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Wear 270 (2011) 591–597

Contents lists available at ScienceDirect

Wear

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ribological properties of copper alloy-based composites reinforced withungsten carbide particles

unji Honga, Bradley Kaplinb, Taehoon Youa, Min-soo Suha, Yong-Suk Kima, Heeman Choea,∗

School of Advanced Materials Engineering, Kookmin University, 861-1 Jeongneung-dong, Seongbuk-gu, Seoul 136-702, Republic of KoreaDepartment of Mining and Materials Engineering, McGill University, Montreal, Quebec H3A 2B2, Canada

r t i c l e i n f o

rticle history:eceived 23 March 2010eceived in revised form5 December 2010ccepted 21 January 2011

a b s t r a c t

In today’s oil/gas industry, use of drill bits in harsh drilling conditions is demanding the pursuit of inno-vated materials for higher performance and efficiency. This paper describes the successful application ofindium doping in tungsten carbide particle reinforced Cu-alloy composites (Cu-alloy/WCp) for PDC (poly-crystalline diamond compact) drill bit body in maximizing wear resistance with relatively low frictioncoefficient. The wear resistance of Cu-alloy/WC composites with novel indium dopant is investigated

vailable online 28 January 2011

eywords:etal-matrix composite

utting toolsear testing

p

by nano-scratch test and pin-on-disc wear test, and is compared with that of conventional materials.Doped indium improved the overall wear performance by 38% under a 10 N normal load with up to asliding distance of 3000 m due mainly to the solid-solution strengthening effect of indium in the Cu-alloymatrix. The combination of ploughing in Cu-alloy matrix, and brittle fracture and fragmentation of WCreinforced particles appear to be the main wear mechanisms of Cu-alloy/WCp composites under macro

cratch testingardness

scale sliding wear.

. Introduction

Drill bits used in today’s oil/gas industry are regularly subjectedo extreme drilling conditions accompanied with sliding, tearingnd gouging motion that can accelerate deterioration of the struc-ures and properties of the bits [1–4]. In actual service, severe wearnd erosion, caused by not only the abrasive but also the high tem-erature and frequent percussion environment, are prime factorshat can lead to premature deterioration of the bits [4]. In order toast longer and be more economical, these bits are comprised of aifferent combination of materials to utilize their respective advan-ages and better withstand against harsh drilling environments. Inarticular, the composite bit body consisting of a metal matrix and aeramic reinforcement is expected to be a promising alternative forpplication in extreme drilling environment to the previously usedteel bit, which has reached the upper limit of their mechanical andconomical limitations due to its relatively poor wear resistance1–6]. Such composites, employing a metallic alloy as the matrix (orinder) and ceramic particles as the reinforcement, are commonly

nown as PRMMC (particle-reinforced metal-matrix composites).he addition of extremely hard but brittle ceramic particles, how-ver, has opposite effects on the performance of drill bits: theres generally a significant increase in hardness and wear resistance

∗ Corresponding author. Tel.: +82 2 910 4417; fax: +82 2 910 4320.E-mail address: heeman@kookmin.ac.kr (H. Choe).

043-1648/$ – see front matter © 2011 Elsevier B.V. All rights reserved.oi:10.1016/j.wear.2011.01.015

© 2011 Elsevier B.V. All rights reserved.

but a substantial decrease in ductility and toughness [5–7]. Accord-ingly, composites with a significant volume fraction of ceramicparticles are rarely used because the ductility and toughness ofthe composites would be intolerably low for general structuralapplications. On the other hand, it was recently shown that the“high-volume” PRMMC, the PRMMC with an unusually high per-centage of ceramic particle reinforcement phase(s), can exhibitfavourable combinations of strength and toughness when pro-cessed appropriately [7–11].

