Preparation of non-spherical silica composite abrasives by lanthanum ion-induced effect and its chemical–mechanical polishing properties on sapphire substrates

Chemical–mechanical polishing is the only technology that can provide a global planarization, and has become widely accepted. Abrasives are one of the important factors influencing chemical–mechanical polishing. In order to improve surface planarization and increase material removal rate of sapphire substrates, non-spherical silica composite abrasives were synthesized by lanthanum ion-induced effect-assisted growth method. Scanning electron microscopy showed the morphologies of non-spherical silica composite abrasives were peanut-shaped, chemical–mechanical polishing tests displayed the material removal rate of the non-spherical silica composite abrasives increased by 32.6% compared with spherical silica composite abrasives, Ambios Xi-100 surface profiler indicated the best surface roughness of sapphire substrate was 1.540 nm, and the element compositions of solids after polishing were analyzed by X-ray photoelectron spectroscopy, which investigated the interactions between abrasives and sapphire substrates. Non-spherical silica composite abrasives may lead to more solid-chemical reactions with sapphire substrates, and higher material removal rate may be also attributed to the mechanical grinding effect enhanced owing to the unique shape to achieve the purpose of material removal.     

Preparation of porous Fe2O3/SiO2 nanocomposite abrasives and their chemical mechanical polishing behaviors on hard disk substrates

Abrasives play an important role in chemical mechanical polishing (CMP) processes. Compact solid silica particles, which have been widely used as abrasive in CMP slurries, may cause surface defects because of their high hardness. Porous silica abrasive exhibits better surface planarization and fewer scratches than traditional solid silica abrasive during the polishing of hard disk substrates. However, the improvement in material removal rate (MRR) was not significant. Therefore, porous Fe₂O₃/SiO₂ nanocomposite abrasives were prepared and their CMP performances on hard disk substrates were investigated. Experiment results indicate that the MRR of slurry containing porous Fe₂O₃/SiO₂ nanocomposite abrasives is obviously higher than that of slurry containing pure porous silica abrasive under the same testing conditions. MRR increases with the increase of the molar content of iron in porous Fe₂O₃/SiO₂ nanocomposite abrasives. Moreover, surfaces polished by slurries containing the porous Fe₂O₃/SiO₂ nanocomposite abrasives exhibit lower surface roughness, fewer scratches as well as lower topographical variations than that by pure porous silica abrasive.     

Removal rate model for magnetorheological finishing of glass

Magnetorheological finishing (MRF) is a deterministic subaperture polishing process. The process uses a magnetorheological (MR) fluid that consists of micrometer-sized, spherical, magnetic carbonyl iron (CI) particles, nonmagnetic polishing abrasives, water, and stabilizers. Material removal occurs when the CI and nonmagnetic polishing abrasives shear material off the surface being polished. We introduce a new MRF material removal rate model for glass. This model contains terms for the near surface mechanical properties of glass, drag force, polishing abrasive size and concentration, chemical durability of the glass, MR fluid pH, and the glass composition. We introduce quantitative chemical predictors for the first time, to the best of our knowledge, into an MRF removal rate model. We validate individual terms in our model separately and then combine all of the terms to show the whole MRF material removal model compared with experimental data. All of our experimental data were obtained using nanodiamond MR fluids and a set of six optical glasses.     

Implications of Polishing Techniques in Quantitative X-Ray Microanalysis

Specimen preparation using abrasives results in surface and subsurface mechanical (stresses, strains), geometrical (roughness), chemical (contaminants, reaction products) and physical modifications (structure, texture, lattice defects). The mechanisms involved in polishing with abrasives are presented to illustrate the effects of surface topography, surface and subsurface composition and induced lattice defects on the accuracy of quantitative x-ray microanalysis of mineral materials with the electron probe microanalyzer (EPMA).     

