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Characteristics of martensitic stainless steel nitrided in a low-pressure RF

Surface and Coatings Technology 163–164(2003)380–385

plasma

S.K.Kim *,J.S.Y oo ,J.M.Priest ,M.P .Fewell a ,a b b

School of Materials Science and Engineering,University of Ulsan,Ulsan 680-749,South Korea

Physics and Electronics,University of New England,Armidale NSW 2351,Australia

Abstract

Martensitic grade stainless steel AISI 420was nitrided in a low-pressure RF plasma using pure nitrogen.With a treatment time of 4.0h at 4008C,the nitrogen-rich layer on the sample was 20m m thick and had a hardness of approximately 4.3times higher than that of untreated material.The layer thickness was much greater than that obtained on AISI 304under identical conditions,reflecting the different Cr content of the two alloys.Below the temperature at which CrN forms,the treated layer retains its martensitic structure,but with a larger lattice parameter than the bulk,a phase that can be termed ‘expanded martensite’,by analogy with the situation with austenitic stainless steel.Kinetics of the layer formation was also investigated which yielded an activation energy of 33.4kJ y mol.

Keywords:RF plasma;Nitriding;Martensitic stainless steel;Nitrogen-rich layer;Expanded martensite

1.Introduction

Martensitic stainless steels are materials of choice in applications where good wear resistance is a key per-formance indicator in addition to the corrosion resistance shown by stainless steels.Such applications include turbine blades,tools,bearings and in surgery,for exam-ple,bone saws for orthopaedic surgery.In all of these situations,improved surface hardness,as can be pro-duced in other alloys by nitriding,is desirable.This motivated some previous studies of nitriding;for exam-ple Sun et al.showed that nitriding improves wear resistance for the martensitic grade AISI 440C w 1x .Nevertheless,there have been fewer works on the nitriding of martensitic grades than on austenitic grades of stainless steel.In particular,the possibility of lowering the process temperature has not been systematically explored.During the last half decade or so,much work on the austenitic grades has highlighted the desirability of treatment temperatures of 4008C and lower w 2–7x .Aside from the obvious benefits of lower cost,faster

*Corresponding author.Tel.:q 82-52-259-2228;fax:q 82-52-259-1688.

E-mail address:sunkyu7@https://www.wendangku.net/doc/b29760626.html, (S.K.Kim ).

turn-around and reduced distortion of the workpiece,it is now clear that process temperatures over ;4808C permit the Cr in the alloy to become mobile;the chromium preferentially forms CrN,the deposition of which certainly increases the hardness,but also results in a reduction in corrosion resistance through the deple-tion of Cr from solid solution in the alloy w 8–10x .

Previous work on the austenitic grade AISI 316has suggested that,as far as working at low temperature is concerned,the low-pressure RF plasma may have the advantage that the thickness of the treated layer falls more slowly with lowering temperatures than with other nitriding media w 7x .In the present paper,we explore this characteristic for the martensitic grade AISI 420.2.Experimental methods

The alloy studied here is AISI 420(C )0.15%,Si -1.00%,P -0.040%,S -0.030%,Cr 12.0;14.0%,Mn -1.00%).The sample consisted of disks 25mm in diameter cleaned in ethanol prior to loading onto the sample table of the hot-wall nitriding reactor at the Australian Nuclear Science and Technology Organiza-tion (ANSTO )w 11x .This reactor is fabricated from stainless steel and pumped by a large-capacity turbo-

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Table 1

Process parameters used in this study

Pre-cleaning

Nitriding RF power and frequency 250W at 13.56MHz Total pressure (mPa )400400Sample bias (V )y 250y 250Time (h )

1.5–

2.0 1.0–16.0H flow rate (m mol s )y 1a 211.9–N flow rate (m mol s )y 12–11.0Ar flow rate (m mol s )

y 1 3.8

–

1.0m mol s s 1.36sccm.

y 1Fig.1.Sections of XRD scans for samples of AISI 420martensitic stainless steel nitrided for (a )4h at the indicated temperatures and (b )4008C for the indicated durations.Results from an untreated sample are included in each panel.

molecular pump.A single-turn inductively coupled antenna,also made from stainless steel is located inside the reactor volume.At an appropriate gas pressure,a diffuse RF glow discharge fills the reactor when RF power is applied to the antenna.

A total of seven treatments were carried out,exploring the variation of treatment time and temperature.Four treatments used the process temperature of 4008C,with the treatment time varied in the range 1;16h,and four

treatments used a process time of 4h,with temperatures in the range 350;5008C.

