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研究生： 葉芊吟
論文名稱： 控制氣氛下熱處理對氮化鋯薄膜性質之影響
指導教授： 喻冀平
黃嘉宏
口試委員:
學位類別： 碩士
Master
系所名稱： 原子科學院 - 工程與系統科學系
Department of Engineering and System Science
論文出版年： 2004
畢業學年度： 92
語文別： 英文
論文頁數： 94
中文關鍵詞： 熱處理 、氮化鋯
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    • 熱處理廣泛的應用於加強氮化鋯薄膜的性質。此篇研究中，氮化
    鋯使用中空陰極離子平版蒸鍍法鍍著在AISI D2 鋼上，實驗的熱處理
    環境，其氣氛包括空氣、氬/氫混合氣體，以及使用鋯和鈦結拖，並
    且探討熱處理下的熱力學以及動力學機制，所有的試片都是在一個控
    制氣氛以減少薄膜的氧化作用之熱處理環境下，作700 ℃，一小時
    的退火處理。在熱處理過後，微結構、氮/鋯比以及堆積因子沒有很
    顯著的變化；但是晶粒有變大，結晶性改善，而且（111）織構係數
    在熱處理之後增強了。和未熱處理的試片相比，薄膜的表面粗糙度稍
    微下降；硬度下降了26 到38 %，可能的原因是在熱處理過後，晶界
    的強度下降了，另一個可能的原因是缺陷減少了。殘留應力在熱處理
    之後釋放了8 到24 %，此可歸因於結晶性變好。腐蝕性質在熱處理
    之後也獲得改善，此點在鹽霧測試及動態極化掃瞄之中可以相互驗
    證。

    Heat treatment processes were applied to enhance the characteristics of ZrN thin films. In this study, ZrN films were deposited on AISI D2 steel using a hollow cathode discharge ion-plating (HCD-IP) technique. Heating environment, including air, Ar/H2, and Zr and Ti getters were discussed with thermodynamic and kinetic analysis. The specimens were heat-treated at 700℃ for 1 hour under optimal atmosphere to reduce oxidation of the thin films. The microstructure, resistivity and packing factor of the heat-treated ZrN thin films were not significantly changed. However, the surface grain size was enlarged and crystalline improved. Preferred orientation of (111) was enhanced after heat treatment. Roughness of the annealed specimens was slightly degraded compared with as-deposited samples. The hardness decreased 26~38 %, this is to be understood that heating reduced the strength of the grain boundary. This also could be attributed to the reduction of defects. The residual stress of the specimens subjected to 700℃ heat treatment was relieved 8~24 % that could be due to the better crystallinity. Corrosion resistance became better after heat treatment; it was confirmed both in salt spray and potentiodynamic scanning.

    Chap 1 Introduction ..................................................................................1 Chap 2 Literature Review .........................................................................5 2.1 Hollow Cathode Discharge Ion-Plating (HCD-IP).........................5 2.2 Characteristics of ZrN.....................................................................6 2.3 Effect of Heat Treatment to the Characteristics of ZrN..................7 2.3.1 Preferred Orientation ...............................................................7 2.3.2 Hardness...................................................................................8 2.3.3 Residual stress of ZrN Film...................................................10 2.3.4 Corrosion property.................................................................11 2.4 Evaluation of Adhesion by Scratch Testing..................................12 2.4.1 Models for the Critical Load..................................................12 Chap 3 Experimental Details ..................................................................14 3.1 Coating Equipment and Specimen Preparation............................14 3.2 Heat Treatment under Controlled Atmosphere.............................15 3.3 Thermodynamics and Kinetic Analysis of Heat Treatment under Controlled Atmosphere ......................................................20 3.4 Structure Characterization ............................................................26 3.5 Compositions ................................................................................26 3.5.1 Rutherford backscattering spectrometry (RBS) ....................26 3.5.2 Auger electron spectrometer (AES).......................................27 3.6 Microstructure...............................................................................27 3.7 Properties......................................................................................27 3.7.1 Hardness.................................................................................27 3.7.2 Roughness..............................................................................28 3.7.3 Residual Stress.......................................................................28 3.7.4 Scratch Test............................................................................29 3.7.5 Resistivity ..............................................................................29 3.8 Corrosion Resistance ....................................................................30 3.8.1 Salt Spray Test .......................................................................30 3.8.2 Potentiodynamic Polarization................................................30 Chap 4 Results ........................................................................................33 4.1 Microstructure...............................................................................33 4.2 Composition..................................................................................33 4.3 Surface Image ...............................................................................38 4.4 XRD..............................................................................................38 4.5 Lattice parameter ..........................................................................44 4.6 N/Zr Ratio and Packing Factor .....................................................44 4.7 Hardness........................................................................................47 4.8 Residual Stress ..............................................................................48 4.9 Resistivity .....................................................................................48 4.10 Corrosion Resistance ..................................................................56 4.10.1 Salt Spray Test .....................................................................56 4.10.2 Potentiodynamic Polarization Scan .....................................59 4.11 Scratch Test .................................................................................66 Chap 5 Discussion ..................................................................................72 5.1 The Depth Profiles of the ZrN Thin Films ...................................72 5.2 Hardness........................................................................................72 5.3 Residual Stress ..............................................................................74 5.4 Corrosion Property........................................................................78 Chap 6 Conclusion..................................................................................89 Reference ................................................................................................90

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