核-壳结构PS/CeO_2复合磨料的制备及其氧化物化学机械抛光性能

以无皂乳液聚合方法制备的聚苯乙烯(PS)微球为内核,硝酸铈为铈源,六亚甲基四胺为沉淀剂,采用液相工艺制备了PS/CeO2复合颗粒.利用XRD、TEM、SAED、FESEM、EDAX等手段,对所制备样品的物相结构、形貌、粒径大小和元素成分组成进行表征.将所制备的复合磨料用于硅晶片热氧化层的化学机械抛光,用AFM观察抛光表面的微观形貌,并测量表面粗糙度.结果表明,所制备的PS/CeO2复合颗粒具有核-壳结构,呈近似球形,粒径在250～300nm,PS内核表面被粒径在5～10nm的CeO2纳米颗粒均匀包覆,壳层的厚度为10～20nm.抛光后的硅热氧化层表面在5μm×5μm范围内粗糙度Ra值和RMS值分别为0.188nm和0.238nm,抛光速率达到461.1nm/min.     

包覆型纳米CeO2@SiO2复合磨料的制备?表征及其抛光性能

以无水乙醇为溶剂,氨水为催化剂,利用正硅酸乙酯(TEOS)水解,并在500℃下煅烧1h,制备了SiO2粉体.将SiO2粉体作为内核浸渍到以硝酸亚铈、乙酰丙酮和正丙醇为原料制备的铈溶胶中,得到包覆型CeO2@SiO2复合粉体.利用XRD、SEM、TEM和FT-IR等测试手段,对所制备样品的物相结构、形貌、粒径大小、团聚情况进行表征.将所制备的包覆型CeO2@SiO2复合粉体配制成抛光浆料用于砷化镓晶片的化学机械抛光,用原子力显微镜(AFM)观察抛光表面的微观形貌,测量表面粗糙度.结果表明,采用浸渍工艺成功制备出单分散球形,粒径在400～450nm,负载均匀的包覆型CeO2@SiO2复合粉体.复合粉体中CeO2的包覆量随着铈溶胶中铈离子浓度的升高而增大.经包覆型CeO2@SiO2复合磨料抛光后的砷化镓晶片表面的微观起伏更趋于平缓,在1μm×1μm范围内表面粗糙度Ra值为0.819nm,获得了具有亚纳米量级粗糙度的抛光表面.     

氧化硅/氧化铁复合磨粒用于硬盘基片的抛光研究

本文以HNO3、NaOH、Fe(NO3)3和SiO2浆料为原料,采用沉淀法制备了1种SiO2/Fe2O3复合磨粒,通过X射线衍射仪(XRD)、飞行时间二次离子质谱仪(TOF-SIMS)和扫描电子显微镜(SEM)对其结构进行表征,结果表明Fe2O3包覆到SiO2的表面,复合粒子具有很好的分散性.用UNIPOL-1502抛光机研究了所制备复合磨粒在镍磷敷镀的硬盘基片中的抛光性能,抛光后硬盘基片的表面粗糙度Ra由抛光前的8.87nm降至3.73nm;抛光后表面形貌的显微镜观测结果表明新制备的复合磨粒表现出较好的抛光性能.     

纳米CeO2颗粒的制备及其化学机械抛光性能研究

以硝酸铈和六亚甲基四胺为原料制备出不同粒径的纳米CeO2粉体颗粒,将纳米CeO2粉体配制成抛光液并用于砷化镓晶片的化学机械抛光.结果表明,不同尺寸的纳米磨料具有不同的抛光效果,采用粒度8 nm的CeO2磨料抛光后微观表面粗糙度最低(0.740 nm),采用粒度小于或大于8 nm的CeO2磨料抛光后其表面粗糙度值均较高.通过简化的固-固接触模型分析,认为当粒度过小时,磨料难以穿透软质层,表现为化学抛光为主,表面凹坑较多,表面粗糙度较高;当粒度大于一定值时,随着磨料粒度增加,嵌入基体部分的深度加大,使得粗糙度出现上升趋势.提出当磨料嵌入晶片表面的最大深度等于或接近于软质层厚度时,在理论上应具有最佳的抛光效果.     

纳米SiO2/CeO2复合磨粒的制备及其抛光特性研究

以尿素[CO(NH2)2]、(NH4)2Ce(NO3)6和SiO2为原料,采用均相沉淀法制备1种新型纳米SiO2/CeO2复合磨粒,通过X射线衍射仪、X射线光电子能谱仪、飞行时间二次离子质谱仪和扫描电子显微镜等分析手段对其结构进行表征,并将SiO2/CeO2复合磨粒配置成抛光液在数字光盘玻璃基片上进行化学机械抛光试验.结果表明所制备的SiO2/CeO2复合磨粒的平均晶粒度为19.64 nm,粒度分布均匀;经过1 h抛光后,玻璃基片的平均表面粗糙度(Ra)由1.644 nm降至0.971 nm;抛光后玻璃基片表面变得光滑、平坦,表面微观起伏较小.     

