Thermal Fatigue Testing of Inconel 617 and Stellite 6 Alloys as Potential Tooling Materials for...

Materials Science and Engineering A 527 (2010) 19381945

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Materials Science and Engineering A

journa l homepage: www.e lsev ier .co

Therm llitmateri

Yucel BirMaterials Instit

a r t i c l

Article history:Received 8 SepReceived in reAccepted 9 No

Keywords:SteelsThixoformingToolingThermal fatigu

ixoforfeedsclingMoVmpero-ph

7 and17 anol stes afte

1. Introdu

Semisolid processing of aluminium and magnesium alloys isalready a well established manufacturing route for the produc-tion of intricate, thin-walled parts with mechanical properties asgood as forged grades [1]. In spite of its potential to upgrade themarket andnet shape fhigh meltindie materiawhen thixoon tool matof forming c

The printo be thermis modest obehaviour o[918] in anhigh tempeprocess temtemperaturthan withwork tool stable replacesteel thixofo

Tel.: +90 2E-mail add

eenare g

are amongpotential candidates. Amongwear-resistant alloys, a Co-based alloy, Stellite 6, retains its hardness and resists oxidation andoffers an excellent resistance to thermal shock, wear and corrosionover a wide temperature range [35]. Inconel 617, a Ni-based super-

0921-5093/$ doi:10.1016/j.provide lightweighting for forged steel parts, this near-orming process has not enjoyed commercialization forg point alloys due to a lack of suitable high temperaturels [2,3]. Cyclic thermal loading on tools is substantialforming steels and confers very specic requirementserials [47]. Thixoforming tools ought to last thousandsycles for industrial application to be attractive.ciple failure mechanism in thixoforming dies is claimedal fatigue as the mechanical loading on the toolingwing to a mushy feedstock [8]. The thermal fatiguef hot work tool steels has been investigated extensivelyattempt to improve their performance in a number of

rature applications such as aluminiumdie casting.Withperatures above 1250 C [46], the surface-to-interioredifferentials in steel thixoformingdies aremuch largerAl [19]. While very affordable, the conventional hoteels proved to be entirely inadequate [2,7,2022]. Suit-ments for hot work tool steels, able to withstand therming environment for an economically acceptable life

62 6773084; fax: +90 262 6412309.ress: [email protected].

alloy,was reported to exhibit superior thermal fatigue resistance indemanding tooling applications [36]. The present work was under-taken to explore the potential of Inconel 617 and Stellite 6 alloysand to compare its performance with that of X32CrMoV33 steelwidely used in the manufacture of conventional forging dies [37].

2. Experimental

The tool steel was supplied as-cast by a major steel com-pany while the Inconel 617 and Stellite 6 alloys were castin the laboratory. Their chemical compositions are given inTable1.X32CrMoV33samplesweremachined fromtheas-receivedblock and were subsequently austenitized at 1025 C for 30min,quenched in circulating air and nally tempered twice at 625 Cfor 2h yielding a hardness of 45 HRC. The Inconel 617 sampleswere solution annealed at 1175 C while Stellite 6 alloy sampleswere stress relieved at 900 C for 4h and slowly cooled to roomtemperature.

The thermal fatigue test involved cyclic heating and coolingof prismatic samples (25mm25mm20mm) machined fromX32CrMoV33 hot work tool steel, Inconel 617 and Stellite 6 alloysbetween the peak die cavity surface temperature and the tem-perature the die was pre-heated to before the forming operation.

see front matter 2009 Elsevier B.V. All rights reserved.msea.2009.11.021al fatigue testing of Inconel 617 and Steals for thixoforming of steels

ol

ute, Marmara Research Center, TUBITAK, Gebze, 41470 Kocaeli, Turkey

e i n f o

tember 2009vised form 9 November 2009vember 2009

e

a b s t r a c t

The principle failure mechanism in thtooling is modest owing to a mushy6 alloys were submitted to thermal cyThe thermal fatigue test of the X32Crto severe surface degradation and teresistance, in spite of favorable thermand Co-based superalloys, Inconel 61hand, was encouraging. The Inconel 6temper softening than the hot work towith few and relatively shallow crack

ction have bwhichm/locate /msea

e 6 alloys as potential tooling

ming dies is thermal fatigue as the mechanical loading on thetock. Samples of X32CrMoV33 steel, Inconel 617 and Stelliteunder conditions which approximate thixoforming of steels.

