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Wear behaviour of thermally sprayed ceramic oxide coatings
Giovanni Bolelli, Valeria Cannillo, Luca Lusvarghi ∗ , Tiziano Manfredini
Dipartimento di Ingegneria dei Materiali e dell’Ambiente, Universit` di Modena e Reggio Emilia, Via Vignolese 905, 41100 Modena, MO, Italy a Received 6 July 2005; received in revised form 9 February 2006; accepted 10 March 2006 Available online 18 April 2006
Abstract The wear resistance of plasma-sprayed ceramic coatings (Al2 O3 , Al2 O3 –13%TiO2 , Cr2 O3 ) has been investigated through pin-on-disk and dry sand-steel wheel tests, has been correlated to microstructural and micromechanical characteristics (microhardness, fracture toughness) and has been compared to well-known platings (such as Cr electroplating and electroless Ni) and HVOF-sprayed cermets (WC–17%Co, WC–10%Co–4%Cr). Plasma-sprayed ceramics are hard but brittle: dry particles abrasion occurs through splats detachment. The toughest coating (Al2 O3 ) displays the highest wear resistance, which in fact overcomes HVOF-sprayed cermets and Cr electroplating, when a low number of wheel revolutions are considered. In pin-on-disk tests, no coating undergoes wear loss against the 100Cr6 ball, that possess lower hardness. Against the alumina ball, Al2 O3 and Al2 O3 –TiO2 coatings show high wear rates and friction coefﬁcients (due to chemical afﬁnity), while Cr2 O3 possesses better wear resistance, lower friction coefﬁcient and inﬂicts less wear on the counterpart. Cr2 O3 wear scar consists in plastically deformed splats and debris forming a quite adherent protective triboﬁlm. © 2006 Elsevier B.V. All rights reserved.
Keywords: Sliding wear; Abrasive wear; Plasma spraying; Ceramic coatings; Friction coefﬁcient
1. Introduction Thermal spraying is often considered as a potential alternative to traditional coating manufacturing techniques (such as hard chrome electroplating) for the production of wear-resistant coatings [1–4]. In fact, a large variety of hard materials (including ceramics and cermets) can be deposited on a cold (or moderately pre-heated) substrate [5,6], thus obtaining very hard coatings while preventing thermal alteration of the substrate itself (which invariably occurs in other hardfacing processes, such as in welding processes), which is a key requirement when design tolerances must be satisﬁed, thin-walled components are being considered, or heat-sensitive materials (like Al and Mg alloys) are being processed. Among the various thermal spraying techniques, plasmaspraying and HVOF-spraying are the most suitable for the production of high-quality wear resistant coatings and they are both technologically mature processes. HVOF was developed to overcome plasma-spraying limits: it is well known that HVOFspraying gives far superior results than plasma-spraying when
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manufacturing cermet coatings, because of the much higher gas jet velocity and lower ﬂame temperature resulting in coatings with extremely low porosity, low splats oxidation and low carbide decomposition and/or dissolution ; in fact, many experimental work concerning HVOF-sprayed cermet coatings tested under various conditions exist [8–13]. However, HVOF has its own limits: it produces high quality metallic alloy and cermet coatings, but these powders are difﬁcult to prepare and very expensive. HVOF sprayed ceramic oxide coatings are still under investigation, but they are not widely used yet, because they must be tested and can be deposited just with few of the commercial torches [14,15]. Thus, plasma spraying is still the most widespread production technique for ceramic coatings, like Al2 O3 , Cr2 O3 . Such coatings are more porous and brittle than HVOF-sprayed cermets, because of intrinsic porosity of plasma-sprayed coatings due to lower particles in-ﬂight velocity and quenching-induced microcracking in the ceramic splats [6,16]. Anyway, they possess very high hardness, due to their purely ceramic nature, they are almost insensitive to many corrosive environments and can stand high temperatures . Thus, if the involved application does not require a liquid tight coating, but just wear resistance, plasma-sprayed ceramic oxide coatings can be a good solution. Besides, manufacturing of atmospheric plasma-sprayed ceramic coatings can be less
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P.0 software).. wear maps should be experimentally obtained. Fracture toughness was determined on thermally sprayed coatings by high-load. 2. Bolelli et al. Image analysis was also performed on SEM images to determine coating porosity (UTHSCSA Image Tool v. Cu K radiation). since such coatings have been studied for a long time [23–27]. The latter was supplied in the “as-plated” state. The crystalline phases of all the three ceramic oxide powders have been studied with X-rays diffraction (XRD. Philips XL30) on polished cross-sections (mounted in resin. For example. even though exceptions may exist and deposition efﬁciency is also a concern. with a NiCoCrAlY (powder: Sulzer-Metco 461NS. The plasma sprayed coatings microstructure was determined by XRD and by scanning electronic microscopy (SEM. have been manufactured onto C40 steel plates (100 mm × 100 mm × 5 mm).5 slpm Cr2 O3 105 Ar. The substrates were grit-blasted with 500 m alumina grits (SulzerMetco Metcolite-C) in a vacuum-operated blasting machine (Norblast) prior to coating deposition. Therefore. many industrial processes make use of plasma-sprayed ceramic coatings. agglomerated and Table 1 Plasma spraying operating parameters Parameters Spray distance (mm) Cooling gas type and pressure Plasma gases ﬂow rates Current (A) × voltage (V) = power (kW) Feeding disk revolution speed (rpm) Carrier gas type and ﬂow Al2 O3 105 Ar. 8 bar Ar: 50 slpm H2 : 15 slpm 560 × 69 = 38. ground with 400. 3. The spraying parama eters for plasma-sprayed oxides are listed in Table 1.85 12 Ar.G. Roma. namely WC–17%Co (powder: Tafa 1343. which could represent an economical alternative to HVOFsprayed cermets in some industrial applications. whose reproducibility is good once the optimal set of parameters has been found. Plasma-sprayed coatings were manufactured with a Sulzer-Metco F4-MB plasma torch. as a ﬁrst step towards wear mapping of such materials. the aim of this study is both to provide an experimental assessment of the wear rates.55 15 Ar. 1000. determining the Ra and Rz parameters (UNI ISO 4287-1). operated in Air Plasma Spraying (APS) mode in a C. Italy).A. however.5 slpm Bond coat 105 Ar. 800. the food and medicine packaging industry does not only need wear resistance. wear mechanisms. HVOF-sprayed cermets and metal platings under various wear conditions. there exist a few works comparing them to the characteristics of other thermally sprayed coatings as well as to other industrially widespread wear resistant coatings. Switzerland). co-shared with Universit` la Sapienza. a thorough study of the wear resistance of thermally sprayed coatings must involve plasma-sprayed ceramics. Roughness measurement was performed by optical proﬁlometry (ConScan proﬁlometer. such as hard chrome electroplating and nickel electroless plating [28.A. without thermal treatment: a heat treatment (5 ◦ C/min heating. 8 bar Ar: 50 slpm H2 : 13 slpm 690 × 65 = 44. agglomerated and sintered) and WC–10%Co–4%Cr (powder: Sulzer Metco 5847. plant (Centro Sviluppo Materiali S. Both Cr electroplatings (on ground substrates) and Ni–P electroless platings (on micro-grit blasted substrates) were industrially manufactured by proprietary processes. 3. −45 + 15 m. but also the absence of heavy metals contamination: Al2 O3 and Al2 O3 –TiO2 are often used for this reason in that ﬁeld. fracture toughness and elastic modulus on coatings polished cross-sections.5 m polycrystalline diamond paste). plasma-sprayed hard ceramic coatings are still studied nowadays [20–22]. 15 s loading time) from SEM micrographs. and of plasma sprayed oxides in particular. A depth-sensing Vickers microindenter (CSM Instruments. as it is currently being done for massive sintered ceramics [30–32].S. −53 + 11 m. namely Al2 O3 (powder: Sulzer-Metco 105SFP. The treatment conditions were chosen following literature indications in order to achieve the highest possible hardness increase through precipitation of nanostructured Ni–P crystals .19]. Much research related to the basic wear mechanisms of plasma-sprayed oxides exists. cracked Vickers microindentations produced with 10 N load (5 N for Al2 O3 –13%TiO2 due to its lower hardness and toughness). in particular under dry sliding conditions and under dry particles abrasion conditions. Italy. Therefore.44 12 Ar. 400 ◦ C treatment temperature for 1h. Furthermore. measuring the indentation diagonals and crack lengths from SEM micrographs and employing the Al2 O3 –13%TiO2 105 Ar. −31 + 3. 3.p. Switzerland) was employed to measure Vickers microhardness. 2. since powder and processing costs are often lower [18.64 10 Ar. Vickers microhardness was calculated on all coatings by measuring the indentations diagonals (1 N load. Al2 O3 – 13%TiO2 (powder: Sulzer-Metco 130. 2000 mesh SiC papers and polished with 3 and 0. Hard chrome electroplating and Ni–14%P electroless plating on C40 steel have also been studied for reference. friction coefﬁcients of various plasma-sprayed ceramic coatings under different sliding wear conditions through pin-on-disk testing. to fully assess the industrial applicability of thermally sprayed coatings. while spraying runs of cermet coatings have been described elsewhere . / Wear 261 (2006) 1298–1315 1299 expensive than HVOF-sprayed cermets in many applications. −15 + 5 m). 2. Materials and characterizations Three plasma-sprayed ceramic coatings. Therefore. slow cooling inside the kiln) was performed on some of the samples (hereafter referred to as Ni–P tt).7 slpm . −53 + 15 m) and Cr2 O3 (powder: Saint-Gobain #3033. −150 + 22 m) bond coat to improve adhesion. 8 bar Ar: 45 slpm H2 : 15 slpm 650 × 67 = 43.29]. Roma.5 slpm sintered). Philips PW3710.5 m). CSM Instruments. 8 bar Ar: 50 slpm H2 : 15 slpm 580 × 68 = 39. and to compare the performance of plasma-sprayed ceramic coatings. Therefore. and two HVOF-sprayed cermet ones.
