Effect of tool pin design on the microstructural evolutions and tribological characteristics of friction stir processed structural steel

In this research, friction stir processing (FSP) technique is applied for the surface modification of ST14 structural steel. Tungsten carbide tools with cylindrical, conical, square and triangular pin designs are used for surface modification at rotational speed of 400 rpm, normal force of 5 KN and traverse speed of 100 mm min⁻¹. Mechanical and tribological properties of the processed surfaces including microhardness and wear characteristics are studied in detail. Furthermore, microstructural evolutions and worn surfaces are investigated by optical and scanning electron microscopes. Based on the achievements, all designed pins were successfully applicable for low carbon steel to produce defect-free processed material. By the microstructural changes within the stirred zone, the processed specimen is obtained higher mechanical properties. This is due to the formation of fine grains as the consequence of imposing intensive plastic deformation during FSP; however, this issue is highlighted by using square pin design. In this case, minimum grain size of 5 μm and maximum hardness of 320 VHN, as well as, maximum wear resistance are all examined for the specimen modified by square pin.     

Wear behaviour of dental enamel at the nanoscale with a sharp and blunt indenter tip

Two different diamond nanoindenter tips, a rounded conical (～1200 nm radius) and a sharp cube corner (20–50 nm radius) were used to abrade bovine enamel. Square abraded areas (2 μm × 2 μm, 5 μm × 5 μm, 10 μm × 10 μm) were generated with loads that varied from 50 μN to 500 μN depending on the indenter tip. In addition normal and lateral forces were simultaneously measured along 10 μm single scratched lines with the sharp cube corner tip. SEM (scanning electron microscopy) and TEM (transmission electron microscopy) were also used to characterise the worn areas and debris. Two different wear mechanisms were observed depending on the geometry of the tip. The rounded tip generates a predominantly elastic contact that mainly compresses and plastically deforms the superficial material and generates severe shear deformation within the sub-surface material which, under certain conditions, fractures and removes material from the sample. The sharp tip cuts into and ploughs the enamel creating a wedge or ridge of material ahead of itself which eventually detaches. This sequence is repeated continuously for every passage of the sharp indenter tip. The different mechanisms are discussed in terms of abrading tip contact angle and enamel microstructure.     

Effects of carbon fiber length on the tribological properties of paper-based friction materials

Four kinds of paper-based friction materials reinforced with carbon fibers of 100, 400, 600 and 800 μm were prepared by paper-making processes. Experimental results showed that the friction materials became porous with fiber length increasing. The friction torque curves were flat except the sample with 100 μm fibers. The wear rate of the sample with 100 μm fibers was only 1.40×10⁻⁵ mm³/J. Tiny debris and fine scratches formed in the worn surface were the reason for excellent wear resistance of friction pairs with 100 μm fibers. The friction pairs with 400, 600 and 800 μm fibers showed typically abrasive wear and fatigue wear.     

Wear characteristics of a diffusion bonded sintered steel with short term surface treatments

A pin on disc machine was used to investigate the tribological behavior of a diffusion bonded sintered steel, with and without surface treatments of steam oxidation and manganese phosphating, over a wide range of speed (0.2–4 m/s) and applied load (4–500 N) in conditions of dry sliding and starved lubrication by oil impregnation of the porous structure of the materials. Besides the calculated wear rates, the wear mechanisms were determined by examination of the components of the rubbing system (sintered pin, disc and generated debris). A transition from a mild to a severe wear regime was identified, denoted by sharp changes of the wear rate. A transient wear regime, interposed between the mild and severe wear regimes, was detected. The rubbing surface quality degradation was in terms of material displacement around the pin circumference due to a delamination wear mechanism. Such regime was detected for the base sintered steel in dry sliding at 1 m/s for the load range 60–80 N and for both surface treatments in oil impregnated sliding at 0.5 m/s for the load range 200–300 N. Oil impregnation of the base sintered steel expanded the mild wear regime towards higher loads throughout the whole sliding speed range compared to dry sliding. For the lower speeds of 0.2 and 0.5 m/s, manganese phosphated samples in dry sliding exhibited higher transition loads compared to the base sintered steel. The lower oil impregnability of the surface treated samples, due to the sealing of porosity by steam oxidation, led to slightly lower transition loads in oil impregnated sliding, compared to the base sintered steel.     

