Microsyst Technol (2008) 14:1839–1846 DOI 10.1007/s00542-008-0696-y

TECHNICAL PAPER

Tribological characterization and numerical wear simulation of microcomponents under sliding and rolling conditions S. Kurzenha¨user Æ V. Hegadekatte Æ J. Schneider Æ N. Huber Æ O. Kraft Æ K.-H. Zum Gahr

Received: 4 December 2007 / Accepted: 25 July 2008 / Published online: 21 August 2008 Ó Springer-Verlag 2008

Abstract Increasing requirements for higher power densities and further miniaturisation in microsystem technology result in highly loaded micromechanical systems. Regarding these applications, the friction and wear behaviour of selfmated Si3N4 ceramic and WC-Co hardmetal has been characterized in laboratory micro tribometers. Experiments under unidirectional sliding and rolling conditions were carried out in air of 50% relative humidity as well as lubricated with water. Results from the model tests were used as input dataset for a numerical simulation tool Global Incremental Wear Model (GIWM) to predict volumetric wear as a function of operating conditions. The laboratory tests indicated that WC-Co as well as Si3N4 are applicable for microsystems running in water, due to their high wear S. Kurzenha¨user (&)  J. Schneider  K.-H. Zum Gahr Institut fu¨r Werkstoffkunde II, Universita¨t Karlsruhe (TH), Karlsruhe, Germany e-mail: [email protected] V. Hegadekatte  O. Kraft Institut fu¨r Zuverla¨ssigkeit von Bauteilen und Systemen, Universita¨t Karlsruhe (TH), Karlsruhe, Germany N. Huber Institut fu¨r Werkstoffphysik und Technologie, Technische Universita¨t Hamburg-Harburg, Hamburg, Germany S. Kurzenha¨user  J. Schneider  K.-H. Zum Gahr Institut fu¨r Materialforschung I, Forschungszentrum Karlsruhe GmbH, Karlsruhe, Germany V. Hegadekatte  O. Kraft Institut fu¨r Materialforschung II, Forschungszentrum Karlsruhe GmbH, Karlsruhe, Germany N. Huber Institut fu¨r Werkstoffforschung, GKSS-Forschungszentrum Geesthacht GmbH, Geesthacht, Germany

resistance and low friction coefficient. Furthermore it was shown, that the numerical simulation can help to reduce the experimental effort by reliable predicting wear under different operating conditions, provided that the active wear mechanisms are comparable.

1 Introduction Success of micromechanical systems and precision engineering is strongly dependant both on the availability of cost-effective manufacturing techniques like micro powder-injection moulding (l-PIM) and the availability of a wide range of different materials like polymers, metals and ceramics (Anon. 2001; Heckele 2004; Piotter 2003). The efficiency of micromechanical systems with movable components, such as micro-pumps, micro-turbines, microengines or micropositioning devices, is considerably limited by the tribological performance of the mated materials. High friction coefficients reduce the efficiency, while adhesion or capillary forces can exceed the externally applied forces and thereby prevent operation of microsystems due to stiction under unfavourable environmental conditions. Even smallest amounts of loose wear debris can result in a loss of operability. Microtribological investigations showed that tribological knowledge from the macro world is not transferable to microsystems without substantial restrictions. With increasing miniaturization the ratio of surface to volume increases strongly, so that the physicochemical characteristics and the interaction of the contacting surfaces attain crucial importance (Zum Gahr 1998, 2001; Kaneko 2000; Scherge 2001; Herz 2002; Kurzenha¨user 2006; Schneider 2005). Thus, systematic investigations of friction and wear behaviour of tribologically loaded material pairings are

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Microsyst Technol (2008) 14:1839–1846

Table 1 Material properties of the test specimens from manufacturers data and own measurements Property

Material Si3N4

WC-Co Ball

Disc

Ball

Disc

Density (g/cm3)

15

14.1

3.2

3.2

Grain size dK (lm)

1.5*

0.4*

0.3*

1.2*

Young’s modulus (GPa)

