射频磁控溅射制备(AlCrTiZrNb)N高熵合金薄膜的微观组织和力学性能

研究了氮含量对(Al Cr Ti Zr Nb)N高熵合金薄膜微观结构和力学性能的影响,利用射频磁控溅射工艺在不同N2和Ar流量比下制备了(Al Cr Ti Zr Nb)N高熵合金薄膜。结果表明,随着氮气流量的升高,(Al Cr Ti Zr Nb)N薄膜的沉积速率逐渐下降,Al Cr Ti Zr Nb合金薄膜的结构由非晶态转变为由Me-N(金属氮化物)构成的面心立方固溶体结构,(Al Cr Ti Zr Nb)N薄膜的择优生长取向为(200)晶面。同时随着N2流量的增加,(Al Cr Ti Zr Nb)N高熵合金薄膜的硬度首先快速升高,随后略微降低。当N2∶Ar=1∶1时,(Al Cr Ti Zr Nb)N薄膜硬度最大值28.324 GPa,此时(Al Cr Ti Zr Nb)N薄膜呈现单一的面心立方固溶体结构,饱和Me-N相的形成与各元素的固溶强化作用是其硬度的增长的主要原因。     

硬质合金表面TiAlZrCr/(Ti,Al,Zr,Cr)N梯度膜的微结构与力学性能

采用多弧离子镀技术,使用Ti-Al-Zr合金靶和Cr单质靶,在wc-8％co硬质合金基体上制备了TiAlZrCr／(Ti,Al,Zr,Cr)N多组元梯度膜.分析了梯度膜的成分、结构和微观组织,并研究了梯度膜的显微硬度和膜／基结合力.研究结果表明,该多组元梯度膜为Bl-NaCl型的TiN面心立方结构;薄膜的成分是以TiAlZrCr合金为过渡层的(Ti,Al,Zr,Cr)N梯度膜;薄膜的组织致密均匀,是典型的柱状晶结构;沉积偏压为-50～-200V时,梯度膜均可获得比(Ti,Al,Zr,Cr)N单层膜更高的硬度(最高值为HV4000)和膜／基结合力(临界载荷大于200 N).     

脉冲偏压对多弧离子镀TiAlN薄膜的成分和结构的影响研究

采用多弧离子镀在高速钢基底上沉积Ti Al N薄膜。利用扫描电镜(SEM)观测薄膜的表面形貌;用EDS分析薄膜表面的成分;用表面轮廓仪测试薄膜的厚度并结合沉积时间计算出沉积速率;用维氏硬度仪测量薄膜的硬度;用XRD表征薄膜的微观结构。结果表明,随着偏压峰值的增大,表面大颗粒逐渐减少,致密性逐渐变好,薄膜硬度也随之增加。沉积参数对薄膜成分有影响,偏压峰值对薄膜中Al含量有较明显的影响,而占空比则主要影响Ti含量。本文对实验结果进行了较详细的讨论和分析。     

Cr,Ni的掺杂对TiAlN基薄膜高温摩擦性能的影响

为了开发具有优异抗摩擦磨损性能的薄膜材料,采用多弧离子镀在4Cr13马氏体不锈钢表面沉积TiAlN薄膜,采用磁控溅射法和多弧离子镀在4Cr13表面分别沉积掺杂Cr和Cr-Ni的TiAlN薄膜.采用扫描电镜(SEM)、X射线衍射仪(XRD)和维氏硬度计分析薄膜的表面形貌、物相和表面硬度,并对不同温度下磨损后的薄膜表面形貌...     

脉冲偏压对304不锈钢表面多弧离子镀CrAlN薄膜结构和耐蚀性能的影响

目前,鲜见有关脉冲偏压对多弧离子镀Cr Al N薄膜耐蚀性能影响的报道。以不同的脉冲偏压在304不锈钢表面多弧离子镀Cr Al N薄膜。采用扫描电镜、显微镜、X射线衍射仪、硬度仪、粗糙度仪分析了Cr Al N薄膜的表面形貌、相结构、硬度、表面粗糙度及耐蚀性能,分析了脉冲偏压对相关性能的影响。结果表明:随着脉冲偏压幅值的增大,Cr Al N薄膜表面大颗粒及凹坑尺寸和数量减少,薄膜质量提高;Cr Al N薄膜主要由(Cr,Al)N相组成,随着偏压增加,Cr Al N薄膜出现(220)择优取向;Cr Al N薄膜表面粗糙度随脉冲偏压增大而减小,显微硬度随脉冲偏压的增大而增大;Cr Al N薄膜在3.5%Na Cl溶液中的耐蚀性随着脉冲偏压的增大而增大,脉冲偏压为400 V时,Cr Al N薄膜与基体304不锈钢的腐蚀速率之比为0.34,薄膜的综合性能最好。     

