The reaction layer formed on steel by additives based on sulphur and phosphorus compounds under conditions of boundary lubrication

Sliding experiments were carried out under constant load and under continuously increasing load using a combination of a high carbon steel and a ball bearing steel with a mineral oil containing a commercial S-P compound under conditions of boundary lubrication. The reacted films formed on the carbon steel under conditions of severe boundary lubrication were examined by light microscopy, electron probe microanalysis and Auger emission electron spectroscopy. The surface products were composed essentially of dispersed thin films containing a high concentration of phosphorus and little sulphur and discontinuously distributed pits containing much more sulphur than the surrounding area. The element distribution on worn surfaces varied considerably with the applied load and the temperature of the contact.     

A specimen carrier, storage disc system for scanning electron microscopy (SEM): evaluation of stainless steel as a substratum for cell culture in vitro

A method of sample preparation for scanning electron microscopy (SEM) studies based on the use of stainless steel discs as a cell culture substratum is described in detail. A number of different cell lines were grown on stainless steel, and the growth patterns and biocompatibility of cells cultured on stainless steel were compared to identical cells cultured on aluminium, glass and plastic substrata. Stainless steel provides cells with an excellent growth surface which allows these cells to retain their normal growth characteristics and appearance. The non-toxic stainless steel discs can be manipulated through any combination of fixatives and organic solvents. The discs have been incorporated into a versatile system of sample preparation for SEM.     

Tribological phenomena in steel-composite brake material friction pairs

The mechanism of the formation of iron layers on brake friction materials sliding over a steel surface has been investigated. The nature of the metallization of friction material specimens and the changes in the surfaces as a result of sliding were studied by optical and scanning electron microscopy, electron probe microanalysis, X-ray diffraction, thermogravimetric analysis, gas Chromatographic analysis and microhardness measurements. A mechanism for the metallization of friction linings (iron layer formation) is proposed. Models of a tribological system for a frictional brake and of the subsurface layers of composite brake materials are described.     

Pattern abrasion of ultra-high molecular weight polyethylene: Microstructure reconstruction of worn surface

The friction and wear behavior of ultra-high molecular weight polyethylene (UHMWPE) sliding against bearing steel (AISI 52100) in a ring-on-block contact mode under the lubrication of aqueous solution of 3.5% NaCl was evaluated. The worn polymer surfaces were analyzed by means of three dimensional profiling, atomic force microscopy, Polarized Raman microanalysis, field emission scanning electron microscopy, and nanoindentation testing. It was found that unusual wavelike abrasion patterns were formed on the worn surface of UHMWPE under properly selected sliding conditions. In the presence of plowing effect, the molecular chains of UHMWPE and short-rod like microcrystalline grains of abrasion pattern were both further oriented along the plowing direction and became tiny and dense owing to microstructure reconstruction. Resultant microstructurally reconstructed worn surface of UHMWPE had a higher nanoindentation hardness and modulus as well as increased wear resistance.     

Atom probe,AFM, and STM studies on vacuum-fired stainless steels

The surface morphology of grades 304L and 316LN stainless steels, after low-temperature bake-out process and vacuum annealing, has been studied by atomic force microscopy (AFM) and scanning tunnelling microscopy (STM). The local elemental composition on the surface before and after thermal treatment has been investigated by atom probe (AP) depth profiling measurements. After vacuum annealing, AFM and STM show significant changes in the surface structure and topology. Recrystallization and surface reconstruction is less pronounced on the 316LN stainless steel. AP depth profiling analyses result in noticeable nickel enrichment on the surface of grade 304L samples. Since hydrogen recombination is almost controlled by surface structure and composition, a strong influence on the outgassing behaviour by the particular surface microstructure can be deduced.     

