Wear of aligned silicon nitride under dry sliding conditions

The wear behaviour of textured silicon nitride (Si₃N₄) ceramics with aligned microstructures was analyzed under abrasive wear conditions. Dry reciprocating self-mated ball-on-flat wear tests were performed to study the influence of different microstructural plane/orientation combinations on the Si₃N₄ tribological behaviour. Textured materials showed superior wear resistance than non-textured reference Si₃N₄ for the whole range of loads and contact pressures, 5–50 N and 1.7–3.6 GPa, respectively, with an increase of about 70% for the maximum applied load. Within textured materials, the plane perpendicular to the extruding direction exhibited a 50% higher wear resistance (4 × 10^?5 mm³ N^?1 m^?1) than the parallel plane where the elongated grains were aligned. The severe wear process involved debonding, fracture and debris formation mechanisms. The progress of this sequence depended on the particular microstructure of each plane/orientation combination. A relationship between abrasive wear resistance and selected microstructural parameters has been established.     

Non-contact temperature measurement of silicon wafers based on the combined use of transmittance and radiance

We propose a non-contact temperature measurement method that combines the temperature dependence of transmittance below 600 °C and radiation thermometry above 600 °C. The combined method uses a polarization technique and the Brewster angle between air and a dielectric film such as SiO₂ or Si₃N₄ grown on silicon wafers. A prominent feature of this method is that both measurements of transmittance and radiance are performed with the same geometrical arrangement.For a semitransparent wafer, the measurement of p-polarized transmittance at the wavelengths of 1.1, 1.2 and 1.3 μm enables temperature measurement in the range from room temperature to 600 °C. For an opaque wafer above 600 °C, the p-polarized radiation thermometry at the wavelength of 4.5 μm allows the temperature measurement without the emissivity problem. The combined method with the use of transmittance and radiance is valid in the entire temperature range irrespective of variations of film thickness and resistivity.     

The tribological characteristics of TiCN coating at elevated temperatures

The tribological behaviour of TiCN coating prepared by unbalanced magnetron sputtering is studied in this work. The substrates made from austenitic steel were coated by TiCN coatings during one deposition. The measurements were provided by high temperature tribometer (pin-on-disc, CSM Instruments) allowing measuring the dependency of friction coefficient on cycles (sliding distance) up to 500 °C. The evolution of the friction coefficient with the cycles was measured under different conditions, such as temperature or sliding speed and the wear rate of the ball and coating were evaluated. The 100Cr6 balls and the Si₃N₄ ceramic balls were used as counter-parts. The former were used at temperatures up to 200 °C, the latter up to 500 °C. The wear tracks were examined by optical methods and SEM. The surface oxidation at elevated temperatures and profile elements composition of the wear track were also measured.The experiments have shown considerable dependency of TiCN tribological parameters on temperature. Rise in temperature increased both friction coefficient and the wear rate of the coating in case of 100Cr6 balls. The main wear mechanism was a mild wear at temperatures up to 200 °C; fracture and delamination were dominating wear mechanisms at temperatures from 300 to 500 °C.     

Friction behaviour of chemical vapor deposited self-assembled monolayers on silicon wafer

Friction characteristics of self-assembled monolayers (SAMs) coated on Si-wafer (1 0 0) by chemical vapor deposition technique were studied experimentally at nano and micro-scales. Four self-assembled monolayers, such as dimethyldichlorosilane (DMDC), diphenyldichlorosilane (DPDC), perfluorooctyltrichlorosilane (PFOTS) and perfluorodecanoicacid (PFDA) coated on Si-wafer (1 0 0) were used as test materials. Nano-scale friction was measured using atomic force microscopy (AFM) in the range of 0–40 nN normal loads, in LFM (lateral force microscopy) mode, using a contact mode type Si₃N₄ tip. Results showed that the friction of SAMs at this scale was influenced by their physical/chemical properties, while that of Si-wafer by its inherent adhesion. Further, micro-scale friction tests were also performed with a ball-on-flat type micro-tribotester under reciprocating motion. Friction was measured in the range of 1500–4800 μN applied normal loads using glass balls of varying radii, viz., 0.25, 0.5 and 1 mm. It was observed that the performance of SAMs was more superior to Si-wafer even at micro-scale, except for PFDA. Evidences obtained using scanning electron microscope showed that Si-wafer and PFDA exhibited wear at this scale. Wear in the case of Si-wafer was due to solid–solid adhesion and that in the case of PFDA due to the influence of humidity (moisture). The micro-scale friction in both these materials was severely influenced by their wear.     