All treatments included a ‘pre-cleaning’step:the reactor was filled with a 50y 50mixture of hydrogen and argon,and an RF glow discharge was maintained as the sample was heated to the process temperature.The length of time required for this varied in the range 1.5;2.0h depending on the desired process temperature and the temperature of the reactor walls at the beginning of the day.At the end of the pre-cleaning and nitriding,the chamber was pumped out and filled with nitrogen for the nitriding step.During all plasma exposure,both pre-cleaning and nitriding,the sample table was biased at y 250V with respect to the reactor walls.Following the treatments,the samples were cooled under vacuum conditions.The range of treatment parameters used herein are given in Table 1.

Following the treatments,the sample were examined by X-ray diffractometry (XRD )and scanning electron microscopy (SEM ),and their surface hardness was measured by an instrumented method.The X-ray dif-

382S.K.Kim et al./Surface and Coatings Technology 163–164(2003)

380–385

Fig.2.Surface hardness of the samples as in Fig.1.

fractometry was performed on the Philips PW 1050diffractometer using CuK a radiation and Bragg–Bren-tanno geometry.Scanning electron microscopy of section samples was used to image the treated layer.A thin cross-sectional slice was cut from each sample and cast in epoxy resin.This was then surface ground and polished.To render the nitrogen-rich layer visible,the polished surface was chemically etched for 10s in Marble’s solution (10g copper sulfate in 100ml of 6.0M hydrochloric acid ).Examination of these samples were carried out in a scanning electron microscope

(JEOL,JSM-820).Measurements of the surface hard-ness of the samples were made with a Nano Instruments instrumented indenter located at ANSTO w 12x ,using loads of 0.05N,0.25N and 1.0N.3.Results and discussion

Fig.1shows X-ray diffractograms from the AISI 420samples.The most unusual feature of Fig.1is the shifting of the 110reflections.These lie in the region of the 111reflection in the X-ray diffractograms for

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S.K.Kim et al./Surface and Coatings Technology 163–164(2003)

380–385Fig.3.SEM micrographs of a cross section of the AISI 420sample treated for 4h at 4008C.The dark band on the left of the image is epoxy resin;the nitrogen-rich layer is rather homogeneous grey band next to

this.

Fig.4.Arrhenius plot for the nitriding of AISI 420in a low-pressure RF plasma.The quantity on the ordinate is d y t ,where d is the thickness 2of the nitrided layer and t is the process duration.

samples of AISI 304austenitic stainless steel nitrided in the same treatments w 13x .However,the treated layer of the 420samples cannot be austenitic,because there are no 200reflections.This indicates that the nitrogen-rich layer also has a ferritic or martensitic structure,and is thick enough,even at low temperature or short treatment time,that the peak from the underlying martensitic substrate is not visible.By analogy with the designation ‘expanded austenite’in the previous results w 14x ,we may call the structure of the treated layer on martensitic stainless steel ‘expanded martensite’.The term may seem odd because martensite is in fact expanded ferrite,

but it is a useful label for the treated-layer structure seen here.

Closer inspection of Fig.1gives a more complicated picture.At the lowest temperature used (Fig.1a,3508C )the diffractogram shows,in addition to the expanded martensite peak,a peak at 38.58.This is possibly due to CrN,but CrN formation at such a low temperature is quite unexpected,particularly as the peak is absent for the samples treated at higher temperature.In fact,trans-formation to CrN and ferrite has clearly occurred at 4508C and the 5008C data show ferrite only.This is a lower transformation temperature than for AISI 304,but it is well known that different alloys show the transfor-mation at different temperatures w 15x .

The time series (Fig.1b )also shows a transformation to CrN and ferrite in the samples treated for 9.0h and 16.0h.This agrees with experience in austenitic alloys showing that the conditions for transformation depends not on temperature alone,but on the combination of temperature and treatment time w 15x .

Fig.2shows the results of instrumented indentation,parallel to Fig.1.In Fig.2,the variation of measured hardness of the treated samples with indenter load reflects the effect of a thin hard layer on a softer substrate.

Electron micrographs of the cross-section of an indent in the sample show that,at an indenter load of 1.0N,the highest load used here,the treated layer is not punctured but is driven into the softer substrate w 16x .The hardness value obtained is therefore intermediate between the true hardness of the treated layer and the hardness of the substrate.Hence,the values at the lightest load (0.05N )give the best indication of the