Subsurface shear instability and nanostructuring of metals in sliding

Dry sliding wear conditions were used to obtain a 500 μm-thick layer of nanosize grains on copper samples. As shown, this layer reveals a flow behavior pattern similar to that of a viscous non-Newtonian fluid. Four structurally different zones were found in the longitudinal cross-sections of samples below the worn surface. Upper two of them are nanocrystalline and consist of many ～1 μm-thick sublayers, which show either laminar or turbulent flow behavior. These sublayers demonstrate different levels of elasticity as compared to each other and may be related to an interplay between work-hardening and thermal softening. Lower two zones undergo usual plastic deformation and severe fragmentation without viscous mass transfer. High level of Young's modulus in the fragmentation zone is evidence of insufficient thermal softening at that depth. We believe that viscous flow zones are the result of shear instability and subsequent shear deformation developed in subsurface layers due to thermal softening. Numerical study has been carried out to simulate friction-induced deformation and shear instability under conditions close to the experiment. As shown, such a situation is possible when deformation-generated heat is taken into account. Another interesting result relates to the sublayers’ strain rate distribution. It was found that 1 μm-thick sublayers may show either high strain rate gradient or zero strain rate as a function of depth below the worn surface. The latter case means that a pack of layers may exist and behave like an elastic body in ductile medium.     

Erosion-oxidation of uncoated,aluminized and chromized-aluminized 9Cr–1Mo steels under fluidized-bed conditions at 550–700 °C

Protective coatings, deposited mainly by thermal spraying and diffusion techniques, are considered a solution to extend the lifetime of many components in the energy production sector, such as heat exchangers. In this paper, some results are presented for uncoated, aluminized and chromized-aluminized 9Cr–1Mo steel, subjected to air and to impacts by 200 μm silica particles at angles of 30° and 90° and speeds of 7.0–9.2 m s^?1 at 550 –700 °C, in a laboratory fluidized-bed rig, to determine whether or not aluminized and chromized-aluminized diffusion coatings could protect the steel under such conditions. Erosion-oxidation damage was characterized by measurement of the mean thickness changes using a micrometer and examination of worn surfaces by scanning electron microscopy.Under most conditions, the coatings provided some protection to the substrate: under 30° impacts, up to 650 °C, and under 90° impacts, at 700 °C, both coatings were effective, whereas under 90° impacts, up to 650 °C, only the chromized-aluminized coating gave significant protection. However, for 30° at 700 °C, the oxide scale on the substrate was protective and the coatings were not needed. Explanations for these observations are presented in this paper, in terms of interactions between the erosion and oxidation processes for the materials.     

Electrogenerated chemical polishing of copper

Stress free polishing method is preferred for a damage free surface of copper with ultra-flatness and ultra-smoothness. Such a surface offers a perfect substrate for integrated circuits and micro-electromechanical systems fabrication. A new polishing method, called electrogenerated chemical polishing (EGCP), is proposed based on the principle of the scanning electrochemical microscope (SECM) and the diffusion controlled chemical reaction. Roughness of a Cu surface is reduced from 100.5 nm to 3.6 nm by the proposed method. To demonstrate the planarization capability of this new method, a patterned Cu surface with an array of micro-columns is planarized with a peak-valley (PV) value from 4.7 μm to 0.059 μm.     

Friction-induced ultra-fine and nanocrystalline structures on metal surfaces in dry sliding

Sliding friction tests of pin-on-disc type were carried out for carbon steel, pure iron and pure copper, and the microstructure and hardness near the sliding surfaces were investigated in detail. It was found that patchy transfer layers with ultra-fine (<200 nm) structures were produced on the disc surfaces. Nanocrystalline grains of 30–50 nm were identified for carbon steel, and submicron sized grains of 100–150 nm were observed in pure copper. The thicknesses of the ultra-fine structures were in the range of 10–50 μm, depending on the specimen material, sliding speed and applied load. The hardness near the sliding surface of pure iron was increased compared with the matrix. It was suggested that the hardening was due to the very fine structure formed by severe plastic deformation, but not due to phase transformation caused by thermal effects.     