33 hot work tool steel was terminated after 1500 cycles duesoftening, both leading to a relatively poor thermal fatigueysical properties. The response to thermal cycling of the Ni-Stellite 6, under steel thixoforming conditions, on the other

d Stellite 6 samples are much more resistant to oxidation andel, providing a superior resistance to thermal fatigue crackingr as many as 5000 thermal cycles.

2009 Elsevier B.V. All rights reserved.

investigated in recent years [8,21,2334]. Superalloysenerally employed for high temperature applications

Y. Birol / Materials Science and Engineering A 527 (2010) 19381945 1939

Table 1Chemical composition of the X32CrMoV33 hot work tool steel and Ni- and Co-based high temperature alloys used in the present work.

Alloy C Si Mn Cr Mo Ni Al Co Cu Nb Ti V W Fe

X32CrMoV33 0.281 0.190 0.200 3.005 2.788 0.221 0.025

1940 Y. Birol / Materials Science and Engineering A 527 (2010) 19381945

Table 2Thermo-physical properties and Youngs modulus values of the tested materials as a function of temperature.

T (C) Conductivity (W/mK) Cp (J/gK) Youngs modulus (GPa) (m/mK)

X32CrMoV33 Inconel 617 Stellite 6 X32CrMoV33 Inconel 617 Stellite 6 X32CrMoV33 Inconel 617 Stellite 6 X32CrMoV33 Inconel 617 Stellite 6

25 16.28 209.6828 207.7282 7.18927 8.66638 9.1189350 18.06

100 21.46 206.5015 204.5025 10.36247 11.14522 11.50619200 21.58 201.4563 199.4289 11.91377 12.48774 12.87849300 22.23 195.493 193.4723 12.40772 13.0512 13.48845400 21.76 188.6115 186.6327 12.81201 13.56039 13.98874500 21.22 180.812 178.9099 13.25921 14.14658 14.51137600 22.72 172.0943 170.3042 13.53733 14.70218 14.98786700 29.23 162.4584 160.8154 13.58018 15.23533 15.46937800 46.99 151.9045 150.4435 13.95789 16.22454 16.44683

a Measured

These twoest temperarespectivelyacross the dthe usual inat the surfaexperimentX210CrW12thus obtaintional hotwbefore the ftion of thethermocoup

The contperature ofame to the30 s (Fig. 2)bring the s30 s. The temples (will brest of thetype thermrespective stively using

The hardwith a loadthermal expdeterminedof 10 C/mimeasuremegas ow atLFA457 insments undeof 5 C/min.

3. Results

Thermo-on the temtate the maheat conduhigh surfacents and exmaterials thigher heating temperchoice baseHowever, tductivity vby the die

g experiments (Fig. 4). The maximum die cavity surfaceratures were in the neighbourhood of 750 C for both hotool steel and Inconel 617 dies. This is believed to be duefact that the thermo-physical properties of the three mate-sted in the present work are not much different below

, i.e. at temperatures which dominate much of the forming

change in temperatures of surfaces A and B with time dur-rmal cycling is illustrated in Fig. 5a. The temperature vs times for the three materials show typically similar features. Sur-ontinuouslywarmsup to themaximumtemperatureduringting step and starts to cool as soon as the sample is elevatedcooling position, while surface B is still warming up as itaccommodate the incoming heat. After about 1520 s, theratures of the two surfaces are equalized when surface A isin contrast to surface B which is still warming up. The lat-starts to cool soon after. Both surfaces keep cooling during

t of the cycle, with surface B temperature running highere than surface A. It takes only a few seconds for surface A2 9.246 11.403 214.9528 9.901 12.525 0.3083 0.4023 0.40935 3 11.579 14.039 0.3814 0.47767 0.46406 209.85342 13.269 15.775 0.3906 0.49697 0.47435 202.40688 14.872 17.197 0.4194 0.51288 0.4797 194.21928 16.555 18.694 0.4382 0.53265 0.49211 185.29067 18.706 19.684 0.4741 0.56354 0.496 175.62097 24.155 22.692 0.5702 0.68715 0.54291 165.21029 27.18 27.666 0.9289 0.70851 0.63111 154.05858a 22.646 29.803 1.8805a 0.75081 0.68442 142.1657

at 750 C.

