等离子体渗氮气压对合金钢渗氮层微观结构和性能的影响

目的 选择M50NiL钢（高合金钢）和AISI 4140钢（低合金钢）2种合金钢,研究渗氮气压对合金钢等离子体渗氮层组织结构、渗层厚度、硬度、韧性和摩擦磨损性能的影响规律。方法 根据离子渗氮GB/T30883—2017,在0～500 Pa渗氮气压范围内选择170、250、350 Pa 3个渗氮气压进行等离子体渗氮,研究渗层微观结构和性能。结果 对于M50NiL和AISI 4140两种合金钢,350 Pa时渗层厚度均最大,170 Pa次之,250 Pa厚度最小。M50NiL钢在350 Pa渗氮和AISI 4140钢在170 Pa渗氮时,表面层具有最优的强韧性。摩擦磨损性能显示,170 Pa和350 Pa气压渗氮的摩擦磨损性能明显优于250 Pa气压渗氮,其中磨损率规律与渗氮层的韧性值测试结果吻合。结论 气压影响了氮离子的能量和分布,从而影响了渗层厚度,钢中的合金元素含量和气压共同影响表面强韧化效果,并且表面强韧化效果直接影响渗氮层的摩擦磨损性能。     

Duplex treatment of AISI 304 austenitic stainless steel using rf nitriding and dc reactive magnetron sputtering of titanium

In this work, duplex treatment has been carried out using radio frequency (rf) plasma nitriding process and direct current (dc) magnetron sputtering of titanium. Nitriding of AISI 304 stainless steel, using rf plasma technique, created a thick modified layer of approximately 20 μm for short plasma processing time of 10 min. After nitriding process, a thin titanium nitride film has been deposited using dc magnetron sputtering of titanium for different nitrogen/argon gas pressure ratios. The treated samples were characterized via glow discharge optical spectroscopy, X-ray diffractometry, scanning electron microscopy, profile meter and Vickers microhardness tester. The elemental composition, thickness and microhardness values of the duplex treated layers are found to be gas composition dependent. The data shows that the microhardness of the duplex treated layer increases to 1.42 fold relative to the associate value of the nitrided one. Moreover, high deposition rate of 110 nm/min is obtained.     

TC4钛合金不同气源激光渗氮行为

在用矩形光斑高功率半导体激光器,在纯氮气和氮氩混合两种不同方式下,通过不同气流量和氮氩混合对Ti-6Al-4V进行表面渗氮,研究气体流量、氮氩混气比对渗氮熔池形态及渗氮组织和力学性能的影响。采用SEM、EDS以及XRD对渗氮层的显微组织、微区成分及相组成进行研究。结果表明:采用纯氮渗氮时,在15 L/min气流量下获得均匀渗氮层,继续增大气流量渗氮熔池流动紊乱,出现贯穿裂纹,且渗氮深度和硬度并未随气流量增加;采用不同氮氩混气比渗氮时,渗氮层的表层硬度均较相同条件下纯氮气渗氮层的有所降低,且渗氮层裂纹倾向减弱,渗氮层组织由表至里在200~800μm内按层深依次存在TiN0.88、TiN0.61、TiN0.3三种稳定相;分别采用纯氮气和不同氮氩混气比渗氮时,渗氮层组织沿层深分布依次均为粗短树枝晶、等轴晶、细长树枝晶、针状晶。     

Cr12钢的稀土诱导离子渗氮工艺

对Cr12钢进行了稀土诱导离子溅射渗氮试验,利用显微硬度计测量了试样表面渗氮层的硬度与层深,结合XRD衍射仪分析了复合渗氮层的相组成,最后用摩擦试验机检测试样表面的摩擦磨损特性。结果表明,稀土能够影响Cr12钢离子溅射渗氮效果,且其效果随两者距离的增加而急剧下降。当稀土与Cr12钢试样距离小于25 mm时,试样表面硬度相对普通离子渗氮工艺明显减小,表面摩擦因数及磨损率略差,但其渗氮层深度却明显增加;当两者距离超过25 mm时,稀土诱导效果明显减弱,试样表面的硬度及摩擦因数与普通离子渗氮工艺基本相同,但磨损率明显增大。分析表明,稀土元素能增大试样表面氮离子的吸附能力且为其渗入提供路径优势,当两者距离过大时稀土离子吸附性减弱,诱导效果消失,同时也使试样表面产生晶格缺陷,降低了其表面抗磨损的能力。     

SURFACE ANALYSES OF NITROGEN ION IMPLANTED Ti6Ai4V ALLOY

The techniques for surface analysis including AES,XPS and SIMS were employed to studythe chemical composition and bond valence of nitrogen ion implanted surface of surgicalimplantation service alloy Ti6Al4V.The depth of implanted nitrogen ions and the sputteringrate of argon beams were determined using a profilometer.It was found that the combinationof injected nitrogen ions with titanium resulted in the formation of hard TiN particles and theprofile of nitrogen concentration approximately displayed gaussian distribution.The totaldepth of implanted nitrogen is about 350 nm and its maximum concentration appears in thedepth of about 140 nm from the surface,in which the concentration ratio of nitrogen totitanium may be up to 1.1.     

