Flatness maintenance and roughness reduction of silicon mirror in chemical mechanical polishing process

As an important optical component in laser system, silicon mirror surface is required to have micron-level flatness and subnanometer-level roughness. The research concentrates on how to improve roughness as far as possible while maintaining flatness of silicon mirror surface during chemical mechanical polishing(CMP) process. A polishing edge effect model is established to explain the reason of flatness deterioration, and a roughness theoretical model is set up to get the limit of perfect surface roughness. Based on the models above, a polishing device is designed to maintain the surface flatness, and the optimized polishing process parameters are obtained by orthogonal tests to get a near-perfect surface roughness. Finally the maintenance of flatness and the improvement of roughness can be achieved at the same time in one step of CMP process. This work can be a guide for silicon mirror manufacture to improve optical reflection performance significantly.     

Effects of chairside polishing and brushing on surface roughness of acrylic denture base resins

The effects of 3 chairside polishing kits and mechanical brushing on the surface roughness of 3 different acrylic denture base resins were compared. Acrylic denture base resins (auto-polymerizing, heat-polymerizing, injected heat-polymerizing resins) were examined after a tungsten carbide bur, and after chairside polishing using 3 polishing kits and pumice. The specimens were subjected to mechanical brushing using a wear tester to simulate 30 000 strokes of brushing. The surface roughness of the acrylic denture base resin specimens was measured using a contact profilometer. After the test, the random polished acrylic resins were evaluated by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Acrylic denture base resins polished using the 3 types of polishing kits had a smoother surface than those finished with the tungsten carbide bur (p<0.05). The surface of the resin polished by a TC cutter exceeded the R _a of 0.2 μm (p<0.05). The auto-polymerizing resin showed a significantly higher surface roughness than the heat-polymerizing resin and injected heat-polymerizing resin (p>0.05). In the case of polishing step wise, there was almost no change in surface roughness after brushing (p>0.05).     

Preparation of Non-spherical Colloidal Silica Nanoparticle and Its Application on Chemical Mechanical Polishing of Sapphire

Non-spherical colloidal silica nanoparticle was prepared by a simple new method, and its particle size distribution and shape morphology were characterized by dynamic light scattering(DLS) and the Focus Ion Beam(FIB) system. This kind of novel colloidal silica particles can be well used in chemical mechanical polishing(CMP) of sapphire wafer surface. And the polishing test proves that non-spherical colloidal silica slurry shows much higher material removal rate(MRR) with higher coefficient of friction(COF) when compared to traditional large spherical colloidal silica slurry with particle size 80 nm by DLS. Besides, sapphire wafer polished by non-spherical abrasive also has a good surface roughness of 0.460 6 nm. Therefore, non-spherical colloidal silica has shown great potential in the CMP field because of its higher MRR and better surface roughness.     

Determination of efficient superfinishing conditions for mirror surface finishing of titanium

To determine mirror surface finishing conditions and efficient and economical superfinishing conditions for pure titanium and titanium alloys, an abrasive film is used when superfinishing is performed under varying conditions. These conditions include the workpiece rotation speed, the oscillation speed, the contact pressure of the roller, the hardness of the roller, and the type of abrasive film. The superfinishing device is applied to polishing a thin and long cylindrical bar. A micro-finishing film and a lapping film were used as abrasive films. Al₂O₃ grains or SiC grains were used as abrasives. The surface roughness of a polished workpiece was measured using a stylus-type surface-roughness measuring instrument. As a result, the conditions to improve the polishing surface efficiently include high values for the workpiece rotation speed, oscillation speed and contact pressure. The roller hardness has no effect on the efficient polishing conditions. The mirror finish of a surface can be created using lapping film of 3 μm with Al₂O₃ grains after polishing to a steady surface roughness under the efficient polishing conditions.     