temperatures are potentially the highest and the low-tures encountered during the thixoforming operation,, and thus give the steepest temperature gradientie. While the die was pre-heated to 450 C, consideringdustrial practice, the maximum temperature attainedce of the die cavity was measured during thixoformings (Fig. 1). Slugs, sectioned from a commercial hot rolledbar, were held isothermally at 1290 C and the slurry

ed was pressed into dies manufactured from a conven-ork tool steel and Inconel 617alloypre-heated to450 Cormingoperation [33]. The temperatures across the sec-die were measured during thixoforming with K-typeles xed into 3mm diameter holes (Fig. 1b).rolled parameter during thermal cycling was the tem-the front face of the sample, heated by an oxyasetilenmaximumdie cavity surface temperaturewithin about

. Cooling was performed by forced air, adjusted so as tourface temperature to around 450 C, during the next

peratures at the front and at the rear faces of the sam-e referred to as surfaces A and B, respectively in thepaper) were measured during thermal cycling with K-ocouples xed into 3mm diameter holes 0.1mm fromurfaces. Thermal fatigue damage was assessed qualita-stereo and optical microscopy.ness of the samples were measured in Vickers unitsof 1 kg (HV1) before and during thermal cycling. Theansion coefcients of the potential die materials werewith a Netzsch 402 PC unit in air at a scanning rate

n. Netzsch 409 PC Lux instrument was used for thent of the specic heat capacities, Cp, under a nitrogen40ml/min at a heating rate of 10 C/min. A Netzsch

trument was used for thermal conductivity measure-r nitrogen gas owing at 100ml/min at a heating rate

and discussion

physical properties of die materials have a big impact

formintempework tto therials te700 Ccycle.

Theing theprolefaceA cthe heato thehas totempecoolingter alsothe resthis timperature gradients across the die, which in turn, dic-gnitude of thermal stresses. High heat capacity and

ctivity help to extract heat from the work piece, avoide temperatures and thereby reduce thermal gradi-tend the service life of the tooling [23]. Of the three

ested in the present work, hot work tool steel offerscapacity and thermal conductivity near the thixoform-ature range and thus appears to be the material ofd on thermo-physical properties alone (Fig. 3, Table 2).he favorable specic heat capacity and thermal con-alues of the hot work tool steel are hardly reectedcavity surface temperatures measured during thixo-

Fig. 3. Changesteel, Inconel 6in (a) heat conductivity and (b) specic heat capacity of X32CrMoV3317 and Stellite 6 alloys with temperature.


Fig. 4. Change in die cavity surface temperatures with time during thixoformingcycle of (a) X32CrMoV33 steel and (b) Inconel 617 alloy.

Fig. 5. (a) Change in temperature at surface A and B and (b) change in temperaturedifference between surface A and B of X32CrMoV33 steel, Inconel 617 and Stellite 6alloy samples during thermal cycling.

Fig. 6. ChangX32CrMoV33

to becomeunderway.

It is indesample whperature gaconguratithermal cycB for the inwarmer thafacewantsbulk and is

Fig. 7. Changecycling of X32e in (a) Youngs modulus and (b) thermal expansion coefcients ofsteel, Inconel 617 and Stellite 6 alloys with temperature.warmer than surface B once the next heating cycle is

ed the temperature gradient across the section of theich is responsible for thermal strains. The largest tem-p occurs between surfaces A and B in the present teston. The change in the temperature gap during a singlele is shown in Fig. 5b. Surface A is colder than surfaceitial several seconds of the thermal cycle but becomesn surface B during the next approximately 30 s. The sur-to expand but is kept fromdoing so by themoremassiveinevitably put under compression when it is warmer

in thermal stresses generated at surface A with time during thermalCrMoV33 steel, Inconel 617 and Stellite 6 alloy samples.

1942Y.Birol/M

aterialsScience

andEngineering

A527 (2010) 19381945

Fig. 8. Features of the front face, surface A, of (a) X32CrMoV33 steel, (b) Inconel 617 and (c) Stellite 6 alloy samples in the course of thermal cycling.