3 Test 4 0. the wear rate of the ball was determined by measuring the worn cap diameter with an optical microscope and the wear rate of the sample was determined by measuring the area of the wear track cross-section by optical proﬁlometry (ConScan proﬁlometer.2 N normal load (Ceramic Instruments AP/87 abrasimeter).3 Test 2 0. Even if the formula has been developed for “halfpenny-shaped” cracks.23 Test 7 0.1 mm diameter Fe360A steel wheel rotating at 75 rpm.1 250 1 Alumina 380 0. the limitation for the use of this formula is that the ratio between the crack and the half diagonal length must be between 0.2 250 5 100Cr6 210 0. 4 N/min unloading rate.5a/c) (2. This condition has been veriﬁed in all the tests.3 Test 6 0. and applying a 40. A minimum of 20 indentations was performed for each hardness.2 250 1 Alumina 380 0. and P is the load (mN). Dry particles abrasion resistance was tested on all thermally sprayed coatings in their “as-sprayed” conditions and on “as-plated” hard chrome for reference (the measurement was not performed on Ni plating due to its low thickness causing the substrate to be quickly exposed) by a simple dry sand-steel wheel test. the friction coefﬁcient was measured on-line by the instrument. by the Oliver–Pharr formula . c the crack length ( m).1 250 1 100Cr6 210 0.5. Switzerland: each area value is the average of four measurements) and calculating the resulting wear volume. Plates are ﬁxed onto a rotating disk: the ball is ﬁxed into a steady ball holder pressed against the sample surface with a normal load (rotating unidirectional sliding). This test is a modiﬁed version of ASTM G65. / Wear 261 (2006) 1298–1315 Test 3 0. it has been demonstrated that it is valid also for Palmqvist cracks .23 for all ceramics and 0.1) where KIC = MPa m0. Ni–P) and cermets. Elastic modulus was determined on all coatings from the unloading part of instrumented indentation loading-unloading curves.5 . Bolelli et al. CSM Instruments. 15 s loading time.2 250 5 Alumina 380 0. Ball-on-disk dry sliding tests were performed with a pin-ondisk tribometer (CSM Instruments. toughness and elastic modulus measurement.1 250 5 Alumina 380 0. the normal load and the counterpart material. FEPA 80 alumina grains (180 m average particle diameter) as abrasive medium with a 1 g/lap mass ﬂux. a 5 N indentation load was chosen. All tests (from tests 1 to 8) were performed on plasma-sprayed ceramic coatings (Table 3): these data will provide important information on wear mechanisms and will serve as a basis for wear mapping of such coatings. with 5 N/min loading rate.3 for metals (Cr. Following preliminary tests (which highlighted some effect of the indentation load on the elastic modulus value.1300 Table 2 pin on disk testing conditions Test 1 Sliding speed (m/s) Sliding distance (m) Normal load (N) Pin material E (GPa) ν 0. especially for plasma-sprayed ceramics).3 Test 8 0.23 G.079(P/a3/2 ) log(4. a the half diagonal of the indentation ( m). The employment of this formula can already be found in literature for plasma spray ceramic coatings  and HVOF cermets . with the main differences consisting in the use of steel wheel instead of a rubber wheel and of corundum in place of Ottawa sand. using Table 3 Pin on disk testing plan (EHC = electrolytic hard chrome) Test 1 As-sprayed Al2 O3 As-sprayed Al2 O3 –TiO2 As-sprayed Cr2 O3 As-sprayed WC–Co As-sprayed WC–Co–Cr As-plated EHC As-plated Ni–P As-plated Ni–P tt Polished Al2 O3 Polished Al2 O3 –TiO2 Polished Cr2 O3 Polished WC–Co Polished EHC × × × Test 2 × × × Test 3 × × × × × × × × a 200.23 Evans–Wilshaw formula : KIC = 0. As reported in literature . The parameters of the various tests (labelled tests 1–8) are listed in Table 2. radius = 3 mm) on (22 mm × 22 mm × 5 mm) coated plates obtained by cutting the (100 mm × 100 mm × 5 mm) plates. varying the sliding speed. For each test. Eight different parameter sets have employed. Switzerland) using 100Cr6 balls (manufacturer’s nominal hardness: 7 GPa. A reduced set of Test 4 × × × × × × × × Test 5 × × × Test 6 × × × Test 7 × × × × × × × × × × × × × Test 8 × × × × × × × × × × × × × .23 Test 5 0. radius = 3mm) and sintered alumina balls (manufacturer’s nominal hardness: 19 GPa.6 and 4. The Poisson’s ratio (required for elastic modulus calculation) was assumed to be 0.2 250 1 100Cr6 210 0.1 250 5 100Cr6 210 0.
while Cr electroplating and HVOF-sprayed cermets chemical and microstructural characteristics have already been described elsewhere . To assess the effect of surface ﬁnishing on the friction and wear behaviour. 1B). 7. 4. 1A). tests 7 and 8 have also been performed on polished plasmasprayed ceramics. Unmolten alumina particles can also be found due to the coarser average particle size of this powder. 3. Obvious microstructural differences appear between the various plasmasprayed ceramic coatings. Table 3): they provide a good amount of data to evaluate the cermets sliding behaviour and are of use as reference values to compare the different performances. they cause splat-stacking faults. . In Al2 O3 –TiO2 . The porosity is still about 6%. in fact. 1A–F describe the microstructures of plasma-sprayed ceramic coatings. These tribological samples were. No glass phase was present in any powder. the alumina one mainly consists in -Al2 O3 Fig. TiO2 was well melted and partly mixed with alumina. notwithstanding the better intersplat adhesion. since SEM micrographs highlight lamellar areas containing different amounts of titania. HVOF-sprayed WC–17%Co and electrolytic hard chrome (Table 3). gas entrapment and unmolten particles. alumina powder in Al2 O3 and alumina–titania powder in -Al2 O3 and anatase. (A and B) Plasma-sprayed Cr2 O3 + NiCoCrAlY bond coat. / Wear 261 (2006) 1298–1315 1301 tests was performed on cermets and on other platings (namely test 3. Microstructure and micromechanical properties SEM micrographs in Fig. laboratory polished using diamond abrasive papers with progressively smaller diamond particles. intersplat adhesion is better than the former coatings. From XRD. the porosity of this coating is the highest among the presently tested ceramic coatings (about 9%). due to these defects.G.1. 8. Thus. The XRD qualitative analysis of the starting powders showed that the chromia powder fully consisted in eskolaite phase (Cr2 O3 ). due to more rounded pores produced by unmolten particles. The overall coating porosity from image analysis is quite low (about 6%): the employment of powder particles with small average grain diameter reduces the average size of pores due to splats stacking faults. Results 3. the chromia coating consists in eskolaite. Therefore.e. down to 2 m. 1. (C and D) plasma-sprayed Al2 O3 + NiCoCrAlY bond coat. (E and F) plasma-sprayed Al2 O3 –13%TiO2 + NiCoCrAlY bond coat. Bolelli et al. the interlamellar cohesion appears higher. splats stacking faults and gas entrapment. while almost no unmolten particles are found (Fig. In Al2 O3 (Fig. but many vertical microcracks are present. titanium dioxide low temperature phase. SEM micrographs of coatings cross-sections. Cr2 O3 markedly exhibits a lamellar microstructure with a prevalence of elongated interlamellar pores. i.