Cavitation erosion of Fe–Mn–Si–Cr shape memory alloys

Cavitation erosion tests of three Fe–Mn–Si–Cr shape memory alloys were carried out at speed 34 and 45 m/s using a rotating disc rig, and their cavitation damage has been investigated by comparison with a referring 13Cr–5Ni–Mo stainless steel used for hydraulic turbine vanes. The research results proved that the cavitation erosion of the Fe–Mn–Si–Cr shape memory alloys is a failure of low cycle fatigue and fracture propagates along grain boundaries. After 48 h cavitation erosion the cumulative mass losses of the studied alloys at speed 45 m/s are more than theirs at speed 34 m/s; however, the effect of velocity on cavitation damage of the Fe–Mn–Si–Cr alloys is much lower than that of 13Cr–5Ni–Mo stainless steel. The cumulative mass loss of the 13Cr–5Ni–Mo stainless steel are 26.3 mg at speed 45 m/s and 3.2 mg at speed 34 m/s, and the mass losses of the Fe–Mn–Si–Cr alloys are within the range of 3.6–7.3 mg at speed 45 m/s and 2.0–4.1 mg at speed 34 m/s. The surface elasticity of the Fe–Mn–Si–Cr shape memory alloys is better than that of the 13Cr–5Ni–Mo stainless steel, and the effect of surface elasticity on cavitation damage increases with velocity. The excellent surface elasticity of the cavitation-induced hexagonal closed-packed (h.c.p.) martensite plays a key role in contribution of phase transformation to the cavitation erosion resistance of the Fe–Mn–Si–Cr shape memory alloys. The cavitation damage of the studied alloys at speed 45 m/s mainly depends on their surface elasticity, and the variation of 48 h cumulative mass loss (Δm) as a function of the elastic depth (h_e) can be expressed as Δm=2.695+[1371.94/(4(h_e−46.83)²+12.751)] with a correlation factor of 0.99345.     

Plastic deformation of 25CrMo4 steel during wear: Effect of the temperature,the normal force,the sliding velocity and the structural state

This article follows a previous study on friction and wear of 25CrMo4 steel [N. Khanafi-Benghalem, K. Loucif, E. Felder, F. Delamare, Influence de la température sur les mécanismes de frottement et d’usure des aciers X12NiCrMoSi25-20 et 25CrMo4 glissant sur du carbure de tungstène, Matériaux et techniques 93 (2005) 347–362]. The aim of our work is to study in more details the process of plastic deformation and the wear rate of this steel in lubricated sliding against cemented tungsten carbide, process observed in the previous work. The considered parameters are the temperature T (from 20 to 200 °C), the normal force P (from 500 to 1500 N), the steel structure (normalised HV 220 and quenched/tempered HV 480 states) and the sliding velocity v (from 0.05 to 0.3 m/s). We measured the friction coefficient and the sample total volume loss. A displacement sensor follows the volume loss evolution during the test; this follow-up is approximate because of the sample plastic flow which leads to the formation of peripheral burrs. All the tests conditions generate a significant plastic deformation of the sample steel, even in the quenched/tempered state: it produces a marked increase of the surface hardness, the work hardened layer being much finer for the quenched/tempered state (15 μm) than for the normalised state (40 μm at 20 °C). For temperatures T ≤ 100 °C in normalised state, the wear follows the Archard's law with an increasing rate with temperature. For T ≥ 120 °C, the wear rate decreases during the test, the global volume of wear being a decreasing function of T. For the quenched/tempered state, the wear rate decreases with the increase of the normal force, this decrease is less than 30% of the normalised state value. The material heating during the wear tests is well correlated with the friction dissipated power, but remains small, except in extreme cases (v maximum, great friction at high temperatures). These results suggest the existence of two wear mechanisms: abrasion by sample debris and burrs emission by plastic flow. The abrasion is probably the dominating mechanism for the tests carried out at the lowest temperatures. The plastic flow becomes a significant component at the highest temperatures. Using a contact model, we discuss to what extent the influence of the temperature and the strain rate on the steel hardness and ductility could explain the temperature and the sliding velocity effect on wear. Other phenomena are probably present: the influence of the steel microstructure and the lubricant on the size and/or the number of particles responsible for abrasion.     

Solid particle erosion behaviour of glass fibre reinforced boric acid filled epoxy resin composites

The tests which involved angular aluminium (Al₂O₃) particles with two different sizes of approximately 200 and 400 μm were conducted at the operating conditions namely different impact velocities of approximately 23, 34 and 53 m/s, two different fibre directions [0° (0/90) and 45° (45/−45)] and three different impingement angles of 30°, 60° and 90°. New composites with addition of Boric Acid filler material at 15% of resin exhibited upper wear than the neat materials without filler material. This means the filler material has decreased the erosion wear resistance. SEM views showing worn out surfaces of the test specimens were scrutinised.     

