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。     

Transmission and scanning electron microscopy studies of deformation at erosion impact sites

Scanning and transmission electron microscopy methods have been employed to study topographic features and subsurface damage associated with erosive-particle impact craters in annealed 310 stainless steel surfaces. Angular Al₂O₃ and spherical glass particles approximately 50 μm in diameter were projected at a velocity of 59 m s^?1 to impact the surface at attack angles of 90° and 20°. Under these conditions, material was found to be displaced but not removed from the surface at isolated impact sites. A comparison was made with damage produced at diamond pyramid hardness indentations. Substantial differences were not observed. In general, a high dislocation density zone a few microns wide was found to surround both impact craters and hardness indentations. The width of this zone varied according to the size and shape of the crater and the direction of particle motion. Deformation twinning occurred at some impact sites. The plastic strain associated with impact craters in 310 stainless steel and copper was also determined by a method that is based on an analysis of selected-area electron channelling patterns.     

Precise fabrication of microtextured stainless steel surfaces using metal injection moulding

In this study, we show a new, cost effective and straightforward method to fabricate stainless steel (SS) microtextures with various geometries. We were able to design and texture a durable Ni mould insert by a microworking robot technique. Furthermore, the obtained microtextures were replicated onto stainless steel surfaces by metal injection moulding. A computer-controlled program enabled precise control of the spacing between the textures giving a broad choice for surface design. Surface geometries, such as micropillars and micropits with different dimensions, were produced on planar and curved surfaces. These results introduce a new platform for mass production of microtextured stainless steel surfaces with high surface control. The obtained surfaces have potential applications by meeting the demands of reducing surface contact and providing surface protection from mechanical damage.     

Electrochemical Analysis of the Slurry Composition for Chemical Mechanical Polishing of Flexible Stainless-Steel Substrates

The surface quality of the stainless steel affects the efficiency of flexible photovoltaics. Chemical mechanical polishing (CMP) is a finishing process that is used to prepare substrates for electronic devices. The CMP slurry composition is an important factor because additives in the slurry generally improve the polishing performance. However, it is limited to find the optimum conditions for the slurry by only experimental approaches. Thus, this study uses electrochemical analysis and friction monitoring to examine the effects of the abrasive, oxidizer, chelating agent, and pH. Electrochemical and monitoring analysis are useful for validating predictions and understanding interactions between the slurry and the stainless steel surface. Good correspondence was found between the predictions and the polishing results in more accurate. The corrosion rate (CR) obtained from the potentiodynamic polarization curve is proportional to the experimental results, as is the behavior of the curve and the coefficient of friction (COF). After only 3 min CMP, the best performing slurry (abrasive 39 wt %, oxalic acid 1 wt %, H₂O₂ 0.03 wt %, pH 1.5) improved the surface quality of 304 stainless steel by 4 nm. As a result, the proposed methods could help reduce the risks involved in stainless steel CMP slurry and these results could provide a reference for optimizing CMP slurry for flexible 304 stainless steel substrates.     

氧化剂含量对304不锈钢化学机械抛光的影响

为了探究氧化剂含量对304不锈钢化学机械抛光的影响及其作用机制,采用过氧化氢作为氧化剂,研究不同氧化剂质量分数下304不锈钢材料去除率及表面粗糙度值的变化规律,并基于接触角和电化学试验分析过氧化氢在抛光过程中的作用机制。结果表明：化学机械抛光过程中过氧化氢含量的增加有利于304不锈钢表面氧化膜的生成,从而有效提高304不锈钢的材料去除率及表面质量;但是过高的过氧化氢含量会导致304不锈钢表面氧化膜致密,使得化学作用与机械作用失衡从而造成304不锈钢表面质量下降;当过氧化氢质量分数为0.04%时,抛光后304不锈钢表面粗糙度值最低,仅有2.5 nm,材料去除率达到324.21 nm/min。     

SEM observations of the sliding behavior of A12O3 and CBN against steel

Both aluminum oxide (A1₂O₃) and cubic boron nitride (CBN) are being used as the abrasive medium in grinding wheels. To compare the effectiveness of these abrasives, a study was made, using the scanning electron microscope (SEM), to observe the sliding behavior and surface damage resulting from single particles of polycrystalline A1₂O₃ and CBN sliding dry against hardened M-50 tool steel. These experiments were run in the chamber of the SEM, which permitted direct observation of the contact areas at high magnifications. Friction force was monitored and videotape recordings were made continuously during these tests. Significantly lower friction and smoother wear tracks were obtained with the CBN. The A1₂O₃ grit produced much sharper ridges and considerable microcracking on the ridges. These microcracks were formed perpendicular to the wear track. The wear tracks obtained in the SEM were compared with the surfaces produced by surface grinding hardened steel with both CBN and A1₂O₃ wheels. At high magnifications, marked similarities between the ground surfaces and the surfaces produced by the basic sliding tests were noted. It is suggested that because of the large number of microcracks formed during the grinding process with the A1₂O₃, the fatigue life of parts ground with an A1₂O₃ wheel would be shorter than those ground with CBN. Practical experience indicates that this is true.     