Rolling contact fatigue using solid thin film lubrication

This paper addresses rolling contact fatigue (RCF) testing in ultra high vacuum (UHV) under high speed conditions. A ball–rod RCF test platform has been adapted for testing in UHV conditions that allows rapid accumulation of stress cycles, over 10 million cycles within 5 h of testing at 130 Hz rotation. The UHV environment and solid lubrication enables good vibration detection for the onset of spall. In this paper, approximately 0.2 μm of silver is applied to the balls and provides sufficient lubrication for up to 25 h of testing, or 50 million stress cycles in high vacuum at 130 Hz. Seventy-nine RCF tests using thin-film silver lubrication have been completed covering two ball sizes, and two rod and ball materials. 9.53 mm diameter Rex 20 steel and silicon-nitride (Si₃N₄) rods were tested against 7.94 mm diameter Rex 20 and 12.7 mm diameter M50 steel balls. It was found that ball size and material hardness did not affect the stress cycle life over a Hertzian contact stress range of 2.1–4.2 GPa and Rockwell C hardness range of 62–77. Rather, the key limiter to test length is lubrication depletion based on 79 tests and an average silver thickness of 0.2 μm. One of the two failure modes were observed for all tests: (i) early life spall of the silver coating, and (ii) depletion of silver lubrication followed by spall failure of both the ball and rod surfaces. A third-body storage model along with the Control Volume Fraction Coverage (CVFC) assumption and analysis was used to predict lubrication availability between asperities on the third body. There is good agreement between calculated and measured post-test lubrication thickness using the third-body storage model.     

Tribological behavior of RH ceramics made from rice husk sliding against stainless steel,alumina, silicon carbide,and silicon nitride

The tribological behavior of rice husk (RH) ceramics, a hard, porous carbon material made from rice husk, sliding against stainless steel, alumina, silicon carbide, and silicon nitride (Si₃N₄) under dry conditions was investigated. High hardness of RH ceramics was obtained from the polymorphic crystallinity of silica. The friction coefficients for RH ceramics disks sliding against Si₃N₄ balls were extremely low (<0.1), irrespective of contact pressure or sliding velocity. Transfer films from RH ceramics formed on Si₃N₄ balls. Wear-mode maps indicated that the wear modes were powder formation under all tested conditions, resulting in low specific wear rates (<5×10⁻⁹ mm²/N).     

Characteristics of a dynamic atomic force microscopy based on a higher-order resonant silicon cantilever and experiments

In order to improve the sensitivity and scanning speed of the dynamic AFM, a surface scanning method using higher-order resonant cantilever is adopted and investigated based on the higher-order resonance characteristics of the silicon cantilever, and the theoretical analysis and experimental verification on the higher-order resonance characteristics of the corresponding dynamic AFM cantilever are given. In this method, the cantilever is excited to oscillate near to its higher-order resonant frequency which is several times higher than that of the fundamental mode. Then the characteristic changes a lot compared with the first-order resonant cantilever. Because of the changes of the quality factor, amplitude and the mode shape of the cantilever, the higher-order resonant AFM gets higher sensitivity and scanning speed. Based on the home-built tapping-mode AFM experiment system, the resolution and the response time of the first and second order resonance measured by experiment are respectively: 0.83 nm, 0.42 nm; 1265 μs, 573 μs. The higher-order resonance cantilever has higher sensitivity and the dynamic measurement performance of the cantilever is significantly improved from the experimental results. This can be a useful method to develop AFM with high speed and high sensitivity. Besides above, the surface profile of a grating sample and its three-dimensional topography are obtained by the higher-order resonant mode AFM.     

In-service behaviour of (Ti,Si,Al)Nx nanocomposite films

This paper reports on the optimization of (Ti,Si_,Al)N_x coatings to improve the performance of coated tools in dry cutting applications. The performance and the wear mechanisms of (Ti,Si_,Al)N_x tungsten carbide coated tools were investigated. Tool life and tool failure modes were thoroughly examined by scanning electron microscopy (SEM) complemented with energy dispersive spectroscopy (EDS) in order to study the wear mechanisms. After 15 min at high cutting speed (200 m/min), the cutting edges of almost all the coatings still remained in good conditions. The results presented on this paper confirmed that nc-(Ti_1?xAl_x)/a-SiN_x nanocomposite coatings offer a significant potential to operate in extreme environments, since this coating outperformed one of the best solutions actually available in the market for high speed turning. An improvement on the tribological behaviour of (Ti,Si_,Al)N_x films was also observed with thermal annealing before the turning tests, due to a self hardening effect as consequence of the spinodal segregation of the (Ti,Al,Si)N metastable phase. On the other hand, no significative increase on the performance of the coated tools was observed with depositing an amorphous Al₂O₃ interlayer.     

