非晶金刚石膜的性能及其应用

非品金刚石薄膜具有超高硬度等一系列优异的特殊性能，为工程界孜孜追求的材料表面镀膜。用百纳科技公司研发制造的过滤阴极真空电弧离子镀膜机镀制的非晶金刚石薄膜，SP^3金刚石结构量≥80％，硬度高，膜／基结合力高，摩擦系数小，耐磨损，耐腐蚀，透光率高，在电子，机械，光学，生物医学上有广泛应用前景。我们已在视窗玻璃，丝锥，模具，硬质合金刀头等产品上成功应用。     

强流脉冲离子束辐照对电弧离子镀TiNbN硬质薄膜摩擦磨损性能的影响

 利用分离靶电弧离子镀工艺在高速钢基体上制备TiNbN多元硬质薄膜,利用TEMP-6型强流脉冲离子束（HIPIB）设备,采用含C/H离子、加速电压300 kV、脉冲宽度70 ns、束流密度60 A/cm2的强流脉冲离子束对所制备的薄膜进行辐照处理,研究辐照前后膜层的摩擦磨损性能的变化。实验结果表明：HIPIB辐照以后,薄膜的表面熔化,摩擦系数降低,晶粒细化,膜层的硬度由HK3444提高到HK3820,膜基结合力由59 N提高到65 N。在测试载荷300 N和600 N条件下,薄膜的摩擦磨损性能均有较大改善。     

铜基大块非晶合金添加微量元素对腐蚀行为的影响机理研究

通过分子动力学方法模拟了Cu-Al合金液相,然后模拟降温过程得到Cu-Al非晶合金.通过计算机编程建立了Cu-Al-M非晶基体、Cu-Al-M非晶表面及吸附O原子Cu-Al-M非晶表面原子结构模型.利用实空间连分数方法,研究了添加微量合金元素Zr,Nb,Ta,V,Y,Sc对Cu基大块非晶合金的腐蚀行为的影响机理.研究发现合金元素Zr,Nb,Ta,V,Sc不向清洁Cu基非晶表面偏聚,但除Y外向有氧吸附的表面偏聚,说明有氧吸附后Cu基非晶表面偏聚发生逆转.键级积分计算表明Zr,Nb,Ta,V,Y,Sc元素均增大与氧之间的结合力,易形成氧化膜,提高Cu基大块非晶的耐蚀性.稀土Y提高Cu基大块非晶的耐蚀性可能是由于它向合金与氧化膜界面偏聚并提高了合金与氧化膜的结合力.     

氢在不锈钢及氧化铬膜复合体中的稳态渗透实验

本文介绍氢在ＨＲ－１不锈钢基体及镀有氧化铬膜的复合材料中的行为研究，包括基体的准备；膜的制备；用不同手段从不同角度对膜进行的分析测试；膜与基体之间的平均结合力测定；用不锈钢材料构成的高温低压渗透回路的建造、调试、密封性能校准；纯ＨＲ－１基体材料中的氢渗透规律研究；有膜复合材料中氢的稳态迁移过程的表现规律实验结果。它们与国外类似的实验符合得较好；膜的分析测试结果反过来对制膜工艺提供了很有用的反馈信息，氢渗透回路的性能通过了有关专家鉴定，主要技术指标已达到国际同类设备的先进水平。为下阶段更广泛深入的研究奠定了良好的基础。     

矫顽力可调的多孔硅基Fe膜

采用电化学腐蚀法制备了不同多孔度的多孔硅(PS),再通过磁控溅射法在该PS衬底上沉积了一定厚度的Fe膜;并对样品进行了X射线衍射的结构分析、扫描隧道显微技术的表面形貌观察和磁光克尔效应的测量.发现在同一Fe膜厚度下，相对于参考样品硅上的Fe膜，多孔硅上Fe膜的矫顽力更大;同时观察到多孔硅基Fe膜随着PS多孔度的增加，矫顽力相应变大;而对于多孔度相同的多孔硅基样品,随着Fe膜厚度的增加矫顽力却逐步减小.得出了多孔硅特有的海绵状疏松结构能有效调节Fe膜矫顽力大小的结论. 关键词： 多孔硅 海绵状结构 Fe薄膜 矫顽力     