Among a variety of available high-volume PRMMCs, tung-sten carbide particle-reinforced composites exhibit excellentmechanical properties [3,4]. In particular, tungsten carbideparticle-reinforced composites with a copper alloy as the matrix(Cu-alloy/WCp) are widely used in drill bit applications for the fol-lowing reasons. First, the two materials have good compatibilitywith each other and show excellent wetting characteristics thatcan form a good interfacial bond between the matrix and reinforc-ing phase [8,12]. Second, copper alloy-based composites exhibitsubstantial wear resistance when reinforced with hard ceramicparticles, such as tungsten carbide [2]. Third, tungsten carbide haslimited solubility in copper and does not form complex interfa-cial intermetallic layers with copper alloys [8,13]. Forth, tungsten

◦

carbide retains the hardness of room temperature up to 1400 Cwithout any phase change [2].

As drilling operations are engaging in increasingly demandingdrilling conditions, Cu alloy-based tungsten carbide compos-ites with further improved mechanical properties are essentially

592 E. Hong et al. / Wear 270

Fb

inabemim

2

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(4t

ig. 1. Schematic diagram of infiltration process for the manufacture of a Cu alloy-ased composite reinforced with tungsten carbide particles.

nevitable. The present work presents the effect of indium as aew dopant to the Cu-alloy/WCp composite to improve its over-ll hardness, strength, and wear resistance, which was fabricatedy a pressureless infiltration process. In order to understand theffect of indium addition and the correlation of hardness andicro/macro wear, the Cu-alloy/WCp composites with and without

ndium dopant are examined using a series of hardness measure-ent, nano-scratch test and pin-on-disc wear test.

. Materials and methods

Tungsten carbide powder (Taegutec, Republic of Korea) with anverage particle size of ∼30 �m was used as the reinforcement. Aopper based alloy (Kennametal, USA) with contents of 14–16 wt.%ickel, 7–9 wt.%zinc, and 23–25 wt.% manganese was used as theatrix. BP-1A flux (Daesong Metal Materials, Republic of Korea)as also added to prevent oxidation from occurring inside the cru-

ible during infiltration. Graphite crucibles (Samjung C&G, Republicf Korea) were used to perform the infiltration process. The cru-ibles were 13.5 cm in height, 5.0 cm in diameter and 0.5 cm inhickness, with an inner diameter of 4.0 cm. As shown in Fig. 1,he tungsten powder acted as the preform and was placed at theottom of the graphite crucible, which was followed by lumps ofhe Cu-based binder alloy, the indium dopant when required, andnally the flux in the form of a powder. The amount of flux and

ndium used was, respectively, 1.0% and 2.0% of the weight of the

opper binder alloy.

The loaded crucibles were placed in a preheated air furnaceKorea Furnace Development, Republic of Korea) at 1177 ◦C for5 min. The first 15 min was considered to be sufficient for the sys-em to re-equilibrate to the set temperature, while the latter 30 min

Fig. 2. Optical micrographs showing the microstructure o

(2011) 591–597

was considered to be the time for the actual infiltration process. Thecrucibles were removed from the furnace immediately after infil-tration, and cooled rapidly in air. Once cooled, the samples wereremoved from the crucibles and cut into pieces for metallographicexamination. The specimens for mechanical testing were machinedusing an electrical discharge machining method, and then sequen-tially mounted, ground, polished, and finally etched using a nitricacid solution for microstructural characterization. The microstruc-ture was characterized using both optical and scanning electronmicroscopy. The size and volume fraction of tungsten carbide phasewere determined by drawing more than 10 random lines of unitlength on optical micrographs and by conducting intercept mea-surements [14].

