Modification of Tribological Properties of Silicon by Boron Ion Implantation

Friction and wear properties of silicon used in the fabrication of microelectromechanical systems (MEMS) are important for their long-term reliability. In the present study, the authors have implanted single-crystal and polycrystalline silicon wafers with boron ions to improve their mechanical and tribological properties. The authors have studied the effects of ion implantation on the crystallinity, microstructure, nanohardness, and friction and wear properties and have found that silicon remains crystalline after ion bombardment at doses up to 2 × 10¹⁷ ions.cm^?2 but with a large amount of defects. The ion bombardment modifies elastic/plastic deformation characteristics and crack nucleation that occurs during indentation. There is a minor increase, ? 10-15 percent, in the nanohardness as a result of boron-ion implantation. Ion bombarded single-crystal silicon exhibits very low friction (0.05) and low wear factor (10^?6 mm³·N^?1m^?1) while slid against a 52100 steel ball. The coefficient of friction of bombarded silicon in dry air and dry nitrogen is even lower.     

A three-point-probe method for measuring resistivity and the Hall coefficient using Hall devices with minimal design complexity

A novel empirical method for express measurement of resistivity and the Hall coefficient, i.e. the sign, the concentration and the bulk mobility of the majority carriers in semiconductor (silicon) wafers is presented and tested. This approach is based on the parallel-field Hall devices with minimal design complexity containing only three contacts–two input and one (Hall) output. The unique simplicity of this three-point-probe method, the lack of numerical coefficients’ calculation and particular requirements for the geometrical dimensions, probe spacing, wafer form, etc. allows to obtain the necessary information following experimentally clear and technically reproducible steps. The data obtained from non-structured n- and p-type silicon wafers at carrier’s concentration of 10¹⁵ ? n; p ? 10¹⁶ cm⁻³ by appropriate probe arrangements corroborate very well with the results from wafers’ certificates and the results obtained using common measurement techniques. The error does not exceed 5–6% which is about the same as the accuracy of other approaches used for this purpose. The results are especially promising in IC fabrication and complementing the classical Van der Pauw method.     

Fretting wear behavior of nitrogen ion implanted titanium alloys in bovine serum lubrication

Nitrogen ion implantation was performed on biomedical titanium alloys by using of the PBII technology to improve the surface mechanical properties for the application of artificial joints. The titanium nitride phase was characterized with X-ray photoelectron spectroscopy (XPS). The nanohardness of the titanium alloys and implanted samples were measured by using of in-situ nano-mechanical testing system (TriboIndenter). Then, the fretting wear of nitrogen ion implanted titanium alloys was done on the universal multifunctional tester (UMT) with ball-on-flat fretting style in bovine serum lubrication. The fretting wear mechanism was investigated with scanning electron microscopy (SEM) and 3D surface profiler. The XPS analysis results indicate that nitrogen diffuses into the titanium alloy and forms a hard TiN layer on the Ti6Al4V alloys. The nanohardness increases from 6.40 to 7.7 GPa at the normal load of 2 mN, which reveals that nitrogen ion implantation is an effective way to enhance the surface hardness of Ti6Al4V. The coefficients of friction for Ti6Al4V alloy in bovine serum are obviously lower than that in dry friction, but the coefficients of friction for nitrogen ion implanted Ti6Al4V alloy in bovine serum are higher than that in dry friction. Fatigue wear controls the fretting failure mechanism of nitrogen ion implanted Ti6Al4V alloy fretting in bovine serum. The testing results in this paper prove that nitrogen ion implantation can effectively increase the fretting wear resistance for Ti6Al4V alloy in dry friction, and has a considerable improvement for Ti6Al4V alloy in bovine serum lubrication.     