静电自组装制备复合磨粒及其 对铜的抛光特性研究

研究苯代三聚氰胺甲醛（BGF）微球与阳离子型聚电解质聚二烯丙基二甲基氯化铵（PDADMAC）、阴离子型聚电解质聚4－苯乙烯璜酸钠（PSS）之间的吸附特性,利用静电自组装技术改变和控制BGF微球的荷电特性,制备出不同形式的PEi BGF/SiO2复合磨粒,以Zeta电位、透射电子显微镜（TEM）和热重分析（TG）等手段对复合磨粒进行了表征,并利用这些复合磨粒制备了铜片抛光用的复合磨粒抛光液。抛光试验表明,吸附在聚合物微球表面和游离于抛光液中的SiO2磨粒在抛光中均起到材料去除作用。传统单一SiO2磨粒抛光液的铜材料去除率为264 nm/min,PE0 BGF/SiO2混合磨粒抛光液的铜材料去除率为348 nm/min,PE3 BGF/SiO2复合磨粒抛光液的铜材料去除率为476 nm/min。经上述3种抛光液抛光后的铜表面,在5 μm×5 μm范围内,表面粗糙度Ra从0.166 μm分别降至3.7 nm、2.6 nm和1.5 nm,峰谷值Rpv分别小于20 nm、14 nm和10 nm,复合磨粒抛光液对铜片有良好的抛光性能。     

Magnetorheological nanofinishing of BK7 glass for lens manufacturing

BK7 is a high-quality crown glass which is used where additional benefits such as temperature sensitive applications of fused silica glass are not required. Due to very low inclusion content with extremely low bubbles, BK7 glass can find its application in lens manufacturing. The present work focuses on nanofinishing of the BK7 glass specimen for ratifying its utility in practical application. A programmable logic controlled 3-axis motions are fed to the magnetorheological (MR) rotating tool for finishing the glass specimen. MR polishing fluid used for nanofinishing consists of deionized water, magnetic iron particles, and cerium oxide powder. Under the influence of magnetic field, the stiffened MR polishing fluid is assisted in reducing the surface roughness of glass up to nanolevel range. Optical properties such as transmittance, absorbance, and reflectance of finished BK7 glass are analyzed and found suitable for lens manufacturing. Results of higher surface quality with excellent finishing are obtained by the present MR finishing process. After 90?min of finishing, the surface roughness values R_a and R_q are reduced to 17 and 27?nm from the initial values of 41 and 57?nm, respectively. To study the surface morphology, scanning electron microscopy is performed on BK7 glass.     

Material sensitive scanning probe microscopy of subsurface semiconductor nanostructures via beam exit Ar ion polishing

Whereas scanning probe microscopy (SPM) is highly appreciated for its nanometre scale resolution and sensitivity to surface properties, it generally cannot image solid state nanostructures under the immediate sample surface. Existing methods of cross-sectioning (focused ion beam milling and mechanical and Ar ion polishing) are either prohibitively slow or cannot provide a required surface quality. In this paper we present a novel method of Ar ion beam cross-section polishing via a beam exiting the sample. In this approach, a sample is tilted at a small angle with respect to the polishing beam that enters from underneath the surface of interest and exits at a glancing angle. This creates an almost perfect nanometre scale flat cross-section with close to open angle prismatic shape of the polished and pristine sample surfaces ideal for SPM imaging. Using the new method and material sensitive ultrasonic force microscopy we mapped the internal structure of an InSb/InAs quantum dot superlattice of 18 nm layer periodicity with the depth resolution of the order of 5 nm. We also report using this method to reveal details of interfaces in VLSI (very large scale of integration) low k dielectric interconnects, as well as discussing the performance of the new approach for SPM as well as for scanning electron microscopy studies of nanostructured materials and devices.     

