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WEAR

ELSEVIER

Effect of lubricationby mineral and syntheticoils on the slidingwear of plasmanitrided AI!31 stainlesssteel 410
Yongqing Fu k,Andrew W. Batchelor.Nee Lam Loh, Koon Woo Tan

1. Introduction Plasma nitriding is a useful method ofenh~ncmg the metallurgical, mechanical and tribological properties of en@ neering materials I I 1. is a thermochemical case hardening II technique where atomic nilrogen is diffused into the surface of specimen from surrounding plasma. During plasma nitriding, the sputtering effectsof the energetic positive ions, which effectively remove the contaminants such as oxide\ from the component surface. nccelerale nitrogen INI+ trimsfer from the plasma to thecomponent 12 Accordingly. plasma nitrid1. ing is particularly suitable for surface modification of stainless steets, where the presence of oxide (i.c.. Cr,O,) on the surface may prevent nitrogen muss transfer during conventional gaseousni&iding.This treatment hasrconomicd,environmental, and metallurgicnl ndv:nt:\ges over other method\

The purpose of the the wear behavior of plasma-nitrided marten\nlc \Liunlc\s steel usmg a pin-on-cylinder wear test rig under both dry and lubricated condition%.The effect of differeru lubricating oils isatso investigated by acomparative lccting of\ynthetic and mineral oils. X-my imaging and scanning electron mlcroscopy (SEM) are used to study the wear in: turhmr hlxlc~. toots and hearings. present work I\ to \tudy mechanisms.

X-ray im:@ng is one of the mai;, methods used in nondeevaluiltion 18.91. It is also ;1novel and potentially v;lluablc technique fortheunalysisofwearmechanisms [ IO]. When X-rays penetrate through the specimen. rhey are difauctwe ferentially metallic ;kwrhed inclusions by discontinuities. or flaws. voids. andnon-

131.
There have been reports on rhe weiir ch;lr;lcteristlcs of nitrided austenitic stainless steel [4-6 However. the wc;u 1. behavior of nirrided manensitic stainless steel has not been syslematically studied \o far [71. Martensiric ctainless steel has found applications in many areas ofengineering. includ-

wear damages in the specimen. The wdiation pa\$ing through the worn specimen and impinging on the tluoresuent xreen placed behind the irradiated specimen reveals the presence of internal defects. Using X-ray imaging. it if pokcible to reveal the subsurface morphology iI\ well ;I\ surfilce WKIF morphology. thereby obtaining much more evidcnc; ot Ihe wear processesrhan from SEM alone IllI* 2. Experimental The marenal used in this work was AISI 410 martensitic stainless \tcel with the following chemical composition:

171) O.II% C, 12.41% Cr. 0.39% Ni. 0.34% Mn. 0.06% MO, 0.44% Si. 0.029% S. 0.019% P, and the balnnce iron. Plnsma nitriding was carried OUI on I commercial IO-EiW plasma processing unit in a 2.5 mbar NJ-H: gs mixture and 550C for 9 h. A Cambridge scnnning electron microscope

(SEM)

was used to analyze the surface morphology and microstructure of the nitrided layer. The microhardness profiles were obtained on cross-section specimens with a load of 100 g. A pin-on-cylinder wear-test system was used in the present investigation, and the dimensions and geometry of pin and cylinder were shown in Ref. and cylinder

[ 121, Both

the pin (specimen)

(counterpart)

were made of 4 t 0 stainless steel

(HV 250) with the surface roughness kept below 0.5 pm. Wear tests were carried out under both dry and lubricated conditions at room temperature (25C) with ambient humidity (50% R.H.). The lubricants include ( I ) mineral oil. Mobil Super 2T with a room-temperature viscosity of 2. I7 Pa s and (2) synthetic oil, Mobil I with a room temperature viscosity of I.24 Pas. The sliding speeds were400 rpm ( 1.03 ~~i/s).6(K)rpmtI.5~mls).800rpm~2.05m/s).lOOOrpm (2.57 m/s) and 1200 rpm (3.08 m/s). The normal loads were I5 N and 25 N and the contact pressures were 6.5 MPa and IO.44 MPa. respectively. Friction force was measured with a strain gage load cell to an accuracy of 0. I N. The wear depth was measured with a linear voltage displacement transducer (LVDT) with an accuracy of I X IO

m. The

tem-

perature rise of the counterface was measured by using a temperature label. which was attached to the counteiiace at l-mm distance from the contact area. Before and after each test. the specimens were weighed by an electronic b;dance to +O.l mg in order to calculate the weight loss. The other experimental details can be found in Ref.

