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.     

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。     

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.     

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.     

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.     

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.     

Effect of plasma nitriding of electroplated chromium coatings on the corrosion protection C45 mild steel

Plasma nitriding is a promising posttreatment technique to create a nitride layer on electroplated chromium coatings for improving their corrosion resistance. In the present study, the effects of plasma nitriding on the corrosion properties of electroplated chromium/C45 mild steel were investigated using electrochemical characterization. The chromium plated samples were nitrided using a pulsed direct current glow discharge in an NH₃ atmosphere. The polarization curve measurement results showed that the plasma nitrided samples exhibited more positive corrosion potentials (E_corr), smaller corrosion currents (I_corr), and evident passivation when compared with unnitrided chromium plating/substrate system. The high value of E_corr and low value of I_corr imply an improvement of the corrosion resistance of the coating/substrate system after plasma nitriding.     

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.     

Effect of Plasma Nitriding on the Performance of WC-Co Cutting Tools

This paper presents the effect of nitriding process parameters on the cutting performance of WC-Co tools. The cutting performance was measured by CNC machining of GG25 cast iron parts. The hardness and phase composition of nitrided layer were determined for different plasma nitriding temperatures and times. The hardness of the nitrided layer increased at all plasma nitrided conditions investigated. However, the machining performance of the cutting inserts varied in the range between a 60% increase and a 40% decrease after plasma nitriding. The maximum number of machined parts was seen when the insert was nitrided at 600 °C-4 h and at 500 °C-4 h.     

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.     

Effects of Temperature on Microstructure and Wear of Salt Bath Nitrided 17-4PH Stainless Steel

Salt bath nitriding of 17-4 PH martensitic precipitation hardening stainless steels was conducted at 610, 630, and 650?°C for 2?h using a complex salt bath heat-treatment, and the properties of the nitrided surface were systematically evaluated. Experimental results revealed that the microstructure and phase constituents of the nitrided surface alloy are highly process condition dependent. When 17-4PH stainless steel was subjected to complex salt bathing nitriding, the main phase of the nitrided layer was expanded martensite (????), expanded austenite (??_N), CrN, Fe₄N, and (Fe,Cr) _x O _y . In the sample nitrided above 610?°C, the expanded martensite transformed into expanded austenite. But in the sample nitrided at 650?°C, the expanded austenite decomposed into ??_N and CrN. The decomposed ??_N then disassembled into CrN and alpha again. The nitrided layer depth thickened intensively with the increasing nitriding temperature. The activation energy of nitriding in this salt bath was 125?±?5?kJ/mol.     

离子渗氮和离子渗硫复合处理表面的摩擦学性能

在４５钢离子渗氮表面,用低温郭了渗硫技术形成具有良好固体润滑作用的渗硫层。采用ＳＥＭ＋ＥＤＸ和ＸＲＤ研究了渗层的组织结构,采用销盘式磨损试验机在油润滑条件下,对原始、渗氮、渗硫以及渗氮渗硫复合处理表面进行了抗擦伤性能及耐磨性能的系统研究。并采用ＥＤＸ和ＡＥＳ分析了摩擦表面边界润滑膜的成分。结果表明：渗硫和渗氮处理均只能在低还条件下提高表面的抗擦伤性能。而复合处理能在各种速度条件下显著提高抗擦伤     

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。     

Low temperature nitriding of AISI 316L stainless steel and titanium in a low pressure arc discharge

AISI 316L stainless steel (SS) and titanium nitriding were studied in a low pressure arc-assisted nitriding process where the substrate temperature and the plasma parameters are uncoupled. Lower nitriding temperature limits were explored for constant plasma parameters in Ar–N₂ gas mixtures and substrates at floating potential. Nitrogen superficial concentration, layer thicknesses and X-ray diffraction analyses were performed on SS specimens nitrided at two temperatures (580 and 680 K) for different times and titanium nitriding was studied in the temperature range 750–1025 K. At low temperature, the nitriding performances are limited by a plasma–surface phenomenon that probably involves recombination of nitrogen atoms.     

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.     

热循环离子渗氮及其强渗作用

用正交试验法研究了３８ＣｒＭｏＡｌＡ钢热循环离子渗氮的特点及其强渗作用。结果表明，渗氮过程受循环参数控制，渗层组织呈层状结构，渗层生长曲线存在长达６ｈ的亚速线性段；在强渗工艺下，该段斜率明显增大。这一动力学特性看来是由热循环催渗和离子轰击加速氮原子扩散的有利作用所致，从而使深层渗氮时间比恒温或分段渗氮缩短了２／３￣１／２。     

Effect of the initial microstructure on the plasma nitriding behavior of AISI M2 high speed steel