050 0. The alumina–titania coating seems to be the most isotropic among all tested coatings.03 12. Cracked Vickers microindentations are shown in Fig. While for ceramic coatings the wear rate remains quite constant independently of the number of disk revolutions.961 0. i. it can be noticed that electrolytic hard chrome and HVOF-sprayed WC–Co rank similarly in this test.67 4. Bolelli et al. Comparing the observed wear rates for the various coatings. due to their high hardness. while Al2 O3 –TiO2 and Cr2 O3 are less tough. while Fig. Ni–P has poor hardness in the as-deposited con- dition.52 11.1302 G.77 ± 0. while electrolytic hard chrome possesses much lower roughness . 2.917 ± – 0. Al2 O3 possesses the best fracture toughness among plasma-sprayed ceramics.50 3.46 Not measurable (ill-shaped microcracks)  Not measurable (coating too thin) Not measurable (coating too thin) E (GPa) 184 141 185 255 257 188 ± ± ± ± ± ± 6 7 13 9 16 8 Ra ( m) 5. do not undergo signiﬁcant plastic deformation-related Fig.65 1. 4 compares the wear rate of plasma-sprayed alumina and of HVOF-sprayed WC–Co cermet as a function of number of disk revolutions. such coatings behave better than plasma-sprayed ceramics.07 ± 0.18 12. both because of the intrinsically lower hardness of -Al2 O3 than -Al2 O3 and because the indentation response of a plasma-sprayed material is governed not only by the intrinsic hardness of the material.66 ± 0.20 KIC (MPa m1/2 ) 2. for alumina and chromia thermally sprayed coatings.547 0.31 Same as Ni–P Rz ( m) ground 2.41 ± 0. R = rutile (TiO2 ). elastic modulus (Oliver–Pharr formula). HVOF-sprayed cermets and electroless Ni–P plating is quite similar.28 3. with similar microcracks propagating both parallel and transverse to the substrate (Fig. 4.121 ± 0.518 ± 0.099 ± 0.66 12. 5.26 ± 1. contributing to the formation of a low melting point glassy phase.036 0. Wear scar analysis also indicates that plasma-sprayed ceramics (in particular Al2 O3 and Cr2 O3 ). X-ray pattern of alumina–titania plasma spray coating.41 0. The roughness of plasma-sprayed Cr2 O3 . = -Al2 O3 . for hard chrome plating and HVOF-sprayed cermets there is a clearly decreasing trend. The abovementioned phenomenon is typical also of HVOF coatings.36 ± 1.70 8.75 ± 0. as a conﬁrmation to the above observations. elastic moduli and roughness parameters of the tested coatings are listed in Table 4. with WC–Co–Cr (the less tough among tested cermets) performing worse.080 ± 0. glassy phase (Fig. but at a low number of revolutions. as SEM micrographs suggested.e.00 ± 0. Cr2 O3 is the hardest of all tested coatings. which is probably responsible for the better intersplat cohesion.57 ± 0. see black arrow) and a minor amount of rutile. where SEM micrographs had already highlighted a low intersplat cohesion.047 0. 2.33 ± 2.45 GPa ).45 1. Al2 O3 has similar hardness to WC–Co.42 ± ± ± ± ± ± 1.967 ± 2.52 ± 0.87 15.102 ± 0.105 ± 0.47 3. being much lower than that of Al2 O3 –TiO2 and Cr2 O3 . but also by the lamellar microstructure. Cermets are much tougher than plasma-sprayed ceramics.25 ± 0.29 1.58 8. which is better highlighted in Fig. oxide ceramics perform deﬁnitely better. indentation fracture toughness.435 ± 2. The wear scar on plasma-sprayed alumina is shown in Fig. The effect of the thermal treatment on electroless Ni is immediately obvious from the huge microhardness increase.16 10. along splat boundaries. This is particularly evident for Cr2 O3 . Ra.29 3.70 30.46 ± 4.055 0.348 0.60 ± 1. The black arrow indicate the broad band caused by the presence of a glassy phase. due to the two-phase nanocrystalline structure.26 0. Electroplated chrome is less hard than all thermally sprayed coatings except for Al2 O3 –TiO2 .51 3. Dry particles abrasion resistance The dry sand-steel wheel test results are listed in Table 5.17 ± 0. crack preferentially propagate parallel to the substrate interface.087 ± – 0.24 Same as Ni–P Ra ( m) ground 0.113 2. with minor quantities of -Al2 O3 and glassy phase.60 ± 1. = -Al2 O3 . the alumina–titania consists mainly in -Al2 O3 with some -Al2 O3 . 3.389 0.70 1. with splat boundaries giving off under load to facilitate the indenter accommodation .62 9.775 ± 0. The very low amount of crystalline TiO2 indicates that it mostly dissolves in molten Al2 O3 . .76 ± 0.71 11. The hardness.46 0.2. but is deﬁnitely improved after the thermal treatment. Both wear volume (mm3 ) and wear rate (mm3 /Nm) for increasing number of steel wheel revolutions have been included. The microhardness of Al2 O3 is lower than that of bulk alumina (HV = 20. 3C). / Wear 261 (2006) 1298–1315 Table 4 Vickers microhardness. 3A–C for plasma-sprayed ceramics: it can be seen that.34 0. Rz for all tested coatings HV1N (GPa) Al2 O3 Al2 O3 –TiO2 Cr2 O3 WC–Co WC–Co–Cr Hard Cr 11.286 Ni–P Ni–P tt 5. Al2 O3 . At a high number of disk revolutions.02 ± 0.09 224 ± 21 184 ± 6 – – – – (due to splats quenching). The labels are the following: = -Al2 O3 . while WC–Co-Cr is slightly less hard.30 ± 0.67 ± 0. It should be noticed that plasmasprayed ceramic coatings have different roughness: roughness seems to be increasing with increasing powder average particle size. fracture toughness.033 Rz ( m) 18.82 8. with the wear rate of the toughest one.
the pin gets progressively worn. maximum sub-superﬁcial shear stress and maximum shear stress depth are all reported in Table 6.20 ± 0.15 21. without any signiﬁcant involvement of the substrate and the coating-substrate interface. E = 380 GPa. even though tested coatings have different thicknesses. Most importantly.97 ± 0.07 38.04 13.76 ± 0.38 10.07 10. as former indentation tests clearly showed.46 ± 1.22 8.24 11.72 ± 0.34 ± 0. SEM micrographs of high-load. which are the weakest link in the material. using the experimentally evaluated elastic moduli in Table 4 for the samples and assuming E = 210 GPa.48 ± 0.64 15.01 8.82 ± 0.64 24.50 14. ν = 0.14 ± 1.02 8.24 ± 1.61 ± 0.15 ± 2. It can be noticed that differences between contact pressures and contact stresses in the various coatings arise due to the different elastic moduli.65 27. the actual contact area increases and the contact pressure consequently decreases.81 ± 0. (A) Plasma-sprayed Cr2 O3 + bond coat.14 Not calculated WC–10%Co–4%Cr 6.17 Not calculated Hard Cr 3.23 for sintered alumina.46 ± 0. cracked Vickers microindentations used for fracture toughness measurement.03 ± 0. the highest shear stress differences being about 25% between WC–Co–Cr and Al2 O3 –TiO2 . (B) plasma-sprayed Al2 O3 + bond coat.96 10. cracks mostly propagate through splat boundaries.65 10.96 ± 1.38 13.73 13.16 9.37 ± 1.18 13.02 ± 0.87 21.3 for 100Cr6 steel.33 16. pin-on-disk test results can be compared. Thus.88 14.88 ± 1.29 20.82 ± 0.70 ± 0. Bolelli et al.79 ± 0.73 ± 1. however..27 5.07 Not calculated .43 ± 0.G. The pin-on- Table 5 wear volumes (mm3 ) and wear rates (×10−3 mm3/Nm) recorded in dry sand-steel wheel abrasion test Test/sample 7 revolutions Wear volume Wear rate 40 revolutions Wear volume Wear rate 60 revolutions Wear volume Wear rate 80 revolutions Wear volume Wear rate Average wear rate Al2 O3 2.35 8. 3. they have been computed from analytical Hertz’s formulae.13 5.11 10.01 10.26 ± 3.02 9. Pin-on-disk wear test Hertzian maximum and average contact pressures.37 ± 0.47 12.93 ± 2.47 ± 1. as the test progresses. / Wear 261 (2006) 1298–1315 1303 Fig.36 ± 0. (C) plasma-sprayed Al2 O3 –13%TiO2 + bond coat.17 5.50 10.26 ± 1.12 ± 0.50 ± 0.04 15.37 ± 0.44 ± 0. Clearly.06 ± 0.12 WC–17%Co 4. 3.3.96 14. the maximum shear stresses always occur within the coating. they always remain the same order of magnitude.85 ± 0. ν = 0.19 ± 0. in fact.01 6.52 ± 0.08 ± 2.47 Cr2 O3 Not measured because the wear rate stays constant 16.63 ± 0.29 Al2 O3 –TiO2 Not measured because the wear rate stays constant 14.30 ± 0.65 ± 1.87 16. phenomena (such as microcutting and microploughing): their only relevant wear mechanism is brittle fracture. such stresses are valid in a static contact condition.82 7.52 ± 1.27 ± 0. in the same test.28 ± 0. which make the contact more severe.22 7.09 ± 1.85 22.01 24.74 ± 1.58 14. and in particular. It must be considered that hertzian stresses and pressures are only valid at the beginning of the test. but do not take into account additional stresses due to friction.