Fig. 9. (a) Oxiafter 1500 cyc

than the reThe state ofsurface A areversed oncolder thantract in thisbulk and is

The magsurface A, d

surface = m

Since the mechanical loading on the tooling is modest owing toa mushy feedstock [8], we can write for thixoforming,

l mechanical (2)

=

anus, reis e

y prompein Fis to bire tetherma

surface

wheremodul[38]. Itis a kewith teshownappearthe entde scale at surface A of X32CrMoV33 steel and thermal fatigue cracksles on sections: (b) at 0.5mm and (c) at 1mm from surface A.

st of the sample, i.e. during much of the heating step.compression at surface A prevails during cooling until

nd B temperatures equalize. The strain distribution isce again during the rest of the cycle when surface A issurface B. The increasingly colder surface wants to con-range but is restricted by the more massive, warmer

put under tension.nitude of stresses generated at the die cavity surface,uring thixoforming can be estimated from,

echanical + thermal (1)

compressivthermal cycInconel 617

Evidentlmuch of theas 550MPawhen surfastresses areis forged inated at theX32CrMoV3and 424MPhand, near tthe bulk antemperaturing operatiodie. The tenfor the X32respectivelsive stressestrength of

The fronmal cyclingX32CrMoV3due to sevethe presentthe surfaceeventuallyto a thermafatigue cracthe surfacealways decoface stock wfrom surfachave exertewide and thcrack resistbe accounte

The poooxidation ato thermalthixoforminperformedFe3O4 has fsurface andThe damaginstrumentwhich relyuous protectake advanas 3wt%.thermal = (T)E(T) (T) (3)

d E are the thermal expansion coefcient and Youngsspectively, both expressed as a function of temperaturevident from Eq. (3) that thermal expansion coefcientperty of potential die materials. The change in and Erature for the three alloys tested in the presentwork areg. 6 and are listed in Table 2. The X32CrMoV33 tool steele at an advantage with a lower expansion coefcient inmperature range. This is essentiallywhy themaximume and tensile stresses that develop at the surface duringling are smaller for the hot work tool steel than for theand Stellite 6 alloys (Fig. 7).

y, compressive stresses dominate at the surface forthermal cycle. These compressive stresses are as high

for the Inconel 617 alloy near the endof theheating stepce A is much warmer than the bulk. High compressivethus to be expected when the thixotropic feedstock

to the die. The maximum compressive stresses gener-die cavity surface, surface A, of Stellite 6 alloy and the3 tool steel are relatively lower, estimated to be 479a, respectively. Tensile stresses dominate, on the otherhe end of the cooling step, once the surface cools belowd during the start of the next heating step before thees of surface A and B equalize. This is when the form-n is over and the thixoformed part is ejected from thesile stresses thus generated are 109, 165 and 258MPaCrMoV33 tool steel, Inconel 617 and Stellite 6 alloys,y. These stresses are much smaller than the compres-s that develop at surface A and fall well below the yieldthe respective alloys.t face, surface A, of the samples submitted to ther-are shown in Fig. 8. The thermal fatigue test of the3 hot work tool steel was terminated after 1500 cyclesre surface degradation (Fig. 8a). Thermal cycling underconditions has produced rather thick oxide scales at

of the X32CrMoV33 hot work tool steel (Fig. 9a) whichstarted to spall off with continued thermal cycling, duel expansion mismatch (Fig. 8a). Deep, branched thermalkswere noted once the oxide scaleswere removed fromof the sample (Fig. 9b and c). These cracks were almostratedwith thick oxide layers even after substantial sur-as removed by grinding and survived at sections 1mme A. The thick oxides on crack surfaces are believed tod a wedging effect which helped to open the cracksus encouraged their growth. The relatively poor fatigueance of the X32CrMoV33 hot work tool steel could thusd for, at least in part, by its inferior oxidation resistance.r resistance of the X32CrMoV33 hot work tool steel tot high temperatures is believed to impact its responsefatigue in the temperature range of interest from steelg point of view. Samples submitted to oxidation testsat 750 C were coated with a thick Fe3O4 scale [39].ailed to sustain the thermal stresses generated at thestarted to spall from the surface after only 500 cycles.

e thus generated at the surface (Fig. 8) is believed to beal in crack initiation. Unlike the high temperature alloyson a minimum Cr content of 20wt% to develop a contin-tive Cr2O3 lm [40,41], the hot work tool steel cannot

tage of such protection with a Cr content only as much

1944 Y. Birol / Materials Science and Engineering A 527 (2010) 19381945

Fig. 10. (a) Chand Stellite 6with depth frocycling.

Howevetool steelw(Fig. 10a). Hmal fatiguecycles. It isof the thermbeen adversat all surprhot work tothe temperagetting as hhot work toperatures thThis ndingresults on vfrom the forhurt the thtool steels.

