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.     

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.     

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‘)。     

Study on the active screen plasma nitriding and its nitriding mechanism

The active screen plasma and DC plasma nitriding of the low alloy steel 722M24 are investigated. Experimental results showed that the metallurgical characteristics and hardening effect on 722M24 steel nitrided by AS plasma nitriding at both floating potential and grounded potential were similar to those nitrided by DC plasma nitriding. Particles sputtered from the active screen and deposited on the specimen surface play the role of the nitrogen carrier in AS plasma nitriding. XRD and high-resolution SEM analysis indicated that the particles with sizes in sub-micron scale were Fe_xN (x > 2). Based on metallurgical analysis and Optical Emission Spectrometer (OES) experimental results, an AS plasma nitriding model has been proposed considering that AS plasma nitriding is a multi-stage process, involving sputtering, physical adsorption, desorption, diffusion and deposition.     

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。     

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.     

304不锈钢双活性屏离子渗氮

目的 考察304不锈钢双活性屏离子渗氮技术的可行性及处理效果.方法 利用双活性屏离子渗氮(DASPN)和普通直流离子渗氮(DCPN)两种技术对304不锈钢进行低温(420℃)硬化处理,对比分析两种工艺所得渗层的组织,对比研究两种工艺所得渗层的相结构、硬度和耐蚀性能.结果 采用DASPN技术可获得比采用DCPN技术更为均匀、致密的渗层,渗层为单一S相层,硬度为763 HV0.25.电化学测试表明,两种渗氮技术相比,DASPN处理获得的渗层耐蚀性能更优.结论 采用DASPN技术对304不锈钢进行低温硬化处理,在试样距双屏的距离为70 mm时能够获得比DCPN更好的渗氮效果.该技术适于工业化推广应用.     

40Cr钢循环离子渗氮工艺及渗层硬度研究

目的探索循环离子渗氮与常规恒温离子渗氮技术的工艺效果。方法先对试样进行调质处理,分组进行离子渗氮,固定氨气和乙醇的流量,改变渗氮时间和渗氮温度两种工艺参数及渗氮工艺,分别测定渗氮后各试样的表面硬度及渗层厚度,观察其金相组织,并分析每组试样渗氮层的性能。结果循环离子渗氮530 6 h℃试样的表面硬度最高,随着渗氮温度的升高和渗氮时间的延长,试样的表面硬度增加,但是当温度超过530℃、时间超过6 h后,试样的表面硬度反而降低。循环渗氮550 10 h℃试样的渗层厚度最厚,随着渗氮温度的升高和渗氮时间的增加,试样的渗层厚度变厚,但时间超过6 h后,渗层厚度的增加较缓慢,6、8、10 h试样的渗层厚度差别不大。相同的渗氮温度下,循环渗氮6 h的试样的渗层厚度基本与常规恒温渗氮10 h试样的渗层厚度一样,相同渗氮时间内,循环渗氮510℃的试样的表面硬度高于恒温渗氮550℃试样的表面硬度,且两者的渗层厚度相差不多。结论循环离子渗氮工艺优于常规的恒温离子渗氮,循环离子渗氮550 8 h℃试样的综合性能最好。     

预氧化+稀土铈对42CrMo钢离子渗氮的影响

针对离子渗氮渗层浅及生产周期长等技术难题,采用预氧化与稀土复合催渗对工程常用结构钢42CrMo进行了离子渗氮。利用显微硬度计、光学显微镜(OM)、扫描电镜(SEM)等对渗氮速率、渗氮层组织、表面形貌等进行了系统的研究。结果表明,经400 ℃×1 h氧化+0.6 cm²/kg(铈表面积/装炉量)稀土的复合催渗工艺具有最佳催渗效果;与无催渗试样相比,优化后的复合催渗不仅提高了渗氮效率,同时减少了脉状氮化物,且降低了渗氮层的硬度梯度。     

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。     

High resolution electron microscopy characterization of nitrides of iron and iron alloys

A study of nitride-phase formation in alloys nitrided by glow discharge plasma nitriding was performed by high-resolution electron microscopy. The iron and steel samples were nitrided above and below the eutectoid transformation point (590 ‡C). After nitriding, the samples were annealed for several treatment times at 400 ‡C. The microstructure and identification of the iron nitrided phases formed by nitriding and annealing were investigated by x-ray diffraction (XRD), optical microscopy (OM) and mainly high resolution electron microscopy (HREM) in a JEOL-4000EX high resolution microscope at 400 kV. The results of the characterization show a surface ε compact nitride layer, which is transformed into ε + γ during cooling. The tempering process affects the surface hardness of the samples. After an initial increase relative to the untreated sample, the microhardness diminishes after long treatment times. This behavior is correlated with the αt’’ phase appearance, growth, and transformation.     

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。     

Active screen plasma nitriding of materials

Abstract

The rapid development and the uptake of plasma nitriding technology into industrial surface engineering have slowed down in recent years. This is attributed to some of the inherent shortcomings of conventional dc plasma technology, for example, difficulties in maintaining a uniform chamber temperature, instability of the plasma and potential surface damage to parts caused by arcing. Efforts in overcoming these problems have led to the development of active screen plasma nitriding (ASPN) technology. This review demonstrates that with all its technological and environmental advantages, ASPN can be used to treat low alloy steels, tool steels, stainless steels and other steels which can conventionally be nitrided with dc plasma technology. In addition, ASPN can be used to treat non-conducting materials such as oxidised steels and polymeric materials which are not suitable for a dc plasma nitriding system. In the longer term, environmental friendly and technologically advanced plasma nitriding will outperform conventional salt bath and gaseous methods. Active screen plasma nitriding is a novel way of possibly achieving the full potential of plasma technology for thermochemical surface engineering.     