Dual-motion fretting behavior of mandibular cortical bone against pure titanium

Dual-motion fretting tests of flat cortical bone specimens from fresh human mandible against pure titanium (TA2) ball were carried out on a modified test rig with tilt angle of 45°. The imposed maximal loads varied from 100 to 200 N. Dynamic characteristics of dual-motion fretting tests were analyzed in combination with micro-examinations via optical microscopy (OM), laser confocal scanning microscopy (LCSM) and scanning electron microscopy (SEM) together with energy dispersive X-ray spectrum (EDX). Two types of F-D curves (the trapezoid and elliptic mode) were recorded during the tests. The examination showed that the wear scars of the dual-motion fretting were asymmetric, and the tangential component of dual-motion fretting was in the mixed fretting regime. Under the lower imposed load, only some detachment of particles and scratches without cracking were observed even after 5×10⁴ cycles. The main wear mechanisms of the dual-motion fretting damage were the abrasive and adhesive wear. Under higher imposed loads, the cracks initiated and propagated mainly at the high stress side of contact edges. The wear mechanisms of the dual-motion fretting of cortical bone under higher imposed loads were the combination of the adhesive wear, abrasive wear, cracking and lubrication of the human bone tissue debris. And the lubrication of the debris played an important role during the dual-motion fretting processes.     

Three-dimensional atom mapping of boron in implanted silicon

The redistribution of boron in highly implanted 〈1 0 0〉 silicon (10 keV; 5×10¹⁵ at/cm²) annealed at 600 °C for 1 h was studied using both laser-assisted wide-angle atom probe (LaWaTAP) and secondary ion mass spectrometry (SIMS). As expected, the concentration was found to increase steeply to 10²¹ boron atoms/cm³ at a distance close to 35 nm and to decrease slowly to 10¹⁹/cm³, a value close to the boron level of the silicon substrate. For depth under 75 nm, the implantation profile of boron as given by LaWaTAP was found very close to that given by SIMS investigations without any calibration of the LaWaTAP data. For larger depth, the LaWaTAP profile is observed above that of SIMS. Detection limits of LaWaTAP for low dopant concentrations are discussed. The contribution of the background noise in the spectrum and sampling errors are considered. Fine-scale fluctuations not detected in SIMS profile and related to clustering were evidenced in LaWaTAP maps and profiles. Numerous boron clusters lying on {0 0 1} planes parallel to the implanted surface, a few nanometer in size, were identified and interpreted as boron interstitial clusters (BICs), in agreement with Cristiano et al. observations. They contained between 50 and 300 atoms (Si and B). This is much higher than that generally assumed in particular in ab-initio modelling where a few atoms BICs are considered. These clusters contained 7 at% of boron in average.     

Surface Hardness and Abrasive Wear Resistance of Ion-Implanted Steels

The hardnesses of nitrogen-implanted steel surfaces have been measured with an abrasive wear technique capable of characterizing surface layers as thin as 25 nm. Treated steel disks and reference disks were abraded with 1–5 μm diamond, and relative wear resistances were calculated from the mass losses. Surface hardness was obtained from a relationship between wear resistance and hardness.

The surface of a hardened and tempered carbon steel implanted with nitrogen ions (10¹⁷/cm²) was significantly harder than with other treatments including quench hardening and nitriding. The hardness decreased to the bulk value over a depth corresponding to the initial implantation depth.

Nitorgen-implanted stainless-steel surfaces wore faster than un-implanted ones, possibly due to interference with transformation hardening which normally occurs during wearing. This “softening” effect persisted to depths several times the depth of implantation, and may help to explain the reduction of sliding wear produced by the implantation of stainless steels. Analyses by Auger electron spectroscopy indicated nitrogen migrated toward the bulk during wear.

Titanium implanted in stainless steel (4.6 × 10¹⁷ ions/cm²) produced a very hard surface with more than 10 times the abrasive wear resistance of the bulk metal.     

