脉冲偏压占空比对TiAlCrN多元复合薄膜微观结构和性能的影响规律

魏永强, 王唯骏, 李永辉, 王道洋, 杨佳乐, 刘畅, 吕怿东, 韦春贝, 钟素娟

表面技术 ›› 2026, Vol. 55 ›› Issue (6) : 40-52.

PDF(18921 KB)
PDF(18921 KB)
表面技术 ›› 2026, Vol. 55 ›› Issue (6) : 40-52. DOI: 10.16490/j.cnki.issn.1001-3660.2026.06.004
腐蚀与防护

脉冲偏压占空比对TiAlCrN多元复合薄膜微观结构和性能的影响规律

  • 魏永强1,*, 王唯骏1, 李永辉1, 王道洋1, 杨佳乐1, 刘畅1,2, 吕怿东1,3, 韦春贝2, 钟素娟3
作者信息 +

Effect of Substrate Pulsed Bias Duty Cycles on the Microstructure and Properties of TiAlCrN Multi-component Composite Films Deposited by Arc Ion Plating

  • WEI Yongqiang1,*, WANG Weijun1, LI Yonghui1, WANG Daoyang1, YANG Jiale1, LIU Chang1,2, LYU Yidong1,3, WEI Chunbei2, ZHONG Sujuan3
Author information +
文章历史 +

摘要

目的 为提升M2高速钢材料的表面性能,研究脉冲偏压占空比对TiAlCrN多元复合薄膜微观结构和性能的影响规律。方法 采用电弧离子镀方法,在M2高速钢表面制备TiAlCrN多元复合薄膜,再通过多种检测表征方法,探究脉冲偏压占空比对TiAlCrN多元复合薄膜微观结构与性能的影响规律。结果 随脉冲偏压占空比的增加,TiAlCrN薄膜表面大颗粒数量整体呈递减的变化趋势;薄膜晶面择优取向发生明显转变,占空比在20%及以下时为(200)晶面,占空比在30%及以上时转变为(111)晶面。当脉冲偏压占空比为10%时,薄膜中Al元素含量(原子数分数)达到峰值21.37%,平均晶粒尺寸最大为6.17 nm,薄膜硬度达到最大值2 381HV,薄膜的结合力最优为74 N;当脉冲偏压占空比为20%时,平均摩擦系数降至最小值0.84;占空比为40%时薄膜中Cr元素含量(原子数分数)最高为22.37%,Cr对薄膜晶粒的细化作用最显著,使薄膜平均晶粒尺寸最小为2.86 nm,致密的薄膜结构可有效阻隔腐蚀介质渗透,自腐蚀电位达到最高值-0.39 V (vs. SCE)。相较于M2高速钢基体,TiAlCrN多元复合薄膜的硬度、耐腐蚀及摩擦磨损性能均实现显著提升。TiAlCrN多元复合薄膜在刀具与模具性能提升方面具有良好的应用前景,研究结果为硬质薄膜沉积工艺优化提供了实验依据。结论 TiAlCrN多元复合薄膜能显著提升高速钢基体的性能,通过调节脉冲偏压占空比可优化其结构与综合性能,其中脉冲偏压占空比为10%时薄膜硬度最高,脉冲偏压占空比为40%时薄膜耐腐蚀和抗摩擦磨损性能最优。

