Microstructure and physical properties of PVD TiN/（Ti, Al）N multilayer coatings

Magnetron sputtered （Ti, Al） N monolayer and TiN/（Ti, Al） N multilayer coatings grown on cemented carbide substrates were studied by using energy dispersive X-ray spectroscopy （EDX）, scanning electron microscopy （SEM）, nanoindentation, Rockwell A indentation test, strength measurements and cutting tests. The results show that the （Ti, Al）N monolayer and TiN/（Ti, Al）N multilayer coatings perform good affinity to substrate, and the TiN/（Ti, Al）N multilayer coating exhibits higher hardness, higher toughness and better cutting performance compared with the （Ti, Al）N monolayer coating. Moreover, the strength measurement indicates that the physical vapour deposition （PVD） coating has no effect on the substrate strength.     

(Ti,Al)N单层和TiN/(Ti,Al)N复合涂层的切削性能研究

借助EDX、SEM、强度测试和切削实验研究了采用磁控溅射在硬质合金基体上沉积的(Ti,Al)N单层和TiN/(Ti,Al)N复合涂层的切削性能。研究表明,两种涂层均与基体结合紧密;TiN/(Ti,Al)N复合涂层则表现出更好的切削性能。     

羟基磷灰石生物涂层材料界面的电镜观察与分析

用扫描电子显微镜和透射电子显微镜对未经热处理的钛合金基体等离子喷涂羟基磷灰石生物材料的显微结构、相组成和界面结合进行了观察与分析. 结果表明 HA涂层的显微结构疏松, 内部有裂纹和孔洞; 涂层的相结构中, HA以结晶态和非晶态两种形态存在; HA和基体的界面结合是以物理结合为主, 界面明显, 没有过渡相, 说明基体和涂层之间化学反应不明显.     

钛合金表面激光熔覆Ti/Ni+Si3N4/ZrO2复合涂层组织与性能研究

目的 提高TA15合金的表面硬度,改善其耐磨性能.方法 以Ti/Ni+Si3 N4/ZrO2混合粉末为原料,利用激光熔覆技术,在TA15钛合金表面制备出以ZrO2颗粒和原位生成Ti5 Si3、TiN为增强相,以金属化合物TiNi、Ti2 Ni为基体的复合涂层.采用X射线衍射仪、扫描电镜及能谱仪等手段分析激光熔覆涂层的显微组织及磨损表面,通过硬度测试、摩擦磨损实验,对熔覆层的显微硬度和耐磨性进行评估.结果 熔覆层与基体形成了良好的冶金结合,熔覆层组织中TiNi和Ti2 Ni金属化合物基体上弥散分布着Ti5 Si3、TiN树枝晶和ZrO2颗粒;与不含ZrO2熔覆层相比,含有ZrO2熔覆层组织的晶粒得到细化;熔覆层中原位生成的TiN桥接在裂纹上,具有增韧的作用;熔覆层的显微硬度分布在835~1050 HV区间内,约为基体硬度的3倍左右;在干滑动摩擦磨损下,熔覆层的磨损量约为钛合金基体磨损量的1/6,其主要磨损机制为磨粒磨损和黏着磨损.结论 熔覆层中高硬度、耐磨陶瓷相和高韧性相的共同配合,显著提高了钛合金表面的硬度和耐磨性.     

Structure and wear resistance of TiN and TiAlN coatings on AZ91 alloy deposited by multi-arc ion plating

In order to investigate the microstructure of TiN and TiAlN coatings and their effect on the wear resistance of Mg alloy, TiN and TiAlN coatings were deposited on AZ91 magnesium alloy by multi-arc ion plating technology. TiN and Ti70Al30N coatings were prepared on the substrate, respectively, which exhibited dark golden color and compact microstructure. The microstructures of TiN and Ti70Al30N coatings were investigated by X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The micro-hardness and wear resistance of TiN and Ti70Al30N coatings were investigated in comparison with the uncoated AZ91 alloy. The XRD peaks assigned to TiN and TiAlN phases are found. The hardness of TiN coatings is two times as high as that of AZ91 alloy, and Ti70Al30N coating exhibits the highest hardness. The wear resistance of the hard coatings increases obviously as result of their high hardness.     