Friction and wear durability studies on the 3D negative fingerprint and honeycomb textured SU-8 surfaces

The effects of two different textures (a 3D negative fingerprint texture and a honeycomb texture) on the tribological performance of SU-8 polymer surface have been investigated with a ball-on-disc tribometer. Friction and wear behaviors of the textured surfaces are conducted against a 4 mm diameter silicon nitride (Si₃N₄) ball counterface. The coefficient of friction for the negative fingerprint textured surface (μ=∼0.08) is much lower than that of the untextured surface (∼0.2) and the honeycomb textured surface (∼0.41) under a normal load of 100 mN and a rotational speed of 2 rpm. The coefficients of friction of the textured surfaces decrease with increasing normal loads between 100 mN and 300 mN. Above the normal load of 300 mN, the coefficient of friction of the negative fingerprint textured surface increases due to the occurrence of plastic deformation. The honeycomb textured surface has shown the highest coefficient of friction. The wear durability tests are also conducted at a normal load of 100 mN and a rotational speed of 500 rpm on the untextured/textured surfaces on SU-8 in the presence of an overcoat of a nano-lubricant, perfluoropolyether(PFPE). Six samples i.e. the untextured surface (Si/SU-8 and Si/SU-8/PFPE), the 3D negative fingerprint textured surface (Si/SU-8/FP and Si/SU-8/FP/PFPE) and the honeycomb textured surface (Si/SU-8/HC and Si/SU-8/HC/PFPE), each with and without PFPE nano-lubricant, have been investigated for their tribological behaviours. The negative fingerprint pattern on SU-8 with PFPE coating has shown the highest wear life of 60,000 cycles under a normal load of 100 mN. The reasons for excellent tribological performance of 3D fingerprinted SU-8 surface are analyzed using the Hertzian contact area calculation.     

Effect of pH on wear and friction of silicon nitride sliding against alumina in water

The influence of the pH in water lubricated sliding contacts was evaluated in terms of friction and wear. The experiments were carried out using a ball-on-disc setup. Si₃N₄ balls and Al₂O₃ discs were tested at temperature of (22±2) °C, sliding speed of (1.00±0.03) m/s and normal load of (54.25±0.17) N. Eight types of water with pHs varying from 3 to 12 were used as lubricant. The running-in period, friction coefficient and wear-volume were shown to be nearly independent of the initial pH values within the DLVO range (4≤pH≤10), since at these range the water׳s pH tends to the same value (7.6±0.3) during the test. Superlubricity could be reached with negligible wear by properly setting the electrochemical properties and operating conditions of the tribosystem.     

Frictional performance and near-surface evolution of nanocrystalline Ni–Fe as governed by contact stress and sliding velocity

While early reports on the wear performance of nanocrystalline alloys have suggested enhanced behavior consistent with their higher hardness compared to conventional microcrystalline alloys, there is still limited understanding of the mechanisms and limits of this enhanced behavior. In the present study, we examine the frictional response of a nanocrystalline Ni–20Fe alloy with 34-nm average grain size compared to the same film annealed to an average grain size of 500-nm. We examine the sliding friction performance of these films in contact with a 3.125 mm diameter Si₃N₄ spherical counterface under a range of normal forces (0.1–1.0 N) and sliding speeds (0.25–3.75 mm/s) in a non-oxidizing dry nitrogen environment. Under all conditions, the initial break-in coefficient of friction (COF) starts high, μ≈0.5–0.8, typical of uncoated metallic friction. However, there is an evolution in the COF which depends on normal force and sliding speed. At low sliding speeds (or normal forces), the steady-state COF decreases to μ≈0.2 whereas at higher sliding speeds and normal forces, the steady-state COF remains high at μ≈0.8. Focused ion beam cross-sectioning and TEM imaging reveal that in all cases, a multilayer substructure is formed in the deforming film: a refined ultrananocrystalline layer at the top surface, over a region of coarsened grains, atop the parent nanocrystalline alloy. The key distinction between the high-friction and low-friction conditions appears to lie in the triggering of a delamination process: high-friction conditions are associated with a thickening of the UNC layer through repeated delamination, whereas low-friction conditions are associated with a thin UNC layer that does not delaminate. Finite element analysis is used to aid in the understanding of how the magnitude and location of stresses drive these two distinct regimes.     