Preparation of porous alumina abrasives and their chemical mechanical polishing behavior

Porous alumina abrasives with different pore sizes were prepared using hydrothermal synthesis method by different hydrothermal temperatures. The pore structure, pore size and pore volume of the products were characterized by transmission electron microscopy and nitrogen adsorption desorption isotherm measurement. The chemical mechanical polishing (CMP) performances of porous alumina abrasives in hard disk substrate CMP were investigated. The results show that, the polished surface average roughness (Ra) decreases when the pore diameter of porous alumina abrasive increases. By comparison with solid alumina abrasive, the prepared porous alumina abrasives give lower Ra, and the porous alumina abrasive with 8.61 nm pore diameter has higher material removal rate under the same polishing conditions.     

Surface effects on Young’s modulus and hardness of fused silica by nanoindentation study

The surface Young’s modulus (E) and hardness (H) of fused silica samples have been studied by nanoindentation. Two factors strongly affect the results of E and H. One factor is the polishing quality of the fused silica surface. Poor polishing quality produces much smaller E and H than the literature values for bulk fused silica. The second factor is surface flatness. Even for a well-polished silica surface, an “arch bridge effect” may hinder the measurements of the true values of E and H. A correction procedure is proposed to eliminate this effect, and the corrected results show substantial improvements.     

Microscale characterization of granular deformation near a crack tip

This paper presents a study of microscale plastic deformation at the crack tip and the effect of microstructure feature on the local deformation of aluminum specimen during fracture test. Three-point bending test of aluminum specimen was conducted inside a scanning electron microscopy (SEM) imaging system. The crack tip deformation was measured in situ utilizing SEM imaging capabilities and the digital image correlation (DIC) full-field deformation measurement technique. The microstructure feature at the crack tip was examined to understand its effect on the local deformation fields. Microscale pattern that was suitable for the DIC technique was generated on the specimen surface using sputter coating through a copper mesh before the fracture test. A series of SEM images of the specimen surface were acquired using in situ backscattered electronic imaging (BEI) mode during the test. The DIC technique was then applied to these SEM images to calculate the full-field deformation around the crack tip. The grain orientation map at the same location was obtained from electron backscattered diffraction (EBSD), which was superimposed on a DIC strain map to study the relationship between the microstructure feature and the evolution of plastic deformation at the crack tip. This approach enables to track the initiation and evolution of plastic deformation in grains adjacent to the crack tip. Furthermore, bifurcation of the crack due to intragranular and intergranular crack growth was observed. There was also localization of strain along a grain boundary ahead of and parallel to the crack after the maximum load was reached, which was a characteristic of Dugdale–Barenblatt strip-yield zone. Thus, it appears that there is a mixture of effects in the fracture process zone at the crack tip where the weaker aspects of the grain boundary controls the growth of the crack and the more ductile aspects of the grains themselves dissipate the energy and the corresponding strain level available for these processes through plastic work.     

Machining and surface finishing of brittle solids

Ceramic materials are finished primarily by abrasive machining processes such as grinding, lapping, and polishing. In grinding, the abrasives typically are bonded in a grinding wheel and brought into contact with the ceramic surface at relatively high sliding speeds. In lapping and polishing, the ceramic is pressed against a polishing block with the abrasives suspended in between them in the form of a slurry. The material removal process here resembles three-body wear. In all these processes, the mechanical action of the abrasive can be thought of as the repeated application of relatively sharp sliding indenters to the ceramic surface. Under these conditions, a small number of mechanisms dominate the material removal process. These are brittle fracture due to crack systems oriented both parallel (lateral) and perpendicular (radial/median) to the free surface, ductile cutting with the formation of thin ribbon-like chips, and chemically assisted wear in the presence of a reactant that is enhanced by the mechanical action (tribochemical reaction). The relative role of each of these mechanisms in a particular finishing process can be related to the load applied to an abrasive particle, the sliding speed of the particle, and the presence of a chemical reactant. These wear mechanisms also cause damage to the near ceramic surface in the form of microcracking, residual stress, plastic deformation, and surface roughness which together determine the strength and performance of the finished component. A complete understanding of the wear mechanisms leading to material removal would allow for the design of efficient machining processes for producing ceramic surfaces of high quality. The research was supported in part by the National Science Foundation through grants MSS 9057082, Jorn Larsen-Basse, Program Director and DDM 9057916, Bruce Kramer, Program Director.     

