金属钛激光气体氮化层组织及表面特征

采用连续波Nd-YAG激光在氮气环境中对金属钛进行激光气体氮化处理.利用SEM,XRD,XPS研究氮化层的显微组织、表面成分、结构.结果表明:通过激光气体氮化可以在金属钛表面得到表面相对平滑、无裂纹的氮化层;氮化层与基体材料之间为冶金结合.氮化层主要由枝晶状TiN组成,同时有TiNxOy,TiO2及TiC存在,外表面有C,O污染或吸附;TiN枝晶密度由表面沿深度方向下降.     

影响内氧化生成Al2O3/Cu表面复合层厚度及组织的因素

采用真空条件,用CuO作氧化剂,在一定的温度下使Cu-Al合金内氧化,获得Al₂O₃/Cu表面复合材料。金相分析发现,在较低温度下内氧化,表面复合层中Al₂O₃颗粒晶界处多于晶内;在较高温度下内氧化,复合层中Al₂O₃颗粒呈弥散状分布;表面复合层厚度随Al含量的增加而减薄,显微硬度随Al含量的增加而升高。     

多弧离子镀TiN/TiCrN/CrN多元多层复合膜的制备及性能研究

采用XH-800多弧离子镀设备在硬质合金刀具表面制备TiN/TiCrN/CrN多元多层复合膜.利用XRD、SEM、显微硬度计、多功能材料表面性能测试仪等对其组织结构与性能进行了研究.结果表明:膜层表面均匀,未出现龟裂现象,色泽光亮度好;膜的相结构组成为TiN和Cr2N,随着Cr靶电流的增大,TiN的择优取向由(200)向(111)转变,膜层出现单质Cr;膜层厚度为5.02μm,具有明显多层特征;显微硬度2536 HV;结合力65 N.     

真空阴极离子镀法制备Ti/TiN/Zr/ZrN多层膜

过去,在不锈钢上沉积10μm以上多元多层软硬交替Ti/TiN/Zr/ZrN厚膜用以提高材料耐腐蚀性能的报道不多.采用阴极电弧离子镀结合脉冲偏压的方法制备了厚度选15 μm的Ti/TiN/Zr/ZrN多层膜.运用扫描电镜(SEM)、X射线衍射(XRD)、显微硬度计、划痕仪等考察了多层膜的形貌、厚度、相组成、硬度以及膜/基结合力,并利用电化学方法评价了基体、单层TiN薄膜以及多层膜的电化学腐蚀性能.结果表明:制备的Ti/TiN/Zr/ZrN多层膜界面明晰、结构致密、晶粒细小;膜/基结合力大于70 N,显微硬度达28 GPa;多层膜比单层TiN膜在提高1Cr11Ni2W2MOV基体的抗腐蚀能力方面具有更显著的作用.     

反应烧结法制备(AlN,TiN)-Al2O3复合材料的研究

以Ti,Al,Al₂O₃为初始粉料,通过750~800℃氮气保护下的中温焙烧,然后在1420~1550℃在氮气氛下反应烧结,制备了不同配比的(AlN,TiN)-Al₂O₃复合材料。研究了组成及烧结工艺对复合材料力学性能、显微结构等的影响。用XRD,SEM等方法分析粉体及烧结体的相组成及微观结构。分析结果表明:AlN,TiN的形成,有助于材料的致密化并使其力学性能提高。组成为20wt%(Al,Ti)-Al₂O₃的粉体在1520℃、30MPa、保温、保压30min热压烧结条件下,与N₂气反应可得到硬度(HRA)为 94.1的高硬度的(AlN,TiN)-Al₂O₃复合材料,该材料的抗弯强度为687 MPa,断裂韧性(K_IC)为6.5MPa·m1/2。     

