Powder Metallurgy Progress, Vol.13 (2013), No 3-4 109 EFFECT OF STATIC PARTNER MATERIAL ON WEAR CHARACTERISTICS OF YTTRIA STABILIZED ZIRCONIA J. Balko, A. Kovalčíková, P. Hvizdoš Abstract Tribological testing and wear damage analysis of yttria stabilized tetragonal zirconia was carried out using the ball-on-disk method. The testing was performed at room temperature in air for dry sliding with different types of ball material (Al2O3, ZrO2, WC-Co, and Si3N4). The coefficient of friction was measured with a load 8 N. Material loss was evaluated using confocal microscopy in terms of volume removed, and specific wear rates were calculated. The measured values of the coefficient of friction were in good agreement with the values in literature for corresponding tribological material pairs. They were lower (0.65) for WC-Co balls, medium (0.73) for the Si3N4 and Al2O3, and higher (0.8) for ZrO2 balls. The highest wear rates were found for the ZrO2/ZrO2 pair which is attributed to the chemical similarity of both tribological partners. Keywords: wear, friction coefficient, static partner, sliding distance, ball-on-disk INTRODUCTION Tribology is the science concerned with studying the processes of friction and wear. In practical circumstances the friction of materials leads to their surface damage and wear. By studying and understanding the mechanisms of wear it is possible to predict the behavior of materials in various applications. Structural ceramic materials have useful tribological properties, such as low density, high corrosion resistance, low coefficient of friction, low thermal expansion and high hardness over a wide range of temperature. Because of these advantages of ceramic materials, their usage is increasing in many of the engineering applications where strong mechanical contact takes place [1-3]. Modern mechanical components and tribosystems must possess the ability to withstand their severe operating conditions, they have to have higher reliability and an excellent performance of their functions. These requirements are related to wear and surface damage of interacting surfaces. Therefore, wear behavior of ceramics have been studied for many years [4]. Polycrystallic zirconia is a ceramic material characterized by high values of fracture toughness, strength and chemical resistance which makes it an attractive material for its use in extreme conditions. It is used as a refractory material for the lining of melting furnaces, the matrix wire drawing, cutting material and as a biomaterial for joint, bone and dental replacements. Ján Balko, Alexandra Kovalčíková, Pavol Hvizdoš, Institute of Materials Research, Slovak Academy of Sciences, Watsonova 47, Košice, Slovak Republic Powder Metallurgy Progress, Vol.13 (2013), No 3-4 110 ZrO2 occurs in three allotropic modifications: monoclinic (m-ZrO2) lowtemperature phase existing at temperatures below 1060C, tetragonal (t-ZrO2) mediumtemperature phase occurring at temperatures from 1060C to 2370C, and cubic (c-ZrO2) high-temperature phase stable at temperatures above 2370C. The phase transformation from t-ZrO2 to m-ZrO2 is accompanied by an increase of volume by 4-5% [5]. This causes local microscopic stresses which can be accompanied by the formation of tension cracks. ZrO2 can be stabilized by adding various oxides (e.g. Y2O3, MgO, CaO). In this way, a metastable microstructure where residual compressive stresses occur is formed. Such material can achieve KIC up to 14 – 20 MPa·m-1/2 which is the highest fracture toughness among monolithic ceramic materials [6]. However, research on the tribological behavior of structural ceramic materials and optimal operating conditions for ZrO2 are hard to find. Therefore, this study was made to collect data on operating conditions of wear against ZrO2 and to investigate the wear behavior and tribofilm formation among four different structural ceramic couples at room temperature in unlubricated sliding [1]. There are many types of experimental set-ups used to more or less closely mimic the real practical situations which differ in the used geometry and loading conditions. In laboratories, one of the most frequently used techniques is a pin-on-disk. If the pin has a spherical shape of the contact part, it is called also ball-on-disk. The measurement is based on the friction of the ball on a sample on a circle track. By measuring the geometry and volume of the wear track, we can study specific wear rate. The linear dependence of wear rate on volume loss can be found. The aim of this work is to measure the basic tribological characteristics (coefficient of friction, wear rate) of zirconia using different ball materials and different loads. An additional goal was to verify whether the volume loss can really be considered to be a linear function of sliding distance, i.e. the wear rate remains constant over the duration of the test. EXPERIMENTAL MATERIALS The experimental material was zirconia stabilized by 3 mol% yttria (3Y-TZP). It was prepared using a commercial powder TZ-3Y- SB, by TOSOH Corp. The powder was cold isostatically pressed at 200 MPa for 3–5 min, then pressurelessly sintered at 1450 °C for 2 h in air. The resulting samples had forms of cylindrical bars with diameters of about 9 mm and length 60 mm. The cylinders were further cut by diamond saw, then ground and polished down to 1 μm finish by diamond paste, so that final test specimens were formed of disks of 1.5–2 mm thick with ~9 mm diameter [7]. As tribological static partners four ball materials were used (Al2O3, ZrO2, WC-Co, Si3N4), all supplied by Spheric Trafalgar Ltd., Ashington UK. EXPERIMENTAL METHODS Vickers hardness was measured under a load of 49.05 N (5 kg). Fracture toughness was calculated from indentation crack lengths using the Anstis equation [8]. E P (1) K IC 0.016 3 / 2 H c where E is modulus of elasticity, E is hardness, P is indentation load and c is the crack length. 111 Powder Metallurgy Progress, Vol.13 (2013), No 3-4 The wear behaviour of the experimental materials was studied in dry sliding in the air at room temperature by means of tribometer THT (CSM Instruments, Switzerland) using the pin-on-disk technique, against a highly polished (roughness Ra < 0.25 µm) Al2O3, Si3N4, WC-Co and ZrO2 balls with 6 mm diameter. The applied load was 8 N, the sliding speed 0.05 m/s and the total sliding distance was 400 m. Every 100 m the test was interrupted and the volume loss was evaluated. The testing was then resumed while great care was devoted to keeping the experimental set-up so that the geometry of the contact before and after the interruption was precisely maintained. The tangential forces during the test were measured and friction coefficients calculated. The material losses (volume of the wear tracks) due to wear were measured by a high precision confocal microscope PLu neox 3D Optical Profiler, by SENSOFAR, and then specific wear rates (W) were calculated in terms of the volume loss (V) per distance (L) and applied load (Fp) according to the standard ISO 20808 [9]: V mm3 (2) W L.Fp m.N At the same time, the worn cap on the counter body was measured by a light microscope, its volume and then its wear rate calculated [9, 10]. RESULTS AND DISCUSSION The tetragonal microstructure of the material (t-ZrO2) consisted of two grain-size: 66% of the material consisted of grains with a size of 0.5 μm – 1.7 μm, the rest were grains with size 2.5 μm – 5 μm. Microstructure of this material was studied and described in detail elsewhere [7]. Basic mechanical properties (hardness, elastic modulus, fracture toughness) of the balls and samples are shown in Table 1. Tab.1. Basic mechanical properties of all ball materials and samples. Material HV 5 [GPa] KIC [MPa·m-1/2] E [MPa] Ball Al2O3 16.8 ± 1.2 5.03 ± 0.12 370 ± 27 Ball Si3N4 17.5 ± 1.1 6.74 ± 0.14 320 ± 29 Ball WC-Co 16.3 ± 1.4 13.75 ± 0.27 450 ± 24 Ball ZrO2 13.2 ± 2.1 6.77 ± 0.14 220 ± 15 Sample ZrO2 12.55 ± 2.0 6.61 ± 0.19 200 ± 12 Coefficients of friction (COF) for all the experimental material pairs were obtained as a function of sliding distance (or time). The tribological measurements showed the unstable initial phase of friction curves, during which stabilization of the system took place, Fig.1. This phase was relatively short, particularly for Si3N4 and ZrO2 balls, where less than 2 m was sufficient. In these two cases the COF was so stable that even the interruptions of the testing run did not lead to changes in the friction and they did not have any observable effect on the COF line. In the other two cases the run-up phases were longer, a few tens of meters, and also after interrupting the test some changes in friction could be observed, Fig.1. This was particularly pronounced in the case of WC–Co as the static partner. Here the coefficient of friction was stabilizing over a longer distance than brittle materials, probably because of the presence of ductile phase – cobalt. 