Characterization of 4H-SiC (0001) surface processed by plasma-assisted polishing

For the finishing of some difficult-to-machine materials, such as silicon carbide, diamond, and so on, a novel polishing technique named plasma-assisted polishing (PAP) was proposed, which combined with the irradiation of atmospheric pressure water vapor plasma and polishing using soft abrasives. In this article, application of PAP to 4H-SiC (0001) substrate was conducted. We used helium-based water vapor plasma to modify the mechanical and chemical properties of the SiC surface. The results of X-ray photoelectron spectroscopy measurements indicate that the surface was efficiently oxidized after plasma irradiation, and the main product was SiO₂. CeO₂ was used as the abrasive material in PAP, the hardness of which was near to that of the oxidized surface. The scanning white light interferometer images of the PAP processed surface showed us that scratches disappeared and surface roughness also decreased from 4.410 nm p-v, 0.621 nm root mean square (rms) to 1.889 nm p-v, 0.280 nm rms. From the atomic force microscopy images, step and terrace structure was observed on the surface after PAP, which means an atomically flat surface was obtained. The PAP processed surface was observed using cross-sectional transmission electron microscope, which indicated that almost no crystallographical defects were introduced.     

Damage-free tribochemical polishing of diamond at room temperature: a finishing technology

Polished surfaces are characterized by a geometric shape and a surface finish, the latter being defined by surface roughness (smoothness) and subsurface damage. In general, mechanically polished surfaces have a high geometric precision and are optically smooth, but they are subjected to surface and subsurface damage. Tribochemical polishing gives smooth surfaces and damage-free subsurfaces, but the surface geometric precision is often poor at the submicron level. Diamond is the hardest material known, and the standard polishing technique for such hard materials is mechanical polishing, causing surface and subsurface damage. In this paper a novel method of tribochemical polishing of natural and synthetic monocrystalline diamond at room temperature is described, which gives very smooth surfaces of, at least, (100) planes, free from surface and subsurface damage within the instrumental detection limits. Such diamond surfaces are van der Waals bondable to other materials. With this novel technology only low material removal rates can be achieved. Therefore, it is mostly adapted as a finishing technique. The described polishing technology can be applied to other (hard) materials as well.     

Investigation of Chemical/Mechanical Polishing of Niobium

A chemical/mechanical method for polishing flat niobium sheets to a mirror finish was developed. Various polishing slurries with different open circuit potentials and pH values were considered. All slurries fell within the niobate region of the Pourbaix diagrams, indicating that slurries are in a thermodynamically stable region. Oxidation characteristics of the niobium in the various slurries were determined by XPS and confirmed previously published work that niobium forms various layers of stable niobium oxides roughly 4.5–4.7 nm in thickness on the surface. A multi-step polishing method that relies on mechanical abrasion of the surface proved to be effective, and particles of different hardness and size were explored. Niobium wafers with initial peak-to-valley (PV) surface roughness of 3 to 7 μm were polished. The multi-step process utilized a slurry containing 1 μm diameter alumina particles to polish this initial roughness down to a submicrometer level. The final polish was provided by a slurry containing smaller particles. The oxide slurry with 70 to 100 nm silica particles gave the best mirror finished surface, with PV = 235 nm, Ra = 32 nm, and RMS = 39 nm. While polishing caused some disorder in the niobium metal, using the oxide slurry gave results closer to those obtained by buffered chemical polish (BCP), which exhibits the highest degree of atomic order based on XPS studies. A polishing process starting with mechanical abrasion, followed by a two-step mechanical polish, is successful for obtaining smooth niobium surfaces on flat wafers.     