630

549

320

305

Hardness HV500

1,503

1,764

1,600

1,650

KIC, MPa m1/2

12



6

7

* Own measurements

necessary under operation conditions comparable to the respective microsystem of interest. A combination of experimental studies and numerical finite-element-simulations proved to be helpful in order to come to a better understanding of the critical operating conditions in tribological loaded microsystems, while, on the other hand, experimental effort can be minimized (Hegadekatte et al. 2006, 2007). Engineering ceramics as well as hardmetals offer, compared to polymers and metals, a unique combination of intrinsically favourable properties due to their high stiffness, hardness, chemical and thermal resistance. Therefore these materials should be applicable for microsystems operating under high load or under harsh environment. Aim of this research was to characterize the tribological performance of self-mated Si3N4 ceramic and WC-Co Fig. 1 SEM micrographs of the microstructure of a WC-6Co and b Si3N4 balls, c WC-12Co and d Si3N4 disc specimens

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hardmetal under unidirectional sliding as well as rolling conditions in air of 50% relative humidity and lubricated with distilled water. Experimental tests were accompanied by numerical wear simulation.

2 Materials, experimental procedures and numerical wear simulation The materials used for the microtribological tests are listed in Table 1. The WC-6Co (Fa. Spheric Trafalgar) and Si3N4 (Fa. Swip) balls for the tribological model tests under unidirectional sliding conditions (Fig. 2a) had a diameter of 1.6 mm and were used as delivered with polished surface. The WC-12Co (TSF44, Fa. Ceratizit) and Si3N4 (SL200BG; Fa. Ceramtec) disc specimens were ground and polished before the tests. For the rolling experiments, a disc with a flat circumferential surface (driven disc) was paired against another one with a curved (r = 4 mm) circumferential surface (driving disc) (Fig. 2b). Si3N4 discs were used as-delivered with polished surface whereas the WC-Co discs had to be ground and polished before the tests. The arithmetic surface roughness Ra was between 0.02 and 0.04 lm for all samples tested. Relevant material properties are listed in Table 1, supplemented by scanning electron microscopy (SEM) micrographs of the etched microstructure of the materials as shown in Fig. 1.

Microsyst Technol (2008) 14:1839–1846

The microtribological model tests under sliding and rolling conditions were carried out in specially designed laboratory tribometers, developed at the Institute for Materials II. A normal force of FN = 800 mN, a sliding speed of v = 400 mm/s and a sliding distance of s = 1000 m were chosen as standard conditions based on a tribological system analysis (Schneider 2005) for the micro planetary gear box used as demonstrator within the frame of the Collaborative Research Centre 499 (SFB 499). Rolling tests (Fig. 2b) were run with a normal load of FN = 250 mN, a sliding speed of v1 = 800 mm/s over 106 revolutions with a slip between 1 and 10%. The model tests were conducted at room temperature both in air of 50% r.h. and under water lubrication. Splash lubrication was used for the sliding contact in water, while a dripping lubrication guaranteed a complete wetting of the contacting surfaces under rolling conditions. After the tests, wear of the specimens was measured by tactile and optical profilometry and the worn surfaces were examined using SEM. For the ball-on-disc setup in unidirectional sliding, the linear wear was measured not only after the experiments but also continuously during the tests as a function of sliding distance by a capacitive detector. For the rolling experiments, the volumetric wear was calculated from profiles perpendicular to the rolling direction of the circumferential surfaces obtained by optical profilometry after the tests. Additional stop experiments were done with self-mated Si3N4 in unlubricated rolling contact to determine the progress of wear with increasing number of revolutions. Continously measured wear data from sliding tests and the wear data obtained from the stop tests in rolling contact were used as input data for the numerical

Fig. 2 Tribological model systems, specimen geometries and operating conditions for a unidirectional sliding and b rolling contact

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wear simulation. The Global Incremental Wear Model (GIWM) developed by Hegadekatte et al. (2006) at the Institut fu¨r Zuverla¨ssigkeit von Bauteilen und Systemen at the Universita¨t Karlsruhe (TH) based on (Archard’s 1953) phenomenological wear model and is described elsewhere in detail (Hegadekatte et al. 2006, 2007). To verify the predictions from the numerical wear simulation in a first step experimental data from tests under standard conditions were used to determine the volumetric wear coefficient kD as fit parameter for the GIWM. Afterwards GIWM was used to predict volumetric wear as a function of the sliding distance or the number of revolutions under various operating conditions, respectively.