Tribological properties of polymer-sheet-adhered metal hybrid gear

A preliminary study was made on the tribology of nylon 66/poly(phenylene ether) polymer sheets adhered to steel gear teeth against a counter steel gear with reference to friction, surface morphology, noise reduction and torque in comparison with a pair of steel gears lubricated with molybdenum grease. Tribological experiments were performed in a gear-testing machine at a rotating speed of 1000 rpm under high torques of the driving and driven gears, recording torque of each gear and noise-frequency profiles. It was found that periodical torque changes in a range of 17–5 N m at 1000 and 3000 cycles (revolutions) turned to 13–8 N m at 5000 cycles, indicating a change to stable cycle and torque conduction, probably due to a plastic surface deformation of the adhered polymer sheet for a smooth contact of pairing teeth. A harsh noise emission in the frequency range of 3–5 kHz was reduced circa 5 dBA as compared with a pair of steel/steel gear. It was found, however, that noise abruptly increased when only one of the adhered polymer sheets was spontaneously removed from the gear surface, probably because of its low adhesive strength against a shear during gear cycle.     

Measurement and statistical analysis toward reproducibility validation of AZ4562 cylindrical microlenses obtained by reflow

This paper presents the statistical analysis applied into the shape of microlenses (MLs) for validating the high-reproducibility feature of their fabrication process. The MLs were fabricated with the AZ4562 photoresist, using photolithography and thermal reflow processes. Two types of MLs arrays were produced for statistical analysis purposes: the first with a cross-sectional diameter of 24 μm and the second with a cross-sectional diameter of 30 μm, and both with 5 μm spacing between MLs. In the case of 24 μm diameter arrays, the measurements showed a mean difference in diameter of 2.78 μm with a standard deviation (SD) of 0.22 μm (e.g., 2.78 ± 0.22 μm of SD) before the reflow, and 2.34 ± 0.35 μm of SD after the reflow. For the same arrays, the mean difference in height obtained was, comparatively to the 5.06 μm expected, 0.76 ± 0.10 μm of SD before the reflow and 1.91 ± 0.15 μm of SD after the reflow, respectively. A mean difference in diameter of 2.64 ± 0.41 μm of SD before the reflow, and 1.87 ± 0.34 μm of SD after the reflow was obtained for 30 μm diameter MLs arrays. For these MLs, a mean difference in height of 0.71 ± 0.12 μm of SD before the reflow and 2.24 ± 0.24 μm of SD after the thermal reflow was obtained, in comparison to the 5.06 μm of height expected to obtain. These results validate the requirement for reproducibility and opens good perspectives for applying this fabrication process on high-volume production of MLs arrays.     

Microstructure,mechanical properties and tribological behavior of tribofilm generated from natural serpentine mineral powders as lubricant additive

Surface-modified serpentine powders with an average size of 1.0 μm were dispersed into mineral base oil to improve the lubricating properties of oil, as well as to generate a thin tribofilm on the worn surface. SEM, TEM, nano-indentation and Stribeck testing were performed to study the morphology, microstructure, micromechanical properties and tribological behavior of the tribofilm, respectively. Results show that a nanocrystalline tribofilm, with a thickness of 500–600 nm, is formed on the worn surface under the lubrication of oil with 1.5 wt% serpentine. The film is mainly composed of Fe₃O₄, FeSi, SiO₂, AlFe and Fe-C compound (Fe₃C). A phenomenological model of the tribofilm generated by serpentine was developed based on the experimental results. The excellent mechanical properties, reinforced phase of embedded particles and porous structure of the tribofilm contribute to the reduction of friction and wear, especially in the case of boundary and mixed lubrication.     

High precision self-alignment using liquid surface tension for additively manufactured micro components

Self-assembly of components using liquid surface tension is an attractive alternative to traditional robotic pick-and-place as it offers high assembly accuracy for coarse initial part placement. One of the key requirements of this method is the containment of the liquid within a designated binding site. This paper looks to expand the applications of self-assembly and investigates the use of topographical structures applied to 3D printed micro components for self-assembly using liquid surface tension. An analysis of the effect of edge geometry on liquid contact angle was conducted. A range of binding sites were produced with varying edge geometries, 45–135°, and for a variety of site shapes and sizes, 0.4–1 mm in diameter, and 0.5 mm × 0.5 mm–1 mm × 1 mm square. Liquid water droplets were applied to the structures and contact angles measured. Significant increases in contact angle were observed, up to 158°, compared to 70° for droplets on planar surfaces, demonstrating the ability of these binding sites to successfully pin the triple contact line at the boundary. Three challenging self-assembly cases were examined: (1) linear initial component misplacement >0.5 mm, (2) angular misplacement of components, and (3) misplacement of droplet. Across all three assembly cases the lowest misalignments in final component position, as well as highest repeatability, were observed for structures with actual edge geometries <90° (excluding 45° nominal), where the mean magnitude of misalignment was found to be 31 μm with 14 μm standard deviation.     