Hardness was measured using a standard Rockwell hardnesstesting machine (Mitutoyo, Japan) by applying a 1.6 mm diametersteel ball with a 100 kg major load for Rockwell hardness scaleB (HRB). A nanomechanical test instrument (Hysitron, USA) wasused to perform nano-mechanical tests on the composite sam-ples. Nano-scratch tests were performed using forces of 300 and1000 �N for durations of 20–30 cycles. The indenter was loaded,forced to scratch the surface of the material by being pulled backand forth for a number of cycles, and then finally unloaded. Thewear tests were carried out using a pin-on-disk tester. Prior tothe wear test, all specimens were ground to 1 �m, cleaned withmethanol and dried. Round specimens with a diameter of 25 mmand a surface area of ∼3.2 cm2 were loaded and slid against anabrasive Al2O3 counterpart ball (Samhwa Ceramics, Republic ofKorea; purity: 93%; Mohs hardness number: 9) at a sliding speedof 0.1 m/s. The applied normal load was fixed at 10 N and the totalsliding distance travelled by the ball ranged from 300 to 3000 m.The mass losses of the specimens were measured on an analyticalbalance with an accuracy of 10−4 g.

3. Results and discussion

3.1. Microstructure

Fig. 2 shows optical micrographs of the etched binder andcomposite microstructures. The binder material had a fairlypronounced dendritic structure, which is typical of Cu-basedalloys. The composite material clearly shows two distinct phases.Almost equiaxed tungsten carbide grains were observed rang-ing in size from approximately 5 to 60 �m with an averageof ∼30 �m. The tungsten carbide particles, which comprise

∼62% of the entire composite, were distributed uniformlythroughout the sample without significant clustering or isola-tion. Scanning electron microscopy did not show evidence ofinterfacial delamination or debonding at the Cu–WC interface(Fig. 3).

f (a) a binder material and (b) infiltrated composite.

E. Hong et al. / Wear 270 (2011) 591–597 593

Fm

3

beopManbitiHitaippmc

3

n(ctraif

Fig. 4. Depth profiles of the nano-scratch tests performed at 300 �N for 20 cycleson (a) the Cu-alloy matrix without indium, (b) Cu-alloy matrix with indium, and

TP

ig. 3. Scanning electron micrograph showing the interface between the Cu-alloyatrix and tungsten carbide.

.2. Hardness measurement

Rockwell hardness measurements were performed for both theinder and composite samples with annealed pure copper as a ref-rence (Table 1). The Cu-alloy binder sample displayed a hardnessf 46.1 HRB, which is much higher than the 8.0 HRB obtained forure annealed Cu, apparently due to the strengthening effects ofn, Sn and Zn [13]. A further hardening effect was achieved by

dding 2 wt.% indium to the Cu-alloy binder showing a higher hard-ess of 52 HRB as compared to a hardness of 46 HRB for the Cu-alloyinder without indium (Table 1). On the other hand, the compos-

te samples showed significantly higher hardnesses (108–110 HRB)han those of the unreinforced binder alloys (46–52 HRB), with thendium-doped composite showing a slightly higher hardness (109.6RB) than the composite without indium (108.4 HRB). The slight

ncrease in hardness in the indium-doped composite is attributedo the solid-solution strengthening effect of indium in the Cu-basedlloy matrix. The increased hardness due to the addition of indiums more apparent in the Cu-alloy matrix than in the composite,resumably because of the stronger influence of tungsten carbidearticles in the composite. The hardness values of the compositeaterials are in good agreement with those reported for similar

omposites in the literature [2,8].

.3. Nano-scratch resistance

Fig. 4 presents the depth displacement charts and images ofano-scratch tests performed on the matrices without indiumFig. 4a) and with indium (Fig. 4b) under a load of 300 �N for 20ycles. The segments simply correspond to half a cycle; naturally,

he scratch depth becomes deeper with each passing segment. Theesults of the nano-scratch tests performed on the matrices withnd without indium showed that the addition of indium clearlymproved the scratch resistance, as the groove depth was smalleror the sample with indium (∼36 nm) than for the sample without

able 1roperties of the materials examined in this study.

