材料的活性屏等离子渗氮

近年来,等离子渗氮技术的迅速发展和在表面工程领域的应用呈现出减缓的趋势,其原因是传统的直流等离子体技术存在一些固有的缺点,例如,炉温难以保持均匀,等离子体不够稳定以及因打弧而引起工件表面损伤等。克服这些不足之处的努力促使了活性屏等离子渗氮(ASPN)技术的发展。本文从技术和环境优势角度证明,ASPN可以应用于低合金钢、工具钢、不锈钢以及能进行传统直流等离子渗氮的其他钢种。此外,ASPN可以处理不适合直流等离子渗氮的非导电材料,如经氧化处理的钢和高分子材料。从长远看,对环境友好且技术先进的等离子渗氮比传统的盐浴和气体渗氮更有优势。活性屏等离子渗氮技术是充分发挥等离子体技术在化学热处理及有关表面工程中应用潜力的新方法。     

Plasma Nitriding of AISI 304 Stainless Steel in Cathodic and Floating Electric Potential: Influence on Morphology,Chemical Characteristics and Tribological Behavior

In direct current plasma nitriding (DCPN), the treated components are subjected to a high cathodic potential, which brings several inherent shortcomings, e.g., damage by arcing and the edging effect. In active screen plasma nitriding (ASPN) processes, the cathodic potential is applied to a metal screen that surrounds the workload, and the component to be treated is placed in a floating potential. Such an electrical configuration allows plasma to be formed on the metal screen surface rather than on the component surface; thus, the shortcomings of the DCPN are eliminated. In this work, the nitrided experiments were performed using a plasma nitriding unit. Two groups of samples were placed on the table in the cathodic and the floating potential, corresponding to the DCPN and ASPN, respectively. The floating samples and table were surrounded by a steel screen. The DCPN and ASPN of the AISI 304 stainless steels are investigated as a function of the electric potential. The samples were characterized using scanning electron microscopy with energy-dispersive x-ray spectroscopy, x-ray diffraction, atomic force microscopy and transmission electron microscope. Dry sliding ball-on-disk wear tests were conducted on the untreated substrate, DCPN and ASPN samples. The results reveal that all nitrided samples successfully produced similar nitrogen-supersaturated S phase layers on their surfaces. This finding also shows the strong impact of the electric potential of the nitriding process on the morphology, chemical characteristics, hardness and tribological behavior of the DCPN and ASPN samples.     

Progress in control of nitriding potential in ASPN process

Abstract

A novel active screen plasma nitriding (ASPN) process provided excellent temperature homogeneity in the load and showed further progress in the control of nitriding potential. In addition to a variation of the nitrogen partial pressure in the process gas commonly used in the conventional plasma nitriding, the applied bias power strongly impacted the nitriding results. In the present work, an application of both methods for the control of nitriding potential in the ASPN process was systematically investigated for a wide range of process parameters to meet the treatment requirements for different types of engineering steel. A two-stage technique based on proper choice of process temperature and required nitriding potential in each stage has been applied in the ASPN process to avoid unnecessary compromises between sufficient thickness of the compound layer, the maximum case hardness and the acceptable nitriding hardness depth.     

Investigation of nitrogen mass transfer within an industrial plasma nitriding system II: Application of a biased screen

Active screen plasma nitriding (ASPN) was conceived in order to reduce negative effects observed in direct current plasma nitriding arising from the application of bias to the components. The mechanism of nitrogen mass transfer in ASPN is still not fully understood. Here, we compare the microstructure, composition and hardness response of AISI P20 and H13 steels after nitriding. A set of samples was nitrided with sample bias applied directly and another set was nitrided at floating potential under an active screen. Similar nitrogen content and hardness profiles were obtained for the samples treated using a bias and under an active screen separated from the samples by 12 mm. When the sample-screen separation was increased from 12 to 70 mm the hardness response improved. The principle processes occurring during ASPN are proposed based on the experimental results. In ASPN, a flux of energetic nitrogen species is generated by the active screen which, provided that the samples are within the range of the energetic species, bombards the surface of the samples being treated. This flux is critical in establishing a nitrogen potential and a satisfactory response in the components.     