Low damage lamella preparation of metallic materials by FIB processing with low acceleration voltage and a low incident angle Ar ion milling finish

Metallic materials are known to be very sensitive to Gallium (Ga) focused ion beam (FIB) processing. Crystal defects formed by FIB irradiation degrade the transmission electron microscope image quality, and it is difficult to distinguish original defects from FIB process-induced damage. A solution to this problem is the low acceleration voltage and low incident angle (LVLA) Argon ion milling, which can be incorporated as an extensional countermeasure for FIB damage removal and eventually for preparation of high-quality lamellae. The transmission electron microscope image quality of iron single crystal could be improved by removing crystal defects using the low acceleration voltage and low incident angle Argon ion milling finish. Lamella quality of the processing result was almost similar with that of the conventional electrolytic polishing. As a practical application of the process, low damage lamella of stainless cast steel could be prepared. Effectiveness of the FIB system equipped with the low acceleration voltage and low incident angle Argon ion milling function as a tool to make high-quality metallic material lamellae is illustrated.     

Electron backscattered diffraction characterization technique for analysis of a Ti2AlNb intermetallic alloy

This investigation was conducted to ascertain the benefits of electropolishing after mechanical polishing for electron backscattered diffraction of a Ti₂AlNb intermetallic Ti−21Al−29Nb (at.%) alloy containing the orthorhombic (O) and body-centered-cubic (BCC) phases. Electropolishing was performed at −40 °C in 6% H₂SO₄ methanol solution. Atomic force microscopy was used to measure the surface topography in attempt to correlate nano-scale surface roughness with electron backscatter diffraction pattern quality. The results suggest that mechanically polishing with colloidal silica (SiO₂) or alumina followed by electropolishing is a sufficient surface preparatory technique for producing quality electron backscattered diffraction patterns for O + BCC microstructures. However, poor pattern quality results after mechanically polishing without electropolishing. High-quality orientation maps for O-dominated O + BCC microstructures were only possible through mechanical polishing followed by electropolishing. The data also suggest that surface roughness, on the order of 50 nm, has less effect on pattern quality than subsurface deformation. Overall, removing the near-surface damage was more critical than reduction of topography.     

Nanoscale machinability and subsurface damage machined by CMP of soft-brittle CdZnTe crystals

Nanoscale machinability and subsurface damage induced by chemical mechanical polishing of three kinds of single crystals were investigated by nanoscratch and high-resolution transmission electron microscope (HRTEM). When the constant loads increase from 800 μN to 3,200 μN, the friction coefficient adjacently linearly increases from 0.199 to 0.292, due to the surface machining hardening effect. As the slight wiping on the surface of Cd_0.9Zn_0.1Te (111) leads to microscratches, the surface turns worse, resulting in the decrease and fluctuation of friction coefficient. Shear band appears on the surface of Cd_0.96Zn_0.04Te (111), while it disappears on the surfaces of Cd_0.96Zn_0.04Te (110) and Cd_0.9Zn_0.1Te (111), replacing with more obvious plastic flow pile-up, and showing the better nanoscale machinability. The cross-sectional HRTEM images show that after CMP the damage layer is 2 nm, and only consists of amorphous state, indicating the main material removal mode of chemical dissolving. While after lapping and mechanical polishing, wear track with width of about 50 nm is still left on the machined surface, and subsurface damage layer is about 10 nm.     

Early stages of wear of copper steel, and electroless nickel against

The early stages of wear of copper, mild steel, an alloy steel, and electroless nickel in the as-deposited and heat-treated conditions, with a load of 50 g against a dry nitrided steel wheel with a surface speed of 0.28 m s⁻¹, were measured using a Talysurf and a precision relocation technique, and the worn surface was examined using scanning electron microscopy. Wear occurred mainly by abrasion. Extensive ploughing with cooper resulted in metal removal and redeposition on the surface. Rapid and severe removal of patches of material occurred witb mild steel, and fragments of the metal were redeposited on the surface. As-plated electroless nickel formed many small cracks in the wear tracks. These were absent in the heat-treated coating when surface damage occurred by brittle fracture of the Ni₃P. Profilometry results taken during the wear tests were analysed and related to the microscopical results and the wear processes.     

Effect of counter materials on coefficients of friction of TiN coatings with preferred grain orientations

In order to investigate the effect of counter materials on the coefficients of friction of TiN coatings with preferred grain orientations, the coefficients of friction against six counter materials (ball) were measured. The ball materials were aluminum (A1050), stainless steel (SUS304, SUS440C), bearing steel (SUJ2), carburized steel (SWRM10), cemented tungsten carbide (WC-Co) and alumina (Al₂O₃). After tests, the worn flat surfaces of balls and the wear tracks of TiN coatings were analyzed by the electron probe micro analysis (EPMA) and the auger electron spectroscopy (AES) to observe the Ti oxide film on each ball material and the adhesion of ball materials to the TiN coatings. The Ti oxide film was observed on the worn flat surfaces of the ball materials and the ball materials did not adhere to the TiN coatings in case that the low coefficients of friction were obtained.     