Influence of drying methods on fractal geometric characteristics of mesoporous silica aerogels

Chemical modification/ambient drying method and freeze drying method were introduced to research the synthesis of mesoporous silica aerogels. By analyzing N2 gas adsorption/desorption isotherms, the fractal geometric characteristics of gels were focused. The overall surface fractal dimensions were determined by analyzing N2 gas adsorption branch and a Frenkel-Halsey-Hill (FHH) equation was empolyed to determine surface fractal dimension Df . It is found that, during ambient drying process, VTMCS/VWetgel ratio plays a crucial role in the changes of geometric feature, the key point is 50%, when the ratio is lower, and surface roughness increases with the ratio, when it exceeds 50%, the surface is almost unaffected by the modification. While freeze drying always tends to get larger Df , freeze drying process could cause a rough surface of the gels. Compared with traditional porosity and specific surface area analyses, fractal geometry may be expected to be favorable for mesoporous structural analyses of materials.     

3D morphology and formation mechanism of fractures developed by true triaxial stressOA

As main part of underground rock mass, the three-dimensional(3D) morphology of natural fractures plays an important role in rock mass stability. Based on previous studies on 3D morphology, this study probes into the law and mechanism regarding the influence of the confining pressure constraints on3D morphological features of natural fractures. First, fracture surfaces were obtained by true triaxial compression test and 3D laser scanning. Then 3D morphological parameters of fractures were calcula...     

低能离子束刻蚀单晶硅表面形貌与粗糙度的研究

研究了低能Ar＋离子束对单晶硅表面的刻蚀效果.使用自制的冷阴极离子源,通过控制离子束的入射能量和刻蚀时间等因素,对单晶硅（100）表面进行刻蚀,采用原子力显微镜（AFM）和非接触式表面测量仪对刻蚀后硅片的表面形貌以及表面粗糙度（RMS）进行测量.实验结果表明：当离子束正入射、束流密度为20μA/cm2、刻蚀时间为30min、刻蚀距离为7cm时,入射能量从800eV增加到1 200eV的过程中,此时表面光滑起主要作用,表面粗糙度逐渐减小;继续增大入射能量到1 600eV时,表面粗糙度开始增大,当入射能量达到1 400eV时,通过AFM观察,硅片表面出现了自组织纳米点状结构,此时表面粗糙起主要作用;延长刻蚀时间同样可以看到粗糙度先减小后增加,延长刻蚀时间到90min,表面的粗糙度达到1.245nm,AFM观察表明,随着时间的增加,由于样片表面原子扩散影响,点状结构排列趋于均匀.     

Influence of CH3SiCl3 consistency on growth process of SiC film by kinetic monte carlo method

CH3SiCl3 (MTS)-H2-Ar system has been applied to prepare SiC film with chemical vapor deposition (CVD) method in this paper. For three facets of SiC film, some significant influence on growth rate, surface roughness, thickness and relative density brought by MTS consistency has been mainly discussed with kinetic monte carlo (KMC) method. The simulation results show that there is a certain scale for mol ratio of H2 to MTS (H2/MTS) with different deposition temperature. When MTS consistency increases, growth rate and surface roughness of three facets all increase, which manifests approximate linearity relationship. Thickness of three facets also increases while increasing trend of three facets thickness is different obviously. Although relative density of three facets all increases, increasing trend shows a little difference with MTS consistency increasing.     

Influence of surface finish and annealing treatment on oxidation behavior of Ti-48Al-8Cr-2Ag alloy

The effect of surface finish and annealing treatment on the oxidation behavior of Ti-48Al-8Cr-2Ag (molar fraction, %) alloy was investigated at 900 and 1 000 °C, respectively in air. Thermal gravimetric analysis (TGA) was conducted for the characterization of oxidation kinetics. The microstructures of oxide scales were studied by scanning electron microscopy (SEM) and transmission election microscopy (TEM) techniques. Unfavorable effect of the annealing treatment on the oxidation behavior of the coating was also investigated. The results indicate that the oxidation behavior of the alloy is influenced by surface finish and annealing treatment. The oxidation rate of ground sample is lower than that of the polished alloy at 1 000 °C in air. The former forms a scale of merely Al₂O₃, and the latter forms a scale of the mixture of Al₂O₃ and TiO₂. Annealing can improve the formation of TiO₂. Foundation item: Project(2007430028) supported by the Science and Technique Foundation of Henan Educational Committee, China     