1I2 1,After

wellr

testing, both SEM and a Fein Focus X-ray microscope FIP-KM).Ol were used to eRamine the surface :md uuhsurfnce wear morphology.

3. Results and discussions

Fig. I shows the surface morphology of pl;t\mil-nitrided 410 shinleu steel. A columnar structure king from the formiuion of a nitride layer can be seen. Fig. 2 I$ ii crosssection morphology of the nitrided layer. showing the typicnl fine microstructure and uniform case hardened Inyer. Fig. 3 showv the microhardnew distribution of the nitridcd layer. The maximum hardness i+ ilbout
0 50 100 150

Distance from Surface (lOJ mm)

I IS0 HV

where;\\ the hard-

ness of the subutrdc il; just 220 HV. The hardcncd zone is approximately X0 pm deep. meilaurcd to SSO HV.

incre;lse in cocfticlent of frick~n at the inihal \tilge ;md thih is attrihutcd to the hreitkiigc (II mcch;lnicnl bundu or local wcldmg between the aspcritics of IWO countcrlhcel;. After that. ;I con~kuit cocfticient of friction i+ ohserved. Fig. 5 \howl; the ccwfticicnt of friction for holh niuided imd lmtreilk!d spccitnm. The coefficient\ ot Iriction for

3.21. Fricricrs, IqwruIw riw rrrd wfwr rrnkr r/r;v vliflirl,~ nitrrdcd \pcclmens ;Irc I~~und hc much lol\\cr than Ihill of IO Fig. 4 shows thr typicul coeflicient of friction curve ils ;I lhc untrc;ded +cimcna. The dynamic hiction during sliding funclion of time after prolonged sliding. There i\ ;I sudden i> UX\I,IIIY brought ahotn hy triction ciltI\cd hy ;Idhcsion nnd

171

y 8

0.6

04
0.2 0

_ -. I

0.2 08 1

deformation

[X1, @niticanr The

krc;\~e

in surhcc

hitrdnc\s

after plasma nitridine can minimix both ;\dhe\;ivc friction and deformation of the a\peritk hetween the tuo c(>nt;lcted surfaces . thus decreGn~~ the coefticient a. z . signiticantly. conditions. the coefticient of friction of friction

For both treated and untrcilted cpecitnenj under dry 4idin; increase5 with JII increase in nominal load as shown in Fig. 5. Thic is becauw

the higher loud increases the contact urea hetwtcn the IWO surfaces and cnuScS the asperities to adhere more Won@q.
More pliistic lmd shear deformation of the nhperities :I< will as adhesion will occur between the two 4xe\. u high coefficient of friction. Fig. 6 shows that the coefticienl
illl

Iexlin~ to

offriction incrc;l\es with

increase in sliding speed under dry shdiq coruhrions for both nitrided and untreated cpecimenj. Thic i4 probably
attributed to the severity of adhesion and platic deformation under high 4iding speed, which cun he deduced from the significant temperature rivz between the tivo countertkes a\ shown in Figs. 7 imd X. From Fig. 7 and 8. it c;m alto he observed thut under dry sliding conditinn. the higher the c\hihit Ioucr aeurweight lossescomparedwith theuntreated specimen\. The degree of improvement in wear resistanceby plasma nitriding was dependent on the applied load and Ihe sliding \peed. An increase in normal load can cause an incrwc in t+tiir volume as shown in Fig, 9. Experimental rcsultr;i&o mdicate that plasma nitridinp was more effective

speed, the more signiticnnt the tempcraturc rk. The higher the load. the higher the temperature rise i\.
Fig. 9 shows the itverage weight losses for$pecitnens tested under dry sliding conditions. The plnsma-nitrided specimens

172

Y. Fir YI rd. / WlW !IY f lYYSl /h9-/7fi

5Nb

15NDly

I5NIWm.

15N,M,n

IINlSyn

15NISvn 200 so0 IWO 1400

tesl Condillons Fig. 9. Average wrtpht Ins under different sliding conditionr \howinp the

signiiicmt iocreare m rliding wear re\istme after plwn~ nitridtng.

Sliding Speed (rpm.)