Tribological properties of Ni-17.5Si-29.3Cr alloy at room and elevated temperatures

The tribological properties of Ni-17.5Si-29.3Cr alloy against Si₃N₄ were studied on a ball-on-disc tribotester between room temperature and 1000 °C. The effects of temperature on the tribological properties of the alloy were investigated. The worn surfaces of the alloy were examined using scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The results indicated that the tribological behavior of the alloy expressed some differences with increase in testing temperature. At low and moderate temperatures (below 800 °C), the alloy showed excellent wear and oxidation resistances, and the wear rate of the alloy remained in the magnitude of 10^?5 mm³/Nm; but at elevated temperature (800–1000 °C), the wear and oxidation resistances decreased, and the wear rate of the alloy increased up to 10^?4 mm³/Nm. The friction coefficient decreased from 0.58 to 0.46 with the rising of testing temperature from 20 to 600 °C, and then remained nearly constant. The wear mechanism of the alloy was mainly fracture and delamination at low and moderate temperatures, and transformed to adhesive and oxidation at elevated temperatures.     

Wear behaviour of iron boride coatings produced by VPS technique on carbon steels

The vacuum plasma spray (VPS) technique is a useful tool for designing the characteristics of the coatings and, thus, the tribological properties of coated components. In the present paper, the wear properties of iron boride coatings produced by means of VPS technique on AISI 1040 steel samples were evaluated as a function of their microstructural characteristics. One coating type was obtained by using Fe₂B pure powder, the other with differentiated FeB + α-Fe blends, with the FeB content increasing and α-Fe content decreasing from the matrix to the surface. Wear tests were performed by means of a tribometer in block-on-ring configuration, without lubricant and in air, by using 40- and 60-N coupling loads and 0.8- and 1.6-m s⁻¹ sliding velocities. On Fe₂B coated samples, wear is essentially oxidative until the failure of the coating, the fragments of which cause a third body abrasion. On the FeB + α-Fe coated samples the wear mechanism is mainly oxidative and the coating totally wears out without spalling as a consequence of its graded structure, which succeeds in both improving the adhesion of the coating to the substrate and reducing the residual stress at the coating–substrate interface.     

Machining with AlCr-oxinitride PVD coated cutting tools

AlCrO_xN_1−x coatings were arc deposited onto HSS drills and WC–Co end mills at N₂/O₂ ratios of 0.9–0.75 using DC or 10 kHz pulse bias. Lower O₂ content coatings had a hardness of 32.5 GPa. whereas 0.25 O₂ ratio coatings were 24–25 GPa. AlCrO_xN_1−x coated 6.35 mm Dia. HSS jobber drills were tested by drilling 2.5D holes in AISI D2. 10 kHz 0.9 N₂ 0.1 O₂ coatings drilled a mean of 17.6 holes/µm, similar to commercial AlCrN coated drills at 17.8 holes/µm, whereas DC 0.75 N₂ 0.25 O₂ coatings drilled 9 holes/µm. AlCrO_xN_1−x coated WC–Co end mills had low steady state wear in milling AISI 316L (70 m/min, MQL) and cut >24 m whereas uncoated tools cut 6 m. In contrast to drilling DC 0.75 N₂ 0.25 O₂ tools had the least corner wear and low adhesion on the rake face.     

The ability of precision hard turning to increase rolling contact fatigue life

In this paper, precision hard turning is proposed for the finishing of the AISI 52100 bearing components to improve rolling contact fatigue life. This finishing process induces a homogenous microstructure at surface and subsurface layers. Fatigue life tests performed on a twin-disk machine show that rolling contact fatigue life increases as R_a value decreases. The bearing components reached 0.32 million cycles for R_a=0.25 μm and 5.2 million cycles for R_a=0.11 μm. In comparison, the bearing components achieved 1.2 million cycles with grinding (R_a=0.2 μm) and 3.2 million cycles with grinding followed by honing (R_a=0.05 μm) respectively.     

Wear characteristics of Cr3C2–NiCr and WC–Co coatings deposited by LPG fueled HVOF

Wear behavior of the HVOF deposited Cr₃C₂–NiCr and WC–Co coatings on Fe-base steels were evaluated by the pin-on-disc mechanism. The constant normal load applied to the pin was 49 N and sliding distance was 4500 m with velocity of 1 m/s, at ambient temperature and humidity. The specific wear rate of WC–Co coating was 3 mm³/N m and Cr₃C₂–NiCr coating was 5.3 mm³/N m. SEM/EDAX and XRD techniques were used to analyze the worn out surface and wear debris. The Fe₂O₃ was identified as the major phase in the wear debris. The wear mechanism is mild adhesive wear in nature.     