Study of the Active Screen Plasma Nitriding

Active screen plasma nitriding (ASPN) is a novel nitriding process, which overcomes many of the practical problems associated with the conventional DC plasma nitriding (DCPN). Experimental results showed that the metallurgical characteristics and hardening effect of 722M24 steel nitrided by ASPN at both floating potential and anodic (zero) potential were similar to those nitrided by DCPN. XRD and high-resolution SEM analysis indicated that iron nitride particles with sizes in sub-micron scale were deposited on the specimen surface in AS plasma nitriding. These indicate that the neutral iron nitride particles, which are sputtered from the active screen and transferred through plasma to specimen surface, are considered to be the dominant nitrogen carder in ASPN. The OES results show that NH could not be a critical species in plasma nitriding.     

Differences in nitrided layer between classic active screen plasma nitriding and active screen plasma nitriding with hemispherical cathodic cage

Abstract

Active screen plasma nitriding (ASPN) is commonly used when regular surface hardening is necessary. The ASPN technique produces a more homogeneous surface coating than direct current plasma nitriding (DCPN) due to different process principles. The term active screen in plasma nitriding refers to a cathodic cage with a defined geometry. The purpose of this work was to study the differences between ASPN using a hemispherical cathodic cage and ASPN using a normal cylindrical cathodic cage. Following some trials using similar parameters, the tests were carried out with three conditions: with DCPN, with a cylindrical cathodic cage in ASPN and with a hemispherical cathodic cage in ASPN. X-ray diffraction and scanning electron microscopy analysis together with energy dispersive spectroscopy were applied to characterise the nitrided layers. The nitrided layers are not the same for each of the conditions used. The ASPN with a hemispherical cathodic cage produced a layer of almost Fe₃N alone, while the other processes gave significant amounts of Fe₄N in the nitrided layer. Scanning electron microscopy analysis showed different surface morphology for each condition.     

纯氮气氛活性屏离子渗氮的研究

在纯氮气氛中，利用活性屏离子渗氮(ASPN)技术对38CrMoAl钢进行了离子渗氮处理，并对渗层的组织结构、硬度、深度等进行了分析。结果表明，只有直流辉光放电电压高于800V时，在纯氮气氛中才能进行活性屏离子渗氮处理。通过对等离子放电空间的粒子进行XRD分析发现，放电电压低于800V时，沉积在基材表面的粒子主要是氧化铁(Fe3O4)；放电电压高于800V时，沉积在基材表面的粒子才是能进行活性屏离子渗氮处理的铁的氮化物(ε，γ‘)。     

Optimization of the ASPN Process to Bright Nitriding of Woodworking Tools Using the Taguchi Approach

The subject of the research is optimization of the parameters of the Active Screen Plasma Nitriding (ASPN) process of high speed steel planing knives used in woodworking. The Taguchi approach was applied for development of the plan of experiments and elaboration of obtained experimental results. The optimized ASPN parameters were: process duration, composition and pressure of the gaseous atmosphere, the substrate BIAS voltage and the substrate temperature. The results of the optimization procedure were verified by the tools’ behavior in the sharpening operation performed in normal industrial conditions. The ASPN technology proved to be extremely suitable for nitriding the woodworking planing tools, which because of their specific geometry, in particular extremely sharp wedge angles, could not be successfully nitrided using conventional direct current plasma nitriding method. The carried out research proved that the values of fracture toughness coefficient K _Ic are in correlation with maximum spalling depths of the cutting edge measured after sharpening, and therefore may be used as a measure of the nitrided planing knives quality. Based on this criterion the optimum parameters of the ASPN process for nitriding high speed planing knives were determined.     

活性屏离子渗氮技术的研究

在真空室内放置一个钢制网状圆筒，并与直流高压电的负极相接，在直流电场的作用下，通过气体离子对圆筒的轰击溅射，产生了一些纳米数量级的活性粒子，利用这些高活性的纳米粒子簇可以对放置在圆筒内的钢件表面进行渗氮处理。试验证明，这些活性粒子是中性的Fe4N粒子，被处理的工件既可以处于悬浮电位，也可以接地。活性屏离子渗氮可以获得和直流离子渗氮同样的处理效果，并解决了直流离子渗氮技术多年来一直存在的许多难以克服的问题。     

富氮层快速离子渗氮工艺及机理研究

利用正交试验法对活性屏快速离子渗氮工艺参数进行优化,并对正交试验预测的优化工艺参数进行了验证。利用Fick第二扩散定律对快速离子渗氮优化工艺的富氮层进行了氮浓度、氮浓度梯度的计算。试验及计算结果表明,高温渗氮温度、高温渗氮时间和低温渗氮时间对渗层厚度的影响较大,选择合适的参数可以在渗氮时间不变、渗层硬度不降低的前提下显著增加渗层厚度。当富氮层厚度为8μm时,采用快速渗氮技术得到试样内表面与基体之间的氮浓度梯度,为传统渗氮模式的20倍以上。     