氮离子注入的Ti6Al4V表面分析

利用表面分析技术(AES,XPS,SIMS)研究了经氮离子注入的外科植入材料Ti6Al4V表面成分与键合态,用轮廓仪的测量结果计算了氮离子注入深度及注入氮离子的Ti6Al4V的刻蚀速率。考虑到该合金的基体效应,对AES的定量结果进行了修正。结果表明,注入到合金中的氮离子与合金中的Ti形成高硬度的TiN,N的分布近似为Gauss形式,注入总深度约为350nm,在距表面约140nm处氮量最大,N与Ti的浓度比可达1.1。     

阴极电压和供氮方式对纯氮离子渗氮的影响

分别研究了在500、600、650和700 V阴极电压条件下采用连续供气抽真空和间歇供氮闭炉的方式进行纯氮离子渗氮的工艺及机理.通过对间歇供氮闭炉离子渗氮层显微组织、相组成和硬度梯度的测定与分析,计算和验证了该工艺中N2分子临界离解能.结果表明,纯氮离子渗氮的活性氮原子来自于经阴极位降区加速的高能N 2与中性N2分子间的非弹性碰撞,离解N2分子的N 2离子临界能为48.64 eV,相应的阴极电压门槛值为650 V.纯氮离子渗氮工艺除要求阴极电压高于650 V外,间歇供气闭炉渗氮也是必备条件,在一定温度和足够高的阴极电压下,只有采用间歇供氮闭炉方式进行离子渗氮,从N2分子才能离解出足够多的活性氮原子,使试样表面产生明显的渗氮效果.     

钽低温离子渗氮工艺参数对渗氮层物相的影响

利用组合的二次回归正交实验设计方案 ,对钽低温离子渗氮条件下 ,表面物相及固溶体中氮的含量随渗氮温度、气氛总压力和氢氮摩尔比的变化进行了系统研究。发现表面渗氮层由化合物Ta6N2 .57、超晶格TaN0 .1和固溶体相组成。氮在钽中的固溶度随气压、温度和氢摩尔分数的增加而增加 ,化合物和超晶格相含量随温度增加而增加 ,同时化合物相随氢摩尔分数增加有一个极大值 ,该极大值随温度增加而下降。     

Influence of process parameters on electrochemical and physical properties of sputtered iron-doped nickel oxide thin films

1Introduction A principal focus of modern research in electrocatalysis is to discover electrode materials that exhibit excellent electrochemical stability and show interesting activity towards typical electrochemical reaction[1?10].It is desirable that th…     

Hydrogen behavior in the iron surface layer modified by plasma nitriding and ion boronising

The effects of the plasma nitriding with the formation of compound nitride and diffusion zones and of the boronising with the different ion doses on hydrogen distribution and hydrogen induced deterioration of a surface layer were examined in the case of Armco iron. Electrochemical studies of hydrogen permeation rate, hydrogen vacuum extraction measurements, optical and scanning microscopy, X‐ray diffraction and elastic recoil detection analysis (ERDA) were used. Accumulation of entering hydrogen within the various constitutent zones of the modified layer inhibits the hydrogen transport into the metal and thus, decreases the mean hydrogen content in the deeper zones and in the core. Hydrogen accumulation within the compact nitride zone causes the expansion of the nitride lattice, nitride phase transformation and deterioration. The ion boronising enhances the hydrogen effects in the plasma nitrided layers. Therefore, modification of the surface layer by plasma nitriding and ion boronising may result in preventing of the bulk metal from hydrogen induced degradation, but may cause hydrogen deterioration of the surface layer, depending on the treatment parameters.     

Tribology and cyclic oxidation behavior of plasma nitrided valve steel

In this study, the tribology and cyclic oxidation behavior of plasma nitrided DIN 1.4871 austenitic valve steel were investigated. For this purpose plasma nitriding treatments were carried out in nitrogen and hydrogen with ratio N₂/H₂: 1/3 at 10 Torr pressure. Nitriding cycles of 400, 450, 500 and 550 °C for 7 h were selected. To remove oxide layer and to enhance diffusion, an effective sputter cleaning procedure was applied in argon and hydrogen gases. The pin-on-disc sliding wear experiments were performed at a load of 6 N and sliding velocity of 0.1 m/s in normal atmosphere under dry condition. Cyclic oxidation tests used to evaluate the oxidation characteristics of the samples consisted of 50 cycles each 30 min at 750 °C. The structure and properties of the samples were examined by optical and scanning electron microscopy (SEM), microhardness measurements and X-ray diffraction. The results indicated plasma nitriding at all temperatures increased the wear resistance of valve steel when sliding against bearing steel. The 550 °C nitrided layer, with CrN, Fe₄N and Fe_2-3N on the surface, was most effective in improving wear resistance. In the case of cyclic oxidation, the results showed that oxidation resistance depends strongly on nitriding temperature. Nitriding at 450 °C produced a layer of predominantly “S” phase which was more effective in improving the oxidation resistance of valve steel.     