单晶SiC的化学机械抛光及其增效技术研究进展

为了解决传统SiC化学机械抛光(CMP)加工效率低的问题,针对单晶SiC表面抛光质量和材料去除率指标,综述了应用传统碱性抛光液、混合磨粒抛光液及含强氧化剂抛光液对单晶SiC进行化学机械抛光的研究现状;为了提高SiC-CMP的化学和机械两方面作用,对SiC-CMP催化辅助增效技术、SiC电化学机械抛光(ECMP)技术、固结磨料抛光、光催化辅助抛光等增效新技术进行了系统综述;对SiC-CMP及其增效技术进行了分析、讨论,指出了当前的研究难点,展望了进一步提高单晶SiC抛光效率的研究方向.     

Formation of Epitaxial Heavy-doped Silicon Films by PECVD Method

Plasma-enhanced CVD(PECVD) epitaxy at 200℃ was used to deposit heavy doped n-type silicon films. Post-annealing by rapid thermal processing was applied to improve the properties of the epitaxial layer. By analyzing the Raman spectra and the imaginary part of the dielectric constant spectra of the samples, it was found that high-quality heavy-doped epitaxial n-type silicon layer can be obtained by optimizing the parameters of the PECVD depositing process. Reducing the electrodes distance of the PECVD had a great effect on the crystallzation of the epitaxialed n-type silicon films. Sillicon films with high-crystallization were obtained with the electrodes distance of 18 mm. Post-annealing process can improve the crystallization and reduce the resistance of the epitaxial films. In our research, it was found that the sheet resistance(R_□) of the post-annealed films with thickness of about 50 nm has a simple relationship with RPH3/SiH_4(ratio of the flow rate of PH_3 and SiH_4) of the PECVD processing: R_□=-184-125 lg(R_(PH3/SiH4)). In the end, high-quality epitaxial n-type silicon film was obtained with R_□ of 15 Ω/□ and thickness of ~50 nm.     

Investigation on the cleaning of KDP ultra-precision surface polished with micro water dissolution machining principle

A potassium dihydrogen phosphate (KDP) optical crystal was machined to an ultra-precision surface with water-in-oil (W/O) micro emulsion polishing fluid. The micro water dissolution principle utilized in the machining process is discussed, its planarization mechanism is illustrated, and an ultra-precision polished surface with 2.205 nm RMS roughness is obtained. However, a substantial quantity of residual contamination remained on the polished surface after machining. This can seriously impact the optical performance of the crystal, and so it must be removed. Fourier transform infrared (FTIR) spectroscopy was used to conduct an investigation into the composition of the surface residue, and the results showed that the residue was comprised of organic chemicals with hydrocarbon chains and aromatic ether, i.e., mostly the polishing fluid. The cleaning method and the principle on which the KDP ultra precision surface investigation is based are discussed in detail, and the cleaning experiments with selected KDP-compatible organic solvents were then performed. FTIR transmittance spectra measurement and microscopic observations were employed to assess the effects of the cleaning process on the surface of the KDP crystal. The results showed that toluene cleaning achieved the most desirable results. This cleaning method produced a surface roughness of 1.826 nm RMS, which allows the KDP crystal to be applied to subsequent engineering applications.     