Abstract

To systematically investigate the effect of the pulsed bias duty cycle, the work aims to deposit TiAlCrN multi-component composite films on the M2 high-speed steel via arc ion plating. The microstructure was characterized by scanning electron microscopy (SEM). Phase identification and texture analysis were performed through X-ray diffraction (XRD). Elemental composition was quantified by energy dispersive spectroscopy (EDS). Microhardness was measured with a Vickers microhardness tester. Adhesion was evaluated via scratch tests on a multifunctional surface properties tester. Tribological performance was assessed with a pin-on-disk testing machine and electrochemical behavior was examined through potentiodynamic polarization tests. Increasing the pulsed bias duty cycle enhanced the ion bombardment intensity over a given period, which reduced the macroparticles. As the pulsed bias duty cycle increased from 10% to 50%, the amount of macroparticles decreased from 547 to 312 due to the stronger repulsive force from the substrate bias. This amount reduction of macroparticles contributed to a lower coefficient of friction and better surface quality. At the pulsed bias duty cycle below 20%, the TiAlCrN multi-component composite films displayed a preferred orientation along the (200) plane. While the pulsed bias duty cycle increased more than 30%, the ion flux density increased and the pull up time of ion flux prolonged, which accelerated TiAlCrN multi-component composite film deposition and led to the internal stress rise. Meanwhile, the strain energy minimization dominated the TiAlCrN multi-component composite film growth and the preferred orientation transited from (200) to (111). At a pulsed bias duty cycle of 10%, the Al content reached a maximum of 21.37at.%, the average grain size and hardness of TiAlCrN multi-component composite films reached the maximum values of 6.17 nm and 2 381HV, respectively. This was attributed to the synergistic effects of solid solution strengthening and the reverse Hall-Petch effect. When the grain size decreased to a critical value, the hardness trend was consistent with the reverse Hall-Petch effect. The relatively coarser grain size corresponded to the maximum hardness. The reduction of strain energy enabled the TiAlCrN multi-component composite film to achieve optimal adhesion 74 N. At a pulsed bias duty cycle of 20%, during sliding friction test process, minimal film delamination limited the wear debris generation, which decreased the average coefficient of friction to 0.84. With the pulsed bias duty cycle increasing to 40%, the Cr element content of TiAlCrN multi-component composite films reached the highest value of 22.37at.%, which promoted the grain refinement and the average grain size reached to the smallest 2.86 nm. This dense microstructure effectively impeded the penetration of corrosive medium. The TiAlCrN multi-component composite film had superior corrosion resistance and the corrosion potential reached to -0.39 V(vs. SCE). With the pulsed bias duty cycle increasing to 50%, the time-dependent enhancement of ion attraction promoted film growth and increased thickness, but the excessive ion bombardment raised internal stress and severely degraded the adhesion to 28 N. Meanwhile, the adhesion reduction of the TiAlCrN multi-component composite film induced the film delamination and accelerated debris generation during the friction process and the coefficient of friction reached to the maximum 0.91. Compared with the uncoated M2 high-speed steel substrate, the TiAlCrN multi-component composite films demonstrated significantly enhanced hardness, superior corrosion resistance and improved tribological performance. These research results provide experimental evidence and key deposition process for optimizing arc ion plating processes. These findings demonstrate the considerable potential of TiAlCrN films for enhancing the performance and durability of cutting tools and molds in advanced manufacturing applications.

关键词

电弧离子镀 / 脉冲偏压占空比 / TiAlCrN多元复合薄膜 / 微观组织 / 性能

Key words

arc ion plating / pulsed bias duty cycle / TiAlCrN multi-component composite film / microstructure / property

引用本文

导出引用
魏永强, 王唯骏, 李永辉, 王道洋, 杨佳乐, 刘畅, 吕怿东, 韦春贝, 钟素娟. 脉冲偏压占空比对TiAlCrN多元复合薄膜微观结构和性能的影响规律[J]. 表面技术. 2026, 55(6): 40-52
WEI Yongqiang, WANG Weijun, LI Yonghui, WANG Daoyang, YANG Jiale, LIU Chang, LYU Yidong, WEI Chunbei, ZHONG Sujuan. Effect of Substrate Pulsed Bias Duty Cycles on the Microstructure and Properties of TiAlCrN Multi-component Composite Films Deposited by Arc Ion Plating[J]. Surface Technology. 2026, 55(6): 40-52
中图分类号: TG174.4   