3 Results 3.1 Unidirectional sliding Figure 3 shows friction coefficient as a function of the sliding distance for self-mated Si3N4 and WC-Co at a normal load of 800 mN and a sliding speed of 400 mm/s in ambient air of 50% r.h. and in distilled water. A friction coefficient of 0.75 was measured for the unlubricated Si3N4 sliding pair at the beginning of the tests. With increasing sliding distance, the friction coefficient dropped down to a quasi-stationary value of 0.54 after about 400 m. After a sliding distance of 1,000 m, profilometric measurements revealed a linear wear W1 of 74 lm for the Si3N4 ball, indicating that this pairing is not applicable for unlubricated sliding contact under the employed loading conditions. The self-mated WC-Co showed a friction coefficient of 0.3 for the first 200 m in unlubricated sliding contact. With increasing sliding distance, the friction coefficient

Fig. 3 Friction coefficient of self-mated Si3N4 and WC-Co as a function of sliding distance in air of 50% r.h. and in distilled water for a normal load of 800 mN and a sliding speed of 400 mm/s

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increased and reached a quasi-stationary value of 0.63. Experiments over a sliding distance of 3,000 m confirmed this value to be stable. A linear wear of 1.2 lm was measured on the WC-Co ball after a sliding distance of 1,000 m. The quasi-stationary wear rate at the end of the test was 0.4 lm/km. Under water lubrication the Si3N4 sliding pair showed a distinct running-in behaviour. During the first 25 m of sliding in distilled water friction coefficient dropped down from a value of about 0.35 to a very low quasi-stationary value of 0.02 with a smooth progression up to the end of the experiments. The continuously measured linear wear indicated that most of the linear wear of 2.7 lm measured at the ball after a sliding distance of 1,000 m occurred during the short running-in period, so that the quasi-linear wear rate was 0.2 lm/km. Lubrication of WC-Co with water resulted in a friction coefficient of 0.13 at the beginning of the tests. A continuous decrease with increasing sliding distance resulted in quasi-stationary values of 0.07 at the end of the tests. After a sliding distance of 1,000 m the linear wear of the WC-Co ball was 1.5 lm which was slightly higher compared to the unlubricated test run. The linear wear rate measured by the capacitive detector was also about 50% higher with values of 0.5 lm/km in the quasi-stationary regime. After none of the sliding tests a measurable wear could be detected for the disc specimens, implying that the linear wear W1 was well below 200 nm. Due to the promising friction and wear behaviour of the water lubricated WC-Co sliding pair, the normal force was varied between FN = 400 mN and FN = 1600 mN in additional experiments (Fig. 4). These tests showed that the friction coefficient slightly decreased from values around 0.09 for 400 mN applied normal load down to a value of 0.06 at 1,600 mN. In contrast to the decrease in

Fig. 4 Quasi-stationary friction coefficient, experimentally deter  and linear wear Wl;GIWM predicted by the mined linear wear Wl;exp GIWM as a function of the applied normal load for self-mated WCCo in sliding contact under water lubrication (sliding speed v = 400 mm/s and sliding distance s = 1,000 m)

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Microsyst Technol (2008) 14:1839–1846

friction, the linear wear measured after a sliding distance of 1,000 m doubled from 1.0 lm at 400 mN normal load to 2.1 lm at 1,600 mN (Fig. 4). The linear wear recorded as a function of sliding distance during the experimental tribological tests with a normal load of 400 mN was fitted using the GIWM. The wear coefficient kD, identified to be 0.75 9 10-11 mm3/ Nmm from this fit, was then used to predict the wear as a function of sliding distance for higher loads. In Fig. 4 it can be seen that the GIWM can predict the experimentally determined wear with a reasonable accuracy considering the scatter of the measurements for the full range of normal loads up to 1,600 mN. 3.2 Rolling contact A clear influence of the chosen slip on the friction coefficient was pointed out for self-mated Si3N4 under rolling conditions in air with a normal load of 250 mN and a speed of 800 mm/s (Fig. 5a). With increasing slip, the friction coefficient measured at the beginning of the tests increased from 0.16 (1% slip) to 0.28 (10% slip). Under all test conditions, the self-mated Si3N4 showed a transition from low to high friction. During the tests with 10% slip, the friction coefficient increased from the very beginning and

Fig. 5 Friction coefficient of self-mated a Si3N4 and b WC-Co in rolling contact as a function of the number of revolutions for tests in air with a relative humidity of 50% at a normal load of 250 mN