高效节能环保渗碳渗氮技术

介绍了四个内容：（1）新型高效、节能、环保渗碳技术,主要包括预抽真空双室多用炉和气氛控制装置,与通常的气体渗碳相比,渗碳速度更快,内氧化、渗碳气体消耗量及 CO2排放量大大减少;（2）控制气氛真空渗碳炉,该炉采用热传导探头和氧探头双探头进行碳势的闭环控制,可实施真空渗碳、气冷、重新加热至850℃淬火的工艺过程,渗层均匀性好,并能有效消除积炭;（3）预抽真空精密控制气氛渗氮炉,该炉采用独特的温度和氮势精确控制系统,可取代QPQ 技术对普通碳钢进行渗氮氧化复合处理,提高其耐磨、耐蚀和疲劳性能;（4）活性屏等离子渗氮技术,其独特之处是,高压直流电源的负极接在真空室内的金属活性屏上,等离子体加热金属屏,由从屏上辐射的热量将工件加热到所需渗氮温度,解决了传统的直流等离子渗氮技术难以克服的工件打弧等问题。     

不锈钢表面含Cu功能梯度复合改性层的制备及抗菌性能

为提高奥氏体不锈钢(ASS)的耐磨性及赋予其抗菌性能,应用改进的活性屏离子渗氮(ASPN)技术,将纯铜冲孔板置于不锈钢冲孔板上面作为活性屏的顶盖,对316奥氏体不锈钢在低温下(430℃)进行表面渗氮处理,在其表面形成由含Cu抗菌沉积层和S相(氮在奥氏体中的过饱和固溶体γ_N)硬质支撑层组成的功能梯度复合改性层。用扫描电镜(SEM)及其所附能谱仪(EDS)、X射线衍射仪(XRD)表征复合改性层的组织形貌、成分及相结构。用显微硬度计和往复摩擦磨损试验机测试了基体和复合改性层的显微硬度和摩擦磨损性能,用金黄色葡萄球菌进行体外抗菌试验评价复合改性层的抗菌性能。结果表明,在偏压达到250 V后,形成了连续分布的硬质S相扩散层和含Cu沉积层组成的复合改性层。改性层表面最高硬度可达928 HV0.05,与Si₃N₄小球对磨时比磨损率较基体降低约57.76%,显著提高了不锈钢的耐磨性。抗菌试验表明,复合改性层与金黄色葡萄球菌接触24 h后,对金黄色葡萄球菌抗菌率提高到98.5%。改进的活性屏离子渗氮技术制备的功能梯度复合改性层可以有效提高...     

IFHTSE global 21: heat treatment and surface engineering in first decades of twenty-first century Part 5 – Modelling based design of surface engineered systems

Abstract

Aspects of surface engineering design, namely, simulation of processing and service behaviour and prediction of properties, are discussed and summarised. Available design techniques are demonstrated by means of examples. Two process simulation modelling approaches, relating to oxidation of Ti alloys and nitriding of steels, are described. A novel optimisation approach to extract Young's modulus, yield strength and work hardening exponent of a power law (load–displacement) material is presented. Design and service behaviour simulation case studies of surface engineered titanium alloy gears for the sports car industry are also presented. It is shown that advances in theoretical principles and computational methodologies and tools, together with the ever increasing abundance and accuracy of thermodynamics and kinetics databases of materials and processing atmospheres, have enhanced the reliability of surface engineering simulations to a level good enough for industrial application. Barriers and development trends in surface engineering design are also addressed.     

离子渗氮新技术的研究现状

为了克服传统离子渗氮的一些固有缺点，近些年来出现一些新的离子渗氮技术，如活性屏离子渗氮、等离子体源离子渗氮、离子注入离子渗氮等，本文简要介绍了这些新技术及其原理、特点，总结了这类技术的共性模型。其中，活性屏离子渗氮技术和等离子体源离子渗氮技术有着明显的设备和工艺优势，可能成为离子渗氮技术的发展方向。     

Influence of oxygen in plasma nitriding

Abstract

The development of low temperature nitriding treatments to enhance wear resistance over the past 40 years is reviewed. The progress achieved is illustrated with evidence from extensive laboratory investigations and industrial trials on textile machine components and other parts. It is demonstrated that small additions of an oxidising component to gaseous nitrocarburising or plasma nitriding/nitrocarburising atmospheres have a beneficial effect on layer formation and on the wear properties of the treated components. The presence of oxygen increases layer formation rates and stabilises the ?-compound layer. The role of oxygen on surface activation is important for chromium containing steels but also on plain carbon or alloyed steels and to neutralise the passivating effect of finishing procedures. Applying a post-oxidation step after nitrocarburising can significantly increase the corrosion resistance of the surface but close control of gas composition and treatment parameters is necessary.     

