Ti-N系薄膜结构研究的若干问题

综述了Ti-N系薄膜结构研究的若干重要问题。着重讨论了δ-TiN的非化学计量性和物理气相沉积过程非平衡性对于Ti-N系膜相组成的影响。从耐磨应用考虑,ε-Ti_2N相或其复相涂层具有优势。透射电镜横截面试样研究阐明了Ti-N膜的分层精细结构,包括其各相的空间分布、择优取向、各层间的取向关系、晶粒度及界面反应层。论述了Ti底层的作用。研究了薄膜结构的一系列力学效应,例如离子轰击、合金化和多层化等引起的薄膜晶粒细化效应;晶粒细化和多层化导致的薄膜硬度增强和韧化,离子轰击追成的膜基界面强化等。上述结果对于改善Ti-N超硬膜性能,扩大其应用,均有重要作用。     

尺寸效应对TiC/α-C∶H涂层织构行为的影响

利用磁控溅射法制备了TiC/α-C∶H纳米复合涂层尺寸效应,并对涂层择优取向的影响进行了研究。通过改变涂层中的C含量来调节晶粒尺寸,发现晶粒尺寸对晶粒的择优取向有着重要影响。随着晶粒尺寸减小,TiC的择优取向从面心立方(111)向(200)转变。这种择优取向的尺寸依赖效应可以用热力学来解释。通过计算与尺寸相关的吉布斯自由能解释了尺寸效应与涂层择优取向的关系。     

尼龙1010在熔融峰温等温结晶生成晶体的热性质和形态结构

用DSC、TEM、ED研究了尼龙1010在熔融峰温等温结晶生成晶体的热性质和形态结构。结果表明该晶体在DSC扫描的时间尺度范围内是稳定的,能保持原有的熔融特性,不是低熔点晶体转化而成的晶体。对该晶体进行的电子衍射,显示出对称清晰的单晶电子衍射斑点,用尼龙1010的晶胞参数标定电子衍射图,证明是单晶的电子衍射图。     

鸵岛蛋壳的微结构研究

用Ｘ射线衍射分析、扫描电镜及透射电镜对鸵鸟蛋壳的晶体结构进行了研究。观察了蛋壳晶体形貌、晶体取向、晶粒尺寸和相邻晶粒的取向关系。发现蛋壳内晶粒存在的择优取向，用取向畸结构解释了蛋壳内存在的择优取向。用扫描电子显微镜观察了蛋壳内有机介质和无机相的形貌。     

沉积温度对磁控溅射制备V-Al-Si-N硬质涂层结构及性能的影响

采用磁控溅射工艺制备了不同沉积温度的V-Al-Si-N涂层,利用X射线衍射、扫描电镜、纳米压痕仪和摩擦磨损试验机对涂层的结构和性能进行了分析。研究结果表明:室温下制备的涂层生长缺陷较多,残余应力较大。适当提高沉积温度至300℃,涂层的晶体结晶性得到提高,柱状晶粗大贯穿整个膜厚,晶粒尺寸变大;继续提高沉积温度至500℃时,涂层呈(200)择优取向,晶粒尺寸变小,涂层致密度提高。随着沉积温度的提高,涂层的硬度略有下降,但是涂层的摩擦学性能得到大幅度提升。500℃制备涂层的硬度为29.7 GPa,磨损率达到6.1×10-17m3/Nm,比室温制备的涂层的磨损率降低了两个数量级。     

聚酞菁锡氧烷晶体结构和晶体形貌的研究

本文用X-射线衍射和电子衍射研究了聚酞菁锡氧烷[Sn(P_c)O]_n的晶体结构,测定出该晶体属体心四方点阵,晶胞参数为a=17.99,c=3.91,和z=2。通过理论衍射强度的计算给出了I 4空间群的晶体结构模型。用扫描和透射电子显微镜对晶体形貌进行了观察,发现聚合物晶粒是由许多板条状基元单晶体以一定方式堆砌而成的。由选区电子衍射确定出在板条晶中分子链排列在平行于晶体的大平面且与其长边方向成约65°角的方向上。     

