非平衡磁控溅射氮化钛薄膜及其性能研究

采用非平衡磁控溅射技术,在钛合金(Ti6Al4V)表面沉积氮化钛薄膜。通过改变氮气和氩气分压比(PN/PAr)和基体偏压,制备出不同结构、性能的氮化钛薄膜。采用X射线衍射技术、原子力显微镜、PS-168型电化学测量系统、CSEM球盘摩擦磨损实验机、HXD-1000 knoop显微硬度仪等研究了薄膜的结构、表面形貌、耐腐蚀性能与机械性能。结果表明,采用非平衡磁控溅射技术制备出了致密的氮化钛薄膜。当PN/PAr较小时,氮化钛薄膜中存在Ti2N时,Ti2N相可以有效提高薄膜的硬度和耐磨损性能;当PN/PAr增加到0.1时,薄膜硬度达到最大,耐磨损性能最优;随着PN/PAr的继续增大,氮化钛薄膜中主要存在TiN相,氮化钛薄膜的复合硬度和耐磨损性能降低。在钛合金(Ti6Al4V)表面沉积氮化钛薄膜可以显著提高其在Hanks类体液中的耐腐蚀性能。     

基底负偏压对直流磁控溅射CrN薄膜择优取向及表面形貌的影响

直流磁控溅射法制备不同基底负偏压下的CrN薄膜,采用XRD分析薄膜相结构,EDS分析薄膜表面成分,SEM观察薄膜表面形貌,并对偏压作用机制进行了探讨。结果表明,当Ar流量6ml/min、N2流量30ml/min时,在基底负偏压增大过程中,CrN薄膜始终由CrN相组成,但薄膜生长发生了(111)(-50V)向(200)(-125V)再向无明显择优生长(-225V)的转变。低偏压时,CrN薄膜[111]向[200]取向转变主要是轰击表面氮离子浓度增加导致;高偏压时,薄膜中Ar浓度大幅增长,高能离子长时间轰击破坏晶粒取向性,使薄膜呈无择优取向。同时,负偏压增加使薄膜表面形貌从具有棱角的不规则形状逐渐变为粒状结构,且晶粒逐渐细小。     

用XPS和AFM等方法研究氮化钛薄膜的物理化学特性

采用反应非平衡磁控溅射方法制备了氮化钛(TiN)薄膜,沉积时的衬底偏压的范围从0V到-500 V.实验结果表明:TiN薄膜的物理特性和力学性能随衬底偏压变化,最佳的薄膜硬度与弹性模量在偏压为-100 V时得到.AFM的测量结果显示薄膜的表面形貌和粗糙度随衬底偏压变化有一个非线性的变化趋势,同样的趋势也出现在Ti2p和N1s的芯态能谱上.特定谱峰的强度和位置的变化预示着偏压引起的薄膜成分和化学态的变化,XPS的结果表明:适当的偏压有助于TiN的成键,稳定的化学结构防止了表面的氧化和扩散,抑制了杂质和缺陷的形成,良好的机械特性归于表面形貌的改善.     

304不锈钢磁控溅射TiNx薄膜不同偏压时的结构和耐蚀性能

基体偏压是影响磁控溅射TiNx薄膜结构和性能的关键因素,且TiNx薄膜的结构与其耐蚀性有极大的关系.利用直流反应磁控溅射技术,通过改变基体偏压在304不锈钢表面制备了具有结构缺陷和不同化学计量比的TiNx薄膜.采用原子力显微镜(AFM)、X射线衍射、场发射扫描电子显微镜、电化学技术研究了TiNx薄膜的表面形貌、相结构和耐蚀性与偏压的关系.结果表明:TiNx薄膜的表面结构与偏压明显相关,适当的偏压有利于获得细小、均匀、致密和光滑的TiNx薄膜;TiNx薄膜为B1-NaCl型面心立方结构,其择优取向为(111)面,增加偏压有利于获得符合化学计量比的TiNx薄膜;致密、光滑和符合化学计量比的TiNx薄膜具有更低的腐蚀倾向;不同化学计量比的TiNx薄膜的腐蚀均为局部剥离,且与该处高密度结构缺陷相关;减少TiNx薄膜的针孔等结构缺陷对于提高其耐蚀性极为重要.     

