研究生: |
張秉書 Chang, Biing-Shu |
---|---|
論文名稱: |
以非平衡磁控濺鍍法製備TiN硬質薄膜之研究 A Study of the Solid Thin Films TiN Deposited by Unbalance-Magnetron Sputtering |
指導教授: |
程金保
Cheng, Chin-Pao |
學位類別: |
碩士 Master |
系所名稱: |
工業教育學系 Department of Industrial Education |
論文出版年: | 2003 |
畢業學年度: | 91 |
語文別: | 中文 |
論文頁數: | 79 |
中文關鍵詞: | 氮化鈦 、非平衡磁控濺鍍 、附著性 、奈米壓痕測試 |
英文關鍵詞: | Titanium nitride, Unbalanced-magnetron sputtering, Adhesion, Nanoindentation |
論文種類: | 學術論文 |
相關次數: | 點閱:447 下載:39 |
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氮化鈦(TiN)硬質薄膜因具有高硬度、耐磨耗、抗腐蝕等特點,因此鍍在某些切削刀具、成型模具及承受高負載的零件上,可明顯延長其使用壽命,同時亦能提升被鍍材表面的平整度。而對這類硬質薄膜而言,為使在工作中能增加壽命,鍍層之要求首重在硬度與附著性。本研究即是以非平衡磁控濺鍍法製備氮化鈦薄膜於SKH9高速鋼基材上,以得到所需之要求。經實驗得知,本機參數設定在OES(%)為60~62%,偏壓為100V,電流值為0.9A,溫度持續加溫在120oC且前處理分別經三氯乙烯、鹼液、去離子水、Freon與氮氣依次清潔,濺鍍TiN階段時間40min的情形下,可得到膜厚2μm,膜層與基材附著力約達67N,硬度在20~24GPa,表面粗糙度在20~40nm的氮化鈦薄膜。另由奈米壓痕測試,除了得到所欲知的硬度值,尚可經由reduced modulus算出楊氏係數值約在290~300GPa。這對氮化鈦膜材抵抗彈性變形之能力提供更進一步的了解。
Titanium nitride (TiN) solid thin film is an important engineering material owing to its excellent hardness, good wear resistance and high corrosion resistance. Because TiN has so many characteristic as above, it has been chosen as hard film material in some applications like cutting tools, forming dies and high loading engineering devices. The TiN films can improve the working life of the substrate material and increase the surface smoothness of the tool. For improving the life of substrate, the hardness and the adhesion of thin film are very important factors. In this study, the unbalanced-magnetron sputtering system was used to deposit single-layer TiN coating on the high-speed steel (SKH9) substrate. Experimental results indicate that the thickness of TiN film was about 2μm and the interface adhesion between TiN film and substrate is about 67N. Moreover, the hardness of TiN film is about 20~24GPa and the roughness of surface varied from 20 to 40 nm. To obtain the above-mentioned results, the test conditions must be controlled. During deposition, the reactive gas of N2 was controlled by optical emission spectrometer (OES) about 60% to 62%. The biasing voltage of substrate was -100V and the target current was 0.9A. The substrate was isothermally at 120oC and the coating time was 40 minutes. Besides, the proper pre-treatment procedure was necessary. By the way, the nanoindentation test not only can obtain exact hardness value of the film, but also can gain the elastic modulus of TiN coatings about 290 to 300Gpa (the reduced modulus Er is known). It can provide advanced knowledge for elastic deformation resistance of TiN coating in MEMS or NEMS field in the near future.
1.Smith, D.L(1995). Thin-film deposition : principles & practice . New York:McGraw-Hill .
2.陳建任(民88)。PVD/CVD 真空鍍膜設備專題研究。高雄:金屬工業中心。
3.Window, B.(1996). Issues in magnetron sputtering of hard coatings. Surface and Coating Technology, 81(1), pp.92-98.
4.Molarius, J.M. , Korhonen, A.S. & Ristolainen, E.O.(1985). Ti-N Phases Formed by Reactive Ion Plating. Journal of Vacuum Science Technology, A3, pp.2419-2425.
5.Grove, W.R.(1840). On Some Phenomena of the Voltaic Discharge. The
Philosophical Magazine,Vol.16, pp.478-482.
6.Berry, R.W. , Hall, P.M. & Harris, M.F.(1968). Thin Film Technology.
New York : R. E. Krieger Publication Company.
7.Wehner, G.K.(1955). Advances in Electronics & Electron Physics.
Vol.7. New York : Academic Press. pp.239.
8. Vossen, John .L. , Kern, Werner(1991). Thin Film Processes II. Boston:
Academic Press.
9.Stuart, R.V.(1983). Vacuum Technology, Thin Film, and Sputtering. New York:Academic Press.
10.Rickerby, D.S. & Mattews, A.(1991). Advanced Surface Coatings.
New York : Chapman & Hall. pp.21.
11.ReactafloTM Instruction Manual.(2001). Huntington : Megatech
Limited Company.
12.Boxman, R.L. , Sanders, D.M. & Martin, P.J.(1995). Handbook of
Vacuum Arc Science & Technology. New Jersey : Noyes Publication.
pp.368-370.
13.Movchan, B.A. & Demchishin, A.V.(1969). Study of the Structure and
Properties of Thick Vacuum Condensates of Nickel, Titanium, Tungsten,
Aluminum Oxide and Zirconium Dioxide. Physical Metal Metallurgy.
Vol.28, pp.83-90.
14.Thornon, J.A.(1974). Influence of apparatus geometry and deposition
conditions on the structure and topography of thick sputtered coatings.