添加Y改善离子镀氮化钛膜的结构与性能

评价了离子镀氮化钛(TiN)和Y改性氮化钛(Ti(Y)N)膜的结合强度和在酸性介质中的耐蚀性能;用X射线衍射,离子探针质谱分析(IMA),透射电子显微镜(TEM)研究它们的显微结构特征;结果表明,添加Y元素富集在Ti(Y)N与A₃钢基材界面区域,并形成厚度约为20nm的亚层,Y的界面改性导致Ti(Y)N膜的X射线衍射线形略有宽化和明显的TiN相(111)面的择优生长取向;这些显微结构特征的改善导致Ti(Y)N膜比TiN膜具有更高的界面结合强度和更好的耐蚀性能。 关键词：     

内表面栅极等离子体源离子注入TiN薄膜及其特性研究

阐述了栅极增强等离子体源离子注入（GEPSII）方法的基本思想.利用GEPSII方法在45号钢 基底上生成了金黄色氮化钛（TiN_x）膜.对不同条件下的TiN膜做电化学腐蚀，X PS，AES， XRD等分析.电化学腐蚀实验显示TiN薄膜改善了45号钢的耐腐蚀性能5—10倍，且在高气压下 效果更好.结构分析显示TiN膜含有TiO₂，TiN成分，主要沿（111）和（200）晶 向生长，深度分析显示膜的厚度只有二十几纳米，膜质地均匀且在基底有一定的嵌入深度. 关键词： 腐蚀 等离子体源离子注入 薄膜 氮化钛     

Co元素对硬质合金基底金刚石涂层膜基界面结合强度的影响

采用基于密度泛函理论的第一性原理平面波赝势方法, 研究了硬质合金刀具基底黏结相Co元素对金刚石涂层膜基界面结合强度的影响机理. 借助Materials Studio软件建立了WC/Diamond膜基界面模型和WC-Co/Diamond膜基界面模型, 采用CASTEP仿真软件计算了WC/Diamond膜基界面模型和WC-Co/Diamond膜基界面模型的最优稳定结构. 通过仿真计算, 获得了WC/Diamond膜基界面模型和WC-Co/Diamond膜基界面模型的界面结合能、电荷密度图及Mulliken重叠布居数. 经对比分析后发现, 硬质合金基底中磁性元素Co的存在能转移金刚石涂层膜基界面处W元素及C元素的电荷, 从而使膜基界面处的原子因失电荷而相斥, 这直接导致了金刚石涂层膜基界面间距变大, 使得金刚石涂层膜基界面结合能降低.     

多孔硅激光染料镶嵌膜的荧光光谱研究

本文对以多孔硅为载体，镶嵌激光染料形成复合膜的光致发光进行了研究，比较了镶嵌膜与其他不同状态下染料发光的差异，发现镶嵌染料荧光光谱线型较其他状态下明显趋于对称，同时考察了衬底情况的改变对镶嵌膜发光的影响。通过对实验结果的分析指出，这种硅基镶嵌膜中的染料的发光主要来自单体的荧光发射。     