离子渗氮用气对后续磁控溅射镀层性能的影响

以40Cr钢为基体材料,进行离子氮化和闭合场非平衡磁控溅射PVD复合表面处理工艺试验。重点探讨用氮、氢混合气体及工业用氨进行离子氮化所得到的白亮层对后续PVD镀层性能的影响。测试了镀层厚度、膜基结合力及摩擦学性能。结果显示,不同渗氮气体得到的复合镀层临界划痕载荷均大于60 N,洛氏压坑边缘均无剥落,但氨处理的压坑边缘有少量坍塌并出现裂纹,表明其白亮层存在缺陷,在球坑试验的试样上也直接观察到缺陷的存在。存在缺陷的白亮层断裂韧性低,压坑试验时,缺陷处启动裂纹并扩展,导致化合物层和PVD镀层的剥落。销盘磨损试验结果表明,用氮和氢混合气体氮化后镀CrTiA lN具有更好的综合摩擦学性能。     

Film characterization of titanium oxide films prepared by high-power impulse magnetron sputtering

Surface modification with a high power glow discharge is an emerging technology that can be used to improve the surface characteristics. Titanium oxide films are prepared using a high-power impulse magnetron sputtering (HPPS-M) glow discharge with a current density of 2 A/cm² and a power density of 1 kW/cm². Observing optical emission spectrum confirms that singly-ionized titanium ions are produced in the plasma. Ions are extracted from the HIPIMS glow plasma by a substrate placed near the plasma source. It is found that the substrate is immersed in the HPPS-M glow plasma. The film is deposited by a HPPS-M, and the results are compared to those of magnetron sputtering operated by a stationary dc power source. The deposition rate is lower by HPPS-M than that by DC-MS. The main structure of the films is rutile, however an anatase structure is also observed. The mixed structure is obtained at an oxygen rate as low as 5%. Anatase structure is not significantly observed in HPPS-M compared to that in DC-MS. The intensity of the XRD profiles becomes weaker with increasing the substrate position due to the collisions of metal species with the plasma species and the background gas particles. The deposition rate of the prepared titanium oxide film is significantly influenced by the production rate of titanium ions, distance of the substrate, and the gas mixture ratio. With regard to the effect of the gas ratio, the difference in the deposition rate is probably based on the argon ion density available to sputter titanium atoms that would eventually contribute to the titanium oxide film deposition.     

Room temperature process for chemical vapor deposition of amorphous silicon carbide thin film using monomethylsilane gas

The silicon carbide thin film formation process, which was completely performed at room temperature, was developed by employing a reactive silicon surface preparation using argon plasma and a chemical vapor deposition using monomethylsilane gas. Time-of-flight secondary ion mass spectrometry showed that silicon-carbon bonds existed in the obtained film, the surface of which could remain specular after exposure to hydrogen chloride gas at 800 °C. The silicon dangling bonds formed at the silicon surface by the argon plasma are considered to easily accept the monomethylsilane molecules at room temperature to produce the amorphous silicon carbide film thicker than monolayer. Thus, the entire silicon carbide thin film formation process at room temperature is possible.     

Effect of nitriding on the electrochemical behaviour of Ti‐Al‐Mn alloy

The effect of technological conditions of nitriding such as process time duration and chemical composition of saturating medium, on the corrosion behaviour of nitrided coatings in 14 M solution of sulphuric acid was analyzed. The investigations were done on the alloy Ti‐5,0 Al‐2,0 Mn. The nitriding was carried out in nitrogen both at atmospheric pressure and rarefied nitrogen pressure (1 Pa) at the temperature 850°C and time processing in the range from 5 to 20 h in nitrogen‐containing gas only, and in powder electrode graphite and nitrogen‐containing gas. It was shown that technological conditions of nitriding determine the protective properties of nitrided coatings. It was indicated that the optimal structure of the nitride layer for best corrosion protection is the thin nitride TiN_x with high surface quality and a gas‐saturated layer. Nitriding in graphite powder effects positively the protective properties of nitride coatings due to reducing the nitride‐forming process.     

