利用薄膜模板成長氮化鈦及二氧化鋯薄膜之研究

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研究生：	鄭雅云 Chang,Ya-Yun
論文名稱：	利用薄膜模板成長氮化鈦及二氧化鋯薄膜之研究 Growth of TiN and ZrO2 Thin Films Using Thin Film Templates
指導教授：	黃嘉宏 Huang,Jia-Hong 喻冀平 Yu,Ge-Ping
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：	2008
畢業學年度：	97
語文別：	英文
論文頁數：	90
中文關鍵詞：	模板、氮化鈦、二氧化鋯
外文關鍵詞：	template, titanium nitride, zirconium dioxide
相關次數：	點閱：2 下載：0
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本次研究發展出一種兩步驟方式利用模板來控制氮化鈦與二氧化鋯薄膜的成長，進而探討模板效應對於薄膜性質與結構之影響。本實驗可分為兩個部分，第一部份為利用不同優選方向之氮化鈦或鈦模板成長氮化鈦薄膜，第二部分則是在高純度氬氣中(99.99%)，用熱處理方式氧化具有不同優選方向氮化鋯薄膜以製備二氧化鋯薄膜；為研究鍍膜製程之影響，使用三種不同鍍膜儀器製備具有(111)優選方向的氮化鋯薄膜試片。藉由X光繞射能譜圖(XRD)的觀察可以發現，使用(200)優選方向的氮化鈦做為模板，可使上層氮化鈦薄膜之優選方向從原來的(111)轉變為(200);至於使用具有(111)優選方向氮化鈦薄膜以及優選方向為(0002)純鈦薄膜做為模板，則有助於上層氮化鈦薄膜之優選方向由(200)轉變為(111)。實驗結果顯示，模板對氮化鈦織構成長的效應較改變製程參數有效。至於熱處理過後的氮化鋯試片，可發現正方晶與單斜晶之二氧化鋯同時出現在薄膜內部，其中高氮鋯比試片產生以正方晶二氧化鋯為主要結晶相，然而在低氮鋯比試片中，主要結晶相為單斜晶二氧化鋯。原本氮化鋯之優選方向對於二氧化鋯的成長影響並不顯著，主要結晶相均為單斜晶之二氧化鋯。在熱處理過後的氮化鋯試片表面發現有空泡產生，本研究使用半定量分析來檢視空泡的生成原因，發現空泡生成之驅動力主要是來自氮化鋯與單斜晶二氧化鋯間體積膨脹所產生的壓應力。

This study developed a two-step method to control the growth of TiN and ZrO2 thin films using thin film templates and explored the effects of template on the structure and properties of the derivative thin films. The experiment was divided into two parts. The first part was to deposit TiN on TiN(111), TiN(200) and Ti(0002) templates. In the second part, ZrO2 thin films were grown by oxidizing ZrN thin films with different preferred orientations in Ar (99.99% purity) atmosphere, where ZrN (111) thin films were prepared by three deposition systems for examining the effect of different deposition methods. The texture of the top TiN thin films revealed by X-ray diffraction (XRD) changed from (111) to (200) as TiN(200) template was used. In the cases of using Ti(0002) or TiN(111) templates, the texture of the derivative TiN thin films switched from (200) to (111). The results indicated that templates were more effective on controlling texture of TiN thin film than adjusting deposition parameters. For the oxidation of ZrN thin film, monoclinic (m-ZrO2) and tetragonal (t-ZrO2) phases of ZrO2 were coexisted in all heat-treated specimens, and t-ZrO2 is the dominant phase in the ZrN specimen with higher N/Zr ratio while m-ZrO2 is prevailed in the ZrN specimens with lower N/Zr ratios. There was no substantial difference in the phase ratio and preferred orientation of m-ZrO2 grown from oxidation of ZrN specimens with different textures. Blisters were observed on the surface of the heat-treated ZrN specimens. A semi-quantitative analysis was proposed to examine the driving force of the blister formation, indicating that blisters may result from the compressive stress induced by the volume expansion from ZrN to m-ZrO2.

致謝    I
摘要    III
Abstract    IV
Chapter 1 Introduction    1
Chapter 2 Literature Review    3
1 Characteristics of TiN, ZrN and ZrO2    3
1.1 Characteristics of TiN and ZrN    3
1.2 Characteristics of ZrO2    3
2 The Control of TiN Thin Film Texture    7
2.1 Models of Preferred Orientation or Texture in TiN Thin Films    7
2.2 Texture Control    9
3 Preparation of ZrO2 Thin Films    12
3.1 The Oxidation of ZrN Thin Film    13
Chapter 3 Experimental Details    16
1 Specimen Preparation and Coating Process    16
1.1 Preparation of TiN and Ti Thin Films    16
1.2 Preparation of ZrN Films    17
1.2.1 Unbalanced Magnetron Sputtering    17
1.2.2 Hollow Cathode Discharge Ion-Plating (HCD-IP)    18
1.3 Heat Treatment    18
2 Characterization Methods    23
2.1 X-ray Photoelectron Spectroscopy (XPS)    23
2.2 Rutherford Backscattering Spectroscopy (RBS)    23
2.3 Auger Electron Spectroscopy (AES)    24
2.4 Field-Emission Gun Scanning Electron Microscopy (FE-SEM)    24
2.5 X-ray Diffraction (XRD)    25
3 Properties Measurement    26
3.1 Hardness and Young’s Modulus    26
3.2 Residual Stress    26
3.4 Color (L*a*b*) and Reflectance    27
3.5 Refractive Index    27
3.6 Electrical Resistivity    28
Chapter 4 Results    30
1 Compositions    30
1.1 XPS    30
1.2 RBS    30
2 Structure    38
2.1 θ/2θ XRD    38
2.2 SEM    48
2.3 AES    53
3 Properties    56
3.1 Electrical Resistivity    56
3.1 Electrical Resistivity    56
3.2 Residual Stress    58
3.3 Hardness    60
3.4 Packing Density    61
3.5 Color and Reflectance    61
3.6 Refractive Index    68
Chapter 5 Discussion    69
1 Template Effect    69
1.1 Structure    69
1.1.1 Texture Evolution    69
1.1.2 The Phase Transition of ZrN to ZrO2    73
1.2 Properties    77
1.2.1 Hardness    77
2 The Formation of Blisters    80
Chapter 6 Conclusions    84

                                

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