贝壳珍珠层中文石晶体择优取向研究

贝壳珍珠层中文石晶体的择优取向是其具有独特力学性能的重要原因．本文采用Ｘ射线衍射方法对我国主要育珠贝（蚌）的贝壳珍珠层中文石晶体的择优取向进行了较系统的研究,结果表明：海水马氏珍珠贝、大珠母贝及企鹅珍珠贝贝壳珍珠层中文石晶体ｃ轴垂直珍珠层面定向排列;淡水三角帆蚌壳珍珠层文石晶体有两种明显择优取向,一种ｃ轴垂直珍珠层层面,另一种ｃ轴与层面斜交,其（０１２）面网方向与层面平行．     

CrAlN抗冲蚀涂层制备及性能研究

为提高钛合金材料抗冲蚀性能,利用真空阴极电弧沉积技术在TC11钛合金上沉积CrAlN涂层,研究靶电流、偏压和气压对涂层结构及性能的影响。采用扫描电镜观察膜层表面和截面形貌,金相显微镜对表面的大颗粒进行定量分析;显微硬度计测量膜层的维氏显微硬度;采用喷砂试验机对涂层的抗冲蚀性能进行测试,通过三维表面轮廓仪测量涂层厚度和侵蚀坑的深度;X射线衍射仪表征涂层中的晶体结构。结果表明:靶电流从70A增大到110A,虽可提高涂层的沉积速率,但会导致涂层表面大颗粒增加,从而降低涂层的抗冲蚀性能;气压从1Pa增大至4Pa,可有效地减少涂层表面颗粒的尺寸及数量,但也会一定程度降低沉积速率及硬度;偏压对CrAlN涂层的结构及性能影响最大,偏压在-50V时涂层呈(200)择优取向,-100V涂层呈(111)择优取向,-200V时,涂层择优取向不明显;且随着偏压的增加,涂层的硬度及抗冲蚀性能增大,在高冲蚀角下,冲蚀的失效机理为脆性失效。结论:工艺参数中靶电流对表面质量的影响最大;涂层的生长取向与偏压密切相关;CrAlN涂层的表面质量及硬度直接影响其抗砂粒冲蚀性能,偏压对涂层抗冲蚀性能影响最大。最终优化的工艺参数为:靶电流90A、偏压-100V、气压4Pa。     

用电子衍射法测定 Au、Ag 的衍射强度

用电子衍射法测定和补充了美国发表的 ASTM 粉末衍射强度数据.并与理论计算进行了比较.初步结论如下:由电子衍射强度是可行的.衍射强度和晶体内原子位置间的变化规律同理论计算结果基本相符.所提供的衍射强度数据,可作电子衍射物相鉴定的参考.另外.实测值和计算值的差异是由子在电子衍射时,晶体吸收较强,导致衍射角增大时,实测值略小于计算值.在电子衍射中,由于原子对电子的散射很强.晶体内产生的衍射束有较高的强度,这些衍射束可看作新的衍射源.在晶体内产生二次衍射.二次衍射可使一些弱衍射变强.一些禁止衍射也可能出现,它给电子衍射强度分析带来困难,也是电子衍射实测值和计算值差异的原因之一.     

纳米多孔Ni-P涂层催化制备螺旋碳纤维研究

以纳米多孔Ni-P涂层为催化剂模板,制备形貌良好、宏量生长的螺旋碳纤维。采用扫描电子显微镜对螺旋碳纤维进行微观形貌观察,采用X射线能量色散谱仪对纳米多孔Ni-P涂层表面进行元素分析,采用X射线衍射仪表征其物相组成。研究了反应温度、升温速率、反应气氛对螺旋碳纤维形貌及纳米多孔Ni-P涂层物相组成的影响。实验结果表明,非晶态的纳米多孔Ni-P涂层在升温过程中会形成结晶Ni相和结晶Ni3P相。随着温度的提高,用纳米多孔Ni-P涂层催化生长的螺旋碳纤维直径出现由大变小的趋势,在600℃时制备的碳纤维其螺旋形貌最佳。螺旋碳纤维的纤维直径、螺旋直径与纳米多孔Ni-P涂层中Ni(200)晶面的择优取向强度相关,这是决定螺旋碳纤维形貌的关键,Ni(200)晶面的择优取向强度越高,生长的螺旋碳纤维的纤维直径和螺旋直径越小。     

Influence of CH4 fraction on the composition, structure, and internal stress of the TiCN coatings deposited by LAFAD technique