NiTi 合金表面激光原位反应合成TiN增强金属基复合材料涂层

采用连续高功率固体Nd-YA G激光辐照, 使预置于NiTi 合金表面的Ti 粉在N₂ 环境中形成TiN 增强Ti 基复合材料涂层。选择适当的激光辐照工艺参数, 获得致密的TiN 增强金属基复合材料激光改性层。SEM 观察及EDAX 成分分析结果表明, TiN/ Ti 金属基复合材料表面改性层与基体NiTi 合金存在良好的冶金结合, 界面处成分均匀过渡, 表面Ni 含量极低。显微硬度测试及磨损实验表明, TiN/ Ti 金属基复合材料改性层显著提高了NiTi 合金的表面硬度和耐磨性, 激光表面改性层可有效地改善NiTi 合金作为生物医学材料使用的表面成分和性能。     

电场激活燃烧合成( TiB2)PNi/Ni3Al/ Ni功能梯度材料

采用电场激活压力辅助合成技术(FAPAS)制备了(TiB₂)_PNi/(TiB₂)_PNi₃Al/Ni₃Al/Ni梯度材料，主要研究电场激活燃烧合成过程中电场对材料合成及层界面扩散连接的作用。分析了梯度材料各层的界面微观组织及相组成和材料的硬度分布。结果表明，采用FAPAS 技术结合机械合金化工艺制备的(TiB₂)_PNi/(TiB₂)_PNi₃Al/Ni₃Al/Ni 功能梯度材料具有快速、简便和组织均匀密实的特点。梯度材料的陶瓷复合层、Ni₃Al层和Ni板的界面区产生成分的互扩散，形成了良好的冶金结合。从Ni板到陶瓷复合层的硬度呈梯度分布。     

Cr3C2粒径对等离子堆焊铁基合金层组织与耐磨性能的影响

在低碳钢表面利用等离子堆焊技术分别制备Fe50堆焊层及添加40％(质量分数)微米和纳米Cr₃C₂的(Fe50+40%微米/纳米Cr₃C₂)复合堆焊层,比较研究添加不同粒径的Cr₃C₂对Fe50合金堆焊层的显微组织与磨损性能的影响。采用X射线衍射仪(XRD)分析堆焊层的相组成,利用扫描电镜(SEM)和能谱分析仪(EDS)观察堆焊层的显微组织形貌及微区成分,通过显微硬度计测试了堆焊层的硬度分布,使用滑动磨损及冲击磨损试验机分别考察了复合堆焊层的磨损性能。结果表明:Fe50等离子堆焊层组织主要由柱状晶α-Fe及其间的网状共晶α-Fe+Cr₂₃C₆组成;而Fe+40%微米/纳米Cr₃C₂堆焊层凝固方式为过共晶,由大量的先共晶碳化物及其间细密、均匀的枝晶与共晶组织组成,并增加了γ-Fe、Cr₇C₃和未熔Cr₃C₂等相;但Fe+40%纳米Cr₃C₂涂层比Fe+40%微米Cr₃C₂涂层析出更多且细小、致密的先共晶碳化物。与Fe50等离子堆焊涂层相比,Fe+40%微米Cr₃C₂涂层的显微硬度、滑动磨损性能及冲击磨损性能分别提高了21%、1.5倍和0.8倍;而Fe+40%纳米Cr₃C₂涂层的显微硬度、滑动磨损性能及冲击磨损性能则分别提高了34.1%、2.4倍和1.7倍,表面的犁沟和剥落及塑性变形明显减少,耐磨性能显著提高。因此,添加纳米Cr₃C₂颗粒可以显著细化铁基合金等离子堆焊层的显微组织并提升其耐磨性能。     

合金化填充材料Ni 对SiCP/6061Al 复合材料激光焊接焊缝显微组织的影响

以N i 片作为合金化填充材料对SiC_P/6061A l 金属基复合材料(SiC_P/6061A lMMC) 进行激光焊接, 研究了激光输出功率、焊接速度等焊接工艺参数对焊缝显微组织的影响。结果表明, 采用金属N i 片作为合金化填充材料对SiC_P/6061A lMMC 进行激光焊接, 可以在一定程度上抑制SiC 颗粒的溶解及针状脆性相Al₄C₃ 的形成, 并获得以Al₃Ni 等相为增强相的焊缝显微组织, 但在焊缝心部有粗大的气孔形成。     