脉冲激光沉积制备的Co80Cr20/Ti90Cr10薄膜的结构与磁性

用脉冲激光沉积(PLD)的方法在硅单晶基片上制备了Ti90Cr10和Co80Cr20/Ti90Cr10薄膜,用XRD研究了Ti90Cr10薄膜的晶体结构与制备温度的关系,结果表明随着温度升高,薄膜从非晶态逐步向晶态转化,并且计算了Ti90Cr10薄膜的晶粒大小以及晶格常数.利用透射电镜对Ti90Cr10薄膜进行了表面和截面形貌的表征.采用纳米压痕仪对Ti90Cr10薄膜的硬度和膜基界面结合力进行了分析,表明薄膜的硬度和膜基结合力随制备条件改变有所变化,制备温度增加,薄膜的硬度和膜基结合力随之增加.利用Ti90Cr10薄膜作为中间层,用PLD制备了Co80Cr20磁性层,获得了很好的垂直磁化性质,膜厚减小,矫顽力和矩形比有所增加,600℃真空条件下制备的Co80Cr20(8 nm)/Ti90Cr10(14 nm)薄膜的矫顽力为65.25 kA/m,矩形比为0.86,并且讨论了Co80Cr20/Ti90Cr10薄膜的磁化性质.     

Pulsed laser deposition of hydroxyapatite film on laser gas nitriding NiTi substrate

A hydroxyapatite (HA) film was deposited on laser gas nitriding (LGN) NiTi alloy substrate using pulsed laser deposition technique. TiN dendrite prepared by LGN provided a higher number of nucleation sites for HA film deposition, which resulted in that a lot number of HA particles were deposited on TiN dendrites. Moreover, the rough LGN surface could make the interface adhesive strength between HA film and substrate increase as compared with that on bare NiTi substrate.     

Synthesis of titanium nitride thin films deposited by a new shielded arc ion plating

Thin films of titanium nitride (TiN) were deposited on stainless steel substrates by a modified deposition technique, double-layered shielded arc ion plating with vicarious circular holes (DL-SAIP). The results show that the TiN film with the distance of 10 mm between the double-layered shield plates had the least droplets. The deposition rate of the films prepared with the new technique was more homogeneous than that of all the other shielded arc ion plating. The film/substrate adhesion and microhardness values of the TiN films were higher than 40 N and 18 GPa, respectively. Thus such TiN thin films can be expected in applications.     

多弧离子镀工艺对TiN/Ti与Cr/Cu界面及微结构的影响

用多弧离子镀技术在铜基上电镀Cr/Ni层进行不同工艺条件下多弧离子沉积TiN/Ti实验.借助X射线衍射(XRD)和扫描电子显微镜(SEM)研究了TiN/Ti与Cr/Cu接触界面形成、微结构及其组分与形貌.XRD分析显示,薄膜表面组分包含TiN,Ti₂N多晶相外,还包含一些Cr-Ti的金属间化合物等.显然,TiN,Ti₂N在表面上已形成.SEM观察指出,在90℃制备的表面膜具有不平整的类枝状结晶结构.随着温度升高至170℃,得到精细TiN/Ti覆盖层表面,XRD峰 关键词： 多弧离子镀 氮化钛 界面形成 微结构     

