偏压对GLC镀层的结构及应力的影响研究

采用磁控溅射离子镀技术制备了类石墨镀层（GLC）,利用扫描电子显微镜（SEM）测量了镀层的厚度、X射线衍射仪（XRD）研究了材料的物相和应力,并结合透射电子显微镜（TEM）观察和分析了材料的组织结构。研究结果表明：不同偏压下得到的镀层结构相同,均为非晶为主的类石墨镀层,并且随着偏压增大,膜厚逐渐减小;在所研究的偏压下,应力变化规律是随着偏压的增加,样品与基体的复合应力先增大,后减小,其中～65V时达到最大值。     

Deposition of dense and smooth Ti films using ECR plasma-assisted magnetron sputtering

We report high quality Ti films grown in a novel electron cyclotron resonance (ECR) plasma-assisted magnetron sputtering (PMS) deposition system. The films are compared with films deposited by conventional direct current (DC) magnetron sputtering. Using ECR-PMS, the argon plasma bombardment energy and Ti film deposition rate can be controlled separately, with the substrate bias voltage under feedback control. Results from SEM, AFM, XRD and PAS (scanning electron microscopy, atomic force microscopy, X-ray diffraction and positron annihilation spectroscopy) show that the properties of Ti films prepared by ECR-PMS are greatly improved compared with conventional sputtering. SEM and AFM confirmed that ECR-PMS Ti films have a dense, smooth, mirror-like surface. Increasing the substrate bias of the ECR plasma from − 23 V to − 120 V while keeping a fixed sputtering bias voltage of − 40 V, the intensity of the (100) reflection of Ti film was a little strengthened, but (002) remained strongly preferred orientation. The XRD peak broadening of ECR-PMS Ti films is more than for conventional magnetron sputtering, due to grain refinement induced by Ar ion bombardment. Doppler broadening of PAS analysis reveals that the Ti films have fewer vacancy defects compared with films prepared by the conventional magnetron.     

Formation of nanocrystalline microstructure in arc ion plated CrN films

Applying negative bias voltages caused significant microstructure changes in arc ion plated CrN films. Nanocrystalline microstructures were obtained by adjusting the negative bias voltage. Structural characterizations of the films were carried out using X-ray diffractometry (XRD) and high-resolution transmission electron microscopy (HR-TEM). The results indicated that increasing ion bombardment by applying negative bias voltages resulted in the formation of defects in the CrN films, inducing microstructure evolution from micro-columnar to nanocrystalline. The microhardness and residual stresses of the films were also affected. Based on the experimental results, the evolution mechanisms of the film microstructure and properties were discussed by considering ion bombardment effects.     

Effect of substrate bias voltage on the texture and microstructure of Cu thin films deposited by ion beam deposition

Cu thin films deposited by non-mass separated ion beam deposition under various substrate bias voltages were investigated. The film textures and microstructure were analyzed by X-ray diffraction and field emission scanning electron microscopy, and the resistivity of the film was measured with the Van der Pauw method. It was found that the optimum negative substrate bias voltage for Cu films was −50 V. The Cu films deposited without substrate bias voltage showed a columnar grain structure with small grains and random orientation. However, when a substrate bias voltage of −50 V was applied, the Cu films had a non-columnar structure with a strong (111) texture and large grains. The electrical resistivity of the Cu films decreased remarkably with increasing negative substrate bias voltage, and reaching a minimum value of 1.8±0.13 μΩ cm at the substrate bias voltage of −50V.     

TA2纯钛H3PO4溶液阳极氧化着色膜的表征和电化学分析

利用恒压控制阳极氧化法在H3PO4溶液中于TA2纯钛表面制备了不同颜色的氧化膜,利用扫描电镜、X射线能谱仪、X射线衍射仪、X射线光电子能谱仪分析了着色膜的形貌、成分、物相和价态,使用电化学工作站在Hank’s模拟体液中研究了着色膜的Tafel极化曲线和电化学阻抗谱(EIS)。结果表明:SEM显示着色膜由一层表面多孔、内层致密的膜层构成;EMAX显示膜层由单一的Ti和O元素构成;XRD和XPS显示膜层主要由Ti4+和O2-组成,呈非晶态TiO2结构;Tafel极化曲线显示随着电压升高,着色膜腐蚀电位正移、腐蚀电流密度下降;EIS显示随着电压升高,着色膜容抗弧半径增大、阻抗值增加,耐腐蚀性提高。     

