織構及鋯介層對奈米晶氮化鋯薄膜之結構與性質的影響

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研究生：	鄧雯文 Wen-Wen Teng
論文名稱：	織構及鋯介層對奈米晶氮化鋯薄膜之結構與性質的影響 Characteristics of Structure and Properties of Nano-crystalline ZrN thin films: Effects of Texture and Zr Interlayer
指導教授：	喻冀平 Ge-Ping Yu 黃嘉宏 Jia-Hong Huang
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：	96
語文別：	英文
論文頁數：	84
中文關鍵詞：	織構、鋯介層、氮化鋯薄膜、硬度、殘留應力、腐蝕性質
外文關鍵詞：	texture, Zr interlayer, ZrN thin film, hardness, residual stress, corrosion resistance
相關次數：	點閱：3 下載：0
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本實驗之目的為研究不同優選方向及加入鋯介層對氮化鋯薄膜之結構與性質的影響。利用非平衡磁控濺鍍系統，於基板溫度為400℃，分別通入1，3，4.2 sccm的氮氣流量，以控制薄膜優選方向為 (111)，隨機，及 (200)，成功地分別鍍著約300nm厚的奈米晶氮化鋯薄膜於P型(100)矽基板及AISI 304不□鋼基板上。此外，於上述三種鍍膜狀況下加入約130nm厚的鋯介層鍍著於不□鋼基板上，以研究鋯介層的影響。鍍膜狀況中雖改變通入氮的流量，但由拉賽福背向散射(RBS)所量測到氮化鋯薄膜中的氮鋯比例為0.8~0.9，因此成份變化的影響不大。
織構變化對於殘留應力與腐蝕性質影響最為顯著。鍍著於矽基板及304不□鋼基板上且具隨機織構的氮化鋯薄膜，顯示較高的殘留壓應力。於1N硫酸水溶液下進行動態極化掃描，量測鍍著於矽基板上的氮化鋯薄膜，得到本質的氮化鋯薄膜腐蝕電位皆為正值，19~149 mVSCE。而鍍著於304不□鋼且具(200)優選方向的氮化鋯薄膜，顯示出最佳保護金屬基板的能力。織構變化對於氮化鋯硬度的影響，可由不同織構氮化鋯鍍著於矽基板的試片發現，並無顯著的不同。
加入厚度130nm的鋯介層具有高度(0002)的優選方向，能將原製程控制具隨機織構的氮化鋯薄膜轉變為(200)織構。而當加入之鋯介層厚度達到240nm時，鋯介層(0002)方向優選程度更高，才能成功把原製程控制具(200)織構的氮化鋯薄膜轉變為隨機織構。鋯介層能改善上層氮化鋯薄膜的結晶性而造成較高的硬度值。同時鋯介層能提高具(111)及random織構的氮化鋯薄膜的抗腐蝕性，由於雙層的薄膜可以有效的阻斷薄膜中孔洞的聯接，防止腐蝕液浸蝕到金屬基板。然而，由殘留應力的量測結果發現，鋯介層並不具有降低上層氮化鋯薄膜中殘留壓應力之能力，相反的，使氮化鋯薄膜中的殘留壓應力提高，並降低氮化鋯薄膜的附著力。

