HiPIMS/DCMS复合磁控溅射(Al0.5CoCrFeNiTi)Nx薄膜结构及性能研究OA
Structure and Properties of(Al0.5CoCrFeNiTi)Nx Thin Films Deposited by Hybrid HiPIMS/DCMS Magnetron Sputtering
目的 探究氮气流量比对(Al0.5CoCrFeNiTi)Nx薄膜化学成分、微观结构及性能的影响规律,提升GCr15轴承钢表面的力学性能和耐腐蚀性能.方法 采用高功率脉冲磁控溅射和直流磁控溅射复合方法,在GCr15轴承钢表面双靶共溅射(Al0.5CoCrFeNiTi)Nx高熵氮化物薄膜,通过X射线衍射仪、扫描电子显微镜、能谱仪、原子力显微镜对薄膜物相结构、微观形貌、化学成分、表面粗糙度进行表征,通过纳米压痕仪器、电化学工作站分别测试硬度(H)、弹性模量(E)和耐腐蚀性能.结果 随着氮气引入与增加,薄膜从非晶态转变为包含TiN、CrN等多种氮化物相的纳米晶结构;随N2/(N2+Ar)比值RN2 增大,"Al原子比"占"高熵元素原子比和"的百分含量由 7.91%提升至 9.89%(逐渐接近高熵靶材设计配比),Ti元素在金属元素中的占比由 47.62%降低至 36.14%;随RN2 增大,薄膜的H、H/E、H3/E2呈增大趋势,当RN2为 40%时达到最大,分别为22.694 GPa、0.069、0.110 GPa.当RN2 为 20%时,耐腐蚀性能最为优异,腐蚀电位较GCr15 基体提升37.895%,较不通氮气薄膜提升 18.146%,腐蚀电流密度较GCr15基体下降68.091%,较不通氮气薄膜下降58.514%.结论 (Al0.5CoCrFeNiTi)N0.2薄膜能够有效提升GCr15 轴承钢的耐腐蚀性能,N元素的引入能够显著提高(Al0.5CoCrFeNiTi)高熵合金薄膜的硬度和耐腐蚀性能.
As a more advanced surface modification technique,HiPIMS/DCMS hybrid magnetron sputtering fully leverages the synergistic advantages of the highly ionized plasma of HiPIMS(which enhances densification and interfacial adhesion of films)and the high deposition rate of DCMS(which ensures process efficiency)compared with individual HiPIMS or DCMS processes.In this study,an innovative method is employed with a high-power impulse power supply to sputter the Al0.5CoCrFeNi high-entropy alloy target,while a DC power supply is concurrently used to sputter the high-purity Ti target,so as to achieve precise control and efficient co-deposition of multiple metallic elements.By systematically adjusting the nitrogen flow ratio(RN2),the influence of reactive gas concentration on film composition evolution,crystalline structure transformation,and performance is thoroughly investigated.A SP-0606ASI magnetron sputtering vacuum coating system is employed for the hybrid deposition experiments.(Al0.5CoCrFeNiTi)Nx high-entropy nitride films are deposited on polished and cleaned GCr15 bearing steel and silicon wafer substrates at different nitrogen flow ratios(0,10%,20%,30%,and 40%by volume).During deposition,a Ti interlayer is first deposited at a constant current of 5 A for 10 minutes,followed by co-deposition of the functional(Al0.5CoCrFeNiTi)Nx high-entropy nitride layer via HiPIMS(constant power:1.5 kW,pulse width:40 μs,pulse frequency:25 000 Hz,deposition time:80 min)combined with DCMS(constant current:7 A,deposition time:80 min).Film microstructure and thickness are characterized by scanning electron microscopy(SEM),elemental composition at selected points is analyzed by energy-dispersive spectroscopy(EDS),and phase composition of the films is characterized by X-ray diffraction(XRD).Film hardness and elastic modulus are measured via nanoindentation(TI980).The electrochemical corrosion behavior of the films in a 3.5%NaCl solution is evaluated with a three-electrode system on a Princeton electrochemical workstation,and the electrochemical impedance spectra are fitted using Zview software.Nanocrystalline(Al0.5CoCrFeNiTi)Nx high-entropy nitride films are successfully fabricated on GCr15 bearing steel and silicon wafer substrates via HiPIMS/DCMS hybrid magnetron sputtering.With the introduction and increase of nitrogen,the films transition from an amorphous state to a nanocrystalline structure consisting of multiple nitride phases such as TiN and CrN.As the N2/(N2+Ar)ratio(RN2)increases,the atomic percentage of Al relative to the total high-entropy elements increases from 7.91%to 9.89%(gradually approaching the designed target composition),while the Ti proportion among metallic elements decreases from 47.62%to 36.14%.With the increasing RN2,film hardness(H)increases from 10.317 GPa to 22.7 GPa,while H/E and H3/E2 values increase simultaneously to 0.069 and 0.110 GPa,respectively.At RN2=40%,the hardness of the(Al0.5CoCrFeNiTi)N0.4 high-entropy nitride film is 119.967%higher than that of the Al0.5CoCrFeNiTi metallic film.At RN2=20%,the film exhibited optimal corrosion resistance:the corrosion potential increasing by 37.895%relative to the GCr15 substrate and by 18.146%compared with the nitrogen-free film,while the corrosion current density decreases by 68.091%and 58.514%,respectively.Simultaneously,its hardness(16.579 GPa)remains 60.696%higher than that of the nitrogen-free film.The introduction of nitrogen significantly improves both the hardness and corrosion resistance of(Al0.5CoCrFeNiTi)high-entropy alloy films.At the optimal nitrogen flow ratio(RN2=20%),the films exhibit the best corrosion performance along with excellent mechanical properties.Appropriate nitrogen incorporation not only enhances interfacial integrity but also effectively inhibits the penetration corrosive media.This study confirms that precise control of nitrogen flow can optimize the structure and performance of high-entropy nitride films,providing essential theoretical and technical guidance for the development of novel protective coatings suitable for harsh service environments.
王建刚;许美琦;刘瑞;王玉江
河北科技大学 材料科学与工程学院,石家庄 050018||河北科技大学 河北省短流程炼钢技术创新中心,石家庄 050018河北科技大学 材料科学与工程学院,石家庄 050018||河北科技大学 河北省短流程炼钢技术创新中心,石家庄 050018河北科技大学 材料科学与工程学院,石家庄 050018||河北科技大学 河北省短流程炼钢技术创新中心,石家庄 050018中国人民解放军陆军装甲兵学院 装备保障与再制造系,北京 100072
矿业与冶金
高熵氮化物薄膜高功率脉冲磁控溅射复合磁控溅射纳米晶硬度耐腐蚀性能
high-entropy nitride filmshigh power impulse magnetron sputteringhybrid magnetron sputteringnanocry-stallinehardnesscorrosion resistance
《表面技术》 2026 (8)
197-207,11
石家庄市科技计划项目(246081487A)2025 年度河北引智项目 the Shijiazhuang Science and Technology Planning Project(246081487A)Hebei High-Level Talent Attraction Program(2025)
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