参考文献

[1] 张权, 耿东森, 许雨翔, 等. 电弧/溅射复合沉积技术的发展及其在刀具涂层中的应用[J]. 表面技术, 2021, 50(5): 20-35.
ZHANG Q, GENG D S, XU Y X, et al.Development of Hybrid Arc/Sputtering Deposition Techniques for Tool Coatings[J]. Surface Technology, 2021, 50(5): 20-35.
[2] 范其香, 林静, 王铁钢. 刀具涂层材料的最新研究进展[J]. 表面技术, 2022, 51(2): 1-19.
FAN Q X, LIN J, WANG T G.The Latest Research Progress of Tool Coating Materials[J]. Surface Technology, 2022, 51(2): 1-19.
[3] WEI Y Q, ZONG X Y, JIANG Z Q, et al.Characterization and Mechanical Properties of TiN/TiAlN Multilayer Coatings with Different Modulation Periods[J]. The International Journal of Advanced Manufacturing Technology, 2018, 96(5): 1677-1683.
[4] 魏永强, 张华森, 张晓晓, 等. N2/Ar流量比对TiZrN/TiN纳米多层薄膜微观结构和性能的影响[J]. 表面技术, 2025, 54(14): 92-104.
WEI Y Q, ZHANG H S, ZHANG X X, et al.Effects of N2/Ar Flow Ratio on the Microstructure and Properties of TiZrN/TiN Nano-Multilayer Films[J]. Surface Technology, 2025, 54(14): 92-104.
[5] 魏永强, 张晓晓, 张华森, 等. 脉冲偏压幅值对TiZrN/TiN纳米多层膜微观结构和性能的影响[J]. 稀有金属材料与工程, 2025, 54(9): 2384-2394.
WEI Y Q, ZHANG X X, ZHANG H S, et al.Effects of Pulsed Bias Voltage on Microstructure and Properties of TiZrN/TiN Nano-Multilayer Films[J]. Rare Metal Materials and Engineering, 2025, 54(9): 2384-2394.
[6] LIU L L, AN X K, GU X L, et al.Nanotwinned CrN Ceramics with Enhanced Plasticity[J]. Nature Communications, 2025, 16: 5934.
[7] 魏永强, 顾艳阳, 范梦圆, 等. 脉冲偏压占空比对TiCrN薄膜微观结构和性能的影响规律[J]. 中国表面工程, 2023, 36(6): 57-67.
WEI Y Q, GU Y Y, FAN M Y, et al.Effects of Pulsed Bias Duty Cycle on the Microstructure and Properties of TiCrN Films[J]. China Surface Engineering, 2023, 36(6): 57-67.
[8] LIN J L, ZHANG X H, OU Y X, et al.The Structure, Oxidation Resistance, Mechanical and Tribological Properties of CrTiAlN Coatings[J]. Surface and Coatings Technology, 2015, 277: 58-66.
[9] WANG Q Z, ZHOU F, YAN J W.Evaluating Mechanical Properties and Crack Resistance of CrN, CrTiN, CrAlN and CrTiAlN Coatings by Nanoindentation and Scratch Tests[J]. Surface and Coatings Technology, 2016, 285: 203-213.
[10] ALBERDI A, MARÍN M, DÍAZ B, et al. Wear Resistance of Titanium-Aluminium-Chromium-Nitride Nanocomposite Thin Films[J]. Vacuum, 2007, 81(11/12): 1453-1456.
[11] 张硕, 范其香, 郝雪卉, 等. 沉积偏压对AlCrTiN纳米复合涂层力学与抗高温氧化性能的影响[J]. 中国表面工程, 2023, 36(2): 104-113.
ZHANG S, FAN Q X, HAO X H, et al.Effect of Bias Voltage on Mechanical and High Temperature Oxidation Resistance of AlCrTiN Nanocomposite Coatings[J]. China Surface Engineering, 2023, 36(2): 104-113.
[12] 林静, 张硕, 马德政, 等. 沉积温度对AlCrTiN涂层组织结构与性能的影响[J]. 中国表面工程, 2021, 34(6): 114-123.
LIN J, ZHANG S, MA D Z, et al.Effects of Deposition Temperature on the Structure and Property of AlCrTiN Coatings[J]. China Surface Engineering, 2021, 34(6): 114-123.