Effect of substrate on structural and transport properties of sprayed Fe:ZnO polycrystalline thin films

ZnO thin films doped with iron have been grown by spray pyrolysis technique on glass and fused silica substrates in order to study the effect of substrate material on the structural, optical, and electro-magnetotransport properties of grown layers. The polycrystalline Fe:ZnO films have different growth orientation according to the substrate, though both films are highly transparent in the visible region of wavelength. The sample grown on glass substrate has larger magnetoresistance and lower electron mobility than that on fused silica substrate.     

Performance Analysis of Ball End Magnetorheological Finishing Process with MR Polishing Fluid

A ball end magnetorheological finishing (BEMRF) process was developed for finishing a flat as well as 3D workpiece surfaces. The BEMRF process has a wide scope in today's advanced manufacturing systems for finishing 3D complex surfaces. Magnetorheological (MR) polishing fluid is used as finishing medium in BEMRF process. The constituent of MR polishing (MRP) fluid includes ferromagnetic carbonyl iron powder, abrasives, and base fluid medium. The workpiece surface is mainly finished by abrasives contained in MRP fluid. Therefore, the different mesh size from 400 to 1200 and volume percent concentration from 5% to 25% of abrasives in MRP fluid were chosen as factors to study their effects on the developed process performance in terms of percent change in roughness values. Silicon carbide abrasives were chosen in the present experimental investigation. Experiments were performed on the ferromagnetic ground surfaces whose initial roughness values (R_a) were measured in the range of 0.428 to 0.767 µm. The experimental results revealed that the MRP fluid with 15 vol % abrasives of mesh number 400 demonstrated better improvements in surface texture of finished surface as compared to other MRP fluid compositions. The finished surface characteristics and textures were studied at microscopic level using scanning electron microscopy and atomic force microscopy.     

Sm掺杂核-壳结构介孔SiO2@CeO2复合颗粒的制备和抛光性能

在低模量介孔SiO2(Mesoporous silica, mSiO2)微球表面负载Sm掺杂CeO2纳米粒子,制备了具有均匀完整核-壳结构的非刚性mSiO2@Ce1-xSmxO2(x=0, 0.23)复合颗粒。借助XRD、 SEM、 HRTEM、 STEM-EDX Mapping、 Raman光谱和N2吸-脱附等技术对产物进行结构表征,利用AFM和三维光学轮廓仪评价Sm元素掺杂处理对mSiO2@Ce1-xSmxO2(x=0, 0.23)复合颗粒抛光效果的影响。讨论了Sm掺杂复合磨粒的高效无损超精密抛光机制。结果表明:掺杂处理可使mSiO2@Ce1-xSmxO2(x=0, 0.23)复合颗粒的抛光效率提高近36%,达到84 nm/min,同时获得具有原子量级精度的加工表面,抛光后SiO2薄膜的粗糙度平均值和均方根分别为0.14和0.17 nm。     

Development of surface finish during the polishing of porcelain ceramic tiles

Polishing tests on a laboratory scale have been used to simulate and study the industrial polishing process for unglazed porcelain ceramic tiles. Tile surface quality was assessed in terms of roughness and optical gloss. Tests with a sequence of progressively smaller silicon carbide abrasive particles showed a general trend of decreasing roughness and increasing gloss during the process. The coarser abrasives (larger than 400 grit number) caused the major change in surface roughness, while the finer abrasives (smaller than 400 grit number) produced the major change in gloss. In these materials the maximum gloss achievable by polishing is limited by the porosity of the ceramic. The rate of material removal during polishing with a coarse abrasive obeyed an Archard-type wear law, being linearly proportional to applied load, although load had little effect on the surface roughness attained after different durations of polishing. In contrast, load had a significant effect on gloss, with higher loads leading to higher values of gloss. The development of both roughness and gloss with polishing time is well described by quantitative empirical models involving a simple exponential function. The same model for gloss evolution is also shown to apply to data reported from industrial-scale polishing experiments in previous work.     