Fig. IO. Coefticicnt of friction under different 4iding speed\ and dtfferettt luhric;lkd ctrndition\ a L ;I rmrnul load ot 25 N.

in improving the wear resistance of the steel under high load and high speed. The improvement of wear resistance by plasma nitriding is brought about by a combination of the high surface hardness. a fine surface microstructure, a rough core and high surface compressive residual stresses which imparts the specimen with good resistance to adhesive, abrasive and fatigue wear 1 I3 1. A hard nitrided layer can suppress adhesion. plastic deformation and severe wear of martensitic stainless steel over a wide range of applied load and sliding speed. value as shown in Figs. 7 and 8. The maximum measured temperature under lubrication conditions is only 37.32, whereas under dry sliding condition the maximum temperature is as high as IoO.7C. There is no significant difference in the cooling ability for both kinds of lubricants as they have similar viscosity. Why does synthetic oil show better performance than mineral oil during sliding wear? This question can be answered in terms of the change in viscosity for the IWO kinds of lubricams during sliding wear. Fig. I la shows the viscosity of both the mineral and synthetic oil measuredusing acontrolled rate rheometer under room temperature. The viscosity of the synthetic oil is much higherthan that of mineral oil indicating the superiority of synthetic oil in lubrication. The viscosity of lubricants decreases as rhe temperature increases. However, as shown in Fig. I lb. the decrease in the viscosity of synthetic oil with an increase in temperature is less than that of mineral oil.

The worn suriaces of untreated specimens exhibit severe scores and deep pmoves, as well as the intense surface/ subsurface cracking and shearing as shown in Fig. 12. These grooves are caused by hard particles, such as nitrides and carbides, w:rich were deeply pressed into the worn surface and subsequenrly ploughed into rhe opposing surface. X-ray images enhanced by the contrast function of worn specimen can show some tracks and the accumulation of the wear debris. An exam@\ If this type of X-ray image is shown in Fig. 1.7. When using the mask processing funcdon to under synthetic oil lubrication is lower than that under minenhance the surface feature of the worn specimens, X-ray images reveal more wear tracks and rhe extrusion of wear debris as is shown in Fig. I4 Fip. 15 shows a typical surface morphology of a worn nitrided specimen. Mild abrasive wear can be observed from eral oil lubrication. especially under high load and high speed for untrealed specimen. Bolh types of luhricams are excellent coolinp agenrs in keeping the temperature at the contachg surface IO a low

173

0.2

c
5 :

gi

0.16

0.1

A-1'
.

+Synlhdlc 01
+-Mineral 011

0.05

oJ(a)

,
Shear

I.E.03tE.02 I.E.01 l.E+OOl.E+Ol lE+02

rate (l/s)

FiE, viwsity of minerul oil and +ynthetlc 1111 ntca+ureduq :I controlled mte rhenmeter under mom temperature. The kinemdic vi+

Il. Ia The I

fhI

Fig. 13. X-my image rbii at ttz edge of rpecinwn.

UK UN

tmck and CXR~L&I Ocwee debris

Fig, IS. Worn nvrphology of nitrided rpecimetl &wing wear.

the mild &aive

174

Y. FII PI ul. / l!Jew !I9 tlY9RI

169-171,

Fig. 15. Transferred layers and particles caused by surface adhesion and plastic deformation are frequently observed on the surfaceofplasma-nitrided specimens asshown in Fig. 16.
This phenomenon indicates that the adhesive wear is one of the dominating wear mechanisms. Most of the transfer materials originate from the drum which is softer than the nitrided surface layer. X-ray images of the top view and cross section of worn specimens shown in Figs. 17 and I8 provide clear evidences of the transfer layer. One mechanism which couldcontribute to the overall wear of the plasma-nitrided stainless steel is delamination wear. This involves the initiation of subsurface or surface cracks, crack propagation and formation of wear particles [ 14,151.

[ 171, Fig. I9 shows a typical delamination morphology of the worn surface. X-ray images also reveal the delamination and near-surfacecracks. The delamination layer is seento be

After plasma nitriding, the nitrided layer is considerately more brittle. The structural mismatch between the nitrided layer and the marrix induces high inherent stressesand even cracks at the interfaces [ 161.Thesecracks start in the nitrided layer and move towards the surface to produce wear particles

-200pm
Fig. 18. X-ray imageofthecross sectionof womnitridedspecimenshowmg the transfer layer.

Fig. 16. Transfer wicks

found on the worn nirrtded specimen caused hy Fig. 19. Delamination morphology found thewornnit&d specimen. on

surfaceadhesionand plastic deformation.

SOOpm
nation mechanism and near-+&ace crack.

Fig. 17. X-ray image of ~hctop view nf worn nitridedqccimcn rhowinp the evidence of the lrabfcr layer.

175

rise in n pin-on-cylinder apparatus followed by SEM and Xray imaging of the worn curfaces revealed the following

conclusions.

i I )Plasma mtridedspecimensexhibited higherwearresistance and better friction control, especially at high levels of
load and speed;

(21The synthetic oil was superior to the mineral oil especially under high load and high sliding speed.