纳米氮化钛薄膜对高频陶瓷窗片二次电子发射率的影响研究北大核心CSCD

纳米TiN薄膜可用来抑制高频陶瓷窗片的二次电子倍增,缩短器件高功率老炼时间,提高微波发射性能。文章通过专用真空镀膜设备,采用同轴圆柱靶和平面靶的直流磁控反应溅射方法,通过优化制备工艺参数,在陶瓷窗片的表面成功制备了纳米氮化钛(TiN)薄膜。采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、X射线光电子能谱仪(XPS)等现代分析手段进行了测试分析,结果表明:纳米TiN薄膜表面晶粒细小,致密度较好;晶面(111)和(200)特征衍射峰峰型规整,峰宽细窄;Ti/N原子计量比接近于1∶1。随着薄膜沉积时间增加,二次电子发射系数(SEY)逐渐增大,溅射时间8.4 s时,SEY为1.72;随着基体偏压的增加,电离效率增加,SEY不断降低,当偏压为350 V时,SEY为1.89;随着N2流量增加,SEY发生变化,当N2流量为38 mL/min时,SEY为1.83。     

氮气流量对CIGS薄膜结构和形貌的影响

采用中频交流磁控溅射方法,在Mo层上沉积了CuInGa(CIG)预制膜.以N2为载气,采用固态硒化法制备获得了Cu(In1-xGax)Se2(CIGS)吸收层薄膜,考察了N2流量对CIGS薄膜结构和形貌的影响.采用SEM和EDS观察和分析了薄膜的表面形貌和成分,采用XRD表征了薄膜的组织结构.结果表明,在不同的N2流量下制备的CIGS薄膜,均具有单一的黄铜矿相结构,薄膜具有(112)面的择优取向.当Ar流量为0.40m3/h时,薄膜表面结构致密,晶粒大小均匀,并且Cu、In、Ga原子含量,处于制备弱p型CIGS薄膜的理想范围.     

烧结NdFeB磁体表面沉积Ni膜及其耐腐蚀性

为改善烧结钕铁硼(NdFeB)磁体的耐腐蚀性能,在磁体表面用磁控溅射方法制备了Ni薄膜。利用扫描电子显微镜(SEM)观察了Ni薄膜的组织形貌,利用电化学测试、中性盐雾试验(NSS)测试了镀膜样品的耐腐蚀性能,研究了溅射功率和负偏压对Ni薄膜组织结构、电化学性能和中性盐雾环境下耐腐蚀性能的影响。结果表明:Ni薄膜的厚度和致密性是影响其耐腐蚀性能的关键因素;随溅射功率增大,Ni薄膜厚度增大,但晶粒尺寸变大、致密性降低,耐腐蚀性能先升高后降低;加负偏压后,Ni薄膜厚度有所减小,但膜层表面更加光滑、组织更加致密均匀,因此镀膜样品耐腐蚀性能有所提高;在溅射功率为100~120 W、负偏压为150 V条件下制备的磁控溅射镀Ni样品具有最好的耐腐蚀性能。     

在室温条件下制备高质量纳米结构TiN薄膜研究

在室温条件下,利用磁过滤等离子体在单晶硅和不锈钢表面上制备了性能优异的纳米结构TiN薄膜.运用原子力显微镜和掠角入射X射线衍射仪对其结构与形貌进行了表征,利用纳米压痕仪测量了TiN薄膜的硬度和弹性模量.结果表明:TiN薄膜表面光滑,致密,无柱状晶;TiN晶粒的平均尺寸为50nm,薄膜硬度达50 GPa,是传统CVD和PVD技术沉积氮化钛的两倍多;XRD衍射试验表明,纳米TiN的衍射角都普遍向小角度移动,TiN晶粒沿(111)择优生长.     

高功率脉冲磁控放电等离子体注入与沉积CrN薄膜研究

采用高功率脉冲磁控放电等离子体离子注入与沉积的方法在不锈钢基体上制备了高膜基结合力的CrN硬质薄膜,并研究了不同的Ar/N流量比对薄膜形貌、结构及性能的影响.采用扫描电子显微镜、X射线衍射对其表面形貌和结构进行分析,发现制备的薄膜表面光滑、致密,相结构单一,主要是CrN(200)相.对薄膜的结合力、硬度、弹性模量、耐磨...     

Cr及Cr-Ni掺杂对不同偏压下TiAlN薄膜性能的影响

为了使4Cr13不锈钢表面性能得到更好的优化和获得镀膜最佳的偏压工艺,在不同的偏压工艺下,采用多弧离子镀技术和磁控溅射技术在4Cr13不锈钢表面沉积掺杂Cr和同时掺杂Cr、Ni的TiAlN薄膜.采用附着力自动划痕仪研究不同偏压条件下薄膜与基体的结合力,采用扫描电子显微镜观察和分析薄膜的表面形貌,采用XRD技术检测薄膜的相结构,采用显微硬度计测量薄膜的显微硬度.结果表明:适当的偏压可以提高薄膜的硬度和结合力,在偏压为-250 V时,薄膜的表面硬度达到最大值2 259 HV0.1 N,结合力为36 N;并且掺杂Ni元素能够起到增强膜基结合力的效果.     