Materials Composition of matrix (wt.%)

Annealed pure copper Pure CuCu-alloy without In Cu–15Ni–8Zn–24MnCu-alloy with In Cu–15Ni–8Zn–24Mn–2InComposite without In Cu–15Ni–8Zn–24MnComposite with In Cu–15Ni–8Zn–24Mn–2In

(c) a tungsten carbide particle. The insets show the surface appearances of the testsamples after 20 cycles, respectively showing the worn volume of ridges and groovesby the abrasive wear.

it (∼49 nm). The increase of scratch resistance is attributed againto the effect of solid-solution strengthening of indium in the Cualloy matrix. The ridge volumes on the two sides around the grooveafter the scratch test are notably distinctive, showing clear concur-rence with the generally known ploughing abrasive wear (Fig. 4).For comparison, an additional nano-scratch test was performed

on a tungsten carbide particle in the Cu–WC composite (Fig. 4c).Although the test was performed under much harsher conditions,i.e., 30 cycles at a force of 1000 �N, the resulting scratch depth wasonly ∼6 nm, which is significantly smaller than those in the Cu-alloy

Rockwell hardness (HRB)

8 ± 3.846.1 ± 1.352.1 ± 1.9

108.4 ± 0.6109.6 ± 0.6

594 E. Hong et al. / Wear 270 (2011) 591–597

0 500 1000 1500 2000 2500 30000.0

0.1

0.2

0.3

0.4

0.5

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Composite without In

Composite with In

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2.5x10-5

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Composite without In (600 m)

Composite with In (600 m)

Load (N)

Wear

rate

(g

m/m

)W

ear

rate

(g

m/m

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Sliding distance (m)

Cu alloy-62WC

(600 m)

Cu-53WC

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Pure Cu

(500 m)

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35003000250020001500100050000.0

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Composite without In

Composite with In

Applied load: 10N

a

b

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where K is the wear coefficient, L is the applied load, and S is the slid-ing distance. Despite the insufficient number of data points to drawa firm conclusion, the composites studied in this paper appeared to

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Composite with In

Vo

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Applied load: 10N

Sliding distance: 3000 m

Sliding distance (m)

ig. 5. Plot of variation in coefficient of friction with increasing sliding distance atn applied load of 10 N.

inders, as expected from its inherently higher hardness property15].

.4. Wear resistance

Shown in Fig. 5 is the frictional behaviour of the Cu alloy-ungsten carbide composites with and without indium during theirear tests. During the initial sliding distance of ∼200 m, the fric-

ional coefficient, �, had remained unstable for both composites,hich thereafter maintained nearly steady state until the termi-ation of the tests. In addition, the general frictional behaviour ofhe composites was assumed to be somewhat influenced by theiromparatively high surface roughness of 1 �m [16]. During theteady state, the average frictional coefficient value was apparentlyower for the In-doped composite than for the composite withoutt as shown in Fig. 5; the frictional coefficient value for the com-osite with In varied between ∼0.23 and 0.35 whereas it variedetween ∼0.28 and 0.41 for the composite without In. The rela-ively high frictional coefficient values for the composites at theow load of 10 N is in good agreement with no application of lubri-ating effect in the wear tests performed in this study [17]. Fig. 6(a)hows the wear rates of the Cu alloy-tungsten carbide compos-tes with a sliding distance of 600 m, along with those of pure Cund Cu-based composites with a similar sliding distance of 500 mrom Ref. [2] for comparison. Both the composites with and with-ut indium displayed much lower wear rates than the Cu–52Wnd Cu–53WC composites under similar conditions, as shown inig. 6(a). The wear rates of the current composites were one orderf magnitude lower than that of the Cu–53WC composite, dueainly to the matrix strengthening effects from the additions of15 wt.% Ni, ∼8 wt.% Zn, ∼24 wt.% Sn, and ∼2 wt.% In as well as

he higher volume fraction of the tungsten carbide reinforcementn the current study (∼62%) than that (∼53%) of Cu–53WC in Ref.2].