Improving the surface properties of A286 precipitation-hardening stainless steel by low-temperature plasma nitriding

Plasma nitriding over a wide range of treatment temperatures between 350 and 500 °C and time from 5 to 30 h on A286 austenitic precipitation-hardening stainless steels has been investigated. Systematic materials characterisation of the plasma surface alloyed A286 alloy was carried out in terms of microstructure observations, phase identification, chemical composition depth profiling, surface and cross-section microhardness measurements, electrochemical corrosion tests, dry sliding wear tests and corrosion-wear tests. Experimental results have shown that plasma nitriding can significantly improve the hardness and wear resistance of A286 stainless steels owing to the formation of nitrogen supersaturated S-phase; the surface layer characteristics (e.g. microstructure, case depth and hardness) of the plasma surface alloyed cases are highly process condition dependent and there are possibilities to provide considerable improvement in wear, corrosion and corrosion-wear resistance of A286 steel.     

双层辉光等离子表面冶金技术

在离子渗氮技术的基础上,发展了双层辉光离子渗金属技术.该技术已成功地将固态合金元素如Ni, Cr, Mo, W, Ti, Al, Nb, Zr以及它们的组合渗入金属材料表面,形成一系列高硬度、耐磨、抗腐蚀合金层.例如在钢铁材料表面形成高速钢和镍基合金;在钛合金表面形成阻燃及耐磨合金等.该技术已获美、英、加等多国专利.本文简要介绍双辉技术的基本原理、主要工艺参数、主要研究结果和应用等.     

Plasma nitriding and nitrocarburising of a supermartensitic stainless steel

Abstract

Supermartensitic stainless steels (SMSSs) are a new generation of the classic 13%Cr martensitic steels, lower in carbon and with additional alloying of nickel and molybdenum offering better weldabilty and low temperature toughness. Several works have shown that plasma nitriding and nitrocarburising of stainless steels at low temperatures produces a hard surface layer which results in increased wear resistance. In this work, SMSS samples were plasma nitrided and nitrocarburised at 400, 450 and 500°C. The plasma treated SMSS samples were characterised by means of optical microscopy, microhardness, X-ray diffraction and dry wear tests. The thickness of the layers produced increases as temperature is raised, for both plasma nitriding and nitrocarburising. X-ray diffraction demonstrates that the chromium nitride content grows with temperature for nitriding and nitrocarburising, which also showed increasing content of iron and chromium carbides with temperature. After plasma treating, it was found that the wear volume decreases for all temperatures and the wear resistance increased as the treatment temperature was raised. The main wear mechanism observed for both treated and untreated samples was grooving abrasion.     

High temperature wear and friction properties of duplex surface treated bearing steels

Duplex treatments by thermo reactive diffusion (TRD) chromizing and puls plasma nitriding were carried out on AISI 52100 and 8620 bearing steels. Tribological behaviors of TRD chromized and duplex treated bearing steels were investigated against Al₂O₃ ball in ball-on-disc system at room temperature and 500 °C. The samples were pack chromized in a furnace at temperature of 1000 °C for 5 h. After chromizing, the samples were puls plasma nitrided for 5 h at 500 °C. The coated steels were characterized using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), scratch and microhardness testing. Plasma nitriding of chromized steels increased the total thickness of the compound layer. The subsequent plasma nitriding increased the surface hardness to 2135 HK_0.025 due to the formation of CrN and Cr₂N. The surface hardness and scratch resistance of coating can be increased with duplex treatment of chromizing followed by plasma nitriding, resulting in high wear resistance. Tribological tests indicated that puls plasma nitriding process decreased the coefficient of friction values and wear rate of the chromized steels at room temperature and 500 °C. Also, examination of the worn surface of the samples showed that particularly at high temperature, the oxidized compact layer occurs and tribo-oxidation played an important role in oxidation behaviour of the steels after the duplex treatment.     

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。