脉冲偏压电弧离子镀制备C_(1-x-y)N_xZr_y超硬复合薄膜

用脉冲偏压电弧离子镀方法在保持石墨靶弧流恒定的条件下,通过同步改变锆靶弧流与氮流量,在硬质合金基体上制备了一系列不同成分的C1-x-yNxZry复合薄膜.随着锆靶弧流与N流量增加,薄膜中Zr与N含量都呈线性增加,同时C含量快速减少.Raman光谱显示所制备的薄膜具有DLC特征,而XRD结果显示薄膜中还存在有明显的ZrN晶体相,说明本实验所制备的薄膜属于在DLC非晶基体上匹配有ZrN晶体相的碳基复合薄膜.随Zr与N含量增加,薄膜硬度先增大后降低,当x=0.19,y=0.28时薄膜具有最高硬度值,为43.6GPa,达到了超硬薄膜的硬度值.     

Influence of Experimental Parameters on Reactive Magnetron Sputtering CN_x Thin Films

Carbon nitride thin films were deposited on Si(001) using unbalanced magnetron sputtering at different experimental parameters. The effects of nitrogen partial pressure, substrate temperature and substrate bias on the deposition rate and nitrogen content are discussed.     

Physical and mechanical properties of reactively sputtered chromium boron nitride thin films

This paper reports on the first study of physical and mechanical properties of reactively sputtered chromium boron nitride coatings as a function of chemical composition, bias voltage and substrate temperature. Several sets of coatings were deposited by reactive unbalanced magnetron sputtering on Si(100) substrates. The chemical composition was deduced from X-ray photoelectron spectroscopy and Auger electron spectroscopy measurements, and was found to be influenced primarily by nitrogen flow rate. The phase composition was determined using X-ray diffraction in conjunction with spectroscopic ellipsometry. Atomic force microscopy was utilized to determine surface roughness and average surface grain size. Both surface roughness and surface grain size were largely independent of the nitrogen concentration and decreased with increasing bias voltage. The nanohardness and elastic modulus of each sample were measured by nanoindentation. The hardest films were produced using −150 V bias voltage and either very low (0.5-1 sccm) or very high (12-15 sccm) nitrogen flow rates.     

Photoacoustic measurement of thermal properties of TiN thin films

Titanium nitride (TiN) thin films were prepared by reactive DC magnetron sputtering under different nitrogen flow rates and at constant substrate temperature as well as at constant nitrogen flow rate and at different substrate temperatures. Photoacoustic measurement of the thermal properties of the films revealed that the thermal diffusivity and thermal conductivity of the TiN thin films are significantly lower than the bulk values and that the grain size of the films has substantial influence on the thermal properties of TiN thin films. The thermal conductivity of the films decreases with increasing nitrogen flow rates and increases with increasing substrate temperature. The above opposing behaviour in the thermal properties is found to be related to the microstructure, especially, the grain size of the films.     

Magnetron sputter deposition of low-stress, carbon-containing cubic boron nitride films using Ar―N2―CH4 gas mixtures

Cubic boron nitride (c-BN) films produced by PVD and plasma-assisted CVD techniques typically exhibit undesired high compressive stresses. One of the effective and feasible methods to reduce stress and hence improve film adhesion has been a controlled addition of a third element into the film during deposition. In the present study, BN films were grown on to silicon substrates using reactive magnetron sputtering with a hexagonal BN target. An auxiliary flow of methane was mixed into argon and nitrogen as the working gas. The deposition was conducted at various methane flow rates at 400 °C substrate temperature, 0.2 Pa total working pressure, and − 250 V r.f. substrate bias. The microstructure of the deposited films was then examined in dependence of the methane flow rate. With increasing methane flow rate from 0 to approx. 2.0 sccm, the fraction of the cubic BN phase in the deposited films decreased gradually down to approx. 75 vol.%, whereas the film stress was reduced much more rapidly and almost linearly in relation to the methane flow rate. At 2.1 sccm methane, the stress became approx. 3 times reduced. Owing to the significantly decreased film stress, adherent, micrometer thick, cubic-phase dominant films can be allowed to form on silicon substrate. The microstructure of the films will be illustrated through FTIR and XRR.     