PTFE@SiO2核壳型添加剂在不同实验条件下的水润滑性能

采用原位聚合法制备了聚四氟乙烯@二氧化硅(PTFE@SiO₂)复合粒子. 利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、粒径分布仪以及傅立叶红外光谱仪(FTIR)对复合粒子的形貌、粒径分布和组成结构进行了分析. 结果表明:所制备的复合粒子呈核壳型复合结构,粒子尺寸处于亚微米级别. 分散性试验表明:该粒子在水中具有良好的分散性和稳定性. 利用LSR-2M往复式摩擦磨损试验机测试了不同试验条件下复合粒子在水环境中的摩擦学性能,结果表明:在常温、0.019 m/s滑动速率以及0.2 μm的钢盘粗糙度下,PTFE@SiO₂润滑剂具有最佳的摩擦学性能;相比于纯水和添加了PTFE/SiO₂的润滑剂,其摩擦系数降低了近80%,磨损体积减小了1~2个数量级. 分析表明:PTFE@SiO₂复合粒子优异的水润滑性能主要与核壳结构的存在以及在摩擦过程中形成的高质量转移膜密切相关.      

核壳结构PS/CeO2复合微球弹性模量的AFM测定

利用原子力显微镜测定了聚苯乙烯(Polystyrene, PS)微球和核壳结构PS/CeO₂复合微球的力-位移曲线,并根据Hertz接触理论计算了微球样品的弹性模量.结果表明:粒径在120 nm左右的PS微球的平均弹性模量约为2.80 GPa,其数值略低于聚苯乙烯块体材料的弹性模量.复合微球的弹性模量随CeO₂壳层厚度的增加而增大,当CeO₂壳厚分别约为8、12和16 nm时,其平均弹性模量依次约为7.93、8.25和10.67 GPa.与纯氧化铈相比,PS/CeO₂复合微球的弹性模量更接近于聚苯乙烯微球.     

磨料对铜化学机械抛光过程的影响研究

利用CP-4型抛光试验机对直径为50.8 mm、表面沉积厚530 nm的铜硅片(表面粗糙度Ra为1.42 nm)进行化学机械抛光(CMP)试验,评价了CMP过程中不同磨料作用下的摩擦系数和材料去除率;利用ZYGO表面形貌分析系统测试含不同磨料抛光液抛光后的硅片表面粗糙度;采用扫描电子显微镜分析CMP后的铜硅片表面损伤形貌.结果表明,磨料的浓度和粒径直接影响CMP过程的摩擦系数:采用5%粒径25 nm硅溶胶为抛光液时的摩擦系数低于超纯水抛光时的摩擦系数;当磨料的添加量和粒度增加时摩擦系数增大.在相同试验条件下,采用10%粒径25 nm硅溶胶抛光材料的去除率为50.7 nm/min;粒径为1μm白刚玉磨料的抛光材料去除率为246.3 nm/min;单纯磨料使铜硅片表面变得粗糙,即用10%粒径25 nm硅溶胶抛光后的表面粗糙度仍大于原始表面(Ra值达3.43 nm);在单纯磨料或超纯水为抛光液抛光下铜硅片表面出现划伤.     

纳米SiO2／CeO2复合磨粒的制备及其抛光特性研究

以尿素[CO(NH2)2]、(NH4)2Ce(NO3)6和SiO2为原料,采用均相沉淀法制备1种新型纳米SiO2/CeO2复合磨粒,通过X射线衍射仪、X射线光电子能谱仪、飞行时间二次离子质谱仪和扫描电子显微镜等分析手段对其结构进行表征,并将SiO2/CeO2复合磨粒配置成抛光液在数字光盘玻璃基片上进行化学机械抛光试验.结果表明:所制备的SiO2/CeO2复合磨粒的平均晶粒度为19.64 nm,粒度分布均匀;经过1 h抛光后,玻璃基片的平均表面粗糙度(Ra)由1.644 nm降至0.971 nm;抛光后玻璃基片表面变得光滑、平坦,表面微观起伏较小.     