多弧离子镀(Cr,Ti,Al,Zr)N多组元超硬梯度膜的结构及性能

(Cr,Ti,Al,Zr)N梯度膜性能优异。采用多弧离子镀技术,使用Ti-Al-Zr合金靶和Cr单质靶在高速钢表面制备(Cr,Ti,Al,Zr)N多元超硬梯度膜,利用扫描电镜、能谱、X射线衍射仪、硬度计、划痕仪对膜层形貌、成分、结构、硬度、附着力进行分析,并通过热震性能试验考察了膜层的抗热震性能。结果表明:制备的膜层为面心立方结构,择优生长取向为(220)面;与TiN,(Ti,Al)N,(Ti,Cr)N,(Ti,Al,Zr)N等硬质膜相比,制备的(Cr,Ti,Al,Zr)N多元梯度膜具有更高的硬度和膜/基附着力,硬度可达4400HV,膜/基附着力大于200N,实现了从硬质膜到超硬膜的转变;膜层中N含量梯度可有效减少应力集中,Cr,Al含量的增加有利于提高膜层抗热震性能;负偏压对膜层硬度影响较大,对膜层成分、结构、抗热震性能影响较小,对膜/基附着力基本无影响。     

多弧离子镀(Ti,Al,Zr,Cr)N多组元氮化物膜的研究

采用多弧离子镀技术,使用Ti Al Zr合金靶和Cr靶,在W18Cr4V高速钢基体上沉积(Ti,Al,Zr,Cr)N多组元氮化物膜.利用扫描电镜(SEM)、电子能谱仪(EDS)和X射线衍射(XRD)对薄膜的成分、结构和微观组织进行测量和表征;利用划痕仪、显微硬度计测评薄膜的力学性能.结果表明,获得的多组元氮化物膜仍具有B1 NaCl型的TiN面心立方结构;薄膜的成分除-50V偏压外,其它偏压下的变化均不明显;增大偏压可减少薄膜表面的液滴污染,提高薄膜的显微硬度及膜/基结合力,最高值可分别达到HV3300和190N.     

多弧离子镀(Ti,Al,Zr)N多元超硬梯度膜的制备及力学性能研究

采用多弧离子镀技术并使用合金靶Ti-Al-Zr制备(Ti,Al,Zr)N多元超硬梯度膜。利用扫描电镜、X衍射仪对(Ti,Al,Zr)N膜层表面、断面形貌、成分、结构进行观察测定;系统考察了沉积工艺对(Ti,Al,Zr)N膜层质量、膜/基附着力和硬度的影响;并对膜层抗热震性进行了研究。通过与TiN,(Ti,Al)N,(Ti,Zr)N等硬质膜进行比较,发现采用Ti-Al-Zr合金靶制备的(Ti,Al,Zr)N多元梯度膜有更高的硬度和膜/基附着力,硬度可达4000 HV,实现了从硬质膜到超硬膜的转变;膜/基附着力大于200 N,同时对沉积工艺有较强的适应性。     

(Ti,Al)N薄膜的升温出气特性研究

介绍了采用多弧离子镀方法在不锈钢表面镀覆(Ti,Al)N薄膜,并对膜的结构、表面成分和形貌进行了简单分析,用热出气方法研究其出气特性,并与不锈钢的热出气性能进行比较,发现在不锈钢表面镀覆一层(Ti,Al)N膜可以有效地阻挡不锈钢体内氢扩散和碳偏析,因此(Ti,Al)N是比较理想的真空材料。     

溅射(Ti,Al)N薄膜的机械性能

运用直流平面磁控反应溅射在抛光淬火的TSA碳素工具钢上沉积(Ti,Al)N薄膜。研究了反应气体N_2流量与基片偏压对形成(Ti,Al)N薄膜的显微硬度的影响。在N_2流量约为10sccm,P_(N2)/P_(Ar),约为0.12与偏压U_B=200V时,(Ti,Al)N薄膜的显微硬度接近极大,可达3000kgf/mm~2。(Ti,Al)N薄膜划痕实验的临界负载L_c约为31N。磨损实验表明,(Ti,Al)N薄膜比淬火的T8A碳素工具钢基底具有好得多的耐磨损特性。微观分析表明(Ti,Al)N薄膜具有良好的抗氧化性能是由于氧化过程中在薄膜表面形成Al-O保护层。     