Wear behavior of AISI D2 steel by enhanced ion nitriding with atomic attrition

An experimental study was performed to investigate the effect of atomic attrition on wear behavior of AISI D2 steel. Wear tests were conducted under three different loads (5, 10, and 20 N) and sliding speeds (100, 200, and 500 rpm), using ball-on-disk type tester and SiC ball. After wear test, the specimen nitrided with ion bombardment showed superior wear behavior. The enhanced hardness by ion bombardment could have a beneficial effect on increased wear resistance. In addition, a wider and more adhesive oxide layer formed on the worn surface of ion-bombarded specimen, because of the rougher structure on the surface by ion bombardment, could lead the surface to withstand wear for longer duration time, acting as a protective layer.     

Evolution of wear,roughness, and friction of Alloy 600 superalloy surfaces in water-submersed sliding

Self-mated wear and friction of Alloy 600 superalloy was studied in a water-submersed ring-on-rod configuration, loading the side of a 6.35 mm diameter rod across the flat surface of a rotating annular ring of 100 mm outer diameter and 70 mm inner diameter producing two sliding contacts along the ring. Tests were conducted at sliding speeds of 0.178 and 0.330 m/s for sliding distances of 100 m. Normal loads of 51 and 204 N were applied, and initial R_a surface roughnesses of the rings along the sliding direction were either smooth (～0.2 μm) or rough (～7.5 μm). Increased initial ring roughness caused a ～20-fold increase in rod wear at the lighter load, whereas at the heavier load increased initial roughness only caused a ～4-fold increase in wear. At lower initial ring roughness the 4-fold decrease in normal load caused a large (one order-of-magnitude) decrease in rod wear, whereas for rings of higher initial roughness the 4-fold decrease in normal load caused only minor (2-fold or less) decreases in rod wear. Wear during this 100 m sliding distance only experienced a minor effect from the 1.8-fold change in sliding speed, as did friction. In all cases friction coefficient rapidly settled into the range 0.6–0.7, except in the cases of lower load on rings of lower initial roughness where friction coefficient remained above 1 for most of this sliding duration. At this lower load the initial ～0.2 μm rod roughnesses increased to nearly 0.8 μm by the 100 m sliding distance, whereas at the higher load this same sliding distance resulted in roughnesses returning near to the initial 0.2 μm. It was hypothesized more highly loaded cases also went through initial roughening prior to smoothening back to 0.2 μm roughness within the 100 m sliding distance, and given additional sliding the more lightly loaded cases would also experience subsequent smoothening. Increasing sliding distance to 400 m, roughnesses indicated a smoothening back to 0.2 μm level during those lightly loaded tests, with friction coefficient correspondingly dropping from 1 into the 0.6–0.7 range observed in all other cases. Extended sliding to 400 m at light loading against rings of lower initial roughness also allowed a rod wear rate which increased with increased sliding distance to be observed, approaching the same rate observed against initially rough rings within the 100 m sliding distance.     

Characteristics of oxidative wear and oxidative mildwear

Dry sliding tests were performed for 45, 4Cr5MoSiV1 steels and 3Cr3Mo2V cast steel at 200 and 400 °C. The wears at 200 and 400 °C are of oxidative wear characteristic due to tribo-oxides formed on worn surfaces. However, the wear at 200 °C presents different wear behaviors and characteristics from the one at 400 °C. The wear at 200 °C is a typical oxidative mild wear, but the wear at 400 °C is beyond oxidative mild wear, here called oxidative wear. The characteristics of oxidative mild wear and oxidative wear were clarified.     

Effect on crystalline structure of AISI M2 steel using tungsten–thorium electrode through MRR,EWR, and surface finish

To investigate on the crystalline structure of AISI M2 steel by using tungsten–thorium electrode in electrical discharge machining (EDM) process was studied. Furthermore, the investigation were carried out for finding the value of material removal rate (MRR), electrode wear rate (EWR) and surface roughness (SR) of tool steel material depending upon three variable input process parameters. On the basis of weight loss, the value of MRR and EWR were calculated at optimized process parameter. Subsequently, surface topography of the processed material were examined through different characterization techniques like scanning electron microscopy (SEM), Optical surface profiler (OSP) and Atomic force microscopy (AFM), respectively. In XRD study, broadening of the peak was observed which confirmed the change in material properties due to the homogeneous dispersion of the particles inside the matrix. Lowest surface roughness and MRR of 0.001208 mg/min was obtained. Minimum surface roughness was obtained 1.12 μm and 2.18427 nm by OSP and AFM study, respectively. Also, minimum EWR was found as 0.013986 mg/min.     

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.