384S.K.Kim et al./Surface and Coatings Technology163–164(2003)380–385

hardness of the treated layer.The results at1.0N load can be regarded as reflecting the thickness of the treated layer.As can be seen in Fig.2b,neither hardness nor layer thickness changes after4.0h treatment,and both decrease at higher process temperature.These effects are correlated with the transformation to CrN observed in the XRD,and indicate the advisability of choosing treatment conditions that avoid this transformation. Fig.3shows a SEM micrograph of cross-section of the nitrided layers of the sample.A thick nitrided layer of approximately20m m was formed in this sample. The earliest study known to us on the plasma nitriding of martensitic stainless steel used pulsed DC-glow nitrid-ing and the alloy AISI410,which is similar to AISI 420,but contains less carbon and more Cr w17x.They used treatment times of2;10h at400;6008C,and a gas mixture of unspecified composition.They obtained hardness increases of a factor of;3.3,compared with the factor;4.3obtained in the present study.Sun et al. also used a pulsed DC glow w1x.They examined the alloy AISI440C,which contains much more carbon and somewhat more Cr than AISI420,and also contains Mo.They obtained a;100-m m-thick layer after nitrid-ing for30h at5108C in a mixture of hydrogen with 25%nitrogen.This compares with20m m after4.0h at 4008C with our process.

Leyland et al.nitrided the martensitic grade AISI17y 4PH in a pulsed triode discharge w18x.This the only previous study known to us to show X-ray diffracto-grams from nitrided martensitic stainless steel.Their results differ from ours in that the treated layer is predominantly austenitic(fcc).This is consistent with the view that nitrogen is an‘austenite stabiliser’,that is, that the nitrogen rich layer tends to have an fcc structure rather than a bcc structure.For example,a study of nitriding the duplex steel AISI318,which is composed of a mixture of ferritic and austenitic grains,found that the treated layer contained only grains with an austenitic structure,and then an effect of the treatment was to convert ferritic grains to fcc w19x.The situation is different in the present work,with the material retaining its martensitic structure while absorbing nitrogen,a structure we have termed expanded martensite,with no indication of a tendency to become fcc.Marchev et al. w20x reported conducting XRD on nitrided AISI410 martensitic stainless steel.They did not show any diffractograms,but reported that sample treated at400 8C‘contain one or more unidentified martensitic phas-

es?’.This would seem to be consistent with our results. By analysing the data of layer thickness against time, an Arrhenius-type plot was constructed(Fig.4).An activation energy of33.4kJ y mol was obtained.To set this in context,the activation energy obtained by Fewell et al.for the low-pressure RF-plasma nitriding of AISI 316is17kcal y mol w7x and by Menthe and Rie for the pulsed-plasma nitriding of the same alloy is31kcal y mol w4x.The first of these used the same nitriding process as the present https://www.wendangku.net/doc/b29760626.html,paring with these values,the activation energy of the420sample is much lower(see also w21x)which indicates that thicker dif-fusion layer can be formed than in austenitic grades.

4.Conclusions

A low-pressure RF discharge using pure nitrogen is an effective medium for nitriding martensitic stainless steel.With a treatment time of4.0h at4008C,the nitrogen-rich layer was20-m m-thick and had a hardness of approximately 4.3times higher than that of the untreated material.The layer thickness was much greater than that obtained on austenitic stainless steel such as AISI304under identical treatment conditions,reflecting the different Cr content of the two alloys.The alloy AISI420was more susceptible to the formation of CrN and ferrite than AISI304.The transformation was evident after9.0h treatment at4008C and completed after only4.0h at4508C.This has a deleterious effect on the hardness again,so that4.0h,4008C is close to the optimum treatment conditions.Under these condi-tions,the treated layer retains its martensitic structure, but with a larger lattice parameter than the bulk.The situation was very similar to that obtained with austenitic stainless steel,and the analogy prompted us to term the newly identified phase‘expanded martensite’.The fact that the treated layer retains a bcc structure is interesting in view of previous evidence that nitrogen promotes a change to fcc.The activation energy obtained for AISI 420is much lower than that of austenitic stainless steels which indicates easy formation of a thicker diffusion layer.

Acknowledgments

This research was supported by the2002University of Ulsan Research Fund.

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优秀党务工作者事迹简介范文优秀党务工作者事迹简介范文 ***，男，198*年**月出生，200*年加入党组织，现为***支部书记。从事党务工作以来，兢兢业业、恪尽职守、辛勤工作，出色地完成了各项任务，在思想上、政治上同党中央保持高度一致，在业务上不断进取，团结同事，在工作岗位上取得了一定成绩。一、严于律己，勤于学习作为一名党务工作者，平时十分注重知识的更新，不断加强党的理论知识的学习，坚持把学习摆在重要位置，学习领会和及时掌握党和国家的路线、方针、政策，特别是党的十九大精神，注重政治理论水平的提高，具有坚定的理论信念;坚持党的基本路线，坚决执行党的各项方针政策，自觉履行党员义务，正确行使党员权利。平时注重加强业务和管理知识的学习，并运用到工作中去，不断提升自身工作能力，具有开拓创新精神，在思想上、政治上和行动上时刻同党中央保持高度一致。二、求真务实，开拓进取在工作中任劳任怨，踏实肯干，坚持原则，认真做好学院的党务工作，按照党章的要求，严格发展党员的每一个步骤，认真细致的对待每一份材料。配合党总支书记做好学院的党建工作，完善党总支建设方面的文件、材料和工作制度、管理制度等。