Microstructure and Mechanical Property of Magnetron Sputtering Deposited DLC Film

A diamond-like carbon (DLC) film was deposited on YT14 substrate using magnetron sputtering (MS). The surface morphologies, roughness and bonding spectra of obtained film were characterized using scanning electron microscopy (SEM), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS), respectively, and its mechanical property and bonding strength were measured using a nanoindentation and scratch tester, respectively. The results show that the C-enriched DLC film exhibits a denser microstructure and smoother surface with lower surface roughness of 21.8 nm. The ratio of C sp2 at 284.4 eV that corresponds to the diamond (111) and the C sp3 at 285.3 eV that corresponds to the diamond (220) plane for the as-received film is 0.36: 0.64, showing that the C sp3 has the high content. The hardness and Young’s modulus of DLC film by nanoindentation are 8.534 41 and 142.158 1 GPa, respectively, and the corresponding bonding strength is 74.55N by scratch test.     

Influence and Optimization of Surface Roughness on Surface Integrity during Turning Using Grey Relational Analysis

Current machining studies have reported effects of prevalent and common factors, while ultra-high finish requires holistic approach to identify all factors and investigate their effects on machining of hard to machine materials. In this work, a less investigated yet important factor, roughness of the uncut surface, was studied, and its effects on the individual response, i.e., surface finish of the machined part, were found to be significant. AISI 316, which is mainly applied in strategic areas, was selected and three effective turning factors, cutting speed (A), feed rate (B), and roughness of the uncut surface (C) on three output responses including surface roughness of the machined surface (R_a), microhardness(HV), and material removal rate (MRR), were reported. Further, single response optimization of the individual output response and multi-response optimization of all the three responses were carried out. Taguchi L₉ orthogonal array based signal-to-noise (S/N) ratio method was used for individual response optimization, and grey relational analysis (GRA) was employed for multi-response optimization. Effects of the process factors on the output responses were evaluated through inclusive statistical analyses. The individual response optimization revealed that there was a considerable effect of roughness of the uncut surface on the machining performance. Results of the GRA illustrated that the speed during the cutting process and the feed rate had substantial trace on the surface integrity (indicated by R_a and HV) and production rate (indicated by MRR), while roughness of the uncut surface did not have a significant effect.     

液流悬浮抛光技术的应用研究

应用液流悬浮抛光技术获得的光电产品表面,不仅具有较好的表面粗糙度,而且抛光面没有亚表面破坏层,并且由抛光引起的表面残余应力极小。同时研制了数控液流悬浮抛光机床,并对硅晶片等材料进行了加工试验。     

Microstrueturc and Mcehanieal Propcrtics of Heat-treated GeSb2Te4 Thin Films

The effect of annealing on microstructure, adhesive and frictional properties of GeSb2Te4 films were experimentally studied. The GeSb2Te4 films were prepared by radio frequency （RF） magnetron sputtering, and annealed at 200℃ and 340℃ under vacuum circumstance, respectively. The adhesion and friction experiments were mainly conducted with a lateral force microscope （LFM） for the GeSb2Te4 thin films before and after annealing. Their morphology and phase structure were analyzed by using atomic force microscopy （AFM） and X-ray Diffraction （XRD） techniques, and the nanoindention was employed to evaluate their hardness values. Moreover, an electric force microscope （EFM） was used to measure the surface potential. It is found that the deposited GeSb2Te4 thin film undergoes an amorphous-to-fcc and fcc-to-hex structure transition; the adhesion has a weaker dependence on the surface roughness, but a certain correlation with the surface potential of GeSb2Te4 thin films. And the friction behavior of GeSb2Te4 thin films follows their adhesion behavior under a lower applied load. However, such a relation is replaced by the mechanical behavior when the load is relatively higher. Moreover, the GeSb2Te4 thin film annealed at 340℃ presents a lubricative property.     