Microsyst Technol (2008) 14:1839–1846

reached a value of about 0.7 after 104 revolutions. For tests with 1 and 4% slip, the friction coefficient remained further on a low level and showed a sharp transition to high values after 5 9 103 (4%) and 104 (1%) revolutions, respectively. At the end of the tests the quasi-stationary friction coefficient was 0.45 (1% slip), 0.62 (4% slip) and 0.72 (10% slip). The friction coefficient for unlubricated, self-mated WC-Co at the beginning of the tests was significantly lower compared to that of the Si3N4 pairing (Fig. 5b) and values between 0.11 (1% slip) and 0.22 (10% slip) were measured. Furthermore no transition occured from low to high friction. The quasi-stationary friction coefficient of self-mated WC-Co after 106 revolutions varied between values of 0.19 (1% slip) and 0.31 (10% slip), which were only half as high as for the self-mated Si3N4. SEM examinations of the worn Si3N4 surfaces of the driven disc after 106 revolutions with 10% slip in air of 50% r.h. showed the formation of compacted wear debris (Fig. 6a). Occasionally grain pull out and cracks perpendicular to the rolling direction were found on the driven disc. The surface of the driving Si3N4 disc showed no visible cracks but it was partially covered with loose wear debris (Fig. 6c). The SEM micrographs of WC-Co tested under the same operating conditions showed small amounts of fine wear debris (Fig. 6b) at the edges of the driven disc’s wear track. The worn surface of the WC-Co driving disc was covered by a layer of compacted wear debris, which was partially delaminating due to cracks (Fig. 6d). Self-mated Si3N4 showed a distinct running-in period of about 104 revolutions under water lubricated rolling conditions (Fig. 7a). Whereas the friction coefficient decreased

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from the very beginning in tests with 4 and 10% slip, the friction coefficient increases to a maximum value of about 0.3 after 2,000 revolutions in tests with 1% slip. After running in, very low values for the friction coefficient around 0.012 resulted for any chosen slip after about 2 9 104 revolutions. Under the same operating conditions, self-mated WC-Co showed a friction coefficient around 0.17 at the beginning of the tests, independent of the amount of slip (Fig.7b). The friction coefficient dropped down with increasing number of revolutions to a quasistationary value of 0.12 for 1 and 4% slip, which was reached after about 2 9 105 revolutions. From around 4 9 105 revolutions on a more pronounced decline was observed for tests with 10% slip resulting in a quasi-stationary friction coefficient of 0.07, which was only about half as high as for the test runs with lower slip. SEM examinations of the worn surfaces after 106 revolutions in water with a slip of 10% revealed a slight smoothening, for both the self-mated Si3N4 (Fig. 8a and c) and the WC-Co (Fig. 8b, d). In the wear track of both materials, small rolls were occasionally found, indicating tribochemical wear as dominating wear process. After none of the rolling tests under water lubrication, as well as for the WC-Co tests in air of 50% r.h., a measurable amount of linear wear could be determined. In order to verify the applicability of the GIWM for wear prediction under rolling conditions, unlubricated long time tests with self-mated Si3N4 were carried out. Figure 9 shows the volumetric wear of driving and driven disc measured after the tests with 4% versus the number of revolutions together with the fitted curves from the numerical simulation

Fig. 6 SEM micrographs of the worn (a, b) driven and (c, d) driving discs of (a, c) Si3N4 and (b, d) WC-Co after 106 revolutions with 10% slip at a normal load of 250 mN and a rolling speed of 800 mm/s in air of 50% r.h. (arrow indicates rolling direction)

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Microsyst Technol (2008) 14:1839–1846

driving (flat) disc showed a good agreement with the experimental data up to 5 9 106 revolutions whereas the wear measured after experiments over 7 9 106 revolutions was considerably higher than that calculated with the wear simulator GIWM. The wear coefficients kD,FD and kD,CD determined from the fitted curves for 4% slip tests were then used for the calculation of the wear in tests with 4 and 10% slip over 106 revolutions. The calculated volumetric wear as a function of the number of revolutions N, together with the experimentally obtained data after 106 revolutions (markers) is shown in Fig. 10 for the different slips. For 10 and 4% slip, a good agreement between calculated and experimentally obtained wear volumes was found both for the driving and the driven disc. For 1% slip the GIWM significantly underestimated the wear volume measured on the samples after the laboratory tests.