[13] WU S, ZHAO Y M, ZHANG L, et al.Effect of C Doping on Structure and Properties of TiAlCrN Coatings by Filter Cathode Vacuum Arc Deposition[J]. Vacuum, 2022, 201: 111093.
[14] LIEW W Y H, LIM H P, MELVIN G J H, et al. Thermal Stability, Mechanical Properties, and Tribological Performance of TiAlXN Coatings: Understanding the Effects of Alloying Additions[J]. Journal of Materials Research and Technology, 2022, 17: 961-1012.
[15] TANG J F, LIN C Y, YANG F C, et al.Effects of Input Power Ratio of AlCr/Ti Target on the Microstructural and Mechanical Properties of AlTiCrN Coatings Synthesized by a High-Power Impulse Magnetron Sputtering Process[J]. Coatings, 2021, 11(7): 826.
[16] MOHAMMADI M, TOLOUEIPOUR M, YAZDANI A.The Effect of Substrate Duty Cycle on the Mechanical and Electrochemical Properties of TiAlN Coatings Deposited by Cathodic Arc Evaporation[J]. Journal of Materials Engineering and Performance, 2025, 34(20): 23867-23876.
[17] ZHAO S S, ZHAO Y H, CHENG L S, et al.Effects of Substrate Pulse Bias Duty Cycle on the Microstructure and Mechanical Properties of Ti-Cu-N Films Deposited by Magnetic Field-Enhanced Arc Ion Plating[J]. Acta Metallurgica Sinica (English Letters), 2017, 30(2): 176-184.
[18] WEI Y Q, GONG C Z.Effects of Pulsed Bias Duty Ratio on Microstructure and Mechanical Properties of TiN/ TiAlN Multilayer Coatings[J]. Applied Surface Science, 2011, 257(17): 7881-7886.
[19] SHI Y J, LONG S Y, YANG S C, et al.Deposition of Nano-Scaled CrTiAlN Multilayer Coatings with Different Negative Bias Voltage on Mg Alloy by Unbalanced Magnetron Sputtering[J]. Vacuum, 2010, 84(7): 962-968.
[20] BOBZIN K, BRÖGELMANN T, KRUPPE N C, et al. HPPMS TiAlCrSiN-Influence of Substrate Bias and Pulse Frequency on Cutting Performance[J]. Surface and Coatings Technology, 2020, 397: 126056.
[21] ZHANG J, LV H M, CUI G Y, et al.Effects of Bias Voltage on the Microstructure and Mechanical Properties of (Ti, Al, Cr)N Hard Films with N-Gradient Distributions[J]. Thin Solid Films, 2011, 519(15): 4818-4823.
[22] HSU C H, LEE C Y, LIN Z H, et al.Bias Effects on Microstructure, Mechanical Properties and Corrosion Resistance of Arc-Evaporated CrTiAlN Nanocomposite Films on AISI 304 Stainless Steel[J]. Thin Solid Films, 2011, 519(15): 4928-4932.
[23] 孔德军, 付贵忠, 王文昌, 等. AlTiCrN涂层结合界面组织特征与结合性能[J]. 工程科学学报, 2015, 37(12): 1624-1629.
KONG D J, FU G Z, WANG W C, et al.Interfacial Structural Characteristics and Bonding Performance of AlTiCrN Coatings[J]. Chinese Journal of Engineering, 2015, 37(12): 1624-1629.
[24] BROWN I G.Cathodic Arc Deposition of Films[J]. Annual Review of Materials Science, 1998, 28: 243-269.
[25] 魏永强, 宗晓亚, 蒋志强, 等. 电弧离子镀中Ti大颗粒空间传输过程中受力变化特征分析[J]. 中国表面工程, 2017, 30(4): 27-35.
WEI Y Q, ZONG X Y, JIANG Z Q, et al.Force Characteristics Analysis of Ti Macroparticles Space Transmission in Arc Ion Plating[J]. China Surface Engineering, 2017, 30(4): 27-35.