Ce0.8Zr0.2O2固溶体磨料对ZF7光学玻璃抛光性能的改善

采用改进的湿固相机械化学反应法制备出超细锆掺杂氧化铈磨料Ce1-xZrxO2(x=0,0.2),运用X射线衍射(XRD)、透射电镜(TEM)等手段表征其物相类型、外观形貌、比表面积、粒度、表面电位等物理性质,通过测定抛光速率和观察表面的微观形貌考察它们对ZF7光学玻璃的抛光性能影响.结果表明,Ce0.8Zr0.2O2固溶体磨料对ZF7光学玻璃抛光性能比纯CeO2磨料有明显的提高,抛光速率达到463 nm/min,5.0 μm×5.0 μm的范围内微观表面粗糙度Rα值达到1.054 nm,而纯CeO2磨料的抛光速率只有292 nm/min,Rα值却增大到1.441 nm.Ce0.8Zr0.2O2固溶体的抛光速率的明显增大和表面粗糙度Rα的下降主要与其负表面电位的增大和颗粒尺寸、粒度的减小密切相关.     

Facile aqueous synthesis and thermal insulating properties of low-density glass/TiO2 core/shell composite hollow spheres

Anatase TiO₂ shells assembled on hollow glass microspheres (HGM) with tunable morphologies were successfully prepared through a controllable chemical precipitation method with urea as the precipitator. Thus, glass/TiO₂ core/shell composite hollow spheres with low particle density (0.40 g/cm³) were fabricated. The phase structures, morphologies, particle sizes, shell thicknesses, and chemical compositions of the composite microspheres were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). The morphology of the TiO₂ shell can be tailored by properly monitoring the reaction system component and parameters. The probable growth mechanism and fabrication process of the core/shell products involving the nucleation and oriented growth of TiO₂ nanocrystals on hollow glass microspheres was proposed. A low infrared radiation study revealed that the radiation properties of the products are greatly influenced by the unique product shell structures. A thermal conductivity study showed that the TiO₂/HGM possess low thermal conductivity that is similar to that of the pristine HGMs. This work provides an additional strategy to prepare low-density thermal insulating particles with tailored morphologies and properties.     

Preparation of nanosized hollow silica spheres from Na2SiO3 using Fe3O4 nanoparticles as templates

Nanosized hollow silica spheres with average diameters from 43 to 70 nm were prepared by removal of Fe₃O₄ templates with hydrochloric acid from silica-coated Fe₃O₄ core–shell composites. The shells of the hollow silica spheres had nanopores with average diameters of 0.92–1.25 nm. When the silica-coated Fe₃O₄ core–shell composites were prepared at a high pH value or with a low mole ratio of Na₂SiO₃ to Fe₃O₄, the resulting hollow silica spheres consisted of highly porous shells. When the silica-coated Fe₃O₄ core–shell composites were prepared with a high mole ratio of Na₂SiO₃ to Fe₃O₄, the resulting hollow silica spheres had large diameters and thick shells. The release rate of herbicide, ammonium glyphosate, could be tuned by using hollow silica spheres with different shell thicknesses.     

Effect of dopants and interlayers on the growth of thin insulating films

Surface morphologies of thin dielectric films deposited on gallium arsenide substrates are studied by atomic force microscopy (AFM). The quasi-periodic mesostructure with a corrugated configuration is found to form during the deposition process. A special dopant and thin interlayer at the film–substrate interface are used to decrease the surface roughness. The corrugated Si_xN_yO_z–SiO₂ film surface disappears by introducing Se atoms into the subsurface layer of the semiconductor. The root-mean-square roughness and the fractal dimension techniques are used for the numerical characterization of the surface morphologies of thin insulator films.     

Visible light photodegradation of methylene blue by AgBr-TiO2/SiO2@Fe3O4 magnetic photocatalysts

Visible photoactive AgBr/TiO2 was immobilized on a SiO2@Fe3O4 magnetic support by solvother- rnal and sol-gel methods to form a AgBr-TiO2/SiO2@Fe3O4 magnetic photocatalyst. Samples were characterized by X-ray diffraction, high-resolution transmission electron microscopy and magne- tometry. Hereto-structured AgBr/TiO2 was well seeded on the shell-core SiO2@Fe3O4 structure. The AgBr-TiO2/SiO2@Fe3O4 magnetic photocatalyst exhibited high photocatalytic activity in the degrada- tion of methylene blue under visible light. The photocatalyst was superparamagnetic, which is beneficial for facile magnetic separation.     