脉冲磁控溅射MoS2涂层的组织结构及摩擦学性能

采用单极性脉冲磁控溅射技术在A286基体表面制备MoS₂低摩擦系数涂层(LFC)。利用XRD、SEM等手段表征涂层的成分与微观组织;采用原位纳米力学测试系统、球-盘式摩擦磨损试验机分析涂层的力学和摩擦学性能,并探讨了脉冲偏压对涂层结构、力学和摩擦学性能的影响。结果表明,脉冲偏压由300V增加到600V,MoS₂涂层择优取向发生了(002)向(100)转变,当脉冲偏压增至800V时又恢复(002)择优取向,;随着脉冲偏压的增加,涂层的硬度及弹性模量出现先减少后增大趋势,摩擦系数在0.065~0.076范围内波动,呈现出先增加后减小趋势;偏压为800V的涂层摩擦学性能最佳,其磨损率仅为基体的13.5%。     

Formation of nanocrystalline microstructure in arc ion plated CrN films

Applying negative bias voltages caused significant microstructure changes in arc ion plated CrN films. Nanocrystalline microstructures were obtained by adjusting the negative bias voltage. Structural characterizations of the films were carried out using X-ray diffractometry (XRD) and high-resolution transmission electron microscopy (HR-TEM). The results indicated that increasing ion bombardment by applying negative bias voltages resulted in the formation of defects in the CrN films, inducing microstructure evolution from micro-columnar to nanocrystalline. The microhardness and residual stresses of the films were also affected. Based on the experimental results, the evolution mechanisms of the film microstructure and properties were discussed by considering ion bombardment effects.     

Effect of negative substrate bias voltage on the nucleation and growth of Cu films during the initial stage of ion beam deposition

We focused the effect of a negative substrate bias voltage on the nucleation and growth of Cu films during the initial stage of ion beam deposition. The resultant microstructure of Cu films was observed by atomic force microscopy (AFM). It was found that Cu films with or without a negative substrate bias voltage have a different dependence of nucleation and growth. It was established that the mechanism of nucleation and growth of Cu films is changed to a progressive nucleation and lateral growth by a sufficient migration of adatoms accelerated by applying a negative substrate bias voltage.     

基片负偏压对Cu膜纳米压入硬度及微观结构的影响

测试了不同溅射偏压下Cu膜的纳米压入硬度，探讨了溅射偏压、残余应力及压痕尺寸效应对Cu膜硬度的影响。结果表明，随着溅射偏压的增大，薄膜晶粒尺寸及残余压应力均减小，导致薄膜的硬度增大，并在-80V达到最大值，随后有所降低。同时薄膜中的压痕尺寸效应对薄膜硬度随压入深度的分布有很大的影响。     

基体脉冲偏压对TiN/Cu纳米复合薄膜组织结构、力学及耐磨性能的影响

本文采用轴向磁场增强电弧离子镀在高速钢基体上沉积了TiN/Cu纳米复合薄膜,研究了基体脉冲偏压幅值对薄膜成分、结构、力学性能及耐磨性能的影响。结果表明,薄膜中铜含量随着脉冲偏压幅值的增加先增加而后降低,在一个较低的范围内(1.3-2.1at.%)。X射线衍射结果表明所有的薄膜均出现TiN相,并未观察到Cu相。薄膜的择优取向随着脉冲偏压幅值的增加而改变。薄膜的最高硬度为36GPa,是在脉冲偏压幅值为-200V时得到的,对应了1.6at.%的Cu含量。与纯的TiN薄膜相比,Cu的添加明显增强了薄膜的耐磨性能。     

Hexagonal diamond formation on steel substrates by negative bias microwave plasma enhanced chemical vapor deposition

This paper reports for the first time the synthesis of hexagonal diamond thin films on high-speed steel substrates by multi-mode microwave plasma enhanced chemical vapor deposition. Before deposition of the films, the substrate surface was treated by scratching with diamond powder. The deposited films were characterized by X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy. The XRD patterns of (100) and (101) planes and the Raman peaks at ~ 1317-1322 cm^− 1 were observed, confirming the formation of hexagonal diamond phase in the prepared films. The effects of voltage bias on the phase formation, microstructure and hardness of the films were also studied by setting the voltage to 0, − 70, − 150 and − 190 V. The highest hardness of 23.8 GPa was found in the film having clusters of size about 550 nm deposited under a bias voltage of − 150 V. These clusters were built up of grains of size about 14 nm.     