Ultrastructural effect of self-ligating bracket materials on stainless steel and superelastic NiTi wire surfaces

Frictional interactions between wires and brackets reduce the efficacy in orthodontic treatments. Self‐ligating brackets (SLBs) are now more often used due to lower frictional forces when compared with conventional‐ligating brackets. In this study, scanning electron microscopy and atomic force microscopy were used to examine the microstructural effects of stainless steel and ceramic SLBs on the surface roughness of stainless steel and superelastic NiTi wires both after in vivo clinical orthodontic treatment as well as in in vitro three‐point bending experiments. A combination of two wires—0.019 in. × 0.025 in. stainless steel wires and 0.016 in. superelastic NiTi wires—and two SLBs—both passive‐type stainless steel SLBs and active‐type ceramic SLBs—was applied for 4 months (bicuspid‐extraction) in an in vivo setting and for 1 month in an in vitro setting (200 g loads). After the SLB treatments, all wires exhibited severe scratches secondary to frictional interactions with the brackets. When used with the stainless steel SLBs (Damon 3MX®), the surfaces of 0.019 in. × 0.025 in. stainless steel (P < 0.0001) and 0.016 in. superelastic NiTi wires (P < 0.05) were significantly smoother than when used with the ceramic SLBs (Clippy‐C®). Such results suggest that orthodontic treatments with stainless steel SLBs are more effective than with ceramic SLBs. Microsc. Res. Tech. 75:1076–1083, 2012. © 2012 Wiley Periodicals, Inc.     

Versatile system for the temperature-controlled preparation of oxide crystal surfaces

We present a versatile system for the preparation of oxide crystal surfaces in the ultra-high vacuum (UHV) at temperatures up to 1300 K. Thermal treatment is accomplished by direct current heating of a tantalum foil in contact with the oxide sample. The sample temperature is measured by a thermocouple at a position close to the crystal and its reading is calibrated against the surface temperature determined by a second thermocouple temporarily attached to the surface. The design of the sample holder is based on a transferable plate originally developed for a commercial UHV scanning probe microscope. The system is, however, also suitable for the use with electron spectroscopy or electron diffraction based surface analytical techniques. We present results for the high-temperature preparation of CeO(2)(111) surfaces with atomically flat terraces exhibiting perfect atomic order and cleanliness as revealed by non-contact atomic force microscopy (NC-AFM) imaging. NC-AFM imaging is, furthermore, used to demonstrate the temperature-controlled aggregation of gold atoms on the CeO(2)(111) surface and their evaporation at high temperatures.     

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.     

The tribological characteristics of JS material under lubrication of oil

A material composed of a steel backing, a sintered porous bronze middle layer and a layer of reinforced PTFE, which is named JS material, was prepared. The friction, wear and limiting PV values of this material under dry friction as well as the lubrication of number 20 mechanical oil were studied using a MPV-1500 friction tester. The worn surface of JS material and the transfer film formed on the counterface of carbon steel were investigated using scanning electron microscopy (SEM) and electron probe microanalysis (EPMA). The results show that the friction, wear and limiting PV values of JS material can be greatly improved with the lubrication of oil. The results of SEM and EPMA analyses indicate that, under dry friction conditions, the solid lubricant PTFE and Pb easily transfer to the steel counterface and results in the reduction of friction and wear; while under the lubrication of oil, little transference of PTFE and Pb to the steel surface occurs and very small friction and wear are achieved. Analyses of frictional surfaces also suggest that the Pb filler gets enrichment on the rubbing surfaces, which is beneficial in increasing the adhesion of the transfer film with the steel surface.     

Loss of grain boundary segregant during ion milling

It is shown that material segregated to grain boundaries can be lost during ion milling. This specimen preparation artifact has been studied in the case of bismuth in copper and has also been observed for phosphorus in stainless steel. The loss is associated with specimen heating during ion milling and can be alleviated by good clamping and cooling of the specimen during milling. Specimen heating permits grain boundary diffusion of the segregating element to the specimen surfaces with subsequent loss of segregant from the specimen by evaporation or sputtering during ion milling. Loss of bismuth during in situ heating to 200–300°C is demonstrated. Therefore, care must be taken in specimen preparation for analytical electron microscopy measurement of such segregation. Similar effects may occur during ion milling of other materials, especially those where low thermal conductivity will result in high beam heating. In these cases, care must be taken to avoid loss of segregant during specimen preparation. Additional tests showed that no significant loss of segregant was observed during X-ray microanalysis, even at nominal room temperature and probe currents five-fold higher than that normally used for microanalysis.     