三、生活朴素，乐于助人平时重视与同事间的关系，主动与同事打成一片，善于发现他人的难处，及时妥善地给予帮助。在其它同志遇到困难时，积极主动伸出援助之手，尽自己最大努力帮助有需要的人。养成了批评与自我批评的优良作风，时常反省自己的工作，学习和生活。不但能够真诚的指出同事的缺点，也能够正确的对待他人的批评和意见。面对误解，总是一笑而过，不会因为误解和批评而耿耿于怀，而是诚恳的接受，从而不断的提高自己。在生活上勤俭节朴，不铺张浪费。身为一名老党员，我感到责任重大，应该做出表率，挤出更多的时间来投入到**党总支的工作中，不找借口，不讲条件，不畏困难，将总支建设摆在更重要的位置，解开工作中的思想疙瘩，为攻坚克难铺平道路，以支部为纽带，像战友一样团结，像家庭一样维系，像亲人一样关怀，践行入党誓言。把握机遇，迎接挑战，不负初心。

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good afternoon everybody! I’m very glad to stand here and give you a short speech about challenge and opportunity,双手交握微笑 So, what’s an opportunity? It’s a great chance to achieve dreams, it’s a platform to show ourselves.Just as now,I’m standing here showing myself,it's one of my dreams,also my opportunity. Then, what about challenge? Challenge is a new or difficult task which test our ability and skill. it is a fighter, a sense of courage, the fearless spirit towards all difficulties, Many people are afraid of being challenged, worrying about change and failure.I used to be a member of them，but now,I find that sth we haven’t done isn’t as difficult as it seems, fear always hindered our courage. Said so much,此刻我最想与你们分享的一句话就是： we should welcome being challenged,and try to enjoy it.它很可能是你进步的机会 Cruel competition isn 't the excuse for failure. No one is regularly on a winner or a loser. To the strong willed, competition is the spring of hope; To the weak minded, it means the winter of despair. So turning into opportunities means taking advantage of these challenges and benefiting from them.In this way,you can be the boss of your life.这句语法有没有错误？指着他，手势 That’s all, thank you!

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人际关系综合诊断量表评分 _________学校，____年级_____专业_____班____号，性别___，姓名_________ 您更多得时间生活在：农村（）或城市（）打“√”的记1分，打“×”的记0分维度题项各栏目总分交谈 1、5、9、13、17、21、25 得分__、__、__、__、__、__、__ 分交际与交友 2、6、10、14、18、22、26 得分__、__、__、__、__、__、__ 分待人接物 3、7、11、15、19、23、27 得分__、__、__、__、__、__、__ 分异性交往 4、8、12、16、20、24、28 得分__、__、__、__、__、__、__ 分合计分常模：总分是0－8分之间，那么说明你在与朋友相处上的困扰较少。你善于交谈，性格比较开朗，主动，关心别人，你对周围的朋友都比较好，愿意和他们在一起，他们也都喜欢你，你们相处得不错。而且，你能够从与朋友相处中，得到乐趣。你的生活是比较充实而且丰富多彩的，你与异性朋友也相处得比较好。一句话，你不存在或较少存在交友方面的困扰，你善于与朋友相处，人缘很好，获得许多的好感与赞同。总分是9－14分之间，那么，你与朋友相处存在一定程度的困扰。你的人缘很一般，换句话说，你和朋友的关系并不牢固，时好时坏，经常处在一种起伏波动之中。总分是15－28分之间，那就表明你在同朋友相处上的行为困扰较严重，分数超过20分，则表明你的人际关系困扰程度很严重，而且在心理上出现较为明显得障碍。你可能不善于交谈，也可能是一个性格孤僻的人，不开朗，或者有明显得自高自大、讨人嫌的行为。（一）交谈方面 0-2分，较高的交谈能力和技巧；3－5分之间，交谈能力一般；6分以上，不善于交谈。（二）交际方面 0-2分，对人较为真诚和热情；3－5分之间，你在被动地寻找被人喜欢的突破口；6分以上，在社交活动与交友方面存在着较大的行为困扰。（三）待人接物 0－2分，较尊重别人，敢于承担责任，对环境的适应性强；3－5分，是个多侧面的人，可以算是一个较圆滑的人；6分以上，缺乏待人接物的机智与技巧。（四）异性朋友交往 0－2分，表明你懂得如何真确处理异性朋友之间的关系；3－4分，与异性同学交往的行为困扰程度一般；5分以上，在于异性交往的过程中存在较为严重的困扰。

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