4 Discussion and conclusions

Fig. 7 Friction coefficient of self-mated a Si3N4 and b WC-Co in rolling contact as a function of the number of revolutions for tests under water lubrication at a normal load of 250 mN, a sliding speed of 800 mm/s and a slip of 1, 4 or 10%

GIWM. The volumetric wear calculated using a wear coefficient kD,CD = 3.3 910-8 mm3/Nmm for the driven (curved) disc and kD,FD = 1.5 9 10-8 mm3/Nmm for the Fig. 8 SEM micrographs of the worn (a, b) driven and (c, d) driving discs of (a, c) Si3N4 and (b, d) WC-Co after 106 revolutions with 10% slip at a normal load of 250 mN and rolling speed of 800 mm/s in distilled water (arrow indicates rolling direction)

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In the present work, the tribological performance of selfmated Si3N4 and WC-Co was characterized under unidirectional sliding and rolling contact in both air of 50% r.h. and distilled water with respect to the application in microsystems. Experimental tests using laboratory tribometers with ball-on-disc and twin-disc geometry were accompanied by modelling approaches using the FEMbased wear simulator GIWM. Self-mated WC-Co showed a high wear resistance under both unlubricated as well as water lubricated sliding and rolling conditions. Friction coefficient for sliding and rolling under water lubrication

Microsyst Technol (2008) 14:1839–1846

Fig. 9 Experimentally determined wear (markers) and wear predicted by the GIWM (lines) of self-mated Si3N4 in rolling contact as a function of the number of revolutions in air of 50% r.h. for 4% slip (FN = 250 mN, v1 = 800 mm/s)

Fig. 10 Experimentally determined wear (markers) and wear predicted by the GIWM (lines) of self-mated Si3N4 in rolling contact as a function of the number of revolutions in air of 50% r.h. for 1, 4 and 10% slip (FN = 250 mN, v1 = 800 mm/s)

was also on a low level and almost independent of the applied normal load and slip, respectively. Enqvist et al. (2000a, b) ascribed the favourable friction and wear behaviour in air and pH-neutral media to the formation of thin WO3 films in the contact area. The results of the SEM examinations of the worn surfaces in this study supported these observations. Self-mated, unlubricated Si3N4 showed high friction coefficients and wear rates both under sliding and rolling conditions. SEM micrographs indicated brittle fracture as dominant wear mechanisms, which was in accordance with the results from (Jordi 2004). A pronounced running-in period was observed for Si3N4 under water lubrication. After the running-in period, both very low friction coefficients of l \ 0.02 and wear rates were observed for self-mated Si3N4 in sliding and rolling contact. In Jahanmir (2004) this behaviour was attributed to the formation of very smooth contact areas by tribochemical wear and the formation of a very thin hydrodynamic lubrication film, who’s bearing strength is enhanced by a

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gradually increasing viscosity towards the surface due to the formation of gel-like silica. However, the relatively high wear intensity during the running-in period in highly loaded sliding contact might become crucial under conditions where sufficient lubrication is not guaranteed, i.e. under transient loading conditions. The numerical wear simulation with GIWM was used to fit and predict volumetric wear data from the laboratory tests. A good agreement between simulation and experiment was achieved for water lubricated unidirectional sliding of self-mated WC-Co at normal loads between 400 and 1,600 mN. For unlubricated rolling of self-mated Si3N4, the discrepancy was significant for tests with 4% slip if the tests were run for more than 3 9 106 revolutions. This was attributed to a change in wear mechanisms accompanied by increased wear intensity. With increasing number of revolutions surface fatigue became more important than micro abrasion and tribochemical reactions resulting in the formation and growth of cracks and grain pull out. For rolling tests with 4 and 10% slip over 106 revolutions the wear predicted using GIWM was in relative good accordance to the experimental data. For tests with only 1% slip the simulated wear was significantly lower than the wear measured after the laboratory experiments. These results point out, that the wear coefficient kD obtained from laboratory tests under certain operating conditions can only be used as fit parameter in the wear simulation to reliably predict wear under different operating conditions, if the active wear mechanism remain the same. Under this assumption the wear simulator GIWM is a powerful tool, which should allow a tribologically optimized geometry design of micro components by the transfer of wear data from laboratory tests to FEM-based component design. Acknowledgments The authors would like to thank the Deutsche Forschungsgemeinschaft (DFG) for financial support within the frame of the Collaborative Research Centre 499 (SFB 499). ‘‘Construction, production and quality assurance of moulded microcomponents made of metallic and ceramic materials’’.