Cu-Ti合金薄膜的微结构和力学性能

通过磁控共溅射方法制备了一系列不同Ti含量的Cu-Ti合金薄膜,采用EDS、XRD、TEM、AFM和纳米力学探针表征了薄膜的微结构和力学性能,研究了化合物对超过饱和固溶薄膜的强化作用。结果表明,由于溅射粒子的高分散性和薄膜生长的高非平衡性,Cu-Ti薄膜形成了超过饱和固溶体,晶格的剧烈畸变使Cu固溶体晶粒迅速细化。随Ti含量的增加,薄膜中产生高分散的细小Cu Tix化合物,并逐步形成Cu超过饱和固溶体纳米晶和细小化合物分布于非晶基体中的结构。与微结构的变化相应,薄膜的硬度随Ti含量的增加持续提高,并在含21.4%Ti(原子分数)时达到8.7GPa的最高值。高分散金属间化合物的存在是Cu-Ti合金薄膜在形成非晶结构后硬度得以继续提高的原因。     

Effect of the aluminium content and the bias voltage on the microstructure formation in Ti1 − xAlxN protective coatings grown by cathodic arc evaporation

The effect of aluminium contents and bias voltage on the microstructure of cathodic arc evaporated Ti_1 − xAl_xN coatings was investigated with the aid of X-ray diffraction experiments and transmission electron microscopy. The coatings were deposited from mixed Ti-Al targets with different Ti:Al ratios (60:40, 50:50, 40:60 and 33:67) at bias voltages ranging between − 20 V and − 120 V. The microstructure of the coatings was described in terms of the phase composition, crystallite size and residual stress and related to the indentation hardness. The microstructure features were found to be related to the uniformity of the local distribution of Ti and Al in (Ti,Al)N, which was controlled, for a certain overall chemical composition of the coatings, by the bias voltage. The consequences of large local fluctuations of the Ti and Al concentrations in Ti_1 − xAl_xN that occurred at higher bias voltages were the phase segregation, which was indicated through the formation of the fcc-(Ti,Al)N/fcc-AlN nanocomposites and the increase of the compressive residual stress in the face-centred cubic (Ti,Al)N. Concurrently, the increasing bias voltage contributed significantly to the reduction of the crystallite size. Higher residual stress and smaller crystallite size increased the hardness of the coatings. The overall chemical composition of the coatings influenced mainly their phase composition. The high concentration of Al in (Ti,Al)N led to the formation of wurtzitic AlN in the coatings.     

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

沉积偏压对涂层的结构与性能具有重要影响,为研究其对AlCrTiN纳米复合涂层成分、组织结构、力学与抗高温氧化性能的影响规律,采用磁控溅射技术,改变沉积偏压(-30、-60、-90、-120 V)制备四种AlCrTiN纳米复合涂层。利用X射线衍射仪、扫描电子显微镜、纳米压痕仪等仪器表征涂层的组织结构、成分、力学性能和抗高温氧化性能。研究结果表明：不同偏压下制备的AlCrTiN纳米复合涂层均为NaCl型fcc-(Al,Cr,Ti)N相结构。随着沉积偏压增大,涂层由沿(111)晶面择优生长转变为无明显的择优生长取向,晶粒尺寸降低,残余应力和硬度增大。偏压为-90 V与-120 V时,涂层表面更加致密,具有更高的硬度和弹性模量。在800℃与900℃氧化1 h后,所有涂层表面均生成一层连续致密的Al₂O₃膜。随着沉积偏压增加,氧化膜厚度逐渐降低,表明抗高温氧化性能逐渐增强,这是因为高偏压下涂层组织更致密,且晶粒更细小。研究成果对AlCrTiN纳米复合涂层的综合性能提升与工程化应用具有一定指导意义。     

脉冲偏压对TiAlCN薄膜结构与力学性能的影响

利用多弧离子镀-磁控溅射复合技术通过改变脉冲偏压在Si片与SS304基体表面制备了TiAlCN薄膜,研究了不同脉冲偏压对薄膜结构和力学性能的影响。薄膜成分、表面形貌、相结构及力学性能分别利用能量弥散X射线谱(EDS)、扫描电镜(SEM)、X射线衍射(XRD)和纳米压痕仪等设备进行表征。结果表明,随着脉冲负偏压的增加,薄膜中Ti元素的含量先减小后增大,而Al元素有相反的变化趋势。适当增大脉冲偏压,薄膜表面颗粒、凹坑等缺陷得到明显改善。物相分析表明TiAlCN薄膜主要由(Ti,Al)(C,N)相,Ti4N3-x相和Ti3Al相组成。薄膜平均硬度与弹性模量随脉冲负偏压的增加先增大后减小,在负偏压-200 V时达到最大值分别为36.8 GPa和410 GPa。     

STUDY ON COMPOSITION, MICROSTRUCTURE AND HARDNESS OF DLC FILMS BY VCAD

DLC super-hard films have been deposited on the substrates of single crystalline Si, pure Ti and stainless steel 18-8 by a method of vacuum cathode arc deposition (VCAD). The composition, microstructure and micro-hardness of the films have been studied in this paper. The results indicate that hardness of the DLC films is different on the different substrates. Hardness of the films increases with decreasing in surface roughness of the films. The maximum value of micro-hardness belongs to the DLC films deposited under the hydrogen pressure of 0.35Pa and the negative bias of 100V.     