6 Test 3–7: 799. 6A as a negative value of the wear rate.8 Test 2–6: 13.1304 G.9 Test 3–7: 1076.6 Test 4–8: 1430.0 Test 4–8: 956. and depth of the point of maximum shear stress.0 Test 4–8: 1357.2 Test 1–5: 560.7 Test 2–6: 421.4 Test 3–7: 707.8 Test 1–5: 620. 6C (average friction coefﬁcients).9 Test 4–8: 839. The alumina pin undergoes lower wear rates (≈10−6 mm3 /Nm) when sliding against Cr2 O3 as well.5 Test 1–5: 14.5 Test 1–5: 373.4 Test 4–8: 831. SEM micrograph of dry sand-steel wheel wear scar on plasma-sprayed Al2 O3 . The SEM micrographs of wear scars of plasma-sprayed coatings tested (test 7) against 100Cr6 (Fig.4 Test 3–7: 1198.9 Test 4–8: 817.7 Test 3–7: 709.4 Test 3–7: 329.4 Test 2–6: 632.8 Test 4–8: 380.4 Test 4–8: 420.2 Test 1–5: 13.5 Test 4–8: 20.8 Test 3–7: 329.9 Test 4–8: 21. for all pin-on-disk test conﬁgurations Maximum hertzian contact pressure (MPa) Al2 O3 Test 2–6: 716. The occurrence of material build-up is indicated in Fig.5 Test 4–8: 1434.6 Test 4–8: 1228.0 Test 2–6: 12. The Cr2 O3 coating causes much less wear on the steel pin (subsequently undergoing much less material transfer from the pin) and displays lower friction coefﬁcients.5 Test 1–5: 173.4 Test 4–8: 20.7 Test 4–8: 19.6 Test 3–7: 21.8 Test 1–5: 622. proof of the brittle detachment of nearby splats.1 Test 2–6: 196.9 Test 4–8: 721.1 Test 3–7: 767.7 Test 3–7: 639.9 Test 3–7: 356.2 Test 4–8: 380. 7B for Cr2 O3 ) conﬁrm that.5 Test 3–7: 800.0 Test 3–7: 24.2 Test 1–5: 414. Overall.0 Test 3–7: 1063.9 Test 4–8: 1225.6 Test 3–7: 1151.4 Test 4–8: 19.8 Test 3–7: 297.4 Test 4–8: 21.1 Test 4–8: 1247.6 Al2 O3 –TiO2 Cr2 O3 WC–Co WC–Co–Cr Cr Ni–P Ni–P tt .1 Test 4–8: 819.6 Test 3–7: 21.8 Test 3–7: 1085.4 Test 4–8: 905.8 Test 3–7: 1201. Black arrows indicate some particularly evident splats. the wear rate against Cr2 O3 never exceeds 10−5 mm3 /Nm.9 Test 3–7: 723.8 Test 3–7: 372. / Wear 261 (2006) 1298–1315 Fig. Bolelli et al.2 Test 4–8: 335.5 Test 3–7: 958. 7A for Al2 O. Fig.8 Test 4–8: 386. Cr2 O3 coating outperforms other plasma-sprayed ceramics in the pin-on-disk test.5 Test 4–8: 444.9 Test 1–5: 192.9 Maximum hertzian shear stress (MPa) Test 2–6: 222.2 Test 1–5: 13.8 Average hertzian contact pressure (MPa) Test 2–6: 477.1 Test 4–8: 953. Al2 O3 and WC–Co wear rates in dry sand-steel wheel tests as a function of number of disks revolutions. maximum sub-superﬁcial shear stress.2 Test 1–5: 413. during Table 6 Hertzian maximum and average contact pressures. Fig. The wear rate of the steel pin against alumina and alumina–titania is 2–10 times higher than that against chromia in all cases (except for Al2 O3 –TiO2 in test 7). 6B (pin wear rate) and Fig. 6A (sample wear rate). 5.1 Test 2–6: 222.4 Test 4–8: 21. concerning both wear rates (undergone and inﬂicted on pins) and friction coefﬁcients.4 Test 4–8: 1259. 4.3 Test 3–7: 22.4 Test 3–7: 371.5 Test 3–7: 336.8 Test 3–7: 1061.4 Test 2–6: 718.8 Test 3–7: 333.4 Test 4–8: 390. Material build-up on the coatings surface is recorded on all samples when tested against 100Cr6 due to steel debris transfer from pin to sample. while the pin undergoes signiﬁcant material loss.0 Test 3–7: 22. disk results for plasma-sprayed coatings are shown in Fig.0 Test 1–5: 192.0 Test 2–6: 479. Fig.9 Test 3–7: 22.9 Test 3–7: 717.7 Test 4–8: 443.2 Test 4–8: 22.1 Test 3–7: 21.3 Test 3–7: 22.8 Maximum shear stress depth ( m) Test 2–6: 12.9 Test 4–8: 1082.
with pin penetration inside the coating. Alumina. 7. instead. 8A–C). besides. some plastically deformed wear debris adheres to the pin. (A) Coatings wear rates. Optical micrographs of pin wear scars are in Fig. 7. which seems to possess low compactness (Fig. SEM micrographs of wear scars on plasma-sprayed Al2 O3 (A) and Cr2 O3 (B) after test no. While Al2 O3 has undergone signiﬁcant material loss. 11A and B represent three-dimensional axonometric projections of wear scars on Al2 O3 and Cr2 O3 after test no. the triboﬁlm on Cr2 O3 is smoother than the original surface and is placed slightly above the mean line of the unworn surface. On Al2 O3 and Al2 O3 –TiO2 coatings (Fig. a triboﬁlm is formed (Fig. (C) friction coefﬁcients. besides plastically deformed splats. 10. consisting in plastically deformed debris from both sample and pin. reproduced from the optical proﬁlometry results. 8A and B). 9C and D). which were also plastically deformed and strongly embedded in this ﬁlm. / Wear 261 (2006) 1298–1315 1305 Fig. and also in plastically deformed ceramic splats (Fig. HVOF-sprayed coatings exhibit an Fig. 9A–D). . When ceramic coatings are tested against alumina pins. They high- light that the steel sample mostly suffered two-body grooving (ploughing and cutting) but also some adhesive wear. some steel debris is transferred to the coatings. the surface ﬁlm is much more compact and smooth in all cases (Fig. which undergoes grooving. with some alumina debris. On Cr2 O3 . Pin-on-disk test results for plasma-sprayed coatings. lot of plastically deformed debris appears in the surface ﬁlm. forming an irregular surface ﬁlm. 8C): it mostly consists in plastically deformed debris and splats (Fig. indicating transferring of steel debris on the coating surface. 8. the test. Negative wear rates indicate material build-up on coating surface due to wear debris sticking. 9A and B). Table 7 sums up the wear rates of all tested samples in the pin on disk wear test. mostly undergoes brittle fracture. 6. Fig.G. (B) pin wear rates. Bolelli et al.