Study of tribological performance of ECR-CVD diamond-like carbon coatings on steel substrates: Part 1. The effect of processing parameters and operating conditions

Diamond-like carbon (DLC) coatings were prepared on AISI 440C steel substrates at room temperature by electron cyclotron resonance chemical vapor deposition (ECR-CVD) process in C₂H₂/Ar plasma. Using the designed Ti/TiN/TiCN/TiC interfacial transition layers, relatively thick DLC coatings (1-2 μm) were successfully prepared on the steel substrates. The friction and wear performance of the DLC coatings was evaluated by ball-on-disk tribometry using a steel counterbody at various normal loads (1-10 N) and sliding speeds (2-15 cm/s). By optimizing the deposition parameters such as negative bias voltage, DLC coatings with hardness up to 30 GPa and friction coefficients lower than 0.15 against the 100Cr6 steel ball could be obtained. The friction coefficient was maintained for 100,000 cycles (∼2.2 km) of dry sliding in ambient environments. In addition, the specific wear rates of the coatings were found to be extremely low (∼10⁻⁸ mm³/Nm); at the same time, the ball wear rates were one order of magnitude lower. The influences of the processing parameters and the sliding conditions were determined, and the frictional behavior of the coatings was discussed. It has been found that higher normal loads or sliding speeds reduced the wear rates of the coatings. Therefore, it is feasible to prepare hard and highly adherent DLC coatings with low friction coefficient and low wear rate on engineering steel substrates by the ECR-CVD process. The excellent tribological performance of DLC coatings enables their industrial applications as wear-resistant solid lubricants on sliding parts.     

Study of TiAlSiN coatings post-treated with N and C + N ion implantations. Part 2: The tribological analysis

Ion implantation has found to be an effective approach to modify surface properties of materials. The present research investigates the effect of (1) nitrogen (N), and (2) carbon subsequently with nitrogen (C + N) implantations on the mechanical and tribological properties of the titanium–aluminium–silicon–nitride (Ti–Al–Si–N) coatings. Superhard TiAlSiN coatings produced by magnetron sputtering, of approximately 2.5 μm thickness, were post-treated by implantations of N or C + N at an energy level of 50 keV. The dose range was between 5 × 10¹⁶ and 1 × 10¹⁸ ions cm^?2. After implantation, the tribological performance of the coatings was investigated by a ball-on-disk tribometer against WC–6 wt.%Co ball under dry condition in ambient air. The wear performance of the samples was examined by a variety of characterization techniques, such as secondary electron microscopy (SEM), 3D profilometry, atomic force microscopy (AFM), and micro-Raman. The results showed that the wear performance of the samples depended strongly on the implanted elements and doses. There was slight improvement on the samples implanted with N whereas significant improvement was found on the C + N implantations. Particularly, the friction coefficient of the sample with 5 × 10¹⁷ C⁺ cm^?2 and 5 × 10¹⁷ N⁺ cm^?2 could reach 0.1. In addition, the specific wear rate of the sample was extremely low (0.85 × 10^?7 mm³/Nm), which was nearly two orders of magnitude below that of the un-implanted coating. The speculation of the mechanical and tribological analyses of the samples indicates that the improvement of the N implanted and C + N implanted TiAlSiN samples could be due to a combined effect of improved hardness, plus enhanced adhesive and cohesive strength. In addition, the improved performance of the C + N implanted samples could be explained by the formation of lubricating implanted-layer, which existed mostly in sp² C–C and C–N forms. The formation of such implanted layer could lead to a change of wear mode from strong abrasive wear to mostly adhesive wear, and result in a drop of friction coefficient and wear rate.     

Tribological Characteristics of Nitrogen (N+) Implanted Iron

The effect of implantation of nitrogen ions (1.5 MeV) on the friction and wear characteristics of pure iron sliding against M-50 steel (unimplanted) was studied in a pin-on-disk sliding friction apparatus. Test conditions included room temperature (～25°C), a dry air atmosphere, a load of ½ kg (4.9 N), sliding velocities of 0.043 to 0.078 m/s (～15 to 25 rpm), a pure hydrocarbon lubricant (n-hexadecane), or a USP mineral oil and nitrogen ion implantation doses of 5 × 10¹⁵ and 5 × 10¹⁷ ions/cm².