[26] LIU J, ZHANG X Y, PELENOVICH V, et al.Effects of Duty Cycle on Microstructure and Mechanical Properties of (AlCrNbSiTi)N High-Entropy Nitride Hard Coatings Deposited by Pulsed Arc Ion Plating[J]. Vacuum, 2024, 225: 113219.
[27] 赵彦辉, 赵鑫, 宋贵宏. 基体偏压幅值对NiCrN薄膜微观结构及力学性能的影响[J]. 材料保护, 2024, 57(12): 122-130.
ZHAO Y H, ZHAO X, SONG G H.Effect of Substrate Bias Voltage Amplitude on the Microstructure and Mechanical Properties of NiCrN Films[J]. Materials Protection, 2024, 57(12): 122-130.
[28] 耿东森, 吴正涛, 聂志伟, 等. 基体偏压对电弧离子镀AlCrSiON涂层结构和热稳定性的影响[J]. 中国表面工程, 2016, 29(6): 60-66.
GENG D S, WU Z T, NIE Z W, et al.Influence of Substrate Bias on Microstructure and Thermal Stability of AlCrSiON Coatings Deposited by Arc Ion Plating[J]. China Surface Engineering, 2016, 29(6): 60-66.
[29] KIMBLIN C W.Erosion and Ionization in the Cathode Spot Regions of Vacuum Arcs[J]. Journal of Applied Physics, 1973, 44(7): 3074-3081.
[30] 丁育胜, 张钧, 田红花. 多弧离子镀高温合金防护层成分离析的研究[J]. 材料保护, 1995, 28(6): 27-29.
DING Y S, ZHANG J, TIAN H H.Study on Composition Segregation of Protective Layer of Superalloy by Multi-Arc Ion Plating[J]. Materials Protection, 1995, 28(6): 27-29.
[31] DAS C R, RANGWALA M, GHOSH A.Influence of Substrate Bias Voltage on Microstructure and Mechanical Characteristics of TiAlSiN Coating Deposited by High Power Impulse Magnetron Sputtering (HiPIMS)[J]. Surface and Coatings Technology, 2023, 458: 129351.
[32] ZHANG M, HU X G, YANG X X, et al.Influence of Substrate Bias on Microstructure and Morphology of ZrN Thin Films Deposited by Arc Ion Plating[J]. Transactions of Nonferrous Metals Society of China, 2012, 22: s115-s119.
[33] TAM P L, ZHOU Z F, SHUM P W, et al.Structural, Mechanical, and Tribological Studies of Cr-Ti-Al-N Coating with Different Chemical Compositions[J]. Thin Solid Films, 2008, 516(16): 5725-5731.
[34] UVAROV V, POPOV I.Metrological Characterization of X-Ray Diffraction Methods for Determination of Crystallite Size in Nano-Scale Materials[J]. Materials Characterization, 2007, 58(10): 883-891.
[35] KOSARI MEHR A, ZAMANI MEYMIAN M R, KOSARI MEHR A. Nanoindentation and Nanoscratch Studies of Submicron Nanostructured Ti/TiCrN Bilayer Films Deposited by RF-DC Co-Sputtering Method[J]. Ceramics International, 2018, 44(17): 21825-21834.
[36] 程芳, 黄美东, 王萌萌, 等. 脉冲偏压占空比对复合离子镀TiCN涂层结构和性能的影响[J]. 中国表面工程, 2014, 27(4): 100-106.
CHENG F, HUANG M D, WANG M M, et al.Effects of Duty-Ratio of Pulsed Bias on the Structure and Properties of TiCN Coatings by Hybrid Ion Plating[J]. China Surface Engineering, 2014, 27(4): 100-106.
[37] PADMANABHAN K A, SRIPATHI S, HAHN H, et al.Inverse Hall-Petch Effect in Quasi- and Nanocrystalline Materials[J]. Materials Letters, 2014, 133: 151-154.