9. 8. Details of wear scars on plasma-sprayed ceramic coatings after testing against alumina pins. test no. Al2 O3 –13%TiO2 (B) and Cr2 O3 (C) after test no. thermally treated Ni–P undergoes a negligible wear rate in all tests. material build-up is recorded from optical proﬁlometry. test no. showing the formation of triboﬁlms. its wear rate becomes negligible in test no. HVOF-sprayed cermets. Remarkably. (A) Plasma-sprayed Al2 O3 . excellent sliding wear resistance: they never undergo a measurable volume loss. . 6. 8. it undergoes very high wear rates both against alumina and against 100Cr6.1306 G. The reasons for this behaviour will be discussed in the following section. / Wear 261 (2006) 1298–1315 Fig. Cr electroplating and Ni–P electroless Fig. white arrows indicate plastically deformed splats. (B) plasma-sprayed Al2 O3 –13%TiO2 . 8. Electrolytic hard chrome displays unfavourable wear and friction characteristics when compared to plasma-sprayed Cr2 O3 and HVOF-sprayed cermets: when tested against sintered alumina. test no. (C and D) plasma-sprayed Cr2 O3 . However. with the appearance of undeformed splats under the triboﬁlm. 12A and B respectively compare pin wear rates and average friction coefﬁcients for plasma-sprayed ceramic coatings. being less hard than steel. SEM micrographs of wear scars on plasma-sprayed Al2 O3 (A). Sometimes. Their performance is therefore comparable to Cr2 O3 . Bolelli et al. Fig. 8. 8. Without thermal treatment. it undergoes a signiﬁcant wear rate (but lower than Al2 O3 and Al2 O3 –TiO2 ).
80 × 10−4 4. located on the higher asperities of the surface.56 × 10−4 −9.29 × 10−4 0 −6. The recorded samples and pins wear rates are listed in Fig. Three-dimensional axonometric representations of wear scars on plasma-sprayed Al2 O3 (A) and Cr2 O3 (B) after test no. Alumina pins undergo both two-body grooving and brittle fracture against HVOF-sprayed WC–Co and thermally treated electroless Ni plating respectively. 10.42 × 10−4 −1. It must be noticed that the sample wear scar after the seemingly anomalous test no. (A) Steel pin after test no.46 × 10−5 Test 4 −4. 3 against Cr2 O3 . EHC is not hard enough to prevent ploughing and cutting by the alumina pin. though it is tough enough to prevent material removal by brittle cracks propagation from pre-existing cracks. possessing low chemical afﬁnity to the counterbody and (probably) high hardness. When sliding against alumina.18 × 10−5 0 0 Note: Negative values indicate material build-up on the sample.02 × 10−3 0 1. Bolelli et al. but lower than that caused by cermets.36 × 10−4 0 −1.14 × 10−4 0 −6. thanks to the formation of a very compact triboﬁlm. 13B.79 × 10−5 −3. No wear rate is indicated for samples tested against 100Cr6. ﬁlls the valleys between adjacent domes.52 × 10−3 −2.17 × 10−5 Test 5 −5. the cermet coatings never undergo signiﬁcant material removal.12 × 10−5 5. Electrolytic hard chrome also causes higher friction coefﬁcients and higher pin wear rates than Cr2 O3 when tested against alumina pins (especially with the lower sliding speed). 11. show deﬁnite morphological differences. which will be hereafter discussed and explained.12 × 10−3 −6.46 × 10−4 0 Test 8 −5. Optical micrographs of pin wear scars. with slightly worn domes caps and Ni–P–O compounds ﬁlling roughness valleys. after a short running-in period in which the domes caps are slightly worn (due to very high localized contact pressures).33 × 10−3 −6. platings.95 × 10−4 3.12 × 10−4 −2.11 × 10−5 −4. Reversing the results for alumina pins.45 × 10−4 −1.72 × 10−4 1.07 × 10−4 Test 2 −4.35 × 10−4 Test 3 −3. 4 against Cr2 O3 . a ﬁlm is formed where an oxidized Ni–P compound. / Wear 261 (2006) 1298–1315 1307 Fig. As far as thermally treated Ni–P electroless plating are concerned.91 × 10−5 1.48 × 10−4 1. respectively. with the latter forming a much smoother wear scar on the pin. 100Cr6 pins undergo one order of magnitude lower wear rates when slid against cermets than when slid against Cr2 O3 .90 × 10−4 −4. HVOFsprayed WC–Co and electrolytic hard chrome.98 × 10−4 −1. .06 × 10−4 4. friction coefﬁcients are indicated in Fig.77 × 10−4 2. comparing the results of tests 7 and 8 performed both on as-deposited and on ground plasma-sprayed ceramics.96 × 10−5 8.G.58 × 10−5 −5. Wear scars of Ni–P electroless platings after tests 4 and 8.64 × 10−4 −1. Table 7 Sample wear rates in mm3 /Nm after pin on disk test on as-deposited (no grinding) coatings Test 1 Cr2 O3 Al2 O3 Al2 O3 –TiO2 Cr WC–Co WC–Co–Cr Ni Ni-tt −1. electrolytic hard chrome displays higher friction coefﬁcient than plasma-sprayed chromia and HVOF-sprayed cermets. 8 is almost identical to that of thermally treated Ni–P.86 × 10−5 7. 13A. The effects of polishing on tribological performance of coatings has been the object of a speciﬁc investigation. In the tests against 100Cr6 pins. 8.33 × 10−3 Test 6 −2.59 × 10−5 −2.25 × 10−5 −3.49 × 10−4 6. (B) alumina pin after test no.02 × 10−4 0 Test 7 −5. because only material build-up Fig. Alumina pins wear rates are higher by almost one order of magnitude when tested against cermets than when tested against plasma-sprayed Cr2 O3 .
14A–D show optical micrographs of some worn alumina and steel pins. however. and ﬁnally by Al2 O3 and Al2 O3 –TiO2 . but WC–Co now causes much less wear than hard chrome and plasma-sprayed Al2 O3 and Al2 O3 –TiO2 . (B) friction coefﬁcients. but surface grinding has made it possible to determine them accurately. 7 and no. approaching the performance of Cr2 O3 . Such very low wear rates could not have been measured on rough samples.3 × 10−5 mm3 /Nm). but only minor surface morphological changes. Thus. 14A). Cr2 O3 remains the ceramic coating inﬂicting less wear to the counterpart. It must also be noticed that wear rates for ground Cr2 O3 and WC–Co tested against alumina have been indicated. Comparison between pin-on-disk tests no. 8 (only positive wear rates indicating effective material removal are indicated) and pin wear rates in test no. / Wear 261 (2006) 1298–1315 Fig. 12. with WC–Co still causing the least wear on the steel pin. ground ones do not show a real wear scar with signiﬁcant material removal from the sample surface. a ﬁlm of transferred material is formed on the pin tested . Bolelli et al. is found in this case. Considering alumina pins. samples wear rates are not signiﬁcantly changed in any case. ering 100Cr6 steel pins. (A) Pin wear rates. while some differences emerge in pin wear rates and friction coefﬁcients. (B) friction coefﬁcients. followed by HVOF-sprayed WC–Co. 7 (steel pin) and test no. electroplated chromium still causes higher wear (comparable to the other ceramic coatings). Thus. thus. Consid- Fig. The wear rates for WC–Co and Cr2 O3 . with Cr2 O3 causing the lowest friction coefﬁcient against alumina. The steel pin undergoes two-body abrasive wear (cutting and ploughing) when tested against chromia (Fig. by hard chrome. their wear performance is still far superior to other tested materials. (A) Sample wear rates in test no. Pin wear rates decrease in all cases (with the exception of 100Cr6 pin against Al2 O3 –TiO2 ). Pin-on-disk test results for all tested coatings. 13. it can be assumed that the overall wear amount undergone by these samples has not actually increased after grinding: like as-sprayed coatings. while a limited material build-up was recorded on as-sprayed coatings. Fig. The friction coefﬁcients against 100Cr6 pins decrease for plasma-sprayed ceramics (which display similar values after polishing) but increase for electrolytic hard chrome and HVOF-sprayed WC–Co. 8 (alumina pin). 8 for as-deposited and ground coatings. are more than two orders of magnitude lower than those for the other coatings. Friction coefﬁcients against alumina pins decrease for all coatings but Al2 O3 and Al2 O3 –TiO2 (which display slightly increased friction) and rankings between coatings remain similar.1308 G. instead. the wear rates that all ceramic coatings and electrolytic hard chrome inﬂict become very similar (about 1.