As expected, the wear rate increased with increasing slidingistance. The primary reason should be that some reinforced tung-ten carbide particles could not sustain but eventually fracturednd fragmented after the cyclic repetitions of loading and unload-ng during the sliding contact. The wear rates of both compositesncreased dramatically at shorter sliding distances from 300 to00 m while they increased rather monotonously at longer slid-

ng distances from 600 to 3000 m. The composite without indiumhowed a higher increasing slope than that with indium at longerliding distances, as shown in Fig. 6(b).

The effect of hardness on the wear resistance in abrasive wearonditions is often discussed using Archard’s law [18], which

Fig. 6. (a) Comparison of the wear rates of the composites with and without indiumto those of pure copper and other composites with similar compositions, as reportedin Ref. [2], and (b) wear rates of the composites with and without indium as a functionof sliding distance.

describes the inverse relationship between the wear volume loss(W) and hardness (H) as shown in Eq. (1).

W = KLS

(1)

9.1x10 9.2x10 9.3x10

Hardness-1

(HRB-1

)

Fig. 7. Plot of volume losses of the composites with and without indium as a functionof inverse Vickers hardness.

E. Hong et al. / Wear 270 (2011) 591–597 595

Fd

fic

phte[iFot(i

Fig. 9. Worn surfaces of the tungsten carbide reinforced Cu-alloy composite with

ig. 8. EPMA images of (a) tungsten carbide, (b) copper, and (c) indium. Indium isistributed uniformly in the matrix of the Cu-based alloy.

ollow the Archard’s relationship as shown in Fig. 7; the compos-te doped with indium showed a 38% lower volume loss than theomposite without indium.

The superior wear resistance of the composite with indium com-ared to the composite without it is in good agreement with itsigher scratch resistance as shown previously in Fig. 4. It is assumedhat the less initial removal of the indium-doped Cu alloy matrixventually slowed down the overall wear rate of the composite19], which may be attributed largely to the solid-solution harden-ng effect by addition of indium to the matrix of the composite [13].

urthermore, indium is known to improve wettability in the joiningf different metallic–ceramic composite systems and microelec-ronic solder joints [20–22]. Apparently from Fig. 8, the EPMAElectron Probe Micro-Analyzer) analysis however revealed thatndium was distributed uniformly in the Cu-alloy matrix and there-

indium showing (a) delamination and detachment of a tungsten carbide particle and(b) particle cracking and ductile wear deformation of Cu-alloy matrix, after a weartest at a sliding speed of 0.1 m/s and a travelled distance of 3000 m under a load of10 N.

fore the superior wear resistance of the indium-doped compositeappeared to originate primarily from the solid-solution strength-ening effect in the matrix, not from its wetting characteristics inthe interface between the matrix and reinforcement. Despite previ-ous studies of indium-doped microelectronic solder joints showingimproved wetting characteristic between the solder ball and padfinish [20–22], there was no sufficient evidence of indium seg-regation into the interfacial regions between the Cu-alloy matrixand tungsten carbide reinforcement in the present composites.Indeed, this observation is in good agreement with a direct cor-relation between the results of nano-scratch and macro-wear testsas shown in Figs. 4 and 6.

On the other hand, the overall wear behaviour of a PRMMC com-posite should be understood by considering contributions fromboth the matrix and reinforcing phases. Even with the apparentengagement of tungsten carbide reinforcement phase in the course

of wear, it is however rather difficult to determine its precise rolein the process of the overall composite wear because the interfa-cial properties between the Cu-alloy matrix and tungsten carbidephase play a significant role but are not well known. Furthermore,even different wear rates and mechanisms can also occur within the

596 E. Hong et al. / Wear 270 (2011) 591–597

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ig. 10. Schematic of all the operative wear mechanisms observed in this study, iloughing of Cu-alloy matrix.

ungsten carbide reinforcement phase depending on the differentrystallographic directions [23].