The purpose of this study is to investigate the effects of texture and the Zr interlayer on the structure and properties of nanocrystalline ZrN thin film. Nanocrystalline ZrN thin films were successfully deposited both on (100) p-type Si and AISI 304 stainless steel at a constant temperature 400℃ with introducing three different N2 flow rate, 1,3, and 4.2 sccm, to control the ZrN film textures as (111), random, and (200) by unbalanced magnetron sputtering system(UBMS). In addition, to understand the effects of Zr interlayer, Zr thin films with thickness of 130 nm were pre-deposited on SS304 substrate and then covered with ZrN thin films which were deposited under the three deposition conditions mentioned above respectively. The N/Zr ratios ranged from 0.8 to 0.9 by Rutherford Backscattering Spectroscopy (RBS) measurements.
The effects of texture were remarkable on residual stress and corrosion resistance. ZrN thin films with random texture deposited both on Si and SS304 substrates showed the higher residual stress than those with (111) and (200) textures. The intrinsic corrosion potentials were obtained by ZrN/Si specimens from potentiodynamic polarization scanning in 1N H2SO4 solution. Intrinsic corrosion potentials exhibit positive values ranging from 19 to 149 mVSCE. ZrN films with (200) texture deposited on SS304 substrate displays the best protection of metal substrate. Different textures showed no distinct effect on hardness for ZrN/Si specimens.
ZrN thin films deposited under random orientation condition showed (200) preferred orientation by introducing a highly (0002) preferred Zr interlayer with thickness of 130 nm. Only with a Zr interlayer which was more (0002) preferred with thickness up to 240 nm, ZrN thin film deposited under (200) preferred orientation condition displayed random preferred orientation. The Zr interlayer improved the crystallinity of the upper ZrN films, which resulted in higher hardness values of ZrN films. In addition, Zr interlayer can promoted the corrosion resistance of upper ZrN films with (111) and random textures due to bi-layer effect which can effectively prevent solution to attack the metal substrate by interrupting the connection of pinholes from film surface to metal substrate. However, Zr interlayer can not help the upper ZrN films to relieve residual stress on the contrary it decreases the adhesion of ZrN films.

致謝    i
摘要    ii
Abstract    iii
Contents    v
List of Figures    viii
List of Tables    xi
Chapter 1 Introduction    1
Chapter 2 Literature review    3
1 Deposition method (Unbalanced Magnetron Sputtering System, UBMS)    .3
2 Characteristics of ZrN films    4
3 Main factors of Texture Evolution    7
3.1 Overall Energy    7
3.2 Surface Energy and Adatom Mobilities    8
3.3 Domain Matching Epitaxy (DME)    10
4 The Effect of texture on properties    13
4.1 Hardness    13
4.2 Residual Stress    13
5 The Effect of metal interlayer on upper film structure and properties    14
Chapter 3 Experimental Details    17
1 Specimen Preparation and Deposition Coating Process for ZrN thin films    17
2 Characterization Methods    21
2.1 Rutherford Backscattering Spectroscopy (RBS)    21
2.2 Field-Emission Gun Scanning Electron Microscopy (FEG-SEM)    22
2.3 Auger electron spectroscopy (AES)    22
2.4 X-Ray Diffraction and Glancing Incident X-Ray Diffraction    22
3 Properties Measurement    23
3.1 Electrical Resistivity    23
3.2  Atomic force microscopy (AFM)    24
3.3 Hardness    24
3.4 Residual Stress    25
3.4.1 Optical Method    25
3.4.2 Modified XRD sin2ψ Method    27
4 Corrosion Resistance    28
5 Coloration    29
Chapter 4 Results    31
1 Structure    31
1.1 N/Zr ratios and packing factor (RBS)    31
1.2 Scanning electron microscopy (SEM)    31
1.3 Auger electron spectroscopy (AES)    32
1.4 X-ray diffraction (XRD)    33
1.5 Glancing incident X-ray diffraction (GIXRD)    34
2 Properties    48
2.1 Electrical resistivity    48
2.2 Roughness    48
2.3 Hardness    48
2.4 Residual stress    49
2.5 Corrosion resistance ( potentiodynamic polarization scan )    50
2.6 Coloration characteristics    51
Chapter 5 Discussion    60
1 Deposition Condition    60
1.1 Deposition Rate    60
1.2 The Development of Texture    61
1.3 Composition and Coloration    62
2 Transition of Preferred Orientation    67
3 Residual Stress    68
3.1 Single Layer ZrN    68
3.2 ZrN with Zr interlayer    69
4 Corrosion resistance    73
Chapter 6 Conclusions    75
References    76
Appendix    83

                                

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