48] can be compared) that the more high-melting-point the ceramic powder is. On the one hand. The low melting point of titania in Al2 O3 –TiO2 coating favours better particle melting. 14B): it is likely that this ﬁlm consists in plastically deformed (and probably also partly oxidized) metallic debris from the pin itself and from the soft Co matrix of the cermet. which spread very well due to their high in-ﬂight velocity and thus possess low mechanical interlocking. 14. with some grain boundaries becoming very evident. Cr2 O3 seems to possess the lowest intersplat cohesion. it improves intersplat adhesion. 4. On the other hand. conﬁrming many literature work [25. 3B) because crack propagation along splat boundaries is more difﬁcult. causing opposing effects. However.G. 1C indicates. Probably it also promotes chemical intersplat bonding as well. 7 against ground electrolytic hard chrome. the better intersplat adhesion also causes more transverse microcracking due to tensile quenching stresses. from the vast literature on plasma spraying of ceramics (for instance. the coarser average powder particle size causes the appearance of a signiﬁcant number of unmolten particles. (A) Steel pin after test no. In the alumina coating.48]. Discussion 4. The wear scar on the alumina pin tested against Cr2 O3 (Fig. the more difﬁcult it is to achieve a dense. overall fracture toughness is higher (Table 4 and Fig. 8 against ground Cr2 O3 . 1A and B) and from fracture toughness measurement. because some metal matrix has been abraded by alumina pin asperities. The as-sprayed coating roughness conﬁrms a very good molten droplets ﬂattening for this coating. the abovementioned phenomena lessen coating anisotropy. against WC–Co (Fig. This is why signiﬁcant cracks both parallel and transverse to the substrate are formed even at a lower load than other plasma-sprayed coatings (5 N instead of 10 N). This phenomenon has already been observed with HVOFsprayed alumina splats . 8 allowed to notice that the surface roughness of Cr2 O3 has decreased because some asperities have been worn out and pores (which have been opened be surface polishing) have been ﬁlled with wear debris. all splats appear well spread. Thus. as emerging from SEM micrographs (Fig. 7 against ground Cr2 O3 .1. The pin suffers both abrasive and adhesive wear in tests against electrolytic hard chrome (Fig. as Fig. (D) alumina pin against test no. Furthermore. (C) steel pin after test no. Bolelli et al. The surface roughness of WC–Co. Besides. Overall. where intersplat cohesion is better. Optical micrographs of pin wear scars after testing against ground coatings. however. instead. has increased. in fact. from the same SEM micrographs. the result is a less tough and less hard coating than . it seems that unmolten particles are not the reason for the low intersplat cohesion of this coating. papers dealing with plasma-sprayed PSZ [43–47] and Al2 O3 –TiO2 [25. Microstructure and micromechanical properties Among plasma-sprayed coatings. 14D) and WC–Co is very smooth. Furthermore. / Wear 261 (2006) 1298–1315 1309 Fig. (B) steel pin after test no. the addition of titania allows the formation a brittle glassy phase inside the coating. 7 against ground WC–17%Co. Proﬁlometry on the wear scar on polished Cr2 O3 and WC–Co samples after test no. leaving the carbide grains protruding out of the surface. It can be argued that the well-spread splats may have too low roughness to allow proper mechanical adhesion of new-coming splats. it is noticeable. 14C). indicating good in-ﬂight melting. the quite high melting point of Cr2 O3 (2330 ◦ C ) causes molten splats to solidify very quickly upon impact and does not allow underlying splats to reach a sufﬁciently high temperature to activate chemical intersplat bonding. low porosity coating. In fact.
So. fracture toughness by itself might not be the best parameter to explain abrasive wear behaviour. P the normal load (N).0290. E the elastic modulus (GPa). the most difﬁcult to melt). with indenting abrasive particles getting progressively embedded in the coating. allowed by much higher particles speed in the supersonic HVOF ﬂame. the wear rate is decreased with increasing sliding distance because embedded particles alter the characteristics of the sample surface.49]. in fracture toughness tests. a2 = 0.33 . along splat boundaries) appeared for Cr2 O3 . the decreasing wear rate of coatings containing metallic phases is caused by abrasive particles which are progressively embedded in metals or cermets due to the ductility of the metallic phase [29. its effect cannot be accounted for and will be considered as a part of the coefﬁcient a.34 Al2 O3 –TiO2 3. Since the normal load has not been changed.1) where a is the material independent constant. a quantity directly related to intersplat cohesion should be adopted. in theory. in such kinds of tests.85 ± 0. but withstands indentation without cracking thanks to its sufﬁcient toughness.28 ± 0. These micromechanical features shall obviously play an important role in explaining the results of tribological tests. It is very important to notice that better as-sprayed coating surface ﬁnishing can be achieved using ﬁner spray powders. wear rates for ceramic coatings can be calculated as the average of measurements performed at different numbers of disk revolutions.e. because it reduces the number of post-deposition mechanical treatments necessary. Ceramic coatings do not undergo ploughing and cutting. instead. The best performance for ceramic coatings is shown by the toughest one. In this way. It would therefore be appropriate to elucidate the relationship between fracture toughness. long cracks in the direction parallel to the substrate (i. a3 = −0. Plasma-sprayed ceramic coatings. in fact.48 Cr2 O3 0. An anomaly is immediately apparent when observing that Al2 O3 –13%TiO2 is more abrasion resistant than Cr2 O3 .2) The coefﬁcient a1 and the a2 . Two facts must be considered to explain this seeming inconsistency: the main wear mechanism is splats detachment along splats boundaries. Vickers microhardness and abrasive wear resistance. a3 . Thus. the steel wheel test can be considered signiﬁcant for them. to quantitatively ascertain the effect of microstructural characteristics on this property.51 ± 0.2. Since the wear rate for ceramic coatings remain quite constant and the wear mechanism is not altered increasing the test duration. but this is not possible for metals and cermets. because of the very high intrinsic hardness of the material. a4 = 1. therefore. The KIC-L /KIC ratio will be employed in a modiﬁed version of the Evans–Marshall formula for abrasive wear rate prediction : w=a (E/H)P 1/8 KIC H 5/8 1/2 (4. It can be seen that the chrome plating is not hard enough to prevent hard alumina grains to wear the surface by grooving phenomena (ploughing. protecting it. The formula will be modiﬁed by multiplying the denominator by the KIC-L /KIC ratio. The resulting expression is as follows: w = a1 (E/H) a2 KIC (KIC-L /KIC )a3 H a4 (4. The coating thus undergoes microcutting. a4 exponents have been evaluated by non-linear least squares ﬁtting of experimental data: a1 = 0.68 ± 0. HVOF-sprayed cermets undergo two and three-body wear as well. thus obtaining an estimation of the crack resistance in this direction.1310 G. Thus. seem a technically appropriate choice when dry particles abrasion is the main wear mechanism involved. microploughing and also microindentation. HVOF-sprayed cermets are tougher than plasma-sprayed ceramics thanks to their composite nature with hard particles in a tough metal matrix and thanks to a better cohesion.23 1. comparable to the one of the abrasive corundum grains. their abrasive wear resistance overcomes that of hard chrome plating and HVOF-sprayed cermets. it is likely that the exponents value shall have to be changed as well. a parameter taking into account the toughness in the direction parallel to the substrate and the coating anisotropy must be introduced. The KIC-L values and the KIC-L /KIC ratio are listed in Table 8. Bolelli et al. with cracks mostly propagating parallel to the substrate. Table 8 KIC-L values and KIC-L /KIC ratios for the plasma-sprayed ceramic coatings Coating KIC-L KIC-L /KIC (MPa m1/2 ) Al2 O3 1. w = wear rate (mm3 /Nm). which is harder and possesses similar toughness. An empirical but simple parameter can be computed by using only the half-diagonal and average crack length in the direction parallel to the substrate in the Evans–Charles formula. cutting). Nonetheless. as already discussed in . thus. This phenomenon has not limited to this speciﬁc test condition. Dry particles abrasion resistance Former research has shown that. they undergo wear due to brittle splats removal. and KIC is the fracture toughness (MPa m1/2 ).40 0. This parameter will be hereafter referred to as KIC-L (MPa m1/2 ). while similar cracks were developed in al directions for alumina–titania. 4. the coatings are still deﬁnitely anisotropic. / Wear 261 (2006) 1298–1315 plasma sprayed alumina alone. even though chromia is the most high melting point among tested ceramics (thus.1290. while at high number of disk revolutions the embedded particles protect the metallic and cermet coatings from further grooving or indenting phenomena. Having a lower as-sprayed surface roughness is very important for technological applications. it is the one for which the best surface ﬁnishing has been obtained in the as-sprayed state.76 ± 0. Therefore. in the latter conditions. Since the formula has been changed. cermets and hard chrome plating wear rate is better than ceramics. The wear mechanism for hard chrome plating under the dry sand-steel wheel test is mixed three-body grooving and two-body rolling (following literature deﬁnitions discussed for instance in ). H the Vickers microhardness (GPa). but it has been also documented under different experimental conﬁguration (microscale abrasion) . for a low number of disk revolutions.30 ± 1.7355.88 0. in view of an optimization for practical application.0121.