电化学机械复合抛光薄膜太阳能电池柔性不锈钢衬底

设计了针对薄膜太阳能电池柔性不锈钢衬底的电化学机械复合抛光法以满足其对表面粗糙度、光反射率和有害物质扩散的要求。首先,设计并制造了一种用于平面加工的复合阴极刀具,理论分析了它的材料去除机理。然后,结合法拉第原理和黏着摩擦理论分析了电化学腐蚀行为和摩擦力作用行为,解决了电化学腐蚀和机械去除钝化膜的匹配一致性问题。最后,以50mm×50mm×0.3mm规格的304不锈钢为阳极工件,对提出的方法进行了实验验证。结果显示:对衬底加工20min后,其表面粗糙度Ra从124nm降到10nm;表面反射率从加工前的56.8%提高到62.4%;表面金属氧化层的形成(氧化铁和氧化铬),有效阻挡了Fe和Cr离子的扩散。实验显示,提出的方法是处理柔性不锈钢表面的有效方法,成本低、效率高。     

硬质粒子摩擦法电铸新技术的研究

提出一种新型的硬质粒子摩擦法电铸技术，从理论上深入探讨了硬质粒子摩擦法电铸技术的沉积机理，并通过金属镍的电铸试验加以验证。理论分析和试验结果表明：硬质粒子摩擦法电铸技术在阴阳极之间引入硬质粒子，并通过电铸芯模的旋转，带动硬质粒子运动，使其不断摩擦、撞击阴极表面，能有效地去除沉积层表面的吸附气泡和积瘤，获得表面平整光亮的电铸层；通过减薄扩散层和扰动结晶过程，能细化晶粒，提高电铸速度。研究结果显示，硬质粒子摩擦法电铸技术在回转体类薄壁零件的电铸成形中有实用价值。     

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.     

Friction of PM ferritic stainless steels at temperatures up to 300 °C

Two ferritic stainless steels (409Nb and 434L) manufactured through powder metallurgical techniques were wear tested at different temperature conditions (up to 300 °C). Two sliding speeds were used, and tests were carried out against a wrought austenitic stainless steel. Materials’ wear performance was characterized through friction coefficients and analysis of wear tracks was carried out through scanning electron microscopy. Results have shown an adhesive wear mechanism. Oxidized ferrite particles have also been found on wear tracks.     

Effect of Modified Silica Abrasive Particles on Nanosized Particle Deposition in Final Polishing of Silicon Wafers

The silane coupling agent γ-aminopropyl triethoxysilane (APTS) and polyethylene oxide (PEO) are proposed to modify the SiO₂ abrasive particles for final polishing of silicon wafers. The effects of the modified silica abrasive particles on nanosized particle deposition, roughness, and removal rate of the silicon wafer are explored in detail. PEO is proved to be a potential modifying agent for controlling deposition of large particles (～410 nm diameter), leading to low roughness (R_a = 0.097 nm), and APTS is found to be effective in controlling deposition of both large and small particles (～410 and ～200 nm diameter, respectively), resulting in lower roughness (R_a = 0.054 nm).     

Influence of Steel Type on the Propensity for Tribochemical Wear in Boundary Lubrication with a Wind Turbine Gear Oil

Tribochemical wear may occur at the interface between a surface and a lubricant as a result of chemical and mechanical interactions in a tribological contact. Understanding the onset of tribochemical wear damage on component surfaces requires the use of high resolution techniques such as transmission electron microscopy (TEM). In this study, two steel types, case carburized AISI 3310 and through-hardened AISI 52100, were wear tested using a ball-on-disk rolling/sliding contact tribometer in fully formulated commercial wind turbine gearbox oil under boundary lubrication conditions with 10% slip. With the exception of steel type, all other test conditions were held constant. Conventional tribofilm analysis in the wear tracks was performed using X-ray photoelectron spectroscopy, and no significant composition differences were detected in the tribofilms for the different steel disk types. However, TEM analysis revealed significant tribochemical wear differences between the two steel types at multiple length scales, from the near-surface material microstructure (depth < 500 nm) to the tribofilm nanostructure. Nanometer-scale interfacial cracking and surface particle detachment was observed for the AISI 52100 case, whereas the tribofilm/substrate interface was abrupt and undamaged for the AISI 3310 case. Differences in tribofilm structure, including the location and orientation of MoS₂ single sheet inclusions, were observed as a function of steel type as well. It is suggested that the tribochemical wear modes observed in these experiments may be origins of macroscopic surface-initiated damage such as micropitting in bearings and gears.