层状Ti3SiC2陶瓷的组织结构及力学性能

利用热压烧结TiH₂,Si和C粉获得了致密度大于98%的层状Ti₃SiC₂陶瓷。利用压痕法,在不同的载荷下测定了材料的维氏硬度, 发现其硬度值随载荷的增加而降低,在最大载荷30kg时,硬度值为4GPa。压痕对角线没有发现径向裂纹的出现。 这归因于多重能量吸收机制——颗粒的层裂、裂纹的扩展、颗粒的变形等。利用三点弯曲法和单边切口梁法测定了材料的强度和韧性分别为270MPa和6.8MPa·m1/2。Ti₃SiC₂材料的断口表现出明显的层状性质,大颗粒易于发生层裂和穿晶断裂,小颗粒易被拔出。当裂纹沿平行于Ti₃SiC₂基面的方向扩展造成颗粒的层裂,当裂纹沿垂直于基面的方向扩展时,裂纹穿过颗粒的同时,在颗粒内部发生偏转,使裂纹的扩展路径增加。裂纹的扩展路径类似人们根据仿生结构设计的层状复合材料。裂纹在颗粒内的多次偏转、裂纹钉扎以及颗粒的层裂和拔出等是材料韧性提高的主要原因。此外,在室温下得到的荷载-位移曲线,说明Ti₃SiC₂材料不象其它陶瓷材料的脆性断裂,而是具有金属一样的塑性。     

Laser Gas Nitriding of Ti-6Al-4V Part 2: Characteristics of Nitrided Layers

The characteristics of laser nitrided layers formed on Ti-6Al-4V are presented in this investigation. It has been determined that titanium nitride (TiN) is formed, which significantly increases the hardness of the nitrided surfaces. The amount of titanium nitride produced depends on the processing parameters such as laser pulse energy and nitrogen concentration. Nitrided layers are much smoother along the laser pass direction than perpendicular to this direction. The shrinkage effect in the laser melt zone produces surface residual tensile stresses in Ti-6Al-4V samples regardless of whether the processing environment is Ar, N₂, or a mixture of these gases. Pre-heating or stress relieving after laser nitriding significantly reduces the residual tensile stress level.     

Metal matrix composite layers formed by laser processing of commercial purity Ti–SiCp in nitrogen environment

Abstract

Metal matrix composite layer formation by means of laser alloying using 6 μm particle size SiC powder (SiC_p) preplaced on titanium surfaces in a nitrogen environment produced golden coloured tracks and a complete solution of SiC_p in the melt zones under a range of processing conditions. The melt layers consisted of dendrites at the top (titanium nitride based) followed by threadlike particle structures (titanium silicides), and the sizes of dendrites and the threadlike particles werefound to increase with increasing laser power density. The surface layer of the dendrites developed a hardness 4·5–9 times that of the base metal (150 HV), and the deep underlying threadlike structures had a plateau of hardness of aboout 2·8–4 times the base hardness. The metal matrix composite layers were found to be 2–4 times thicker than those produced previously in a helium environment under similar processing conditions. The exothermic reactions due to the formation of titanium nitride, titanium carbide, or titanium carbonitride along with titanium silicide during laser melting of SiC_p coated titanium surfaces under a nitrogen environment are considered to be responsible for the greater melt depth and complete dissolution of ceramic particles, by increasing the temperature of the melt.