No differences in wear rates were observed in the low-dose (5 × 10¹⁵ ions/cm²) experiments. In the high-dose experiments (5 × 10¹⁷ ions/cm²), small reductions in initial (～40 percent) and steady-state (～20 percent) wear rates were observed for nitrogen-implanted iron riders as compared with unimplanted controls. No differences in average friction coefficients were noted for either dose.

Auger electron spectroscopy combined with argon ion bombardment revealed a subsurface Gaussian nitrogen distribution with a maximum concentration of 6 atomic percent at a depth of 8 × 10^?7 m (0.8 μm). Similar analysis within the wear scar (～2.0 × 10^?5 m subsurface) of an implanted rider after 20 μm of wear yielded only background nitrogen concentration. No inward migration of nitrogen ions was observed.     

Study on carrier mobility measurement using electroluminescence in frequency domain and electrochemical impedance spectroscopy

In this paper, the two methods, electroluminescence in frequency domain and electrochemical impedance spectroscopy, have been applied to investigate the carrier mobility in single layer polymer light-emitting diode employing the polymer MEH-PPV (Poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene]) as the light-emitting layer. The carrier mobility μ is 1.64 × 10⁻⁶ cm²/V s under the electric field 8.3 × 10⁵ V/cm measured by the method of electroluminescence in frequency domain. The electrochemical impedance spectroscopy results indicate that the carrier mobility μ is 1.08 × 10⁻⁶ cm²/V s under the electric field 7.5 × 10⁵ V/cm. A significant advantage of the two methods is that both of them can be applied to measure the carrier mobility in the thin film.     

Study of tribological performance of ECR-CVD diamond-like carbon coatings on steel substrates: Part 2. The analysis of wear mechanism

This paper describes the tribological performance of diamond-like carbon (DLC) coatings deposited on AISI 440C steel substrates by electron cyclotron resonance chemical vapor deposition (ECR-CVD) process. A variety of analytic techniques were used to characterize the coatings, such as Raman spectroscopy, atomic force microscopy (AFM) and nano-indentation. The sliding wear and friction experiments were carried out by the conventional ball-on-disk tribometry against 100Cr6 steel counterbody at various normal loads (1-10 N) and sliding speeds (2-15 cm/s). All the wear tests were conducted under dry sliding condition in ambient air for a total rotation cycle of 1 × 10⁵ (sliding distance ∼2.2 km). Surfaces of the coatings and the steel balls were examined before and after the sliding wear tests. The DLC coatings that had been tested all showed relatively low values of friction coefficient, in the range of 0.1-0.2 at a steady-state stage, and low specific wear rates (on the order of 10⁻⁸ mm³/Nm). It was found that higher normal loads or sliding speeds reduced the wear rates of the coatings. Plastic deformation became more evident on the coating surface during the sliding wear test at higher contact stresses. The friction-induced transformation of the coating surface into a graphite-like phase was revealed by micro-Raman analysis, and the flash temperature of the contact asperities was estimated. It was suggested that the structural transformation taking place within the wear tracks was mainly due to the formation of compact wear debris layer rather than the frictional heating effect. On the other hand, an adherent transfer layer (tribolayer) was formed on the counterface, which was closely related to the steady-state friction during sliding and the wear mechanisms. Fundamental knowledge combined with the present tribological study led to the conclusion that adhesive wear along with abrasion was probably the dominant wear mechanism for the DLC/steel sliding systems. Additionally, fatigue processes might also be involved in the wear of the coatings.     