直流负偏压对类金刚石薄膜结构和性能的影响

利用直流-射频-等离子体增强化学气相沉积技术在单晶硅表面制备了类金刚石薄膜，采用原子力显微镜、Raman光谱、X射线光电子能谱、红外光谱、表面轮廓仪和纳米压痕仪考察了直流负偏压对类金刚石薄膜表面形貌、微观结构、沉积速率和硬度等性能的影响。结果表明：无直流负偏压条件下，薄膜呈现有机类聚合结构，具有较低的SP3含量和硬度；叠加上直流负偏压后，薄膜具有典型的类金刚石结构特征，SP3含量和硬度得到了显著的提高；但随着直流负偏压的升高，薄膜的沉积速率和H含量逐渐降低，而SP3含量和硬度在直流负偏压为200V时出现最大值，此后逐渐降低。     

Influence of microstructure and chemical composition of sputter deposited TiO<Subscript>2</Subscript> thin films on in vitro bioactivity

Functionalisation of biomedical implants via surface modifications for tailored tissue response is a growing field of research. Crystalline TiO₂ has been proven to be a bone bioactive, non-resorbable material. In contact with body fluids a hydroxyapaptite (HA) layer forms on its surface facilitating the bone contact. Thus, the path of improving biomedical implants via deposition of crystalline TiO₂ on the surface is interesting to follow. In this study we have evaluated the influence of microstructure and chemical composition of sputter deposited titanium oxide thin films on the in vitro bioactivity. We find that both substrate bias, topography and the flow ratio of the gases used during sputtering affect the HA layer formed on the films after immersion in simulated body fluid at 37°C. A random distribution of anatase and rutile crystals, formed at negative substrate bias and low Ar to O₂ gas flow ratios, are shown to favor the growth of flat HA crystal structures whereas higher flow ratios and positive substrate bias induced growth of more spherical HA structures. These findings should provide valuable information when optimizing the bioactivity of titanium oxide coatings as well as for tailoring process parameters for sputtered-based production of bioactive titanium oxide implant surfaces.     

装饰薄膜ZrN的中频反应磁控溅射沉积工艺研究

利用中频反应磁控溅射技术在1Cr18Ni9Ti不锈钢基底上沉积ZrN薄膜。通过控制N/Ar、溅射功率和基体偏压等参数,得到不同实验条件的ZrN膜层。通过对膜层颜色测量和AES分析,研究N分压强对ZrN膜层质量的影响。实验结果表明：工作气压0.3Pa,溅射功率5kW,基体偏压-150V、占空比50%等工艺参数一定的前提下,N分压强在不同的范围内,可以分别制备出视觉效果类似于18K、23K和纯金的氮化锆膜层。     

On the dependence on bias voltage of the structural evolution of magnetron- sputtered nanocrystalline Cu films during thermal annealing

The nanostructural evolution during heat treatments of DC magnetron-sputtered Cu films deposited at different substrate bias voltages was experimentally studied. A growth chamber equipped with two magnetrons and Kapton windows for in-situ X-ray diffraction was mounted on a six-circle goniometer at a synchrotron beam line. Using Bragg-Brentano X-ray diffraction, the grain size, the texture, and the lattice constant were monitored during thermal annealing. Increasing the substrate bias voltage, the grain growth rate lowered, and the change in texture with time became smaller due to a decrease in the defect concentration. Furthermore, the grain size in the as-deposited films decreased with increasing bias voltage. The activation energy for grain growth was, within experimental errors, the same in all the films.     

射频磁控溅射沉积高质量ZnO薄膜的工艺研究

在室温下利用射频磁控溅射法在硅(100)基片上制备ZnO薄膜,利用X射线衍射(XRD)和扫描电子显微镜(SEM)对其结晶性能进行分析。研究了制备条件对薄膜沉积速率的影响。分析了薄膜沉积速率对薄膜结晶状况的影响及源气体中的氧气和氩气的流量比对薄膜结晶状况的影响。研究结果表明,薄膜的生长速率强烈依赖于射频功率和工作气压,薄膜的结晶性能强烈依赖于薄膜的沉积速率和反应气体中氧气和氩气的流量比。制备高结晶质量的ZnO薄膜的最佳工艺参数为靶到衬底的距离为4cm,输入功率为250W,源气体中氩气和氧气的流量比n(Ar)∶n(O2)为5∶20,溅射工作气压为2Pa。在最佳工艺条件下所制备的薄膜表面平整致密,接近单晶,在可见光区的透射率高达90%。