According to the literature and experimental observation, theverall wear behaviour of both composites appeared to be some-hat associated with the delamination wear mechanism, which

s generally defined as the detachment of reinforcement particlesn the form of sheets or flakes due to sub-surface crack propaga-ion along the sliding direction [24,25]. In particular, delaminationear is known to be a dominant mechanism in PRMMC at inter-ediate to high loads as in this study, and is generally observed

y the presence of scratches on the worn surfaces, and crackingnd detachment of reinforced particles [25,26], as shown in Fig. 9a.ore importantly, the overall wear behaviour of both composites

ppeared to be further associated with severe plastic deformationy ploughing and ductile flow of Cu-alloy matrix as is often reporteds a major wear mechanism for metallic materials [27] and is alsovidenced in Figs. 4 and 9b, which is in the latter stage of wearindered by the much harder tungsten carbide phase. While theungsten carbide phase is highly resistant to shear localization, theynally crack, fragmentize, and fracture as shown in Fig. 9b [5,16].onsidering the interface between the Cu-alloy matrix and tung-ten carbide phase of Cu-alloy/WCp composites does not appear toe particularly weak, the combination of ploughing wear in metallicatrix and brittle fracture in ceramic reinforcement should be theajor wear mechanism of Cu-alloy/WCp composites. Aforemen-

ioned wear mechanisms that are operative in this study are alsohown schematically in Fig. 10.

Furthermore, in the absence of any experimental evidence, it isarefully assumed that the effect of oxidative wear should be min-mal in pure copper or Cu-based alloys and instead, the most wearccurred due primarily to the mechanical damage in our materials,nlike highly reactive metals such as titanium in which case theormation of TiO2 on the worn surface can influence the frictionalehaviour of the titanium [17,27].

. Conclusions

Using a pressureless infiltration technique, composites con-isting of copper alloy-based matrix and tungsten carbideeinforcement with and without indium were manufactured. Theollowing conclusions can be drawn from this study:

. Microstructural analysis revealed a uniform distribution oftungsten particles in the Cu-alloy matrix with no cracks ordelamination at the interface between the particles and matrix,indicating good bonding between the matrix and reinforcement.Nano-scratch and pin-on-disc wear tests were performed toclarify the correlation between the nano/micro-scale and macro-scale wear behaviours.

. The addition of indium resulted in increases in the Rockwellhardness of the Cu-alloy matrix and composite. Furthermore, the

nano-scratch and wear tests showed that the addition of indiumenhanced the nano-scratch and wear resistances of the Cu-alloymatrix and the composite, respectively.

. The nano-scratch test showed that the addition of indiumnotably enhanced the wear resistance and reduced the amount

[

[

[

ng delamination/pull-out and cracking/fracture of tungsten carbide particles, and

of ploughing wear on Cu-alloy matrix. The addition of indiumalso enhanced the macro-wear, mainly because of the uniformindium dissolution in the Cu-alloy matrix, confirmed by EPMAanalysis.

4. The wear rates of the composites increased with increasingsliding distance. The wear rates of both composites increaseddramatically at shorter sliding distances from 300 to 600 m,whereas they increased monotonously at longer sliding dis-tances from 600 to 3000 m. The composite without indiumshowed the higher coefficient of friction and wear rates than thecomposite with indium, particularly at higher sliding distances.

5. The major wear mechanism is considered to be ploughing wearin Cu-alloy matrix and fracture/fragmentation of tungsten car-bide particles. Some degree of delamination wear was alsoobserved by particle pull-out and cracking/detachment on theworn surfaces of the specimens.

Acknowledgements

This research was supported by the International Research &Development Program of the National Research Foundation ofKorea (NRF) funded by the Ministry of Education, Science and Tech-nology (MEST) of Korea (Grant number: 2007-00717). Authors arethankful to Prof. Wayne D. Kaplan at Technion University in Israelfor useful discussion and manuscript review. HC also acknowledgespartial support from the Priority Research Centers Program throughthe National Research Foundation of Korea (NRF) funded by theMinistry of Education, Science and Technology (2009-0093814).

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