MST/3208     

The effect of laser surface nitriding with a spinning laser beam on the wear resistance of commercial purity titanium

Laser nitriding of commercial purity titanium using various concentrations of helium and nitrogen has been carried out. The surface appearance and microstructure of a treated layer were found to be dependent on the beam power density, interaction time, velocity and concentration of nitrogen. X-ray diffraction analyses have led to the conclusion that the dendrite layer in the resolidified zone of the nitrided specimens consisted mainly of TiN. The surface roughness of specimens after various laser treatments was investigated by SEM and a surface profilemeter. Using optical microscopy, the dendrite TiN and needle-like structure in the melt zone, and the large grain structure in the heat affected zone, were investigated. The surface wear resistance of nitriding CPTi was significantly improved compared to the untreated or laser glazed material, and the wear data were found to correlate with scanning electron microscopy observations. Two layers, having different microstructures, thickness and abrasive wear resistance were identified. Further, 100% overlapping considerably improved the wear resistance of the nitrided specimens.     

Laser Gas Nitriding of Ti-6AI-4V Alloy

Laser gas nitriding of Ti-6A1-4V has been investigated with both CO₂ and Nd:YAG lasers. Results indicate that Nd:YAG laser in pulse mode provides a better surface finish and a lower cracking severity than CO₂ laser. A crack-free nitrided layer has been obtained by optimizing the processing parameters. Titanium nitride (TiN) significantly increases the hardness of the nitrided surfaces. The amount of titanium nitride produced depends on the processing parameters, such as laser pulse energy and nitrogen concentration. With optimized parameters, the nitrided surface is somewhat rougher than the polished base metal but much smoother than the shot peened surface. The shrinkage effect in the laser melt zone produces surface residual tensile stresses regardless of the processing environment. Preheating or stress relieving after laser nitriding can significantly reduce the residual tensile stress level.     

Diffusion kinetics of explosively treated and plasma nitrided Ti-6Al-4V alloy

Ti-6Al-4V alloys, which were exposed to an explosive shock process, were nitrided in nitrogen plasma in the temperature range of 700-900°C for 3-12 h. During the plasma nitriding, the surface layer consisted of TiN (δ), Ti₂N (ε) and nitrogen solid solution layers (α-Ti). The growth rate of nitride and solid solution layers were found to be controlled by the diffusion of nitrogen. An effective nitriding was achieved due to high dislocation density and vacancy concentration. Based on the present layer growth data, an analytical model for multiphase diffusion was used to estimate the effective nitrogen atom diffusion coefficient in the nitride layers. The interface velocity equations were derived from Fick's law and a numerical method has been used to compute the diffusion coefficients of nitrogen in a binary multiphase Ti-TiN system. Depending on temperature and layer thickness, the activation energies of nitrogen in TiN and Ti₂N phases were found to be 18,950 (±2116) and 27,925 (±1105) cal/mole, respectively.     

Ion-nitriding behaviour of Fe-Ti alloys in theα-phase region

The ion-nitriding behaviour of four iron alloys containing between 0.11 and 1.48 wt% titanium was investigated in the-phase region to discuss kinetics of the growth of the nitriding layer. The ion-nitriding experiments have been made at 823 K. Two nitriding layers were observed: a thin surface layer which mainly consists of Fe₄N; an internal nitriding layer beneath the surface layer, where the nitride formed was found to be TiN. The growth of the internal nitriding layer is controlled by a diffusion process of nitrogen in the matrix metal. The apparent diffusion coefficient of nitrogen in the nitriding layer, evaluated using the rate equation proposed for internal oxidation, increases linearly with the volume fraction of titanium nitride. Furthermore, by excluding the effect of the titanium nitride from the apparent diffusion coefficient, the diffusion coefficient of nitrogen in-iron was calculated, being in good agreement with that reported so far. In addition, the increase in hardness in the internal nitriding layer has been discussed.     