Plasma Spray Deposition Enhancement of Titanium Nitride Layer Using Nitrogen-Contained Plasma Irradiation of Titanium Substrate as a Pre-spraying Method

Reactive plasma spray of TiN ceramic coating attracts much attention over the years because of its ability to deposit thick layers on various metal surfaces. However, some mechanical properties of the coating such as its hardness should be improved. In this study, initially a thin layer of titanium nitride was prepared on a titanium substrate during irradiation of titanium substrate by a thermal DC nitrogen-contained plasma jet. Then, during reactive plasma spraying, Ti particles were injected into plasma jet, converted to titanium nitride and huddled on to the substrate. This new hybrid method (primary plasma irradiation and post-reactive plasma spraying) for deposition of TiN coatings would combine the advantages of both plasma-enhanced chemical vapor deposition and reactive plasma spraying methods in part. It resulted in a thick and hard layer of titanium nitride film. Sample produced by this method was analyzed with x-ray diffraction confirming titanium nitride production. Vickers hardness was measured using optical microscopy which was around 1319 H_v300g. To study the cross section of the layer, optical microscopy and scanning electron microscopy (SEM) were used.     

Effects of Ti_(0.5)Al_(0.5)N coatings on the protecting against oxidation for titanium alloys

Ti0.5Al0.5N coatings were deposited on TC11(Ti-6.5Al-3.5Mo-1.5Zr-0.3Si) and silicon substrates using a cathode arc ion-plating system.The microstructure, composition, phase structure, and oxidation-resistance of the alloys and nitride coatings were investigated by scanning electron microscopy, X-ray diffraction, transmission electron microscopy, Auger electron spectroscopy, and thermal analyzer.The results show that the oxidation resistance of the titanium alloy is relatively limited;the compound structures of Ti mixed with Al oxides are formed during the heating process.The phases of the Ti0.5Al0.5N coatings are composed of a TiN solid solution phase.The oxidation kinetics obeys the parabolic law.During the oxidation process, the selective oxidation of Al occurs, thus protecting the underlying coating and substrate.     

The microstructural characterization of the nitrided layers prepared by direct current nitrogen arc

The characteristics of nitrided layers prepared on commercially pure titanium substrates by direct current nitrogen arc are presented by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) micrographs as well as X-ray diffraction (XRD). The titanium nitride (TiN) dendrites were fully developed with interconnected cellular morphologies at the top surface but grew almost perpendicular to the interface with coarser arms in the middle area. Also less TiN was found near the interface. The energy inputs had an obvious effect on the microstructures and the hardness of the nitrided layers. The maximum micro-hardness was 2 500 HV at the top surface which was over 9 times higher than that of the substrate.     

On the mechanochemical activated synthesis of nanocrystalline in-situ Ti(Al)N

This paper reports on our study of the synthesis of titanium nitride solid solution by the reduction of aluminum nitride with titanium by mechanical alloying (MA) using a planetary ball mill. A nanostructure composite of in-situ titanium nitride solid solution was produced through exchange reaction between Ti and AlN. X-ray diffraction (XRD), scanning electron microscopy (SEM), electron probe micro analysis (EPMA), transmission electron microscopy (TEM), energy dispersive X-ray analysis (EDX) and particle size analysis (PSA) were used to characterize the product. It was found that, with increased milling time, Al resulted from decomposition of aluminum nitride dissolved in the Ti lattice, leading to the formation of Ti(Al) solid solution and a reduction of the Ti lattice interplanar distance. Consequently, the Ti(Al) solid solution reacted with nitrogen to form in-situ Ti(Al)N nano particles. The milled powder had a spheroid shape and a very narrow size distribution of about 1 μm at the end of milling. In-situ Ti(Al)N particles with an average size of 10 nm were attained at a ball-to-powder weight ratio of 10:1 and a Ti:AlN molar ratio of 1:1.     

Deposition,microstructure and hardness of TiN/(Ti,Al)N multilayer films

In this work, TiN/(Ti,Al)N multilayer films were deposited on stainless steel substrates with alternatively switching Ti and TiAl alloy targets sources on and off by pulse biased arc ion plating. The crystallography structures and cross-sectional structures of TiN/(Ti,Al)N multilayer films were evaluated by X-ray diffraction analysis (XRD) and by TEM, respectively. The hardness and film/substrate adhesion were determined by nanoindentation and scratch test, respectively. A complex set of microstructures has been found between TiN and (Ti,Al)N layers, at the interface, another layered interfacial region which consists of extremely fine sub-layers, which results from the rotation of the specimen in the deposition chamber. The hardness values of the multilayers exhibit higher hardness compared with that of monolithic (Ti,Al)N film.     