Use of cathodic cage in plasma nitriding

Cylindrical samples of 1020 steel and 316 stainless steel were nitrided under the conditions by conventional dc plasma nitriding (DCPN) and by a new technique denominate cathodic cage plasma nitriding (CCPN). The 1020 and 316 stainless steel samples were treated during 3 h and 5 h, respectively, in 773 K and 360 Pa. The samples were characterized by optical microscopy, X-ray diffraction and microhardness testing. All the samples nitrided by DCPN process presented erosion rings on the surface exposed to the plasma. In comparison, in samples nitrided by CCPN, the erosion rings were completely eliminated, without loss of the mechanical properties in the different phases of existence in the nitrided layer.     

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.     

冷轧预处理对TC4合金540 ℃渗氮组织的影响

TC4钛合金经820 ℃固溶处理及室温下冷轧得到10%、20%、30%、40%、50%不同变形量的试样,之后在540 ℃进行渗氮复合时效处理8 h。利用光学显微镜、X射线衍射仪、扫描电镜等分析了不同变形量下合金渗氮组织和时效组织的变化特点以及渗氮试样表面的相结构和形貌的变化。试验结果显示,渗氮处理后,试样表面生成了TiN、Ti₂N等高硬的氮化物颗粒,变形量越大,试样表面生成的氮化物颗粒越多且尺寸越大;经固溶处理后,TC4合金的室温组织为α相+亚稳β相,经渗氮复合时效处理后,亚稳β相分解为α相,同时α相向β相转化,变形量越大,析出的β相越多,且这种趋势不如单纯的时效处理明显。     

Investigation into some tribological properties of plasma nitrided hot-worked tool steel AISIH11

Interest in the tribological properties of plasma nitriding has increased substantially over the past years because plasma nitriding provides a high nitride depth and improved hard facing. The present study examines the tribological properties of AISI Hll plasma nitrided, hot- worked steel. Different nitriding temperatures and durations were considered. Characterization of the composite structures was investigated with wear tests, x-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), and microhardness tests. The depth profile of the nitrided zone was measured using the nuclear reaction analysis (NRA) technique. Plasma nitriding affected the microhardness, wear properties, and morphology considerably. Increase in process temperature increased the nitride zone depth.     

Effect of DC plasma nitriding temperature on microstructure and dry-sliding wear properties of 316L stainless steel

A wear resistant nitrided layer was formed on 316L austenitic stainless steel substrate by DC plasma nitriding (DCPN). The structural phases, micro-hardness and dry-sliding wear behavior of the nitrided layer were investigated by optical microscopy (OM), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDS), micro-hardness tester and ring-on-block wear tester. The results show that a single expanded austenite layer (S-phase) and a single CrN nitride layer were formed at 400 °C and 480 °C, respectively. In addition, the S-phase layers formed on the samples exhibited the best dry-sliding wear resistance under ring-on-block contact configuration test. Wear of the untreated 316L was sever and characterized by strong adhesion, abrasion and oxidation mechanism, whilst wear of the DCPN-treated 316L was mild and dominated by plastic deformation, slight abrasion and frictional polishing.     

脱碳层对38CrMoAl钢离子渗氮的影响

对表面残存不同厚度脱碳层的38CrMoAl钢塔形试样进行离子渗氮,借助显微硬度计、光学显微镜、扫描电镜等多种手段,对试样渗速、硬度及渗氮前后的微观组织进行研究。结果表明,在残余的脱碳层里存在较严重的魏氏组织;残余脱碳越严重魏氏组织越多;离子渗氮的渗速随着表面脱碳层厚度的增加先增加后降低;魏氏组织中大量的铁素体为氮原子扩散提供了快速渗入通道及形成大量氮化物的场所,在渗层表面形成大量的鱼骨状、网状、脉状氮化物,数量随着脱碳层的增加而增加,并且不断向渗层深处延伸。38CrMoAl钢表面残存脱碳层虽然有加快渗速的作用,但会增加渗层的不良组织,增加渗层剥落的风险。故38CrMoAl钢制工件做普通调质应适当加大加工余量。     

Corrosion properties of active screen plasma nitrided 316 austenitic stainless steel

AISI 316 austenitic stainless steel has been plasma nitrided using the active screen plasma nitriding (ASPN) technique. Corrosion properties of the untreated and AS plasma nitrided 316 steel have been evaluated using various techniques, including qualitative evaluation after etching in 50%HCl + 25%HNO₃ + 25%H₂O, weight loss measurement after immersion in 10% HCl, and anodic polarisation tests in 3.5% NaCl solution. The results showed that the untreated 316 stainless steel suffered severe localised pitting and crevice corrosion under the testing conditions. AS plasma nitriding at low temperature (420 °C) produced a single phase nitrided layer of nitrogen expanded austenite (S-phase), which considerably improved the corrosion properties of the 316 austenitic stainless steel. In contrast, AS plasma nitriding at a high temperature (500 °C) resulted in chromium nitride precipitation so that the bulk of the nitrided case had very poor corrosion resistance. However, a thin deposition layer on top of the nitrided case, which seems to be unique to AS plasma nitriding, could have alleviated the corrosion attack of the higher temperature nitrided 316 steel.