Lubrication of Silicon Nitride and Silicon Carbide by Water: Running in,Wear and Operation of Sliding Bearings

The purpose of this work was to establish the conditions for the operation and break-in of water-lubricated ceramic bearings. The experiments consisted of sliding 1/4 silicon nitride or—carbide balls against pre-polished disks of the same material in water until tribochemical wear generates smooth conformal surfaces that allow hydrodynamic lubrication (<0.002) by very thin water films. This running in was performed at various sliding speeds (0.01-4m/s) and loads (0.5-20N). The minimum sliding speed for low friction were 0.04m/s for silicon nitride and 0.5m/s for silicon carbide, much lower than for conventional bearings. The load carrying pressures were 60-80MPa, which is higher than the usually pressures of thrust bearings. The hydrodynamic fluid film thickness was estimated with a standard integration of Reynolds' equations modified for circular geometry, it was to be 5-15nm for silicon nitride, 25nm for silicon carbide. Operation over long distances (80km) allowed us to measure the wear rate during hydrodynamic lubrication; this was found to be <2×10^–11mm³/nm, a rate acceptable for industrial application. A novel method completed during this work allows the determination of the wear rate during run-in. It varies with sliding velocity for silicon nitride, from 1 to 6×10^–5mm³/nm; it is constant at 4×10^–6mm³/nm for silicon carbide.     

Mechanical properties of the alloy Ti-6Al-4V irradiated with swift Kr ion

The radiation damage effect on the friction coefficient, wear, and microhardness of the alloy Ti-6Al-4V after 250 MeV krypton ion irradiation was studied. Tribological measurements were made in air, oxygen, and argon atmospheres and in a vacuum. The smallest friction coefficient for the irradiated samples occurred in argon and the vacuum. The wear of the unirradiated samples and those irradiated with low fluences (<10¹³ cm⁻²) increased in the vacuum and argon atmosphere. Wear was significantly reduced after irradiation with the fluence of 10¹⁴ cm⁻². The microhardness of the alloy Ti-6Al-4V increased by over 25% after irradiation with a large fluence.     

Investigation on the tribology of Zr ion implanted tool steel

AISI D3 tool steel was ion implanted with zirconium and the improvement in surface tribological properties investigated. The Zr ion implantation was done using a metal vapor vacuum arc (Mevva) broad-beam ion source, with a mean ion energy of 130 keV and at doses of 3.6×10¹⁶, 5×10¹⁶ and 1×10¹⁷ ions/cm². Wear, friction and hardness of the implanted samples were measured and compared to the performance of unimplanted steel. The wear resistance was increased by about a factor of two, the friction remained about the same or was possibly increased by a small amount and the near-surface hardness was improved by a factor of five or more by the ion implantation. We also investigated the effect on the Zr implantation profile of the multi-component energy distribution of the ion beam.     

Thermal diffusivity measurement of Au nanofluids of very low concentration by using photoflash technique

In this paper, the application of photoflash technique to measuring the thermal diffusivity of gold nanofluids of very low concentration at room temperature was presented. The nanofluid samples were prepared from the pulse laser ablation procedure. The thermal diffusivity was obtained by fitting the theoretical temperature signal to the experimental data, and it was found to increase linearly from 1.47 × 10⁻³ cm² s⁻¹ to 1.68 × 10⁻³ cm² s⁻¹ as the concentration increased from 1.11 mg/L to 3.18 mg/L. The increase in thermal diffusivity in these multidispersed nanofluids was attributed to the higher nanoparticle concentration as well as to the increasing presence of the smaller size nanoparticles.     

Accelerator of the НГ-12И neutron generator as an implanter of hydrogen ions

The use of an updated accelerator of the -12 neutron generator as a high-current implanter of hydrogen ions (protons and deuterons) with energies of 175–210 MeV into wafers made of crystalline silicon is described. The ion-beam scanning system used ensured nonuniformity in the irradiation of wafers with a diameter of 100 mm of <10%, which allowed the production of silicon-on-insulator wafers by the hydrogen splitting technique. The required particle fluence was 10¹⁷ cm^–2. A slight refinement of the setup allows wafers with diameters of up to 200 mm to be irradiated. The design features of the setup as they apply to different temperature conditions (down to a temperature close to that of liquid nitrogen) of the irradiation of 100-mm-diameter wafers are described.Translated from Pribory i Tekhnika Eksperimenta, No. 1, 2005, pp. 126–129.Original Russian Text Copyright © 2004 by Stepovik, Mokichev, Magda, Kiryushkin, Kozikov, Semkov, Kurochkin, Lukin, Khmelnitskii, Popov.     