Au/TiN复合薄膜制备及其表面增强拉曼光谱研究

表面增强拉曼散射光谱(SERS)已用于环境监测、生物医药、食品卫生等领域,而高活性SERS基底是表面增强拉曼散射光谱技术应用的关键。TiN作为新型等离子材料具有较强的SERS性能,同时化学稳定性及生物相容性较好,但其SERS性能不如贵金属金强。该研究采用氨气还原氮化法和电化学沉积法,在TiN薄膜表面沉积贵金属Au纳米颗粒制备出Au/TiN复合薄膜。在Au/TiN复合薄膜中单质Au和TiN两种物相共存;随着电化学沉积时间延长,TiN薄膜表面单质金纳米颗粒数量逐渐增多,金纳米颗粒尺寸增大,颗粒间距减小。由于金与TiN两者的本征表面等离子共振耦合作用,Au/TiN复合薄膜的共振吸收峰发生了偏移。利用罗丹明6G为拉曼探针分子,对Au/TiN复合薄膜进行SERS性能分析,发现Au/TiN复合薄膜上的R6G探针分子的拉曼峰信号强度随沉积时间延长呈现先增大后减小的规律;当电化学沉积时间为5 min时,R6G拉曼信号峰较高,复合薄膜样品的SERS活性最大。将Au/TiN复合薄膜和Au薄膜分别浸泡在10-3,10-5,10-7,10-8及10-9 mol·L-1 R6G溶液5 min,进行检测限分析,发现Au/TiN复合薄膜检测极限达10-8 mol·L-1,增强因子达到8.82×105,与Au薄膜和TiN薄膜相比,Au/TiN复合薄膜上对R6G探针分子SERS活性最高。这得益于Au/TiN复合膜中表面等离子体产生的耦合效应,使得局域电磁场强度增强,从而引起R6G探针分子拉曼信号增强。通过2D-FDTD模拟电场分布发现Au/TiN,Au及TiN薄膜具有电场增强作用,其中Au/TiN复合薄膜的增强作用尤为显著,这也证实了氮化钛与金纳米颗粒之间存在耦合效应。另外发现TiN与Au之间可能存在电荷转移,促进了4-氨基苯硫酚氧化反应,进而证实了TiN与Au薄膜的协同作用。此外,Au/TiN复合薄膜均匀性较好,相对平均偏差仅为7.58%。由此可见,采用电化学沉积制备的Au/TiN复合薄膜具有作为SERS基底材料的应用潜力。     

Optimization of plasma parameters for high rate deposition of titanium nitride films as protective coating on bell-metal by reactive sputtering in cylindrical magnetron device

Nano-structured titanium nitride (TiN) thin film coating is deposited by reactive sputtering in cylindrical magnetron device in argon and nitrogen gas mixtures at low temperature. This method of deposition using DC cylindrical magnetron configuration provides high uniform yield of film coating over large substrate area of different shapes desirous for various technological applications. The influence of nitrogen gas on the properties of TiN thin film as suitable surface protective coating on bell-metal has been studied. Structural morphological study of the deposited thin film carried out by employing X-ray diffraction exhibits a strong (2 0 0) lattice texture corresponding to TiN in single phase. The surface morphology of the film coating is studied using scanning electron microscope and atomic force microscope techniques. The optimized condition for the deposition of good quality TiN film coating is found to be at Ar:N₂ gas partial pressure ratio of 1:1. This coating of TiN serves a dual purpose of providing an anti-corrosive and hard protective layer over the bell-metal surface which is used for various commercial applications. The TiN film's radiant golden colour at proper deposition condition makes it a very suitable candidate for decorative applications.     

In situ identification of organic components of ink used in books from the 1900s by atmospheric pressure matrix assisted laser desorption ionization mass spectrometry

Transport of N, O, and Ti during dc magnetron sputtering deposition of nanoscopic TiN/Ti and TiN structures on plasma nitrided M2 tool steel, as well as transport of metallic species composing the plasma nitrided steel substrates were investigated. N and O depth distributions were determined with subnanometric resolution using narrow resonant nuclear reaction profiling, whereas Ti was profiled, also with subnanometric depth resolution, by medium energy ion scattering. The surface elementary compositions of the TiN/Ti/nitrided steel and TiN/nitrided steel structures were determined by low energy ion scattering. The chemical compounds formed during deposition were accessed by X-ray photoelectron spectroscopy, indicating the presence of TiN, TiO₂, Ti oxynitrides, as well as other metallic nitrides and oxynitrides, but no metallic Ti was observed. Owing to the observed intensive atom mobility, the compositions of the deposited films on plasma nitrided steel structures varied continuously on a nanoscopic scale, from the core of the steel substrate to the bulk of the stoichiometric TiN films. The Ti interlayer assists interdiffusion of all species, in contrast to the TiN film layer, which is known to be a diffusion barrier. The improved adhesion of TiN hard coatings to plasma nitrided steel under working conditions is discussed in terms of the gradual compositional change around the interfaces and the atomic mobility during their formation.     