Deposition of TiN films on Co–Cr for improving mechanical properties and biocompatibility using reactive DC sputtering

This study reports the deposition of TiN films on Co–Cr substrates to improve the substrates’ mechanical properties and biological properties. In particular, the argon to nitrogen (Ar:N₂) gas flow ratio was adjusted to control the microstructure of the TiN films. A Ti interlayer was also used to enhance the adhesion strength between the Co–Cr substrate and TiN films. A series of TiN films, which are denoted as TiN-(Ar/N₂)1:1, Ti/TiN-(Ar/N₂)1:1, and Ti/TiN-(Ar:N₂)1:3, were deposited by reactive DC sputtering. All the deposited TiN films showed a dense, columnar structure with a preferential orientation of the (200) plane. These TiN films increased the mechanical properties of Co–Cr, such as the critical load during scratch testing, hardness, elastic modulus and plastic resistance. In addition, the biological properties of the Co–Cr substrates, i.e. initial attachment, proliferation, and cellular differentiation of the MC3T3-E1 cells, were improved considerably by deposition of the TiN films. These results suggest that TiN films would effectively enhance both the mechanical properties and biocompatibility of biomedical Co–Cr alloys.     

工艺参数对磁控溅射ZrN膜耐腐蚀性能的影响

为寻求真空磁控溅射ZrN膜耐蚀性与其溅射工艺间的规律,在1Cr18Ni9Ti不锈钢表面以不同的工艺参数真空磁控溅射了系列ZrN膜。通过中性盐雾试验确定了不同工艺参数所得ZrN膜的耐蚀性等级。结果表明:ZrN膜耐蚀性随N2流量的增加先增加,但超过15 mL/min后,膜的耐蚀性反而下降;ZrN膜耐蚀性随反应温度升高而增强;ZrN膜的耐蚀性随反应时间的增加越来越好,但超过15 min后,膜的耐蚀性不再增强;以ZrN膜的耐蚀性为依据,最佳溅射工艺参数为N2流量15 mL/min,反应时间15 min,反应温度200℃。     

钛合金表面加弧辉光离子渗镍铬及其性能研究

采用加弧辉光离子渗金属新技术处理钛合金Ti5Al2.5Sn表面,研究了渗层的相组成特点,成分分布情况,评价了改性层的磨擦摩损性能,及与钛合金基体间的接触腐蚀相容性等。结果表明加弧辉光离子渗技术可以快速地在钛合金表面获得NiCr镀渗复合层。渗层由Ni3Ti等金属间化合物组成,其硬度、耐磨性能均高于离子注氮层,具有较高的抗含Cl^-1水溶液腐蚀性能,在含Cl^-1腐蚀环境中与钛合金基体接触相容。     

Cr在多弧离子镀(Ti, Cr)N复合膜中的作用

利用AIP-01多弧离子镀膜机,通过改变铬靶电流,在高速钢基体上沉积出不同Cr含量的(Ti,Cr)N复合膜涂层,用扫描电子显微镜、微纳米力学测试仪和X射线对薄膜的表面颗粒、硬度及内应力进行了分析.结果表明薄膜中添加Cr能减小表面颗粒尺寸,提高硬度,当Cr的含量达到31%(wt%)时,薄膜硬度达到最高值,此时薄膜的内应力也最大.     

氮离子束轰击对电弧离子镀TiN膜层的作用

电弧离子镀膜层中"大颗粒"的存在,降低了膜层质量,限制了其进一步应用.采用俄罗斯UVN 0.5D2I离子束辅助沉积电弧离子镀设备,对高速钢W18Cr4V上沉积的TiN膜层进行了氮离子束轰击.结果表明:TiN膜层表面"大颗粒"完全消失,凹坑浅而平整,粗糙度降低.膜层中较软的Ti和Ti2N向TiN转变,TiN(111)取向逐渐减弱,而(200)取向逐渐增强.膜层的显微硬度由原来的1 980 HV1N升高到2 310HV1N.     