[38] NI L, YANG T E, XIONG J, et al.Structure and Mechanical Properties of TiAlCrSiN Coatings Deposited on Ti(C, N)-NbC-Ni Cermets with Varied Mo2C Contents[J]. International Journal of Refractory Metals and Hard Materials, 2020, 86: 105083.
[39] 张冬青, 刘艳梅, 王子铭, 等. Mo含量对AlCrMoSiN涂层微观结构和性能的影响[J]. 表面技术, 2025, 54(1): 32-41.
ZHANG D Q, LIU Y M, WANG Z M, et al.Effects of Mo Content on Microstructure and Properties of AlCrMoSiN Coatings[J]. Surface Technology, 2025, 54(1): 32-41.
[40] 周琼, 王涛, 黄彪, 等. TiAlSiN涂层力学性能改善措施的研究现状及进展[J]. 表面技术, 2024, 53(8): 40-51.
ZHOU Q, WANG T, HUANG B, et al.Research Status and Progress of Improving Mechanical Properties of TiAlSiN Coatings[J]. Surface Technology, 2024, 53(8): 40-51.
[41] HUANG B, ZHANG E G, DU H M, et al.Effects of Annealing Temperature on the Microstructure, Mechanical and Tribological Properties of CrAlTiN Coatings[J]. Surface and Coatings Technology, 2022, 449: 128887.
[42] SUN P L, HSU C H, LIU S H, et al.Analysis on Microstructure and Characteristics of TiAlN/CrN Nano- Multilayer Films Deposited by Cathodic Arc Deposition[J]. Thin Solid Films, 2010, 518(24): 7519-7522.
[43] 田灿鑫, 邹长伟, 王泽松, 等. 基底偏压对电弧离子镀制备AlCrVN涂层微结构及力学性能的影响[J]. 表面技术, 2023, 52(3): 181-188.
TIAN C X, ZOU C W, WANG Z S, et al.Influence of Substrate Bias Voltage on Structure and Properties of AlCrVN Coatings Deposited by Cathodic Arc Ion Platings[J]. Surface Technology, 2023, 52(3): 181-188.
[44] FAN Q X, WANG T G, LIU Y M, et al.Microstructure and Corrosion Resistance of the AlTiN Coating Deposited by Arc Ion Plating[J]. Acta Metallurgica Sinica (English Letters), 2016, 29(12): 1119-1126.
[45] 付志强, 苗志玲, 岳文, 等. 脉冲偏压占空比对电弧离子镀TiAlN涂层的影响[J]. 稀有金属材料与工程, 2018, 47(11): 3482-3486.
FU Z Q, MIAO Z L, YUE W, et al.Influence of Duty Ratio of Pulsed Bias on TiAlN Coatings Deposited by Arc Ion Plating[J]. Rare Metal Materials and Engineering, 2018, 47(11): 3482-3486.
[46] DING X Z, TAN A L K, ZENG X T, et al. Corrosion Resistance of CrAlN and TiAlN Coatings Deposited by Lateral Rotating Cathode Arc[J]. Thin Solid Films, 2008, 516(16): 5716-5720.
[47] HOCHE H, PUSCH C, OECHSNER M.Establishing PVD-Coatings for the Corrosion Protection of Mild Steel Substrates for Complex Tribological and Corrosive Stresses[J]. Surface and Coatings Technology, 2019, 376: 74-83.
[48] INMAN S B, WISCHHUSEN M A, QI J, et al.Variation of the Passive Film on Compositionally Concentrated Dual-Phase Al0.3Cr0.5Fe2Mn0.25Mo0.15Ni1.5Ti0.3 and Implications for Corrosion[J]. Metallurgical and Materials Transactions A, 2024, 55(12): 4776-4795.

基金

国家自然科学基金(51401182); 中国国家留学基金项目(CSC202108410274); 河南省自然科学基金项目(242300420053); 河南省高层次人才国际化培养资助项目; 广东省基础与应用基础研究基金项目(2024A1515010753); 新型钎焊材料与技术国家重点实验室开放课题项目(SKLABFMT-2023-09); 郑州航空工业管理学院科研团队(23ZHTD01010); 郑州航空工业管理学院研究生教育创新计划项目(2025CX88)

PDF(18921 KB)

Accesses

Citation

Detail

段落导航
相关文章

/