Facile aqueous synthesis and thermal insulating properties of low-density glass/TiO2 core/shell composite hollow spheres

Anatase TiO2 shells assembled on hollow glass microspheres(HGM)with tunable morphologies were successfully prepared through a controllable chemical precipitation method with urea as the precipitator. Thus,glass/TiO2 core/shell composite hollow spheres with low particle density(0.40 g/cm3)were fabricated.The phase structures,morphologies,particle sizes,shell thicknesses,and chemical compositions of the composite microspheres were characterized by X-ray diffraction(XRD),scanning electron microscopy (SEM),and energy dispersive X-ray spectroscopy(EDS).The morphology of the TiO2 shell can be tailored by properly monitoring the reaction system component and parameters.The probable growth mechanism and fabrication process of the core/shell products involving the nucleation and oriented growth of TiO2 nanocrystals on hollow glass microspheres was proposed.A low infrared radiation study revealed that the radiation properties of the products are greatly influenced by the unique product shell structures. A thermal conductivity study showed that the TiO2/HGM possess low thermal conductivity that is similar to that of the pristine HGMs.This work provides an additional strategy to prepare low-density thermal insulating particles with tailored morphologies and properties.     

Synthesis of mesoporous γ-AlOOH@Fe3O4 magnetic nanomicrospheres

Mesoporous γ-AlOOH@Fe₃O₄ magnetic nanomicrospheres were synthesized using superparamagnetic Fe₃O₄ nanoparticles as the core and aluminum isopropoxide (AIP) as the aluminum source. The obtained magnetic nanomicrospheres were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), N₂ adsorption–desorption and vibrating sample magnetometry (VSM). The effects of preparation parameters such as hydrolysis time of AIP, concentration of AIP and coating layer number on microspheres were investigated. The results indicated that the mesoporous γ-AlOOH@Fe₃O₄ magnetic nanomicrospheres consisted of a mesoporous γ-AlOOH shell and a Fe₃O₄ magnetic core. The diameter of γ-AlOOH@Fe₃O₄ nanomicrospheres was about 200 nm, the thickness of mesoporous γ-AlOOH shell was about 5 nm and the average pore size was 3.8 nm. The thickness of the mesoporous γ-AlOOH shell could be controlled via layer-by-layer coating times. The formation mechanism of the mesoporous γ-AlOOH shell involved a “chemisorption–hydrolysis” process.     

Preparation of SiO2/TiO2 Janus particles by electrostatic assembly,hydrolysis and calcination

This paper describes a novel chemical method for preparing SiO₂/TiO₂ Janus particles. First, polystyrene (PSt)/SiO₂ particles with a raspberry-like structure are prepared by electrostatic assembly. The influences of the reaction time of sulfonation and the treatment times of polyelectrolyte solutions (PDADMAC, PSS) on PSt and SiO₂ are investigated with respect to the surface charge density of the particles. SiO₂/TiO₂ Janus particles are then obtained by hydrolysis of butyl titanate on the surface of PSt/SiO₂ particles followed by a calcination process. Particle size analyzer, Zeta potential instrument, FTIR, TEM and SEM are used to characterize the particle size, the amount of charge on the surface of PSt and SiO₂ particles and the compositions and morphologies of PSt/SiO₂, SiO₂/TiO₂ and PSt/SiO₂/TiO₂. The diameters of the PSt, SiO₂, PSt/SiO₂ and SiO₂/TiO₂ particles are 2.0 μm, 303 nm, 2.7 μm and 330 nm, respectively.     

Real-Time Stress Measurement in SiO<Subscript>2</Subscript> Thin Films during Electrochemical Lithiation/Delithiation Cycling

Oxide coatings have been shown to improve the cyclic performance of high-energy density electrode materials such as Si. However, no study exists on the mechanical characterization of these oxide coatings. Here, thin film SiO₂ electrodes are cycled under galvanostatic conditions (at C/9 rate) in a half-cell configuration with lithium metal foil as counter/reference electrode, with 1 M LiPF₆ in ethylene carbonate, diethyl carbonate, dimethyl carbonate solution (1:1:1, wt%) as electrolyte. Stress evolution in the SiO₂ thin film electrodes during electrochemical lithiation/delithiation is measured in situ by monitoring the substrate curvature using a multi-beam optical sensing method. Upon lithiation SiO₂ undergoes extensive inelastic deformation, with a peak compressive stress of 3.1 GPa, and upon delithiation the stress became tensile with a peak stress of 0.7 GPa. A simple plane strain finite element model of Si nanotube coated with SiO₂ shell was developed to understand the mechanical response of the core-shell type microstructures under electrochemical cycling; measured stress response was used in the model to represent SiO₂ constitutive behavior while Si was treated as an elastic-plastic material with concentration dependent mechanical properties obtained from the literature. The results reported here provide insights and quantitative understanding as to why the highly brittle SiO₂ coatings are able to sustain significant volume expansion (300%) of Si core without fracture and enhance cyclic performance of Si reported in the literature. Also, the basic mechanical properties presented here are necessary first step for future design and development of durable Si/SiO₂ core shell structures or SiO₂-based electrodes.