不同工作週期對直流脈衝電漿化學氣相沉積法蒸鍍 DLC 薄膜於氮氧化處理 JIS SKD11 工具鋼之研究 Characteristics of DLC Films Coated on Oxynitriding-treated JIS SKD11 Tool Steel 1 2 3 4 5 S.H. Chang, C.R. Huang, C.M. Liu, C.K. Peng, C.C. Yu JIS SKD11 (Diamond-like Carbon, DLC) SKD11 DLC 8% Hv 0.025 2621.0 0.05 m s -1 200 g (5.20 10-3 mm 3 ) /DLC 3.5 wt% NaCl (I corr =1.83 10-5 A cm -2 ) (R p =4811.1 cm 2 ) JIS SKD11 tool steel is commonly used as cold work tool steel. In order to improve the tool life, a thin film is used to protect the integrity of the inner material. In this study, the diamond-like carbon (DLC) thin film was prepared by DC-pulsed PECVD. We used Raman spectroscopy analysis, wear tests, hardness tests and corrosion resistance inspections to evaluate the properties of the DLC films coated on the oxynitriding/ DLC-treated SKD11 tool steel. Experimental results showed that all the DLC films have excellent adhesivity. The duplex coating layers had optimal properties when the work cycles maintained at 8% of unipolar negativepulsed voltage: highest surface hardness (Hv 0.025 2621.0) and lowest wear volume loss (5.20 10-3 mm 3 ) when the sliding speed maintained at 0.05 m s -1 and load of 200 g. The optimal oxynitriding/dlc duplex coating had the lowest corrosion current (Icorr = 1.83 10-5 A cm -2 ) and the highest polarization resistance (Rp = 4811.1 cm 2 ) in 3.5 wt% NaCl solutions. 關鍵詞 : SKD11 Key words: SKD11 tool steel, DC-pulsed PECVD, DLC, oxynitriding and wear 一 前 言 PVD CVD 1 2 4 5 3 1,2,4,5 Department of Materials and Mineral Resources Engineering, National Taipei University of Technology 3 Department of Chemical and Material Engineering, Lunghwa University of Science and Technology -42-
(1,2) (ONC ) Nitrex (Micro-pores) 500 / (1,2) (3) 500 C Fe 3 O 4 (Diamond-like Carbon, DLC) sp 3 sp 2 sp 2 sp 3 (4-7) DLC (PECVD) DLC PECVD DLC JIS SKD11 DLC 二 實驗方法 JIS SKD11 HRC 61-63 (Oxynitriding, ONC ) XRD (DC-pulsed PECVD) (DLC) (Raman Spectroscopy Analysis) (Wear test, Pin-on-Disk ASTM G99) (8) (Vickers) SEM DLC 5% 8% 10% 12% 15% (10 khz) 90 (-1.5 kv) (CH 4 5 sccm) 三 結果與討論 480 /8 hrs (480 /30 min) SKD11 43 µm (9) 鑛冶 59/1-43-
SKD11 46 µm SKD11 XRD 1 Fe 3 N ε Fe 4 N γ' Fe 3 O 4 1 SKD11 XRD SKD11 2 Hv 0.05 1399.3 95 µm Hv 0.05 710 3 2 SKD11 SKD11 488 nm sp 2 /sp 3 sp 2 sp 3 8% DLC G-peak sp 2 sp 3 D-peak sp 2 (1332 cm -1 ) sp 3 D-peak D-peak G-peak (I D /I G ) sp 3-44-
sp 3 G-peak (10-12) 4 SKD11 8% I D /I G (0.63) G-peak (1540.39 cm -1 ) sp 3 / sp 2 8% 3 DLC sp 3 sp 3 sp 3 8% DLC 0.05 m s -1 200 g 4 5 SEM 5(b) 5(c) 8% 10% sp 3 5(b) 5(c) 8% 10% 5(a) 5(d) 5(e) 5% 12% 15% 5(e) 15% DLC 6 10% (7.07 10-3 mm 3 ) 8% (5.20 10-3 mm 3 ) sp 3 鑛冶 59/1-45-
5% 12% 15% 7.90 10-3 7.57 10-3 8.40 10-3 mm 3 5 0.05 m s-1-200 g SEM (a)5% (b)8% (c)10% (d)12% (e)15% 3.5 wt% NaCl 7 Tafel - -46-
DLC 1 10-5 A cm -2 8% (I corr =1.83 10-5 A cm -2 ) 3.5 wt% NaCl (R p ) 8% DLC (R p =4811.1 cm 2 ) 8% 3.5 wt% NaCl 6 0.05 m s -1-200 g 7 3.5 wt% NaCl 鑛冶 59/1-47-
1 I corr ( 10-5 A cm -2 ) E corr (Volts) R p ( cm 2 ) 5% 4.24-1.15 2416.9 8% 1.83-1.14 4811.1 10% 2.84-1.16 3723.2 12% 3.73-1.20 2349.2 15% 3.31-1.18 3183.9 四 結 論 JIS SKD11 CH 4 5 sccm -1.5 kv 10 khz 90 8% 1 µm Hv 0.025 2621.0 I D /I G (0.63) G-peak 1540.39 cm -1 200 g 0.05 m s -1 8% DLC 5.20 10-3 mm 3 8% /DLC 3.5 wt% NaCl 1.83 10-5 A cm -2 4811.1 cm 2 JIS SKD11 四 參考文獻 (1) DLC ASP23 2013 (2) Alsaran, Effect of Post-Oxidizing on Tribological and Corrosion Behavior of Plasma Nitrided AISI 5140 Steel, Surface and Coatings Technology, vol. 176, 2004, pp. 344-348. (3) 1996 310 (4) DC 2007 (5) M. Kahn, M. Čekada, T. Schöberl, R. Berghauser, C. Mitterer, C. Bauer, W. Waldhauser and E. Brandstatter, Structural and mechanical properties of diamond-like carbon films deposited by an anode layer source, Thin Solid Films, vol. 517, 2009, pp. 6502-6507. (6) Z. Lin, S. B. Lv, Z. J. Yu, M. Li, T. Y. Lin, D. C. Ba, C. K. Choi and I. S. Lee, Effect of bias voltage on Diamond-like carbon film deposited on PMMA substrate, Surface and Coatings Technology, vol. 202, 2008, pp. 5386-5389. (7) R. Sharma, P. K. Barhai and N. Kumari, Corrosion resistant behavior of DLC films, Thin Solid Films, vol. 516, 2008, pp. 5397-5403. (8) ASTM, Standard Test Method for Wear Testing with a Pin-on-Disk Apparatus, Designation: G99-03. (9) SKD11 2009 (10) Andrea Carlo Ferrari, Determination of bonding in diamond-like carbon by Raman spectroscopy, Diamond and Related Materials, vol. 11, 2002, pp. 1053-1061. (11) A. C. Ferrari and J. Robertson, Resonant Raman spectroscopy of disordered, amorphous, and diamond like carbon, Physical Review B, vol. 64, 2001, pp. 1-13. (12) 2012 19-48-