Spraying TiN by a Combined laser and low-pressure plasma spray system

The formation of a TiN-Ti composite coating by thermal spraying of titanium powder with laser processing of the subsequent coating in a low-pressure N₂ atmosphere was examined. A low-pressure plasma spray system was used in combination with a CO₂ laser. First, the coating was plasma sprayed onto a mild steel substrate using a N₂ plasma jet and titanium powder in a controlled low-pressure N2 atmosphere. The coating was then irradiated with a CO₂ laser beam in a N₂ atmosphere, and the coating was heated with a N₂ plasma jet. The amount of TiN formed in the coating was characterized by X-ray diffraction analysis. The influence of plasma spraying conditions such as plasma power, flow of plasma operating gases, chamber pressure, and laser irradiating conditions on the formation of TiN was investigated. The effect of TiN formation in the titanium coating on Vickers hardness of the coatings was examined. It was evident that coating hardness increased with an increase in TiN content in the coating and that a TiN-Ti composite coating with a hardness of more than 1200 H V can be obtained with the use of laser irradiation processing.     

Microstructure and Tribological Properties of TiB2/TiB/TiNx（x=1,0.3）/Ti Composite Coating Produced on Pure Ti by Laser Surface Alloying

TiB2/TiB/TiNx(x=1,0.3)/Ti composite coating was prepared on pure Ti by laser surface alloying by using powders of boron as starting materials.The composite coating was examined by X-ray diffraction(XRD),high-resolution transmission electron microscopy(HRTEM)and scanning electron microscopy(SEM).The friction and wear properties of the composite coating were examined using a pin-on-disk tester under dry sliding wear condition.The results showed that the top surface of the composite coating was mainly composed of TiB2,TiB,TiN0.3,TiN and Ti phases,while the interface of the composite coating was composed of TiB and Ti phases.The composite coating showed sticklike structure near the top surface,and dendrites structure near the interface.The friction and wear test showed that the composite coating had better wear resistance than pure Ti due to their higher microhardness than that of pure Ti substrate.     

Surface characterization and mechanical property of TiN/Ti-coated NiTi alloy by PIIID

A hard and adherent TiN/Ti thin film of approximately 3 μm in thickness was deposited on the surface of Ti-50.6 at.% Ni alloy by the PIIID technique. The surface composition and chemical state of the coated samples were evaluated by XPS. The XPS results indicate that titanium oxide and titanium oxynitride were present on the TiN surface. The spectra of Ti 2p, N 1s, O 1s and C 1s electrons before and after the film being sputter etched were also discussed. Scanning electron microscopy (SEM) and energy disperse spectroscopy (EDS) analyses demonstrate that an interfacial layer, containing Ti, N and Ni, was formed at the interface between the TiN and Ti coatings. Sliding wear tests show that the TiN coating significantly reduces the friction coefficient and improves wear resistance of the NiTi alloy.     

Dependence of Microstructure and Hardness of Nanocomposite Coatings of nc-(Ti_(1-x)Al_xN)/a-Si_3N_4 on Aluminum Contents

HARD COATINGS are finding a widely applicationin machining industries as tools and moulds since1980s[1].Hard coatings consisting of a variety of thetransition metal nitrides,for instance,TiN,TiC,TiCN,TiBN,TiAlN,CrN etc,usually service as a protectioncoatings that requires some better properties ofwear-resistance,corrosion-resistance and also highfatigue-strength especially at elevated temperature(formore details see Ref.2-6).The generic concept for the design of novelsuper-hard(>40G…     

真空退火对TC4钛合金表面Ti/TiN多层复合涂层性能的影响

金属基体材料表面硬质膜层在服役过程中,残余应力在膜基界面以及膜层内部界面之间的积聚会导致膜层发生界面剥落失效。以TC4钛合金基体表面Ti/TiN多层复合膜层为研究对象,探讨真空退火对复合膜层结构及性能的影响,并表征退火前后复合膜层的界面划痕失效以及抗粒子冲蚀性能。结果表明,真空退火促进了膜层内部以及膜基界面两侧原子的热扩散,使得界面结构特征明显弱化。界面状态的改变使得复合膜层的表面显微硬度降低以及膜基结合强度提高。在划痕载荷作用下,复合膜层抵抗裂纹沿界面扩展的能力得到增强。真空退火有助于提高膜层的强韧性匹配,可有效抵抗小角度冲蚀粒子的犁削以及大角度粒子冲蚀下的疲劳,因此Ti/TiN多层复合膜层表现出较好的抗冲蚀性能。     

A study on microstructure and properties of calcium phosphate coatings processed using ion beam assisted deposition on heated substrates

In this study a set of thin Hydroxyapatite (HA) [Ca₁₀(PO₄)₆(OH)₂] coatings was deposited on heated silicon and titanium substrates using Ion Beam Assisted Deposition (IBAD). The effects of substrate temperature and processing parameters on the microstructural properties and composition of the coatings are being studied. Analytical techniques include transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM) with an energy dispersive X-ray spectroscopy (EDS), as well as scanning electron microscopy (SEM) with EDX, X-ray diffraction (XRD), and Fourier Transform Infrared Spectroscopy (FTIR). The current results indicate that as substrate temperature increases the Ca/P ratio of the coatings both on titanium and silicon substrates increases. The crystallinity of the coatings and the number of calcium phosphate compounds within the coating including HA also increases. STEM-EDS revealed an atomically diffused intermediate layer at the interface between the coating and substrate. XRD results along with TEM selected area diffraction (SAD) revealed that the coatings are composed of HA, other calcium phosphate, and calcium oxide compounds.     