Reference Anon. (2001) Reports on micro and nano technologies. In: MINATECH. Proc conference on micro and nano technologies 2001. Teltow, Germany Archard JF (1953) Contact and rubbing of flat surfaces. J Appl Phys 24:981–988. doi:10.1063/1.1721448 Enqvist H, Beste U, Axe´n N (2000a) The influence of pH on sliding wear of WC-based materials. Int J Refractory Met Hard Mater 18:103–109. doi:10.1016/S0263-4368(00)00007-X Enqvist H, Ho¨gberg H, Botton GA, Ederyd S, Axe´n N (2000b) Tribofilm formation on cemented carbides in dry sliding conformal contact. Wear 239:219–228. doi:10.1016/S00431648(00)00315-X

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1846 Heckele M, Schomburg W (2004) Review on micro molding of thermoplastic polymers. J Micromech Microeng 14:R1–R14. doi:10.1088/0960-1317/14/3/R01 Hegadekatte V, Huber N, Kraft O (2006) Finite element based simulation of dry sliding wear. Tribol Lett 24:51–60. doi: 10.1007/s11249-006-9144-2 Hegadekatte V, Kurzenha¨user S, Huber N, Kraft O (2007) A predictive modeling scheme for wear in pin-on-disc and twindisc tribometers. In: Proc 34th Leeds–Lyon-symp Herz J, Schneider J, Zum Gahr K-H (2002) Tribologische Untersuchungen an Gleitpaarungen aus ZrO2, POM und Stahl fu¨r den Einsatz als wassergeschmierte mikromechanische Bauteile. Mat Sci Eng Tech 33:415–424 Jahanmir S, Ozmen Y, Ives L (2004) Water lubrication of silicon nitride in sliding. Tribol Lett 2004:409–417. doi:10.1023/ B:TRIL.0000044489.44053.be Jordi L, Iliev C, Fischer T (2004) Lubrication of silicon nitride and silicon carbide by water: running in, wear and operation of sliding bearings. Tribol Lett 17:367–376. doi:10.1023/B:TRIL. 0000044485.77019.fb Kaneko R (2000) Some recent progress in microtribology in Japan. Tribol Lett 9:89–96. doi:10.1023/A:1018812612458

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Microsyst Technol (2008) 14:1839–1846 Kurzenha¨user S, Schneider J, Zum Gahr K-H 2006. Untersuchungen zum Haft-und Gleitverhalten von Tribopaarungen fu¨r die Mikrotechnik. In: Proc Tribologie Fachtagung 2006. Gesellschaft fu¨r Tribologie, Go¨ttingen, pp 12/1–12/9 Piotter V, Gietzelt T, Merz L (2003) Micro powder-injection moulding of metals and ceramics. Sadhana Acad Proc Eng Sci 28:299–306 Scherge M (2001) Scale dependence of friction. In: Proc world tribology conference 2001. Vienna, pp 489/1–489/7 Schneider J, Zum Gahr K-H, Herz J (2005) Tribological characterization of mold inserts and micro components. Adv Micro Nano Syst 3:579–604. doi:10.1002/9783527616732.ch9 Zum Gahr K-H (1998) Tribological aspects of microsystems. In: Fukuda T, Menz W (eds) Micro mechanical systems—principles and technology. Elsevier, Amsterdam, pp 83–113 Zum Gahr K-H, Blattner R, Hwang D-H, Po¨hlmann K (2001) Microand macro-tribological properties of SiC ceramics in sliding contact. Wear 250:299–310. doi:10.1016/S0043-1648(01) 00595-6

Tribological characterization and numerical wear ...

adhesion or capillary forces can exceed the externally applied forces and thereby prevent operation of microsys- tems due to stiction under unfavourable ... Institut für Werkstoffphysik und Technologie, Technische. Universität Hamburg-Harburg, Hamburg, Germany. S. Kurzenhäuser Á J. Schneider Á K.-H. Zum Gahr.

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