Structural and optical characteristics of Al x Ga1- x N/AlN superlattice

AlN/Al_0.3Ga_0.7N superlattices were grown on (0001) sapphire substrate by metal-organic chemical vapor deposition (MOCVD). The superlattice period varies from 6 to 30. The layer thickness of different period stack was designed. GaN or AlGaN template was employed for growing AlN/AlGaN superlattices. Reflectivity, SEM, AFM and XRD data of the Al _x Ga_1-x N/AlN superlattices are presented. It is found that the templates used have an intensive impact on surface roughness and interfacial properties of following AlN/AlGaN superlattices. The result of atomic force microscopy indicates that AlN/AlGaN superlattices grown on GaN template exhibit quasi-two-dimensional growth mode. The resulting superlattice has a smooth surface morphology and distinct interface. No crack is observed in the area of a 2-inch wafer. Supported by the Special Funds for Major State Basic Research Project (973 Project) (Grant No. 2006CB6049), the Hi-tech Research Project (Grant Nos. 2006AA03A103, 2006AA03A118, and 2006AA03A142), the National Natural Science Foundation of China (Grant No. 60676057), and the Research Fund for the Doctoral Program of Higher Education of China (Grant No. 20050284004)     

Atomic scale KMC simulation of {100} oriented CVD diamond film growth under low substrate temperature—part Ⅱ Simulation of CVD diamond film growth in C—H system and in Cl—containing systems

The growth of {100}-oriented CVD diamond film under two modifications of J-B-H model at low substrate temperatures was simulated by using a revised KMC method at atomic scale,The results were compared both in Cl-containing systems and in C-H system as follows:(1) Substrate temperature can produce an important effect both on film deposition rate and on surface roughness;(2) Aomic Cl takes an active role for the growth of diamond film at low temperatues;(3){100}-oriented diamond film cannot deposit under single carbon insertion mechanism,which disagrees with the predictions before;(4) The explanation of the exact role of atomic Cl is not provided in the simulation results.     

Atomic scale KMC simulation of {100} oriented CVD diamond film growth under low substrate temperature-Part II Simulation of CVD diamond film growth in C-H system and in Cl-containing systems

The growth of {100}-oriented CVD diamond film under two modifications of J-B-H model at low substrate temperatures was simulated by using a revised KMC method at atomic scale. The results were compared both in Cl-containing systems and in C-H system as follows: (1) Substrate temperature can produce an important effect both on film deposition rate and on surface roughness; (2) Aomic Cl takes an active role for the growth of diamond film at low temperatures; (3) {100}-oriented diamond film cannot deposit under single carbon insertion mechanism, which disagrees with the predictions before; (4) The explanation of the exact role of atomic Cl is not provided in the simulation results.     

Boosting Hydrogen Evolution and Oxygen Reduction Performances of Pd/C upon Surface Phosphorization

表面磷化策略提高 Pd/C 的析氢和氧还原性能

朱桐桐， 王海鸽， 李小鹏， 廖耀祖， 朱美芳

（东华大学 材料科学与工程学院 纤维材料改性国家重点实验室，上海 201620）

中文说明：构筑金属异质结构是实现高性能电催化剂的有效途径之一，共轭微孔聚合物（CMP）是一种具有可设计孔隙率的功能新材料。基于此，本文提出利用CMP 客体化学方法来制备具有双功能电催化活性的PdP2@Pd/C 异质结构。该异质结构的形成依赖于由氮基团组成的 CMP前体，它允许结合 Pd 物质并引入磷掺杂剂。原位形成的 Pd 负载CMP 前体在热解过程中可直接转化为氮和磷化物掺杂的多孔碳（NPC），而 P 则扩散到 Pd/C 界面导致Pd颗粒表面磷化。所制备的由 PdP2@Pd/C（Pd 含量 4 wt.%）异质结构组成的 NPC 表现出显著增强的电催化性能，包括具有高析氢活性（58mV @ 10 mA cm^-2）和接近商业化 20 wt.% Pt/Cd电极的氧还原活性以及出色的循环稳定性。该研究指出了CMP作为客体，在构筑异质结构的电催化剂方面展现的巨大潜力。

关键词：共轭微孔聚合物，钯磷异质结构，双功能电催化剂，析氢反应，氧还原反应