Coating titanium on carbon steel by in-situ electrochemical reduction of solid TiO2 layer

Ti coating on A3 steel was successfully prepared by direct electrochemical reduction of high-velocity oxy-fuel (HVOF) thermally sprayed and room-temperature dip-coating titanium dioxide coating on A3 steel in molten CaCl₂ at 850 °C. The interfacial microstructure and mutual diffusion between coating and steel substrate were investigated using scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy. The results show that the precursory TiO₂ coating prepared by HVOF has closer contact and better adhesion with the A3 steel substrate. After electrolysis, all of the electro-generated Ti coatings show intact contact with the substrates, regardless of the original contact situation between TiO₂ layer and the steel substrate in the precursors. The inter-diffusion between the iron substrate and the reduced titanium takes place at the interface. The results demonstrate the possibility of the surface electrochemical metallurgy (SECM) is a promising surface engineering and additive manufacturing method.     

激光熔覆-激光氮化复合法制取TiNi-TiN梯度材料

将激光熔覆与激光表面氮化技术相结合制取TiNi-TiN梯度材料。采用先进的六孔同轴送粉喷嘴系统,分别将纯Ti、Ni粉末按一定比例送入激光熔化区,在粉末熔化过程中发生Ti、Ni间高温合成反应,原位合成一定厚度的TiNi金属间化合物熔覆层,然后将原位合成的熔覆层在富氮气氛中进行激光氮化处理,表面形成一层金黄色的TiN。利用光学显微镜和扫描电镜观察了熔覆层组织,并测量了熔覆层及氮化层的厚度。对不同工艺参数获得的熔覆层用X射线衍射仪进行了物相鉴定,并对氮化试样的熔覆层进行了显微硬度分布测试,得出了较好的制取TiNi-TiN梯度材料的工艺参数为:激光功率600 W,扫描速度0.5 m/min,钛送粉量2.5 g/min;镍送粉量3.2 g/min。     

涂层IrO2+Ta2O5钛阳极在析氧过程中的形貌和成分变化

作者用热分解法制备钛基IrO2+Ta2O5涂层阳极,涂层制备态在373 K马弗炉中长时间时效处理,然后在0.5mol/L H2SO4介质中、4A·cm-2电流密度下进行强化寿命试验.用自带能谱仪(EDS)的场发射高分辩电子扫描显微镜(SE-SEM)和X射线衍射仪(XRD)进行电解前后的表面形貌和成分分析.研究结果显示涂层制备态在373K马弗炉中长时间时效处理时,金红石IrO2织构优先生长且晶面间距随时效时间延长而增加;电解过程中涂层的失效过程为气体氧对涂层界面的冲刷造成涂层逐层腐蚀消耗,接着涂层产生裂纹和扩展,导致涂层剥落;化学成分方面,涂层氧化铱优先消耗和氧化钛逐步积累.     

CFRP表面激光熔覆TC4 + AlSi10Mg复合涂层的组织与性能

采用激光熔覆技术在碳纤维增强热塑性塑料(carbon fiber reinforced thermoplastics, CFRP)表面成功地制备了TC4 + AlSi10Mg复合涂层. 通过扫描电镜、能谱仪和透射电镜分析了TC4 + AlSi10Mg复合涂层与CFRP基体连接的界面层微观结构、元素成分分布及相组成. 采用纳米压痕仪对复合涂层到基材的硬度变化规律进行测试. 结果表明,通过激光熔覆技术可以快速在CFRP材料表面形成连续的、均匀的TC4 + AlSi10Mg复合涂层. TC4 + AlSi10Mg复合粉末在激光作用下,受热熔化渗透到CFRP基体内部,形成良好的冶金结合,并在碳纤维-树脂-复合涂层之间形成连续的界面层. TC4 + AlSi10Mg复合涂层与CFRP基体连接的界面层相成分为TiC,Ti₃Al,TiS₂和Ti₃AlC相. CFRP基体的平均硬度为10.15 HV,涂层的最高硬度可达1914 HV. 基于试验观察和理论分析,得出CFRP表面激光熔覆TC4 + AlSi10Mg复合涂层主要的界面反应机理为Ti(s) + C(s)→TiC(s),Al(l) + 3Ti(s)→Ti₃Al(s).