High load AFM friction and wear experiments on V2O5 thin films

High load friction and wear experiments by means of atomic force microscopy were carried out at the surface of highly (0 0 1) oriented vanadium oxide V₂O₅ thin films deposited on silicon by reactive magnetron sputtering. Microscopic friction coefficient was estimated for wide range of loads. The nature of surface wear due to multiple, high load scanning is presented and discussed.     

Influence of Cr content on tribological properties of Ni3Al matrix high temperature self-lubricating composites

High temperature self-lubricating composites Ni₃Al-BaF₂-CaF₂-Ag-Cr were fabricated by powder metallurgy technique. In this paper the effect of Cr content on tribological properties at a wide temperature range starting from room temperature to 1000 °C was investigated. It was found that Ni₃Al matrix composite with 20 wt% Cr exhibited low friction coefficient of 0.24-0.37 and a wear rate of 0.52-2.32×10⁻⁴ mm³ N⁻¹ m⁻¹. Especially at 800 °C it showed the lowest friction coefficient of 0.24 and a favorable wear rate of 0.71×10⁻⁴ mm³ N⁻¹ m⁻¹. This implied that 20 wt% Cr was the optimal Cr content and its excellent tribological performance could be attributed to the balance between strength and lubricity.     

Photo-enhanced field emission study of TiO2 nanotubes array

Aligned TiO₂ nanotubes were synthesized by simple anodization of the Ti foil surface. The as-anodized product is further characterized by SEM, XRD, and PL. The tube inner diameter is found to be ≈60-80 nm with the average wall thickness ≈30 nm and areal density ≈15×10⁶/ cm². FE studies of the aligned TiO₂ nanotubes are carried out at base pressure of ≈1×10⁻⁸ mbar. The turn-on field observed for an emission current density of ≈10 μA/cm² is found to be ≈1.7 V/μm and current density of ≈44 μA/cm² is obtained at an applied field of ≈2.3 V/μm. Photo-enhanced FE study is carried out by shining visible and UV light on the cathode. The aligned TiO₂ nanotubes show sensitivity to both the light sources. The FE current shows fast switching response to the visible light. The increment in the preset current upon UV illumination can be attributed to the band edge excitation of the electrons. The free excitons associated with band gap of the TiO₂ nanotubes array may be responsible for the visible light sensitivity. TiO₂ nanotubes are also grown on the Ti wire and exhibit similar photo-enhanced behavior. The FE and photo-enhanced FE properties demonstrate the applicability of the aligned TiO₂ nanotubes in the FE based micro/nanoelectronic devices.     

Nano-wear of the diamond AFM probing tip under scratching of silicon, studied by AFM

In order to improve such a widely used microtribological testing procedure as surface scratching by an AFM diamond tip, an experimental study has been carried out using single-crystalline silicon as the tested material. Wear of the AFM diamond tip under scratching was observed by a decrease in the scratch depth with increasing wear cycles and by the direct imaging of the diamond tip shape using a Si₃N₄ AFM tip. It was shown that the current widely used experimental method, which assumes the diamond tip to be non-wearable, introduces uncontrollable error into the obtained values for the tested material's wear rate. The harder the tested material, the larger may be the tip wear, and, therefore, the bigger may be its effect on the obtained wear rate values. The specific wear rates for the diamond tip and a silicon wafer were estimated to be 1.4 × 10^-9 and 4.5 × 10^-4 mm³/(N m), respectively.