Artifacts in sample preparation of transmission electron microscopy

Two types of typical artifacts induced by ion milling, damage on the surface and temperature elevation, were investigated. The ion-induced damage layer on the surface reached as high as 3.46 nm when 5 keV argon ions were bombarded at 75 degrees of incidence from the surface normal of Si(001). Cleaning up the surface using 250 eV argon ions could minimize the surface damage close to the level of natural oxide thickness. The local temperature was measured from samples with thermocouples mounted in two different ways. The temperature reached 296°C when a single ion gun was used to mill the sample at 5 keV with 80 degrees of incidence angle, while the sample with thick substrate was heated up to 198°C. A gold thin film was investigated to confirm the ion beam-induced annealing as an artifact. Possible ways to reduce the thermal load in the sample are suggested.     

Surface Modification of C17200 Copper-Beryllium Alloy by Plasma Nitriding of Cu-Ti Gradient Film

In the present work, a copper-titanium film of gradient composition was firstly fabricated by the dual magnetron sputtering through power control and plasma nitriding of the film was then conducted to modify C17200 Cu alloy. The results showed that the prepared gradient Cu-Ti film by magnetron sputtering was amorphous. After plasma nitriding at 650 °C, crystalline Cu-Ti intermetallics appeared in the multi-phase coating, including CuTi₂, Cu₃Ti, Cu₃Ti₂ and CuTi. Moreover, even though the plasma nitriding duration of the gradient Cu-Ti film was only 0.5 h, the mechanical properties of the modified Cu surface were obviously improved, with the surface hardness enhanced to be 417 HV_0.01, the wear rate to be 0.32 × 10^?14 m³/Nm and the friction coefficient to be 0.075 at the load of 10 N, which are all more excellent than the C17200 Cu alloy. In addition, the wear mechanism also changed from adhesion wear for C17200 Cu substrate to abrasive wear for the modified surface.     

Characteristics of copper oxide films deposited by PBII&D

Copper oxide films were deposited by plasma based ion implantation and deposition using a copper antenna as rf sputtering ion source. A gas mixture of Ar + O₂ was used as working gas. During the process, copper that was sputtered from the rf antenna reacted with oxygen and was deposited on a silicon substrate. The composition and the chemical state of the deposited films were analyzed by XPS. The structure of the films was detected by XRD. It is observed that Cu₂O film has been prepared on the Si substrate. It is found that the microstructure of the deposited film is amorphous for the applied voltage of − 5 kV. The surface layer of the deposited films is CuO. This is because the surface layer absorbs the oxygen from ambient air after the treated sample was removed from the vacuum chamber. An appropriate applied voltage, 2 kV under the present conditions, brings the lowest resistance. It is also seen that the maximum absorbance of the deposited films moves to a lower wavelength with increased applied voltage.     

Improvement of Mechanical Properties of Martensitic Stainless Steel by Plasma Nitriding at Low Temperature

A series of experiments were carried out to study the influence of low temperature plasma nitriding on the mechanical properties of AISI 420 martensitic stainless steel. Plasma nitriding experiments were carried out for 15 h at 350℃ by means of DC- pulsed plasma in 25%N2＋ 75%H2 atmosphere. The microstructure, phase composition, and residual stresses profiles of the nitrided layers were determined by optical microscopy and X-ray diffraction. The microhardness profiles of the nitridied surfaces were also studied. The fatigue life, sliding wear, and erosion wear loss of the untreated specimens and plasma nitriding specimens were determined on the basis of a rotating bending fatigue tester, a ball-on-disc wear tester, and a solid particle erosion tester. The results show that the 350℃ nitrided surface is dominated by c-Fe3N and ON, which is supersaturated nitrogen solid solution. They have high hardness and chemical stabilities. So the low temperature plasma nitriding not only increases the surface hardness values but also improves the wear and erosion resistance. In addition, the fatigue limit of AISI 420 steel can also be improved by plasma nitriding at 350℃ because plasma nitriding produces residual compressive stress inside the modified layer.     

Self-propagating high-temperature synthesis of complex nitrides of intermetallics

In our previous papers, the Self-Propagating High-Temperature Synthesis (SHS) of aluminium and titanium nitrides was studied. In this paper the synthesis of the complex nitrides of intermetallics, based on titanium, aluminium and nickel, was carried out. The samples were produced by the direct SHS of nickel–aluminium and titanium–aluminium mixtures in a nitrogen atmosphere, as well as by the SHS synthesis of nickel–aluminium and titanium–aluminium intermetallics followed by pulsed plasma ion nitriding. Composition of products was studied by chemical analysis, as well as by X-ray diffraction and X-ray photoelectron spectroscopy. Experiments revealed that the highest extent of nitridation was achieved during direct one-stage SHS synthesis of the complex intermetallic nitrides.