a higher local temperature is reached in the contact point. a deﬁnite chemical afﬁnity between the two metallic surfaces of electroplated chromium and 100Cr6 certainly exists. the harder one wears the softer one: since all tested coatings but Ni–P plating without treatment are harder than 100Cr6. while. the contact area becomes much larger and also involves the soft Co matrix. while the new equation (Fig. a greater number of points should have been employed. for ceramic coatings. because the overall extent of the actual contact area is increased. it appears that contact stresses have not been high enough to cause such phenomenon. Bolelli et al. The only way by which material could be removed from samples surface would be by crack formation and propagation by cyclic contact fatigue. 4. the steel surface is more rapidly oxidized. while it is coarser and thicker on the others. Furthermore. This explains the lower friction coefﬁcient recorded on the as-sprayed chromia coating. although it remains lower than that for hard chrome and as-deposited Ni–P. where a transferred steel ﬁlm is formed. the ﬁlm is thinner and smoother on the Cr2 O3 one. Dry sand-steel wheel test results for plasma-sprayed ceramic coatings ﬁtted with Eqs.2). After polishing. both because of transfer material oxidation and because a large part of the cermet surface consists of ceramic WC particles possessing low chemical afﬁnity for steel. / Wear 261 (2006) 1298–1315 1311 Fig. thus. chemical afﬁnity between the surfaces must be considered. Although there exist doubts concerning the effective usefulness of such predictive theoretical or semiempirical formulae for thermally sprayed coatings [53. On the electrolytic hard chrome plating. When ceramic coatings are ground. instead. because they all form a quite smooth and thin ﬁlm of transferred material. in the current work. thus. reducing wear caused by the hard coating asperities. however. once the correlations between operating parameters and micromechanical properties shall be fully elucidated by further fundamental research. The ﬁt results. a ﬁlm of transferred material is formed on the pin itself and the friction coefﬁcient increases. In many cases. under a higher contact load the transferred ﬁlm on the sample surface is more rapidly built up. A very peculiar situation occurs for cermet coatings: in the as-sprayed condition. (B) wear rates plotted against (E/H) a2 (KIC (KIC-L /KIC )a3 H a4 ). 15. the friction coefﬁcient slightly increases. The same considerations are valid for as-deposited Ni–P platings as well. a steel–steel contact governs tribological phenomena. While ceramic coatings have no chemical afﬁnity for the 100Cr6 pin. In this situation. the steel pin forms a ﬁlm of transferred material on the coatings.54]. (4. reducing the friction coefﬁcient. (A) Wear rates plotted 1/2 against (E/H)P 1/8 /(KIC H 5/8 ). Therefore. they can be a useful reference for a simple estimation of the performance of a coating. no signiﬁcant transferred ﬁlm is formed. The friction coefﬁcient and pin wear rate decrease with increasing contact load for almost all coatings and with increasing sliding speed as well. therefore. Pin on disk wear test It is a basic principle that. the chemical afﬁnity between the soft Co matrix and the steel pin becomes relevant. for a proper statistical analysis. This is conﬁrmed by optical micrographs indicating adhesive wear taking place on the steel pin in this case. Considering as-sprayed ceramic and cermet coatings.1) and (4. For electrolytic hard chrome. 15A shows that the Evans–Marshall equation fails in predicting the abrasive wear rates of the various coatings. which possess the lowest surface roughness. after the thermal treatment. and a basis for a future a-priori process design. reducing the friction coefﬁcient.G. after a runningin period. where no signiﬁcant transferred . It should be noticed that. The above considerations only seek to indicate a new way for the microstructural interpretation of abrasive wear test results of plasma-sprayed coatings. should not be considered as being valid in general. so that the pin is initially worn by few protruding carbide particles and the steel debris form a transfer ﬁlm on the coating. thus adding no further source of friction and wear. The morphology of the transferred ﬁlm is inﬂuenced by coating surface ﬁnishing: considering as-sprayed ceramic coatings. but the friction coefﬁcient is the highest among tested coatings: in this case. The latter event also occurs for increased sliding speed. they never undergo a wear loss except for Ni–P without thermal treatment. (4. the appearance of the Ni3 P phase and the formation of oxidized phases on the coating surface deﬁnitely lowers the chemical afﬁnity. the contact is localized on coating surface asperities. when the chrome plating is polished. 15B) ﬁts the experimental data.2). only three points have been employed to ﬁt Eq. under a higher normal load. they all cause a similar friction coefﬁcient and pin wear against the 100Cr6 pin. Tribological phenomena in couplings between the steel pin and tested coatings seem to be inﬂuenced by the coating roughness. Fig.3. in a tribological coupling between two different surfaces.
a high overall grain boundary surface provides a great amount of shear faults for plastic deformation. This ﬁlm prevents any further wear on the coating. plastically deformed coating material or in a surface chemical alteration of the coating. once formed. On plasma-sprayed Cr2 O3 . below this ﬁlm. The hardness of these carbide particles. while. it is continuously removed and reformed and does not protect the coating. the occurrence of a triboﬁlm has already been documented in literature [56. splats are less free to deform plastically and are more easily cracked due to elastic stresses accumulation. some wear debris from coating material is transferred to the alumina pin.24. . moreover. The measured wear rate (<10−7 mm3 /Nm) and the smooth pin wear scar. on Al2 O3 and Al2 O3 –TiO2 . is only beneﬁcial if the triboﬁlm itself possesses adequate cohesion. 10B. The detached metal debris (together with some very small WC fragment) mix with the alumina debris and acts as bonding phase. Thus. as the above mentioned literature works report and the present observations of alumina pin wear scars conﬁrm. 9C and D) indicate that. Such particles slightly protrude out of the metal matrix and. ﬁlm areas consisting in alumina particles and WC fragments held by metal matrix are found next to the protruding particles. on other coatings. the splats themselves seem to undergo extensive plastic deformation: it is known that. the compact ﬁlm effectively protects the surface from damage. some of which have been cracked but. which are due to heat generation by friction and to poor thermal conductivity of ceramic materials. SEM micrographs (Fig. Another reason for the lower friction coefﬁcient might be the appearance of CrO2 and CrO3 on the very surface of the ﬁlm. with rougher wear scars for higher recorded wear rates. The plastically deformed metal strongly holds the small carbide particles. favouring plastic deformation. With this assumption. is plastically deformed around contact points because of high contact stresses. Friction coefﬁcient and pin wear are quite high for electrolytic hard chrome and for Al2 O3 and Al2 O3 –TiO2 coatings: for these latter. the plastically deformed ﬁlm is very thin and compact. the ﬁlm smoothness may partly account for the lower friction coefﬁcient recorded in this case. The pin undergoes grooving phenomena (ploughing and cutting) which are probably due to the formation of a thin. The pin wear rate seems to be increasing both with normal load. accounting for the higher wear rate. Furthermore. On cermets. as for electrolytic hard chrome and as-deposited Ni–P. at the same time. Tests against alumina pins also allow to evaluate the wear resistance of the various coatings. and also undergoes a limited extent of brittle cracking and grain pull-out. since alumina is hard enough to inﬂict wear on most of them. plastic deformation without sub-surface cracking is more favoured in the Cr2 O3 coating. the ﬁlm has a quite loose structure. which increases ﬂash temperature in the contact point favouring thermal shock cracking . and with sliding speed. because of the quite high initial surface roughness. For hard chrome. If a triboﬁlm is not formed. is much different from the one in plasma-sprayed coatings: in massive ceramics. reducing the contact pressure on surface asperities by sample grinding lowers wear alumina pin wear rates and also lowers friction coefﬁcients. the present alumina pin wear seems in a border-line situation between mild and severe wear.29]. It appears that surface triboﬁlms formation is an important tribological phenomenon in most cases: these triboﬁlms consist in plastically deformed wear debris. there are unaltered splats. During the test.55] and massive [30–34] ceram- ics conﬁrm the occurrence of microscale plastic deformation in ceramics: material sliding at discrete “shear faults” (for instance. Obviously. as explained in . high local temperatures lessen the asperities hardness. chemical afﬁnity is likely to be the dominating effect. and. the higher hardness of the Cr2 O3 coating implies the compact triboﬁlm. which are harder than the alumina counterbody. Tribological studies on both plasma-sprayed [23.24]. however. cannot be easily abraded by pin surface asperities or loose debris. although a few