高脉冲功率能量PLD法制备MgZnO薄膜中的沉积机理

用PLD法成功制备了一系列高质量的MgZnO薄膜。实验中发现高脉冲能量沉积薄膜的结构和发光特性随基片温度的变化规律与低脉冲能量下的结果不一样:基片在室温时高脉冲能量制备薄膜的XRD峰的半峰全宽比高基片温度时的结果相对更小;AFM显示其颗粒变大,柱状生长突出;PL谱紫峰与绿峰强度比最大,结晶质量反而提高。另一方面,与低脉冲能量时相反,增大氧气压强后高脉冲能量沉积的薄膜XRD半峰全宽变窄。结合实验现象和表征,合理解释了高脉冲能量沉积的机理。室温制备高质量MgZnO薄膜的PLD沉积机理对于以后在柔性衬底上沉积薄膜的研究有重要的参考价值。     

GaSb基PECVD法制备SiO2薄膜的应力研究

为了实现在GaSb衬底上获得低应力的SiO₂薄膜,研究了等离子体增强化学气相沉积法（PECVD）在晶格失配较大的GaSb衬底上沉积SiO₂薄膜的应力情况。通过改变薄膜沉积时的工艺条件,如反应温度、射频功率、反应压强、气体流量比,并基于曲率法模型,对镀膜前后的曲率半径进行了实验测量,利用Stoney公式计算相关应力值并绘制应力变化曲线。详细讨论了PECVD工艺条件的改变对SiO₂薄膜应力所产生的影响。同时通过在Si衬底上沉积SiO₂薄膜,对比分析了导致薄膜应力产生的因素及变化过程。实验结果表明,在沉积温度为300℃、射频功率为20 W、腔体压强为90 Pa、气体流量比SiH₄/N₂O为125/70 cm³·min^-1的工艺参数下,PECVD法在GaSb衬底上沉积的SiO₂薄膜应力相对较小。     

Effect of active screen plasma nitriding pretreatment on wear behavior of TiN coating deposited by PACVD technique

Titanium based alloys are used extensively for improving wear properties of different parts due to their high hardness contents. Titanium nitride (TiN) is among these coatings which can be deposited on surface using various techniques such as CVD, PVD and PACVD. Their weak interface with substrate is one major drawback which can increase the total wear in spite of favorite wear behavior of TiN. Disc shaped samples from AISI H13 (DIN 1.2344) steel were prepared in this study. Single TiN coating was deposited on some of them while others have experienced a TiN deposition by active screen plasma nitriding (ASPN). Hardness at the surface and depth of samples was measured through Vickers micro hardness test which revealed 1810 Hv hardness as the maximum values for a dual-layered ASPN–TiN. Pin-on-disc wear test was done in order to study the wear mechanism. In this regard, the wear behavior of samples was investigated against pins from 100Cr6 (Din 1.3505) bearing steel and tungsten carbide–cobalt (WC–Co) steel. It was evidenced that the dual-layer ASPN–TiN coating has shown the least weight loss with the best wearing behavior because of its high hardness values, stable interface and acceptable resistance against peeling during wearing period.     

Condensation Surface Temperature as a Means for Studying Film Formation Mechanisms

A rise in the condensation surface temperature during film growth is a result of energy dissipation on the condensation surface. An example of energy dissipation is the dissipation of chemical reaction heat, which releases during film deposition by reactive magnetron sputtering. The monitoring of the surface temperature during TiN film deposition by reactive (Ti–in–N₂) and nonreactive (TiN–in–Ar or TiN–in–N₂) sputtering methods has shown that this temperature is higher in the reactive case and decreases in the (TiN–in–Ar)–(TiN–in–N₂) sequence of nonreactive sputtering modifications. It has been found that the composition and crystal structure of TiN films do not depend on the growth method and are identical to those of bulk titanium nitride. Based on these results, a formation mechanism of films obtained by the above methods has been suggested. In the case of reactive sputtering, the film was supposed to grow on the condensation surface through a reaction between titanium and nitrogen atoms. In the cases of nonreactive sputtering, the film forms from TiN molecules.