The mechanism of the initial stage of selective transfer during frictional contact

The initial stages of selective transfer during frictional contact between copper alloys and steel using three types of test configuration were studied by optical microscopy, scanning electron microscopy and electron probe X-ray microanalysis. A mechanism of selective transfer and its implications under conditions of boundary lubrication when the lubricant is also an electrolyte is proposed.     

Scanning electron microscopy and microprobe investigation of high speed sliding wear of aluminum oxide

Using two types of pin and disk apparatus the mechanisms of wear of single crystal spheres of aluminum oxide of controlled orientation against steel were investigated by scanning electron microscopy and electron probe X-ray microanalysis.The different mechanisms of wear and their controlling factors are discussed.     

Wear and corrosion wear of medium carbon steel and 304 stainless steel

Wear and corrosive wear involve mechanical and chemical mechanisms and the combination of these mechanisms often results in significant mutual effects. In this paper, tribological behavior, X-ray peak broadening, and microstructure changes of carbon steel AISI 1045 and stainless steel AISI 304 samples under simultaneous wear and corrosion were investigated and the results were compared with those obtained from dry wear tests. 3.5 wt.% NaCl solution was used as the corrosion agent and a pin-on-disk tribometer was employed to perform wear and corrosive wear tests.X-ray diffraction measurements have shown that by increasing the applied load, the worn surfaces of carbon steel samples reached a constant strain at which fracture and wear occurred. Whereas in 304 stainless steel samples, by increasing the applied load, broadening of X-ray diffraction peaks was decreased.Wear tests of carbon steel and stainless steel samples have shown smaller weight losses and lower friction coefficient in the presence of corrosive environment. Study of worn surfaces suggested that depending on wear environment and applied load, different features of wear mechanisms were involved.     

Oxide formation and alloying elements enrichment on TRIP steel surface during inter-critical annealing

The gas atmosphere in continuous annealing and galvanizing lines alters both composition and microstructure of the surface and sub‐surface of sheet steels. The alloying element enrichments and the oxide morphology on transformation‐induced plasticity steel surfaces are strongly influenced by the dew point of the furnace atmosphere and annealing temperature. The formation of a thin oxide film and enrichment of the alloying elements during annealing may result in surface defects on galvanized sheet products. The present contribution reports on the use of microanalysis techniques such as electron backscatter diffraction, glow discharge optical emission spectroscopy and electron probe micro‐analysis for the detailed surface analysis of inter‐critically annealed transformation‐induced plasticity steel such as oxide phase determination, microstructure and microtexture evolutions.     

Microstructure and mechanical properties of similar and dissimilar stainless steel electron beam and friction welds

Microstructure and mechanical properties of similar and dissimilar welds of austenitic stainless steel (AISI 304), ferritic stainless steel (AISI 430), and duplex stainless steel (AISI 2205) have been studied. Welding processes electron beam welding and friction welding were used. Optical, scanning electron microscopy, and electron probe microscopy were carried out to study the microstructural changes. Residual stress, hardness, tensile strength, and impact toughness testing were conducted to study mechanical behavior. Dissimilar metal electron beam welds of austenitic–ferritic, ferritic–duplex, and austenitic–duplex stainless steel welds contained coarse grains, which are predominantly equiaxed on austenitic, duplex stainless steel side, and they are columnar on the ferritic stainless steel side. Diffusion of elements was significant in electron beam welding and insignificant in friction welds. Austenitic–ferritic stainless steel exhibited tensile residual stress on the ferritic stainless steel side adjacent to the interface, compressive stresses on the austenitic stainless steel side that matches with the delta ferrite microstructure observed in this region. High compressive stresses were noted on duplex stainless steel side interface compared to austenitic stainless side interface. The highest tensile strength was observed in duplex–austenitic stainless steel joints. The impact strength and notch tensile strength of electron beam weldments are higher than the friction weldments. All electron beam and friction welds showed toughness lower than parent metals.     