电弧离子镀TiN及其复合膜的腐蚀机理探讨

利用电弧离子镀在高速钢基体上制备了TiN及其复合膜（Ti，Cr）N，通过盐水全浸泡试验测量了薄膜的腐蚀速率。利用SEM观察了薄膜腐蚀后的表面形貌及断口形貌，并用其自带的能谱分析仪测量复合膜中Cr的含量，讨论了带有宏观熔滴颗粒的TiN及其复合膜（Ti，Cr）N的腐蚀机理。结果表明：高速钢表面电弧离子镀TiN和（Ti，Cr）N复合膜均可提高其耐腐蚀性能，薄膜的腐蚀主要有小孔腐蚀、缝隙腐蚀及电偶腐蚀。     

Al含量对(Ti,Al)N涂层结构性能的影响

(Ti，A1)N是20世纪80年代末期在TiN基础上发展起来的一种新型多元涂层材料。由于加入Al元素，(Ti，Al)N不但硬度、耐磨性优于TiN，而且大大改善了涂层的抗高温氧化性能。综述了Al元素在(Ti，Al)N涂层中的作用机理，以及Al含量对(Ti，Al)N涂层的晶体结构、抗高温氧化、硬度和耐磨性的影响。指出当Ti和Al的比例近似为1：1时，(Ti，Al)N涂层将获得优越的综合使用性能。     

室温磁控溅射制备(Ti,Zr)N薄膜及其性能研究

采用直流反应磁控溅射工艺,在载波片和Al基材上制备出金黄色的(Ti,Zr)N薄膜.(Ti,Zr)N薄膜具有比TiN薄膜更高的硬度和更强的耐腐蚀性能.用XRD衍射方法和扫描隧道显微镜对薄膜的晶体结构、微观表面形貌和电子结构进行了测试分析.XRD结果表明,(Ti,Zr)N薄膜为多晶态,存在TiN和ZrN两种分离相;从表面形貌可知,薄膜表面平整,晶粒排列致密且无连接松散的大颗粒;STS谱表明,Zr掺杂后,禁带宽度仍为1.64eV,但在禁带内增加了新能级,新能级的宽度分别为0.33eV和0.42eV,这也正是掺杂Zr后,薄膜仍呈现金黄色的主要原因.     

Morphological changes induced by thermal anneals in NiFe/Ag multilayers; their relation to the resistive and magnetoresistive properties

(Ti, Al)N films have drawn much attention as alternatives for TiN coatings, which are oxidized easily in air above 500 °C. We have investigated the effect of Al content on the oxidation resistance of (Ti_{1 − x}Al_x)N films prepared by r.f. reactive sputtering.

(Ti_{1 − x}Al_xN films (O ≤ x ≤ 0.55) were deposited onto fused quartz substrates by r.f. reactive sputtering. Composite targets with five kinds of Al-to-Ti area ratio were used. The sputtering gas was Ar (purity, 5 N) and N₂ (5 N). The flow rate of Ar and N₂ gas was kept constant at 0.8 and 1.2 sccm, respectively, resulting in a sputtering pressure of 0.4 Pa. The r.f. power was 300 W for all experiments. Substrates were not intentionally heated during deposition. The deposited films (thickness, 300 nm) were annealed in air at 600 900 °C and then subjected to X-ray diffractometer and Auger depth profiling.

The as-deposited (Ti_{1 − x}Al_x)N films had the same crystal structure as TiN (NaCl type). Al atoms seemed to substitute for Ti in lattice sites. The preferential orientation of the films changed with the Al content of the film, x. Oxide layers of the films grew during annealing and became thicker as the annealing temperature increased. The thickness of the oxide layer grown on the film surface decreased with increasing Al content in the film. For high Al content films an Al-rich oxide layer was grown on the surface, which seemed to prevent further oxidation. All of the films, however, were oxidized by 900 °C annealing, even if the Al content was increased up to 0.55.     

Effects of bias voltage on the microstructure and mechanical properties of (Ti,Al,Cr)N hard films with N-gradient distributions

(Ti,Al,Cr)N hard reactive films were deposited on high speed steel substrates by multi-arc ion plating (MAIP) technology using pure Cr and Ti-50Al(at.%) alloy targets. The partial pressure of N₂ was raised step by step in each deposition process. The surface morphology, the cross-sectional morphology of fracture sample, the surface compositions and the phase structure of the (Ti,Al,Cr)N films were investigated by scanning electronic microscope (SEM) and X-ray diffraction (XRD). The dense columnar microstructure was obtained in all of the (Ti,Al,Cr)N films, though micro-droplets evidently existed on the surface of the films. The micro-hardness of the film surface, the adhesive strength of the film/substrate and the thermal shock resistance were investigated. The results revealed the effects of bias voltage on the composition, phase structure, and mechanical properties. The improved balanced properties of a micro-hardness of about 50 GPa, an adhesive strength larger than 200 N and a thermal shock resistance of 7-8 cycles were reached at a bias voltage of 150 V. The present super-hard (Ti,Al,Cr)N films with N-gradient distribution may be an actual substitution of TiN, (Ti,Al)N, (Ti,Cr)N and single-layer (Ti,Al,Cr)N hard films.