Titanium nitride laser-beam surface-alloying treatment on carbon tool steel

In order to improve the wear resistance of tool steel, a study of TiN surface-alloying treatment on 1% carbon steel by irradiation with a CO₂ laser beam was performed. Argon and nitrogen were used as shielding gases, and their effects on the formation of the surface-alloyed layer were investigated. The effect of cobalt additions to the TiN powder on the hardness of the alloyed layer was also investigated. When argon was used as shielding gas, the depth of the alloyed layer was increased compared with the depth when nitrogen was used as a shielding gas. A portion of the TiN decomposed into titanium in the argon environment, the nitrogen apparently being lost as a gas. The structure of the surface-alloyed layer was composed of a ferritic phase without martensitic structure even at high cooling rates. When this layer was annealed at 1000 ° C for 3 h, part of the titanium precipitated as TiC particles. The hardness of the annealed alloyed layer increased to about 500 Hv. This increase in hardness was accompanied by the appearance of martensite. When nitrogen was used as shielding gas, decomposition of TiN was suppressed and the hardness of the alloyed layer reached 850 Hv. These layers had a martensitic structure. Thus, nitrogen is preferable to argon as a shielding gas if a martensitic structure is desired in this system. When 5% cobalt was added to the TiN powder, the hardness of the alloyed layer increased to 1100 Hv. This increased hardness is caused by stabilization of the martensitic structure caused by an increase in theM _s temperature.     

X-ray reflectivity study on TiN/Ti/Si structures before and after annealing

X-ray reflectivity was employed as a powerful tool for studying the surface and interface roughness and thickness, as well as density, of TiN/Ti/Si layers. X-ray reflectivity of the as-deposited samples, with nominal thickness of 17.5 nm of Ti and 3.0 nm of TiN, shows uniform oscillations. When the samples are annealed at 710°C, residual strongly attenuated oscillations are still observed, while the 850°C-annealed sample does not show oscillations, indicating high surface and interface roughness of the formed nitride and silicide layers. It is demonstrated that increased interface roughness, even for a layer with a larger average electron density difference, reduces the oscillations in the reflectivity curve very rapidly. For comparison, cross sectional transmission electron microscopy was employed to find the thickness of the surface and interface layers in silicide structures, which are in good agreement with the X-ray reflectivity results. The work was also supported by tapping mode atomic force microscopy observations, where we have observed nearly flat structures for the as-deposited sample surface and needle-like protrusions for the annealed samples. The surface roughness of the top TiN layer was used to obtain simulated X-ray reflectivity spectra in good agreement with the experimental results. Preliminarily, the crystallography of the layers in the samples was determined by the grazing angle X-ray diffraction technique, to acquire knowledge on the Ti and Si compounds formed in the samples after the annealing.     

Effect of N2/Ar gas flow ratios on the nitrided layers by direct current arc discharge

Nitrided layers were prepared on titanium substrates by direct current (DC) arc discharge technique. The effect of nitrogen to argon flow ratios on the microstructures and mechanical properties of the samples was investigated. The X-ray diffraction results show that the surfaces of the layers consist mainly of TiN and a very little TiN_0.3 (101) under the condition of nitrogen/argon gas mixture. A strong TiN (200) preferential orientation in nitrided layers can be seen. With increasing the nitrogen concentration ratio in nitrogen/argon gas mixture, the density and size of TiN dendrites in the nitrided layers, and the hardness and wear resistance of the layers enhanced significantly.     

氮氩混合比对TA2真空氮化层结构与性能的影响

采用间歇式真空氮化技术对TA2钛合金进行渗氮处理。探究氮氩混合比对合金氮化层结构和性能的影响规律。结果表明:表面渗氮层主要由TiN和TiN0.3相组成,氮氩比越低其有效硬化层越厚,但会降低有效活性N原子的相对含量,不利于渗层的致密性。适当的氮氩混合比能在TA2表面形成氮化物,N原子有效地向纵深扩散,氮化物层与扩散层结合紧密,过渡良好,硬度梯度平缓;腐蚀电位随着氮氩比的增加呈现逐渐上升趋势,从氮氩比为1∶5时的-0.622V提升到氮氩比为5∶1时的-0.549V,腐蚀电流和腐蚀速率则呈现出逐渐降低的趋势。