表面微观形貌对疲劳强度影响的定量分析

利用原子力显微镜对表面定量测量的结果,通过建立有限元模型,分析了表面微观形貌表征参数对微应力集中的影响,研究了四种不同表面处理方式对lCrllNi2w2MoV不锈钢疲劳性能的影响。结果表明:各表征参数包括微缺陷温度、微缺陷的谷底半径和单峰平均间距对微压力集中都有影响,仅靠表面粗糙度参数无法真实反映表面微观形貌对微应力分布的影响;不同表面微观形貌所引起疲劳性能的变化与其表征参数的变化是一致的,利用表面形貌参数可以定量分析不同表面所导致的疲劳性能的改变。     

环保型缓蚀剂壳寡糖对304不锈钢化学机械抛光的影响

为研究环保型缓蚀剂壳寡糖对304不锈钢化学机械抛光过程和抛光效果的影响,探讨其在抛光过程中与金属表面的作用方式及吸附机制,采用化学机械抛光试验、接触角测量、扫描电子显微镜(SEM)和X-射线色散能谱仪(EDS)分析等方法,研究壳寡糖有机分子对304不锈钢化学机械抛光的影响,采用量子化学计算研究壳寡糖分子的全局反应参数,分析计算反应活性位点,采用分子动力学模拟有机分子在金属表面的吸附并分析活性原子的径向分布。结果表明：CMP抛光过程中添加壳寡糖能够通过吸附作用在304不锈钢表面形成一层疏水性的薄膜,抑制氧化剂对不锈钢表面的刻蚀,提高抛光后的表面质量;在壳寡糖质量浓度为400 mg/L时得到表面粗糙度为1.65 nm的最佳表面质量。量子化学研究表明,壳寡糖的活性反应位点主要为O原子,能够在金属表面形成多中心吸附。分子动力学模拟表明,壳寡糖有机分子能够平行吸附在金属表面,有机分子中的O原子能够与铁原子形成配位键,在吸附中占据主导地位。     

Acceleration of corrosive wear of duplex stainless steel by chloride in 69% H3PO4 solution

Plots of corrosive wear loss with load and anodic polarization curves during friction were examined for duplex stainless steel (DSS) in 69% H₃PO₄ solution with or without Cl⁻ by a pin-on-ring apparatus. Morphology of tracks and debris was observed in a scanning electron microscope. Variation of Vicker hardness of worn surface was also tested. The defects in wear subsurface were analysed by means of the positron annihilation technique (PAT) and a transmission electron microscope (TEM). The results show that the acceleration of chloride on corrosive wear of the steel is due to the brittle-fracture of the worn surface.     

Influence of Surface Roughness on the Lubrication Effect of Carbon Nanoparticle-Coated Steel Surfaces

In the present study, a systematic evaluation of the influence of the surface roughness on the lubrication activity of multi-wall carbon nanotubes (MWCNT) and onion-like carbon (OLC) is performed. MWCNT and OLC are chosen as they both present an sp²-hybridization of carbon atoms, show a similar layered atomic structure, and exhibit the potential to roll on top of a surface. However, their morphology (size and aspect ratio) clearly differs, allowing for a methodical study of these differences on the lubrication effect on systematically varied surface roughness. Stainless steel platelets with different surface finishing were produced and coated by electrophoretic deposition with OLC or MWCNT. The frictional behavior is recorded using a ball-on-disk tribometer, and the resulting wear tracks are analyzed by scanning electron microscopy in order to reveal the acting tribological mechanisms. It is found that the lubrication mechanism of both types of particles is traced back to a mixture between a rolling motion on the surfaces and particle degradation, including the formation of nanocrystalline graphitic layers. This investigation further highlights that choosing the suitable surface finish for a tribological application is crucial for achieving beneficial tribological effects of carbon nanoparticle lubricated surfaces.     

Corrosion-wear behaviour of thermal sprayed nanostructured FeCu/WC-Co coatings

The corrosion and corrosion-wear behaviour of a thermal sprayed nanostructured FeCu/WC-Co coating were investigated in a Hank's solution and compared to stainless steel AISI 304 and nanostructured WC-Co coatings. Electrochemical noise and potentiodynamic polarization measurements were conducted along with an ex situ scanning electron microscopy to unfold the response of these materials under these corrosive and corrosion-wear test conditions. The multiphase structure of the FeCu/WC-Co coating induces a complex corrosion behaviour. Under corrosion-wear conditions, the nanostructured FeCu/WC-Co coating exhibits a depassivation/repassivation behaviour comparable to the behaviour of stainless steel AISI 304 and nanostructured WC-Co coatings.