TiCN coatings were deposited using a large area filtered arc deposition (LAFAD) technique from Ti targets in a mixture of N₂ and CH₄ gases. CH₄ fraction was varied from 0 to 50% to change the C content in the coatings. Scanning electron microscopy (SEM), x-ray photoelectron spectroscopy (XPS), x-ray diffraction (XRD), and substrate bending method were used to characterize the dependence of the CH₄ fraction on the surface morphology, composition, bonding structure, crystalline structure, and internal stress in the deposited coatings. It was found that TiCN coatings consist of nano-sized clusters and the cluster size increases with CH₄ fraction. XPS results show that with increasing CH₄ fraction, the N content in the coatings decrease continuously, the C content increases to 9.3 at.% at a CH₄ fraction of 30% followed by a slight decrease with the additional increase in the CH₄ fraction. With an increase of the C content in the coatings, there is a decrease in the Ti-N bonding content and an increase in the Ti-C and C-N bonding contents in the coatings. XRD results indicate that with increasing CH₄ fraction, the growth orientation of the TiCN coatings changes from (111) to (220) preferred orientation. The TiN (220) peak shifts to a lower diffraction angle, and the grain size decreases continuously. The internal stresses in all TiCN coatings are compressive and increase linearly with increasing C content in the coatings. The decrease in the grain size and the increase in the C content correspond to the continuous increase in the internal stress in the coatings.     

Effect of Thickness on the Structure and Tribological Properties of MoSx Coating

MoSx coatings were prepared by bipolar-pulse DC unbalanced magnetron-sputtering system with the variation of coating thickness at different Ar pressures.The composition and surface morphology were determined by using energy dispersive X-ray and scanning electron microscopy;the structural characterization was analyzed by X-ray diffraction.The friction and wear properties were investigated by fretting tests in air with less than 10% and 50% relative humidity.At 0.40 Pa pressure,(002) basal plane orientation was formed throughout the coatings.At 0.88 Pa and 1.60 Pa pressures,(002) basal plane orientation was only noticed in the first stage of coating growth(around 0.20 μm in thickness), and then edge orientations with their basal planes perpendicular to the surface would be evolved in the coatings.Humidity has a minor influence on the coatings that have(002) basal plane orientation,whereas the tribological properties of MoSx coatings with edge orientations are greatly affected by humidity.The mechanisms of coating growth and friction and wear processes are discussed.     

Influence of Ni content on the structure and properties of Cr-Ni-N coatings prepared by direct current magnetron sputtering

Cr-Ni-N coatings were deposited on 304 stainless steel substrates using a conventional direct current magnetron reactive sputtering system in nitrogen-argon reactive gas mixtures. The influence of Ni content (0 ≦ x ≦ 20 at.%) on the coating composition, microstructure, and tribological properties was investigated by glow discharge optical spectroscopy, X-ray diffraction and transmission electron microscopy, scanning electron microscopy (SEM), nano-indentation, and pin-on-disk tests. The results showed that microstructure and properties of coatings changed due to the introduction of Ni. The ternary Cr-Ni-N coatings exhibited solid solution structures in spite of the different compositions. The addition of Ni strongly favoured preferred orientation growth of <200>. This preferred orientation resulted from the formed nano-columns being composed of grains with the same crystallographic orientation, as confirmed by SEM cross-sectional observations. The mechanical properties including the nano-hardness and reduced Young's modulus decreased with increasing Ni content. Pin-on-disk tests showed that low Ni content coatings presented higher abrasion resistance than high Ni content coatings.     

Electrophoretic deposition of composite hydroxyapatite-chitosan coatings

Cathodic electrophoretic deposition has been utilized for the fabrication of composite hydroxyapatite-chitosan coatings on 316L stainless steel substrates. The addition of chitosan to the hydroxyapatite suspensions promoted the electrophoretic deposition of the hydroxyapatite nanoparticles and resulted in the formation of composite coatings. The obtained coatings were investigated by X-ray diffraction, thermogravimetric and differential thermal analysis, scanning and transmission electron microscopy, potentiodynamic polarization measurements, and electrochemical impedance spectroscopy. It was shown that the deposit composition can be changed by a variation of the chitosan or hydroxyapatite concentration in the solutions. Experimental conditions were developed for the fabrication of hydroxyapatite-chitosan nanocomposites containing 40.9–89.8 wt.% hydroxyapatite. The method enabled the formation of adherent and uniform coatings of thicknesses up to 60 μm. X-ray studies revealed that the preferred orientation of the hydroxyapatite nanoparticles in the chitosan matrix increases with decreasing hydroxyapatite content in the composite coatings. The obtained coatings provided the corrosion protection for the 316L stainless steel substrates.     