The resploys, Inconeon the othecolouring, tthe Inconelthat they artool steel. Tsamples suidentied tSiO2 [39]. Thave sustaiout spalling

Weight gain as a function of temperature of the three alloys used in thework.

tion was reported to be good at high temperatures [43,44].content of the two alloys, above 20wt%, facilitated the for-of a continuous Cr2O3 lmduring thermal fatigue providingte protection, much like it does in high temperature alloys

]. Oxides of aluminium and silicon are also well establishedighly protective for alloys intended for high temperaturetions [41]. Further evidence for the above account is avail-the TGA tests (Fig. 11). The resistance to oxidation of theange in hardness of X32CrMoV33 hot work tool steel, Inconel 617samples with increasing number of thermal fatigue cycles and (b)m surface A of X32CrMoV33 steel samples before and after thermal

Fig. 11.present

protecThe Crmationadequa[40,41to be happlicaable inr, the underlying issue with the conventional hot workas the substantial drop inhardnessupon thermal cyclingardness of surface A,whichwas 442HVbefore the ther-test, dropped to approximately 275 HV after only 400inferred from the hardness prole across the sectional fatigue sample that a surface layer 10mm deep hasely affected by thermal exposure (Fig. 10b). This is not

ising considering the temper resistance of the presentol steel, reported to deteriorate above 650 C [42] andtures surface A must withstand during thermal cycling

igh as 750 C. The temper resistance of theX32CrMoV33ol steel is apparently not sufcient to sustain the tem-ixoforming dies experience during forming operations.of the present work is in full agreement with earlier

arious hot work tool steels [2022]. It is fair to concludeegoing that temper softening and severe oxidationbothermal fatigue resistance of the conventional hot work

onse to thermal cycling of theNi- andCo-based superal-l 617andStellite6,under steel thixoformingconditions,r hand, was an encouraging one. Aside from a slighthere was hardly any oxidation on the front face of617 and Stellite 6 samples (Fig. 8b and c) suggestinge much more resistant to oxidation than the hot workhe oxides formed on Inconel 617 and Stellite 6 alloybmitted to oxidation tests performed at 750 C wereo be predominantly chromium oxide, with Al2O3 andhese slowly growing adhesive oxides are believed toned the thermal stresses generated at the surface with-. The plasticity of the chromium oxide, essential for

Fig. 12. (a) Thand (b) Stelliteis obtained byermal fatigue cracks on sections parallel to surface A of Inconel 6176 after 5000 cycles. The section seen is at 0.2mm from surface A andsand paper grinding.


X32CrMoV33 tool steel is clearly inferiorwith respect to the Inconel617 and Stellite 6 alloys which behave very similarly over this tem-perature range. The adhesive oxides are claimed to contribute tothe superior thermal fatigue performance of these alloys.

Softening upon thermal cycling was noted also in these alloys(Fig. 10). The average hardness of surface A, 306 HV before the test,dropped to268HVafter1500cycles and remainedmoreor less con-stant for the rest of thermal cycling in Inconel 617. Likewise, thehardness ofthermal cyhot work toThe extentsuperalloyscycles. Besiner. Howevand Stellitecracking. Thshallow craWhile the tlite 6 samplthose in theily removedthe Stellite617 alloy owoxidation reat the frontbe responsithis sample

4. Conclus

Sampleswere submiimate thixoevery 602the X32CrMcycles dueboth leadinof favorablecycling of Ining conditio617 and Steto oxidationviding a suand relativeIt is concludtooling mattance to higcracking.

Acknowled

F. Alageyiments. ThithixoforminPlaning Org

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ions

of X32CrMoV33 steel, Inconel 617 and Stellite 6 alloystted to thermal cycling under conditionswhich approx-forming of steels, i.e. between 75010 and 45010 C,s for a total of 5000 cycles. The thermal fatigue test ofoV33 steel had to be terminated, however, after 1500to severe surface degradation and temper softening,g to a relatively poor thermal fatigue resistance, in spitethermo-physical properties. The response to thermalconel 617 and Stellite 6 alloys, under steel thixoform-ns, on the other hand, was encouraging. The Inconelllite 6 samples were found to be much more resistantand temper softening than the hotwork tool steel, pro-

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Thermal fatigue testing of Inconel 617 and Stellite 6 alloys as potential tooling materials for thixoforming of steelsIntroductionExperimentalResults and discussionConclusionsAcknowledgementsReferences

Thermal Fatigue Testing of Inconel 617 and Stellite 6 Alloys as Potential Tooling Materials for...

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