(3) The combination of synthetic oil as lubricant and plasma nitrIding resulted in the lowest wear rate.
t 4) X-ray lmagng and SEM verified that the controlling wear mechanisms of the nitrided steel are adhesion. abradve
Weilr and delaminution.

Acknowledgementi
Ilf unlrclllcd qxllacn

The author\ would like to thank Doxon Engineering for providing plama-nitrided specimens. The support of the School nf Mechnnlcal Production and Engineering, Nanyang Technological University. is also acknowledged.

References

III P..A Dc.nilc).


mrnt\. I4l-lhh

l. Bell. F. Hornbeck. Plasna aqusteddiffu~mn treat.

Suri,ct \IodiCcauon Technotogier VI. m: T.S. Sudmhan. J.F.

Br;l/.l Ed\. I, The blmmla. Metal\ and Marenal Society. 1993, pp.

I! I K T. RIG. E I11 Grun. H.J R.

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\trlutlclnr .md hmitq. Mater. Sci. Eng. A I4 I 1991 I 4?544. 141 R D Whulls. V.D. Scott. B.S. Yilha. A.Z. Sahin. S.A.M. Said. J. Nickel. r\ Cub. lnvesugation inlo wome trihologrcal pmpalies of pla\ma nurldcd hot-worked 1001steel AISI HI I. I Mater Enp. Perfum,a~cc 5 19%) !ZJ.

151 MB
U!.

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on the dry

IhI ACohen. A. Rosen, The influence of the nunding prce\\


made up of many sublayers which h;J been piled on the top of each other. Shear deformation lines beneath the worn surface can also be observed as shown in Fig. 20. Under lubricated conditions, only mild itbri\k wear and scratch marks can be found on the surface of worn specimens as is shown in Figs. 2 I and 2. To summarize, both SEM and X-ray imaging contirm that
ItI?

uc:s rc\l\l;mcc nf IS-S PH +tainlos steel. Werr IO8 ( 19861 IS-

[7 ]

Y. Sun. T Bell. G. Wucxl. Wca hehakinr nf phrma-nnndcd msrten-

ac aunlc\~ #{eel. Wei I711 IWI 131-1~8. I ( Xl A Grccnc. ASM Metal lbdhook. Vol. 17. Nnndeslruollvc E~sluatmn and Qu;duy Control. ASM bernatmnal. 1992. pp. 295-357. [ 1)1 Y Q Fu. H T Xing. M.Chaddwekann. A.W. B;llchelnr.Optlmiralinn of Id\er prrrcaing pauneterr hy X-my Imaging. J. Mater. Sci. Lea. Ihl 1Y97) 11119-1112.

the bait

wear mechanisms of the nitrided specimens are

[IO MCh;ldn\&ur~n. I

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of \liding

(tear lertr of hulyl ruhtterin presenceof lubrbntr man liKu\ in~hument, Wear !I I I I I I Y Q Fu, A W Batch&

adhesive wear. delamination and abrasive wear. 4. Conclusion A tribological study of plasma nitrided stainless steel involving measurements of friction. wear and temuerature

X-ny micro-

ItW71

3543.

N.L. Lnh. X-my unagmg and SEM ;m;lly+s of I&h Intemahnmd Confer-

ef qorn pl;~qua&u!ed 316 \tamle\\ hteel, m: T.S. Sudurshrm.K.A. Khur. M Jcnrdin Eds. ). &ceding\ cute cln Surf.ce Mndilbtion 1% Fmplpurc. pp. %3-973. ,.

Technnlqr*

ISMT-IOI.

2-1 Sep.

176

Y. uru/./Wvr/r?IY 16Y-I?/, AI (IY98)

[ 121 PK. Aw. A.W. Batchelor. N.L. Lrrh. Structure nnd trihrQzical propenit\ of plasma nirrided surf;rc tilw on Incc1ncl7lH. Surf. Coutinp Trchnal. 89 1997 70-76.

[ IS) II, D.T. GilWne. W~arcl~ar~cteri~tiver~fpl:~~n~:~-~~itritledCrMr~~teul S.


under mlxed and houndwy
luhrwted cmditim.

1. M&r

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[I.11

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t 1992 I 19%206.

1141 N.P. Sub. A rtww (19771 12.

of 1111 dcl;w~;ltinn thwry of war. Wwr 44

1 I71

pIarm gearing +teul. Wear I61 IIOY3) nitrlded


nitridcd fnwncl7lX

IO9-?lK

P.K. Aw. A.W. Bukhclnr. N.L. Lull. Ftiilurt mrch;tnirnl\ of pltiamu tilm. Wca 208 1997) 2212%

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