製程參數對高功率脈衝磁控濺鍍製備氮化鉬薄膜結構與性質之影響

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研究生：	張庭恩 Zhang, Ting-En
論文名稱：	製程參數對高功率脈衝磁控濺鍍製備氮化鉬薄膜結構與性質之影響 Effects of Process Parameters on Structure and Properties of Molybdenum Nitride Thin Films by High-Power Impulse Magnetron Sputtering
指導教授：	黃嘉宏 Huang, Jia-Hong
口試委員:	張銀祐 Chang, Yin-Yu 李志偉 Lee, Jyh-Wei 林郁洧 Lin, Yu-Wei
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：	2021
畢業學年度：	109
語文別：	英文
論文頁數：	112
中文關鍵詞：	氮化鉬、高功率脈衝磁控濺鍍、織構、殘留應力
外文關鍵詞：	Molybdenum nitride, High-power impulse magnetron sputtering, Texture, Residual stress
相關次數：	點閱：1 下載：0
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本研究之目的為使用高功率磁控脈衝濺鍍(HiPIMS)鍍覆緻密且高硬度的單相γ-Mo2N薄膜；並且透過調控製程參數，改善 HiPIMS高殘留應力和低沉積速率的缺點。實驗調控的參數有佔空比、工作壓力和氮氣流量，分別影響峰值功率、平均自由徑和鉬金屬殘留量。結果顯示，隨著佔空比和工作壓力降低，能夠製備出緻密的薄膜。試片D10（10% 的佔空比）和 P05（5 mTorr 的工作壓力）所使用參數最佳，均為具有高硬度 (約24 GPa) 的單相 Mo2N薄膜，且幾乎沒有殘留應力。此結果亦指出高壓應力並不是高硬度的必要條件。此外，Mo2N薄膜的優選方向可以藉由改變製程參數，在 (200) 和 (111) 之間切換。(200)的織構係數隨著佔空比和工作壓力的減少而增加。在佔空比 ≥10%時，競爭成長理論和離子干擾效應可用來解釋織構的變化機制。(200)面上的氮空缺可能有利於(200)取向的晶粒形成，因此當N2+/(N2+N2+)的比例13%時，尚能出現(200)的織構。隨著佔空比縮小到 5%，高能量的氣體離子引起離子穿隧效應，因此薄膜呈現(200)主導的織構。隨著工作氣壓增加，使得離子能量降低，因此減少了離子穿隧效應，而離子干擾效應開始起作用。在高工作氣壓(10 mTorr)的低能量沉積條件下可以製備具有(111) 織構的薄膜。在HiPIMS製程中，減少佔空比和工作氣壓能夠引起顯著的離子轟擊效應，進而增加Mo2N薄膜的壓應力，使薄膜變得更緻密，增加其硬度及降低其電阻率。

The objectives of this study were to produce single phase γ-Mo2N thin films with dense structure and high-hardness by high power impulse magnetron sputtering (HiPIMS), in which high residual stress and low deposition rate could be controlled by adjusting the process parameters. Duty cycle, working pressure and nitrogen flow rate were selected as the controlling process parameters, which were respectively related to peak power, mean free path and the amount of retained Mo metal. The results showed that dense Mo2N thin films could be produced as the duty cycle and working pressure decreased. Mo2N samples D10 (10% duty cycle) and P05 (5 mTorr working pressure) were deposited with the optimum process parameters, where the films possessed single phase Mo2N with high hardness (~ 24 GPa) and almost no residual stress, indicating that high compressive residual stress was not a necessary condition for high hardness. The preferred orientation of Mo2N thin films could be tailored from (200) to (111) by controlling the process parameters. The texture coefficient of (200) increased as the duty cycle and working pressure decreased. The texture evolution could be explained by the competitive growth theory and ion interference effect for the samples deposited with duty cycle 10%. The N vacancies on the (200) plane might facilitate the formation of (200)-oriented grains, and thus (200) peak appeared when the N2+/(N2+N2+) ratio  13%. As the duty cycle decreased to 5%, the high-energy gas ions caused the ion channeling effect, leading to the (200)-dominant texture. As the working pressure increased, the energy of the ions decreased, thereby the ion channeling effect becoming less effective and the ion interference effect being functioning. The (111)-dominant texture could be prepared at low energy deposition condition with high working pressure (10 mTorr). Decreasing duty cycle and working pressure in HPPMS process could induce significant ion peening effect, and thereby increase the compressive stress and densify the Mo2N thin film, which could increase the hardness and decrease the electrical resistivity of the thin film.

摘要    i
Abstract    ii
致謝    iii
Content    iv
List of Figures    vi
List of Tables    vi
Chapter 1  Introduction    1
Chapter 2  Literature Review    3
2.1 Characteristics of Molybdenum Nitride    5
2.1.1 Structure of Molybdenum Nitride    5
2.1.2 Properties of Molybdenum Nitride    7
2.2 High-power impulse magnetron sputtering (HiPIMS)    9
2.3 Texture evolution    10
2.3.1 Overall Energy Model    10
2.3.2 Competitive Growth Theory    11
2.3.3 Ion Channeling Effect    12
2.4 Residual Stress    12
Chapter 3  Experimental Details    14
3.1 Experimental Design    14
3.2 Substrate Preparation    14
3.3 Deposition Procedures    14
3.3.1 High power impulse magnetron sputtering system (HiPIMS)    15
3.4 Measurement of Chemical Compositions and Structure    20
3.4.1 Chemical Composition    20
3.4.2 Binding Energy    20
3.4.3 Crystal Structure, Preferred Orientation and Crystalline Size    21
3.4.4 Lattice Parameter    22
3.4.5 Film Thickness and Microstructure    22
3.4.6 Surface Roughness    23
3.5 Measurement of Properties    23
3.5.1 Hardness and Young's modulus    23
3.5.2 Residual stress    24
3.5.3 Electrical Resistivity    25
Chapter 4  Results    27
Part I: The Effect of Duty Cycle (D-series)    27
4.1 Plasma composition    29
4.2 Cathode Voltage and Peak Current    31
4.3 Chemical Compositions and Structure    32
4.4 Properties    40
Part II: The Effect of Working Pressure on HiPIMS (P-series)    43
4.5 Cathode Voltage and Peak Current    43
4.6 Chemical Compositions and Structure    47
4.7 Properties    55
Part III: The Effect of Nitrogen Flow Rate on HiPIMS (N-series)    58
4.8 Cathode Voltage and Peak Current    58
4.9 Chemical Compositions and Structure    61
4.10 Properties    70
Chapter 5  Discussion    73
5.1 Effect of process parameters on texture evolution    75
5.1.1 Effect of duty cycle    75
5.1.2 Effect of working pressure    80
5.1.3 Effect of nitrogen flow rate    82
5.1.4 The relationship between texture and process parameters    84
5.2 Effect of process parameters on residual stress and hardness    85
5.2.1 Effect of duty cycle    85
5.2.2 Effect of working pressure    86
5.2.3 Effect of nitrogen flow rate    87
5.2.4 The relationship between intrinsic stress and process parameters    90
Chapter 6  Conclusions    91
References    93
Appendix A  AFM images of specimens    103
Appendix B  XPS spectra    106
Appendix C  Optical spectra    108
Appendix D  Heat Dissipation Estimation of the HiPIMS sputtering gun    110

                                

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