Friction and wear behavior of laser composite surfaced aluminium with silicon carbide

The present study concerns the wear behavior of laser composite surfaced Al with SiC and Al + SiC particulates. A thin layer of SiC and Al + SiC (at a ratio of 1:1 and dispersed in alcohol) were pre-deposited (thickness of 100 μm) on an Al substrate and laser irradiated using a high power continuous wave (CW) CO₂ laser. Irradiation leads to melting of the Al substrate with a part of the pre-deposited SiC layer, intermixing and followed by rapid solidification to form the composite layer on the surface. Following laser irradiation, a detailed characterization of the composite layer was undertaken in terms of microstructure, composition and phases. Mechanical properties like microhardness and wear resistance were evaluated in detail. The microstructure of the composite layer consists of a dispersion of partially melted SiC particles in grain refined Al matrix. Part of the SiC particles are dissociated into silicon and carbon leading to formation of the Al₄C₃ phase and free Si redistributed in the Al matrix. The volume fraction of SiC is maximum at the surface and decreases with depth. The microhardness of the surface improves by two to three times as compared to that of the as-received Al. A significant improvement in wear resistance in the composite surfaced Al is observed as compared to the as-received Al. The mechanism of wear for as-received vis-à-vis laser composite surfaced Al has been proposed.     

Wear behavior of electroless Ni–P–B4C composite coatings

In this research, the wear of electroless Ni–P and Ni–P–B₄C composite coatings was reviewed. Auto catalytic reduction of Ni in nickel sulfate and sodium hypophosphate bath including suspended B₄C particles with different concentration was used to create composite coatings with 12, 18, 25 and 33 vol.% of B₄C particles. Coatings 35 μm thick were heat treated at 400 °C for one hour in an argon atmosphere and the wear resistance and friction coefficient of heat-treated samples were determined by block-on-ring tests. All wear tests were carried out at 24 °C, 35% moisture, 0.164 m/s sliding speed and about 1000 m sliding distance. Graphs show that an electroless Ni–P–B₄C composite coating with 25 vol.% of B₄C had the best wear resistance against a CK45 steel counterface.     

Measurement of highly reflective surface shape using wavelength tuning Fizeau interferometer and polynomial window function

In this study, a 5N − 4 phase shifting algorithm comprising a polynomial window function and a discrete Fourier transform is developed to measure interferometrically the surface shape of a silicon wafer, with suppression of the coupling errors between the higher harmonics and the phase shift error. A new polynomial window function is derived on the basis of the characteristic polynomial theory by locating five multiple roots on the characteristic diagram. The characteristics of the 5N − 4 algorithm are estimated with respect to the Fourier representation in the frequency domain. The phase error of the measurements performed using the 5N − 4 algorithm is discussed and compared with those of measurements obtained using other conventional phase shifting algorithms. Finally, the surface shape of a 4-in. silicon wafer is measured using the 5N − 4 algorithm and a wavelength tuning Fizeau interferometer. The accuracy of the measurement is discussed by comparing the amplitudes of the crosstalk noise calculated by other algorithms. The uncertainty of the entire measurement was 34 nm, better than that of any other conventional phase shifting algorithms.     

Friction and wear properties of αFeSi2–Si alloy,ReSi1.8 and MoSi2 in ethyl alcohol

In this study, Fe–X at% Si alloy (X=70.5, 80.0 and 96.0), Re–64.3 at% Si and Mo–66.7 at% Si disk specimens were prepared by spark plasma sintering, and their friction and wear properties were investigated when they were slid against Si₃N₄ ball specimens in ethyl alcohol. The friction and wear properties of Si ingots were also examined. Fe–70.5 at% Si, Fe–80.0 at% Si, Fe–96.0 at% Si and Re–64.3 at% Si disk specimens exhibited friction coefficients as low as 0.15. It is considered that the low friction of the Fe–70.5 at% Si, Fe–80.5 at% Si and Fe–96.0 at% Si disk specimens was due to the formation of low friction silicon alkoxide and polyoxysilane on the worn surfaces of the disk specimens and the paired ball specimens. Re–64.3 at% Si disk specimens exhibited the highest microvickers hardness of all the disk specimens prepared in this study. In addition, the microvickers hardness of the Fe–X at% Si (X=70.5, 80.0, 96.0 and 100) disk specimen increased with increasing the Si content. Moreover, it was difficult to obtain dense Fe–90.0 at% Si disk specimens by sintering the annealed and crushed Fe–90.0 at% Si powder. However, dense Fe–96.0 at% Si disk specimens could be obtained by sintering the Fe–90.0 at% Si powder at 1403 K.