................................................................................XXVI
壹、前言.....................................................................................................1
貳、文獻回顧.............................................................................................4
1 薄膜鍍製技術..................................................................................4
1.1 物理氣相沉積............................................................................4
1.2 濺鍍原理....................................................................................6
1.3 反應式濺鍍................................................................................7
1.4 射頻濺鍍....................................................................................9
VIII
1.5 磁控濺鍍..................................................................................10
1.6 薄膜沉積與附著機制..............................................................13
1.7 薄膜微結構..............................................................................14
2 薄膜的發展與種類........................................................................19
2.1 薄膜發展概況..........................................................................19
2.2 薄膜分類與介紹......................................................................22
2.3 薄膜硬化機制..........................................................................29
3 高熵合金薄膜................................................................................30
3.1 高熵合金簡介..........................................................................31
3.2 高熵合金之性質與特色..........................................................33
參、實驗流程...........................................................................................38
1 實驗設計........................................................................................38
1.1 基底合金之優化設計..............................................................40
1.2 增添一元耐火元素Nb 之設計.............................................43
1.3 硬度及抗氧化性之綜合性質..................................................44
IX
2 薄膜準備........................................................................................47
2.1 靶材製備..................................................................................47
2.2 基板準備..................................................................................48
2.3 薄膜鍍製..................................................................................50
3 薄膜基本性質分析........................................................................57
3.1 成分分析..................................................................................57
3.2 晶體結構分析..........................................................................58
3.3 微結構分析..............................................................................59
3.4 表面粗糙度分析......................................................................59
4 薄膜機械性質分析........................................................................61
4.1 硬度和楊氏模數分析..............................................................61
4.2 薄膜附著性分析......................................................................63
4.3 薄膜抗磨耗性質分析..............................................................65
5 薄膜抗氧化性分析........................................................................67
6 銑刀切削測試................................................................................67
X
肆、結果與討論......................................................................................73
1 減Si 成分之結果與討論.............................................................73
1.1 T6.7 及T11.7 靶材成分分析.............................................74
1.2 T6.7 及T11.7 氮化膜之基本性質分析................................75
1.2 T6.7、T11.7 及W 氮化膜之表面形貌及微結構比較.....78
1.3 T6.7、T11.7 及W氮化膜之機械性質比較......................79
2 不同氮氣流率對Nb5 氮化膜的影響.........................................81
2.1 鍍率分析..................................................................................81
2.2 成分分析..................................................................................82
2.3 晶體結構分析..........................................................................84
2.4 表面形貌與微結構分析..........................................................89
2.5 表面粗糙度分析......................................................................93
2.6 機械性質分析..........................................................................96
3 不同基板偏壓對N40 及N50 氮化膜的影響..........................99
3.1 鍍率分析..................................................................................99
XI
3.2 成分分析................................................................................101
3.3 晶體結構分析........................................................................103
3.4 表面形貌與微結構分析........................................................108
3.5 表面粗糙度分析....................................................................113
3.6 機械性質分析........................................................................120
3.7 抗氧化性分析........................................................................124
3.8 綜合性質分析........................................................................130
4 不同基板溫度對N40 及N50 氮化膜的影響........................132
4.1 鍍率分析................................................................................132
4.2 成分分析................................................................................134
4.3 晶體結構分析........................................................................136
4.4 表面形貌與微結構分析........................................................140
4.5 表面粗糙度分析....................................................................143
4.6 機械性質分析........................................................................149
4.7 抗氧化性分析........................................................................153
XII
4.7.1 於1000 ºC 持溫兩小時大氣退火爐冷.............................153
4.7.2 於1000 ºC 持溫兩小時大氣退火空冷.............................158
4.8 綜合性質分析........................................................................159
5 最佳製程參數之N40 及N50 氮化膜附著力測試................161
5.1 HRC附著性測試.................................................................162
5.2 刮痕測試................................................................................169
6 最佳製程參數之N40 及N50 氮化膜磨耗試驗....................181
7 最佳製程參數之N40 及N50 氮化膜切削試驗....................194
7.1 低速切削試驗........................................................................195
7.2 高速切削試驗........................................................................207
伍、結論.................................................................................................224
陸、本研究之貢獻................................................................................226
柒、未來研究方向................................................................................227
參考文獻.................................................................................................228
                                

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