Application of BIB polishing technology in cross-section preparation of porous,layered and powder materials: A review

For the accuracy of experimental results, preparing a high quality polished surface and cross-section of the materials for further analysis using electron backscattered diffraction (EBSD), electron probe microanalysis (EPMA), and scanning probe microscopy (SPM) is extremely important. Broad ion beam (BIB) polishing, a method based on the principle of ion bombardment, has irreplaceable advantages. It makes up for the drawbacks and limitations of traditional polishing methods such as mechanical polishing, electrochemical polishing, and chemical polishing. The ions will not leave the bombardment area during polishing, which makes the BIB method suitable for porous materials. The energy of the ion beam can be adjusted according to the sample to reduce the deformation and strain of the polishing area, especially for fragile, soft, and hard materials. The conditions that need to be controlled during BIB polishing are simple. This paper demonstrated the unique advantages of BIB polishing technology in porous, layered and powder materials characterization through some typical application examples, and guided more researchers to understand and utilize BIB polishing technology in the development of new applications.     

The Nature of Mechanically Polished Surfaces of Copper

Surfaces of copper polished with diamond abrasives were examined by transmission electron microscopy; surfaces abraded on silicon carbide papes were also studied for comparison. There was no evidence of an amorphous layer, known as the Beilby layer, on any of the polished surfaces; the surface layers were crystalline and all showed evidence of plastic deformation. Slab-shaped cells were present at the surfaces that appear to correspond to the microbands or shear bands that have been observed in heavily cold-rolled copper. Some recrystallization occurred in the surfaces polished with 6-μm diamond abrasive, indicating some relaxation and modification of the microband-shear band structure; small subgrains were also observed, and it is concluded that they were also recrystallized grains. The degree of deformation at the surface decreased with increasing fineness of polish (i.e., from 6-μm diamond abrasive to 1 μm). The abraded surfaces consisted almost entirely of small subgrains, indicating that the shear band structure at these surfaces had nearly all recrystallized. It was concluded, however, that the highest surface temperature was attained when polishing with 6-μm diamond abrasive and then was only 100-150°C.     

Protection by diamond-like carbon films on fused silica slides from erosion by the impact of solid particles

Measurements were made with a new test for improved quantitative estimation of the mechanical protection of thin films on optical materials. The mechanical damage was induced by a sandblasting system using spherical glass beads. Development of the surface damage was measured by the changes in the specular transmission and reflection and by inspection using a surface profilometer (and a scanning electron microscope). The changes in the transmittance with the duration of sandblasting were measured for uncoated and coated fused silica slides. It was determined that the diamond-like carbon films double the useful optical lifetime of the fused silica. Conclusions were obtained for the fused silica surface removal mechanism and for the film removal mechanism.     

Glassomer—Processing Fused Silica Glass Like a Polymer

Fused silica glass is one of the most important high‐performance materials for scientific research, industry, and society. However due to its high chemical and thermal resistance as well as high hardness, fused silica glass is notoriously difficult to structure. This work introduces Glassomer, a solid nanocomposite, which can be structured using polymer molding and subtractive technologies at submicrometer resolution. After polymer processing Glassomer is turned into optical grade fused silica glass during a final heat treatment. The resulting glass has the same optical transparency as commercial fused silica and a smooth surface with a roughness of a few nanometers. This work makes high‐performance fused silica glass components accessible to high‐throughput fabrication technologies and will enable numerous optical, photonic and medical applications in science and industry.     

辐照对红外熔石英性质的影响(英文)

研究了高能电子、高能质子辐照对红外熔石英性质、光学面形的影响。研究了高能电子对红外熔石英面形的影响 ,结果表明 ,没有明显的面形变化。研究了高能质子对红外熔石英面形、可见和红外反射特性的影响。研究结果表明 ,没有观察到高能质子辐照对红外熔石英面形和反射特性的影响