Journal of Vacuum Science Technology. Vol.11, pp.666-670.
15.Messier, R. , Giri, A.P. , & Roy, R.A.(1984). Revised Structure Zone Model for Thin Films Physical Structure. Journal of Vacuum Science Technology. A2(2), pp.500-503.
16.Bland, R.D. , Kominiak, G.J. & Mattax, D.M.(1984). Journal of Vacuum Science Technology. A2(4), pp.671.
17.Window, B. , Savvides, N.(1986). Charged particle fluxes from planar magnetron sputtering sources. Journal of Vacuum Science Technology. A4(2), pp.196.
18.Freller, H. , Lorenz, P.(1986). Electrochemically measured porosity of
magnetron sputtered TiN films deposited at various substrate orientation . Journal of Vacuum Science Technology. A14, pp.2691.
19.Monaghan, D.P.(1991). Surface and Coating Technology. Vol.59, pp.21-25.
20.Spencer, A.G. , Howson, R.P. & Lewin, R.W.(1988). Pressure stability in reactive magnetron sputtering. Thin Solid Films. Vol.158, pp.141.
21.Ives, M. , Cawley, J. & Books, J.S.(1993). Surface and Coating Technology. Vol.6, pp.127.
22.Slwyn, G.S.(1993). Optical Diagnostic Techniques for Plasma Proce-
ssing. New York : American Vacuum Society.
23.竹田博光著,賴耿陽編(民83)。陶瓷材料覆膜技術,2-19。台南 : 復漢出版社。
24.Nicolet, M.A.(1978). Diffusion Barriers in Thin Films. Thin Solid Films. 52, pp.415.
25.Roberts, B. , Harrus, A. & Jackson, R.L.(1995). Interconnect Metall-
ization for Future Device Generations. Solid State Technology. Vol.Feb, pp.69-78.
26.Toth, L.E.(1971). Transition Metal Carbides and Nitrides. New York :
Academic Press.
27.Wang, Y.K. , Wang, W.M. , Cu, X.H. , Cheng, X.Y. & Li, B.S.(1993). A study of the oxide layer on the surface of a TiN coating. Materials Chemistry and Physics. Vol.36, pp.80-83.
28.Nicolet, M.A. , Sondgren, J.E.(1978). Diffusion barriers in thin films. Thin Solid Films. Vol.52, pp.415-443.
29.Mumtaz, A. , Class, W.H.(1982). Color of titanium nitride prepared by
reactive DC magnetron sputtering. Journal of Vacuum Science Techno-
logy. Vol.20, pp.345-348.
30.Perry, A.J. , Georgson, M. & Sproul, W.D.(1988). Variations in the reflectance of TiN , ZrN and HfN. Thin Solid Films. Vol.157, pp255-265.
31.Perry, A.J. , Schoenes, J.(1986). Vacuum. Vol.36, pp.149-155.
32.池 永勝。今後的熱處理技術(日文)。
33.TÖrÖk, E. , Perry, A.J. , Chollet, L. & Sproul, W.O.(1987). Young’s
modulus of TiN , TiC , ZrN and HfN. Thin Solid Films. Vol.153, pp.37-43.
34.呂登復(民75)。實用真空技術。新竹 : 國興出版社。
35.Laimer, J. , Stori, H. & Rodhammer, P.(1989). PACVD of TiN in a
Capacitively Coupled RF Discharge. Journal of Vacuum Science
Technology. A7(5), pp.2952.
36.Heinke, W. , Leyland, A. , Matthews, A. , Berg, G. , Fridrich, C. &
Broszeit, E.(1995). Evaluation of PVD nitride coatings, using impact,
scratch and Rockwell-C adhesion tests. Thin Solid Films. Vol.270,
pp.431.
37.SST-101 Scanning Scratch Tester operational manual(1985). Tokyo:
Shimadzu Corporation(島津製作所).
38.Burnett, P.J. & Rickerby, D.S.(1987). Thin Solid Films. Vol.148,
pp.41.
39. Burnett, P.J. & Rickerby, D.S.(1987). Thin Solid Films. Vol.148,
pp.51.
40. 吳文發 (民91)。化學氣相與物理氣相沉積技術。載於國科會國家奈米元件實驗室主編「積體電路製程技術訓練班講義(I)」,頁 5-9。
41.鄭昌瓊等(2002)。簡明材料辭典,頁56。北京:科學出版社。
42.Oliver, W.C. & Pharr, G.M.(1992). An Improved Technique for Determining Hardness and Elastic Modulus Using Load and Displacement Sensing Indentation Experiments. Journal of Materials Research. Vol.7, No.6, pp.1564-1583.
43.Pharr, G.M., Oliver, W.C. & Brotzen, F.R. (1992). On the generality of the relationship between contact stiffness, contact area, and elastic modulus during indentation, Journal of Materials Research. Vol. 7, No. 3, pp.613.
44.Hertz, H. & Reine, J. (1882). Angew. Math. Vol.92, pp.156.
45.Tbor, D.(1948). Proc. R. Soc.Vol. A192, pp247.
46.Vijgen, R.O.E. & Dautzenberg, J.H.(1995). Mechanical Measurement of the Residual Stress in Thin PVD Films. Thin Solid Films. Vol.270, pp.264-269.
47.Schneider, D. & Tucker, M.D.(1996).Non-destructive characterization and evaluation of thin films by laser-induced ultrasonic surface waves. Thin Solid Films. Vol.290-291, pp.309.