exceptions exist in the present experimental data set. being very small and close to each other. in fact. instead. This is particularly obvious for the WC–Co cermet: the wear rate it inﬂicts on the alumina pin decreases by more than two orders of magnitude after grinding. grain boundary sliding) is thought to be the cause of such phenomenon. due to rapid cooling. with few debris embedded in grain boundaries. Besides. In plasma-sprayed coatings. so that a metal–metal contact arises. in fact. softer surface ﬁlm consisting in wear debris. Let us examine the case of as-sprayed ceramic coatings. it is likely that the increased contact point temperature favours metallic surfaces oxidation. The metal matrix. nonetheless. Their triboﬁlm consists in plastically deformed splats and wear debris: plastic deformation is caused by high local contact pressures and by high local contact temperatures. the contact is localized on WC particles. However. the wear scar appearance in massive ceramics. therefore. it is able to inﬂict wear on them and. allowing debris sticking onto the cermet surface. Thus. Comparing the present wear rates and wear mechanisms with literature work on wear of sintered ceramics [30–32]. Therefore. and part of the soft metal is abraded by asperities on the counterbody.1312 G. the coating cannot oppose to continuous material removal by the harder counterpart asperities. Fig. in fact. are still embedded. A signiﬁcant compressive stresses distribution appears just below the surface at contact points because of high contact pressures: it is known that. it undergoes much less wear than 100Cr6 (wear rates ≤10−5 mm3 /Nm). splat boundaries themselves may constitute favourable areas for plastic slipping [23. slightly reducing chemical afﬁnity troubles. a thicker ﬁlm appears. ceramics can plastically deform at the microscale. increasing the friction coefﬁcient. / Wear 261 (2006) 1298–1315 steel ﬁlm appears. thus. reducing the friction coefﬁcient . prevent further abrasion of the metal matrix. Furthermore. under high idrostatic stress. Bolelli et al. surface splats on the chromia coating are quite free to deform plastically without sub-surface cracking. The triboﬁlm formation. its formation and its compactness are the effect of the exceptional ductility of the Co-based metal matrix. splats consist in very small crystals (≤1 m) . which favours brittle cracking. Sintered alumina is harder than all tested ceramic coatings. where splat cohesion is lower. with a higher amount of debris on all the contact surface: this is probably due to material detachment from surface asperities. with no brittle cracking. clearly indicates the occurrence of a mild pin wear regime (according to [30–32]) in tests against ground WC–Co and Cr2 O3 . since brittle fracture is involved in alumina pin wear. Besides.
plasma-sprayed Cr2 O3 and HVOF-sprayed cermets are the best performing coatings under all aspects and are all candidate coatings for electrolytic hard chrome replacement. The contact temperature must have been high enough to cause nanocrystallization along the contact area. • In the pin-on-disk test. no triboﬁlm formation occurs because the favourable condition of carbides slightly protruding out of the metal matrix has already been accomplished by the grinding operation: the ground surface itself acts as the triboﬁlm. a very smooth wear scar appears. Among the thick (≥100 m) coatings tested in this study. . It is practically unusual to ﬁnd application where hertzian contact pressures are allowed to exceed 1 GPa . has the ability to form a compact triboﬁlm by splats plastic deformation. so that in the contact area. As a result. plasma-sprayed Al2 O3 shows the best dry particles abrasion resistance. carbide particles are already slightly protruding. the ﬁlm only consists in plastically deformed splats. with few debris ﬁlling open pores. its employments are suggested under such conditions. have been characterized in terms of microstructure and micromechanical properties. 12A). seems an interesting solution. Thus. Cermets have similar performance to electrolytic hard chrome.G. Cr2 O3 . related to the crack propagation resistance in the direction parallel to the substrate (i. As far as thermally treated Ni–P is concerned. intersplat cracking). on the ground surface. Besides. pin wear rate and friction coefﬁcient. the contact pressure was not high enough. The smoothness of the wear scars. Some strict rules have been recently issued in USA due to this problem . Conclusions Three plasma-sprayed oxide ceramic coatings. thus. the contact is already located on the very hard carbide particles. no further wear occurs on the coating. deserve a special comment.58] indicates that wear due to brittle crack propagation could occur: in this case. On WC–Co. Al2 O3 –13%TiO2 is the most isotropic but also the less hard and less tough one. the ability to form a smooth and compact surface ﬁlm by local plastic deformation is the key property determining coatings performance. This accounts for the absence of material build-up on the surface and for the very low measured wear rate. but only a very low wear rate. It is interesting to observe how an improves surface ﬁnishing alters the wear behaviour. its performances are comparable to HVOF-sprayed ceramics. A combination between KIC-L and Vickers microhardness is suggested to predict the dry particles abrasion resistance of plasma-sprayed ceramics. is not a good parameter to predict plasma-sprayed ceramics dry particles abrasion resistance: the parameter KIC-L . due to the formation of an alumina–titania glassy phase which favours intersplat adhesion but turns out to be quite brittle. However. by itself. In particular. Plasma-sprayed Al2 O3 and Al2 O3 –13%TiO2 do not form an adequately compact triboﬁlm and therefore show unfavourable properties in terms of sample wear rate. / Wear 261 (2006) 1298–1315 1313 on the other hand. In particular. Al2 O3 –13%TiO2 . performing similarly to cermet coatings though having potentially lower production costs. as shown in Section 3. must be introduced. although more expensive than most ceramic ones (at least thrice more expensive than alumina). crack propagation was reported to be caused by metal matrix embrittlement due to carbides dissolution: in this case. friction coefﬁcient) have been compared to the behaviour of two HVOF-sprayed cermet coatings (WC–17%Co and WC–10%Co–4%Cr). namely Cr2 O3 . the contact point temperature is high enough to form oxidized Ni–P–O compounds which deﬁnitely lessen the friction coefﬁcient and contribute (together with the high hardness and toughness of the nanostructured coating) to arrest any further coating wear. may cause some wear on the pin (Fig. the higher actual contact area prevents local plastic deformation of the metal matrix around surface asperities. are cheaper than cermets. Cr2 O3 powders. On Cr2 O3 . the higher actual contact area reduces initial contact stresses around surface asperities. • Plasma-sprayed ceramics are the better-performing coatings in dry particles abrasion conditions. so that less debris appears. Their dry particles abrasion resistance (dry sand-steel wheel test) and pin-on-disk wear test response with 100Cr6 steel and sintered alumina counterbodies (sample wear rate. Plasma-sprayed chromia. because they never undergo abrasive grooving but only splats detachment. thus. The response from the Ni–P electroless plating in test 8. but.e. thanks to a ductile metal matrix and to a composite microstructure. The experimental results lead to the following conclusions: • Cr2 O3 coating is the hardest and most anisotropic among plasma-sprayed ceramics. Fracture toughness. as it happened in as-sprayed coating. Al2 O3 . so that the coating is tough enough to prevent crack propagation under reasonable contact loads. potential disadvantages. little amount of wear debris and no material build-up for ground Cr2 O3 and WC–Co coatings is consistent with the onset of a mild wear regime for the alumina pin. instead. pin wear rate. Thus. the triboﬁlm is formed by chemical alteration of the coating surface: once the domes caps are smoothed by high contact pressures. WC–17%Co and WC–10%Co–4%Cr are also anisotropic. and no material build-up is recorded. because the soft Co matrix is much more easily ground and removed. Besides. untreated and thermally treated electroless Ni–P coatings. the coating behaves almost exactly like the thermally treated one. 5. The only noticeable wear phenomenon is the removal of a small amount of Co matrix by the highest counterpart asperities: once the carbide particles are protruding out enough and the counterpart surface asperities are worn away. due to low interlamellar cohesion. Further development of this research should also involve more environmental friendly alternatives to thermally sprayed Cr2 O3 able to reproduce its excellent wear behaviour. the optimal choice of spraying parameters prevented an excessive extent of carbides dissolution. which must be considered in a proper coating choice. include the rather low deposition efﬁciency of Cr2 O3 (≤45% in conventional APS ) and environmental problems due to possible formation of Cr6+ by in-ﬂight thermal alteration of the coating material during spraying. Some literature work [57. are tougher than plasma-sprayed ceramics. Thus. where the pin and sample wear rate and friction coefﬁcient resemble thermally treated Ni–P. Bolelli et al. electrolytic hard chrome.
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