112 Powder Metallurgy Progress, Vol.13 (2013), No 3-4 1,0 0,9 0,8 0,7 COF [-] 0,6 0,5 0,4 0,3 Al2O3 Si3N4 WC-Co ZrO2 0,2 0,1 0,0 0 100 200 300 400 Sliding distance [m] Fig.1. Coefficient of friction curve of each material during the tests. Table 2 shows the values of COF, averaged over the stable parts of COF lines. Satchowiak et al. [11] specifies the COF of ZrO2/ZrO2 pair as ~0.75 which is slightly lower than in our case which can be caused using a lower load. The highest coefficient of friction was observed with ZrO2 ball due to the chemical similarity with tested material, then Al2O3 and Si3N4. The lowest COF was in a test using WC-Co ball due to the presence of the softer ductile metallic phase. Tab.2. Friction coefficients of each sample/static partner pair. Material COF [-] Ball Al2O3 0.72 ± 0.15 Ball Si3N4 0.73 ± 0.09 Ball WC-Co 0.65 ± 0.21 Ball ZrO2 0.81 ± 0.18 When calculating wear rates it is usually assumed that the wear rate is constant over the sliding distance, as it is the case also in the standard [10]. Our interrupted testing intended to assess how reliable such an assumption is. An example of evolution of the wear track with the sliding distance is shown in Fig.2 where the steady growth, wear track width, depth and area can be seen. Almost linear growth of the wear track profile area for all experimental tribological pairs can be seen in Fig.3. Evaluation of the volume loss showed its linear increase with the sliding distance. Consequently, the wear rate (W ≈ V/L) is really basically constant, which means it is a quantity useful for evaluation of the obtained results, as is stipulated in the ISO 20808 standard. 113 Powder Metallurgy Progress, Vol.13 (2013), No 3-4 2 0 Track depth [m] -2 -4 100 m -6 200 m -8 - 10 300 m - 12 - 14 400 m - 16 - 18 0 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 Track width [m] Fig.2. Evolution of wear track in ZrO2/ZrO2 test. 24000 Al2O3 Si3N4 WC-Co ZrO2 20000 Wear track profile [m] 16000 12000 8000 4000 800 600 400 200 0 100 150 200 250 300 350 400 Sliding distance [m] Fig.3. Wear track profile area as a function of the test sliding distance for each experimental tribological pair. The highest wear rate (3.62 x 10-5 mm3/N·m) was observed for tribological partners ZrO2/ZrO2 because of chemical similarity and therefore an active tribo-chemical reaction can be assumed to occur. Chih-Chung [12] reported the wear rate of the ZrO2/ZrO2 pair as 2.5 mm3/N·m which is in good agreement with our results. The wear rate of zirconia/zirconia tribo-pair was about two orders of magnitude higher than the other tribological pairs. The wear was less intense for Al2O3 (5.55 x 10-7 mm3/N·m), than the Si3N4 ball (4.68 x 10-7 mm3/N·m), and the lowest one was observed for WC-Co (1.60 x 10-7 mm3/N·m) Fig.4. 114 Powder Metallurgy Progress, Vol.13 (2013), No 3-4 1E-5 Al2O3 Si3N4 WCCo ZrO2 3 Sample wear rate [mm /N.m] 1E-4 1E-6 1E-7 1E-8 100 150 200 250 300 350 400 Sliding distance [m] Fig.4. Wear rates of ZrO2 disks in tests with different static partners in various testing stages. Ball wear rates show that the highest wear has the zirconia ball due to the chemical similarity with the sample. The lowest values of wear were for the Al2O3 and WC-Co balls. Fig.5. This is most probably connected to the very high chemical stability of the alumina on one hand and to the lower friction (as shown by lower COF) of WC-Co on the other hand. 1 3 Ball wear rate [mm /N.m] 0,1 0,01 1E-3 1E-4 1E-5 Al2O3 Si3N4 WC-Co Material Fig.5. Ball wear rates of all static partners. ZrO2 Powder Metallurgy Progress, Vol.13 (2013), No 3-4 115 CONCLUSION The tribological characteristics were studied: the coefficient of friction, specific wear rate. Tests were realized on ZrO2 disks with ZrO2, Si3N4, Al2O3 and WC-Co balls as friction counterparts. The measured values of friction and the calculated values of specific wear rate are in agreement with the literature data. • The lowest COF had a ZrO2/WC-Co pair, 0.61, thanks to the presence of a metallic phase. • The highest values of both friction (0.81 ± 0.18) and wear were observed in tests with the ZrO2 ball, because of chemical similarity and tribo-chemical reaction of the surfaces in contact. In the other tribological pairs the wear rates of the ZrO2 disk were similar. • Wear rates of the alumina and WC-Co balls were the lowest probably due to their high chemical stability (Al2O3) and lower friction (WC-Co), respectively. • Wear rate after each sliding period was calculated and it was shown that it can be considered to be a constant over the test sliding distance. Acknowledgements This work was supported by the Slovak Grant Agency, projects VEGA 2/0075/13, VEGA 2/0043/14 and APVV-0108-12. REFERENCES [1] Miner, JR., Grace, WA., Valori, R.: Lubr. 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