The nitriding behavior of AISI M2 steel was studied on samples previously submitted to two different heat treatments in order to investigate the effects of the initial microstructure on the thickness and hardness of nitrided layer. Prior to nitriding, one group of samples was fully annealed while the other group was quenched and tempered, thus acquiring the lowest and highest hardness respectively. Plasma nitriding was performed at 450 °C for 8 h with a mixture of N₂ and H₂ in a plasma reactor working under floating potential. Structural and mechanical properties of nitrided layers were characterized using X-ray diffraction (XRD), optical microscopy and microhardness testing. Variations in surface roughness were obtained by 3D surface profilometry analysis. The thicker nitrided layer was obtained for the fully annealed samples, in which the nitrided layer is composed of γ′-Fe₄N and ε-Fe_2-3N phases plus a diffusion zone. For the hardened-tempered samples, the nitrided region mainly consisted of a diffusion zone. Plasma nitriding increased the surface hardness of the fully annealed samples by 330% and that of the quenched-tempered samples by 50%. The nitrided depth was also estimated using cross-sectional microhardness profiles; giving about 140 µm and ∼ 70 µm for the fully annealed and quenched-tempered samples, respectively. Due to the grain to grain nitrogen diffusion, plasma nitriding also increased the surface roughness. The largest roughness was obtained for the fully annealed samples, in accordance with the largest nitrided depth. The difference in the nitriding behavior was explained on the basis of the microstructural aspects of the substrates such as the concentration of the freely dispersed alloying elements and the level of compressive residual stresses.     

Improvement of corrosion and wear resistances of AISI 420 martensitic stainless steel using plasma nitriding at low temperature

The influence of low temperature plasma nitriding on the wear and corrosion resistance of AISI 420 martensitic stainless steel was investigated. Plasma nitriding experiments were carried out with DC-pulsed plasma in 25% N₂ + 75% H₂ atmosphere at 350 °C, 450 °C and 550 °C for 15 h. The composition, microstructure and hardness of the nitrided samples were examined. The wear resistances of plasma nitrided samples were determined with a ball-on-disc wear tester. The corrosion behaviors of plasma nitrided AISI420 stainless steel were evaluated using anodic polarization tests and salt fog spray tests in the simulated industrial environment.The results show that plasma nitriding produces a relatively thick nitrided layer consisting of a compound layer and an adjacent nitrogen diffusion layer on the AISI 420 stainless steel surface. Plasma nitriding not only increases the surface hardness but also improves the wear resistance of the martensitic stainless steel. Furthermore, the anti-wear property of the steel nitrided at 350 °C is much more excellent than that at 550 °C. In addition, the corrosion resistance of AISI420 martensitic stainless steel is considerably improved by 350 °C low temperature plasma nitriding. The improved corrosion resistance is considered to be related to the combined effect of the solid solution of Cr and the high chemical stable phases of ?-Fe₃N and α_N formed on the martensitic stainless steel surface during 350 °C low temperature plasma nitriding. However, plasma nitriding carried out at 450 °C or 550 °C reduces the corrosion resistance of samples, because of the formation of CrN and leading to the depletion of Cr in the solid solution phase of the nitrided layer.     

渗扩时间比对AISI 316不锈钢渗氮层组织与性能的影响

采用真空两段渗氮工艺,在不同的强渗、扩散时间下对AISI 316不锈钢进行渗氮处理,通过X射线衍射(XRD)、扫描电镜(SEM)、光学显微镜(OM)、显微硬度测试和摩擦磨损试验等分析了渗氮层的组织和性能。结果表明,经过12 h的真空渗氮后,AISI 316不锈钢表面形成了一层由γ′-Fe₄N、ε-Fe_2-3N和CrN等相组成的渗氮层,其表面硬度和耐磨性能相较于基体均有明显的提高。其中,渗扩时间比为1∶1(强渗6 h、扩散6 h)时的渗层厚度约为96 μm,表面硬度约为1069 HV0.5,是基体表面硬度的4.5倍,在20 N载荷下的磨损量约为基体的1/3;渗扩时间比为1∶2(强渗4 h、扩散8 h)时的渗层厚度约为120 μm,ε-Fe_2-3N相衍射峰增强,在20 N载荷下的磨损量约为基体的1/30。延长扩散时间能增加渗氮层厚度,改善表面形貌,进一步提高不锈钢的耐磨性。     

PH13-8Mo钢的离子渗氮工艺

对PH13-8Mo钢离子渗氮工艺参数进行了研究,其中包括渗氮温度、渗氮时间及渗氮件表面粗糙度。结果表明:随渗氮温度的升高、渗氮时间的延长、零件表面粗糙度的降低,PH13-8Mo钢渗氮层厚度增加;渗氮零件表面粗糙度对渗氮层脆性等级影响较大,渗氮零件表面粗糙度为6.3 μm时,其脆性等级达到III级;渗氮时间、渗氮温度及零件表面粗糙度对渗氮层硬度影响甚微。渗氮温度540 ℃,渗氮时间22 h,零件表面粗糙度0.8 μm时,PH13-8Mo钢可获得良好的渗氮层,渗氮层厚度可达197.5 μm,渗氮层硬度可达1083 HV0.2,脆性等级为II级。