Improvement of the wear resistance of titanium alloyed with boron nitride by electron beam irradiation

Surface alloying of commercially pure titanium was carried out with an electron beam (EB) apparatus using a boron nitride powder which was previously deposited on its surface by Atmospheric Plasma Spraying (APS) in order to produce a composite layer with high wear resistance.Electron beam surface alloying is an important surface engineering routine that involves melting of a pre-deposited layer or concomitantly added alloying elements/compounds with a part of the underlying substrate by direct energy electron beam irradiation to form an alloyed zone characterized by a novel microstructure and composition.The present study is concerned with the influences of EB-remelting process on the wear resistance of the alloyed titanium material. The microstructure, corrosion resistance and phase analysis were also examined. Scanning electron microscopy (SEM), light microscopy (LM) and X-ray Diffraction (XRD) were performed to characterize the phase modification and morphology after the EB treatment. The sliding wear as well as the hardness of the remelted material was significantly improved (in comparison with pure Ti) through this alloying technique. The corrosion behaviour of the modified surfaces was compared with that of Ti in order to demonstrate that its initial good corrosion resistance is not strongly influenced due to surface alloying.     

多弧离子镀Ti-Al-Zr-Cr-N系双层膜的结构与力学性能

采用多弧离子镀技术和Ti-Al-Zr合金靶及Cr单质靶,在WC-8%Co硬质合金基体上制备了(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N和Cr N/(Ti,Al,Zr,Cr)N 2种四元双层氮化物膜。利用扫描电镜(SEM)、能谱仪(EDS)和X射线衍射仪(XRD)分析2种双层膜的微观组织、成分和结构;利用划痕仪和显微硬度计对比2种双层膜的力学性能。结果表明,获得的2种双层膜均具有B1-NaCl型的TiN面心立方结构;双层膜的组织均是典型的柱状晶结构;沉积偏压为–50~–200 V时,双层膜的力学性能均优于(Ti,Al,Zr,Cr)N单层膜,并与Ti-Al-Zr-Cr-N系梯度膜的力学性能相当,同时(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N双层膜可获得更高的硬度(HV_(0.01)最高值为41 GPa),而CrN/(Ti,Al,Zr,Cr)N双层膜可获得更强的膜层与基体间结合力(所有值均大于200 N)。     

纯钛表面激光熔覆铁基耐磨涂层结构及摩擦学性能(英文)

利用激光熔覆技术在纯钛表面制备铁基涂层。用 XRD、SEM、TEM分析涂层的相组成和晶体结构。在UMT-2MT摩擦磨损试验机上对铁基涂层在不同载荷和不同滑动速度下的摩擦磨损性能进行测试。用SEM和3D表面轮廓仪分析铁基涂层磨损后的表面形貌和磨屑形貌。结果表明:钛表面激光熔覆制备的铁基涂层的显微硬度约为860HV0.2,具有优异的耐磨性能,磨损率为(0.70～2.32)×10-6mm3/(N·m),可以显著提高纯钛基材的耐磨性能;涂层的磨损机理为轻微的磨粒磨损和粘着磨损。     

Structure and properties of Ti–Al–Y–N coatings deposited from filtered vacuum-arc plasma

Ti_0.5Al_0.5N coatings with a small amount of Y (up to 1 at.%) were deposited by filtered vacuum arc plasma at pulsed high voltage negative substrate bias potential with amplitude up to 2.5 kV and their microstructure was studied. X-ray fluorescence analysis showed that this deposition method allows ensuring well the conformity of the elemental composition of the metallic components of cathodes and films. X-ray diffraction measurements of the films with yttrium revealed a solid solution (Ti,Al)N phase with a cubic NaCl-type structure as the only crystalline phase. The films deposited with an amplitude of the substrate bias potential in the range of 1–1.5 kV were characterized by a strong axial texture [110]. In these films an increase of the yttrium content leads to the reduction of the nitride lattice parameter and growth of coherent scattering zone dimension as well as to a decrease of the surface roughness. Coatings containing 1 at.% Y exhibited high hardness of 32–36 GPa and oxidation resistance.