射频磁控溅射法制备TiB2涂层及其性能分析

利用射频磁控溅射技术在硅和钢片上沉积了TiB2涂层.采用场发射电子扫描显微镜(FESEM),小掠射角x射线衍射(GAXRD)及X射线光电子能谱(XPS)分别研究了涂层的横截面形貌,晶体结构以及涂层中的元素和化学状态.同时,对涂层的显微硬度和残余应力进行了表征.结果表明, 利用射频磁控溅射法制备的TiB2涂层平整光滑,结构致密,沿[001]晶向择优生长,具有纳米晶结构,硬度显著提高,而且残余压应力较低.     

偏压对磁控溅射沉积Al—Zn镀层成分和结构的影响

采用扫描电镜（SEM）、X射线衍射仪、X射线能谱（EDS）和俄歇电子能谱仪（AES）,研究了基片偏压对磁控溅射沉积Al-Zn镀层组成和结构的影响。随着基片偏压的增加镀层的Zn含量呈降低趋势,在不同基片偏压下可获得不同择优取向的Al-Zn镀层。     

Structure and Anomalous Magnetic Properties in Fe-N/Ti-N Nano-multilayers

DC-magnetron sputtering was employed to prepare Fe-N/Ti-N periodic nano-multilayers . Magnetic properties were studied by vibrating sample magnetometry and structure by TEM and X-ray diffraction for the films. A strong enhancement of the saturation magnetization was found in multilayers containing thinner Fe-N layers. The coercivity was found to be nearly constant. A kind of anomalous hysteresis loops was found in some samples     

The effects of pre-implantation of steel substrates on the structural properties of TiN coatings

We have studied the effects of nitrogen pre-implantation of AISI C1045 steel substrates on the microstructure and microhardness of deposited TiN coatings. The substrates were implanted at 40 keV, to the fluences from 5 × 10¹⁶ to 5 × 10¹⁷ ions/cm², which was followed by deposition of 1.3-μm thick TiN coatings by reactive sputtering. Structural characterization of the samples was performed by standard and grazing incidence X-ray diffraction analysis, Rutherford backscattering spectroscopy and transmission electron microscopy. Microhardness was measured by the Vicker’s method. Nitrogen implantation up to 2 × 10¹⁷ ions/cm² induces the formation of Fe₂N phase in the near surface region of the substrates, which becomes more pronounced for higher fluences. Microstructure of the deposited TiN coatings shows a strong dependence on ion beam pre-treatment of the substrates. The layers grown on non-implanted substrates have a (200) TiN preferential orientation, and those grown on implanted substrates have (111) TiN preferential orientation. The change in preferred orientation of the layers is assigned to a developed surface topography of the substrates induced by ion implantation, and possible effects of distorted and altered crystalline structure at the surface. Ion implantation and deposition of TiN coatings induce an increase of microhardness of this low performance steel for more than eight times.     

Microstructure and properties of TiAlSiN coatings prepared by hybrid PVD technology

TiAlSiN coatings with different Si content were prepared by hollow cathode discharge (HCD) and mid-frequency magnetron sputtering (MFMS) hybrid coating deposition technology. The chemical composition, microstructure, mechanical properties of these coatings were systematically investigated by means of energy dispersive spectrometry (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), nanoindentation measurement, scratch and high speed milling hardened steel tests. The coatings prepared by this method showed the structure of crystalline phase was corresponding to that of TiAlN, however, different preferred orientation with addition of Si. Proper content of Si into TiAlN led to increase of microhardness and adhesion. TiAlSiN coated end mill with Si content of 4.78 at.% had the least flank wear, which was improved about 20% milling distance than TiAlN coated end mill.     

电沉积Ni-SiC纳米复合镀层的显微组织分析

采用超声波辅助脉冲电沉积复合镀技术在铜基表面制备Ni-SiC纳米复合镀层.研究了超声波的施加和不同电极摆放方式对镀层显微组织和性能的影响.结果表明:超声波和第二相颗粒共同作用可以显著细化复合镀层显微组织,显微硬度可达到HV760;复合镀层镍衍射品面(200)和(220)峰位的变化,说明晶粒生长过程中的择优取向得到了抑制...