Fabrication of Hollow or Macroporous Silica Particles by Spray Drying of Colloidal Dispersion

In this study, hollow silica particles were fabricated by atomizing the dispersion of silica nanocolloids synthesized by modified Stober method and self-organization of the particles by spray drying technique. Rapid evaporation of the droplet containing the silica nanoparticles resulted in the formation of hollow microparticles at high evaporation temperature due to hydrodynamic instability of the droplet. Similar strategy was adopted for the fabrication of macroporous silica particles by the sol spray drying of the hetero-colloidal dispersion of polystyrene nanospheres and commercial silica nanoparticles. The morphologies of the porous particles were observed by scanning electron microscope with varying drying temperature. As a demonstrative purpose, the results using emulsion droplets as confining geometry was compared with the porous particles obtained from spray dryer. Collectively, spray drying was found to be more efficient manner to prepare the porous materials with continuous way in the view of production efficiency and time.     

电解质诱导聚集初级粒子制备介孔SiO_2材料

在无模板剂的条件下,通过在Stber合成过程中引入外加电解质成功地制备了具有介孔结构的SiO2粒子.实验结果表明,通过电解质的加入可以诱导Stber过程中初级SiO2粒子的聚集,从而得到了具有介孔结构和较强表面吸附能力的SiO2粒子.     

The Effect of Gelatin on the Preparation of Silica Coated Iron Particles

A method is described for coating fine iron particles(～1μm) with a uniform silica layer,produced by the hydrolysis of tetraethyl orthosilicate.The presence of a small amount of gelatin on the surface of the iron particles facilitates this process.The X-ray photoelectron measurements indicated that the gelatin interacted with the surface of the iron particles by means of both nitrogen(in -NH2 groups) and oxygen(in -COOH groups) and then bound to the silica.The silica coating increases the resistance of the iron particles to oxidation on heating in air,which makes the temperature at which an observable oxidization occurs from 330 ℃ to 400 ℃ raised.     

Preparation of Silver Nanoshells on Silica Particles by a Simple Two-step Process

A simple two-step method was developed to prepare silver nanoshells coated on silica paticles. The method involves two steps: concentration of reaction precursor (AgNO3) on particle surfaces and subsequent reduction by formaldehyde. The obtained composite particles were characterized by TEM, ED, and SEM-EDS measurements. The results show that the silver nanoshell is coated on silica particle surface in the form of a polycrystalline (cubic structure) layer with average thickness of 20 nm and weight percentage of 1.9%.     

Research of Silica Particles Dispersion in Polymer Matrix Under Acoustic Levitation

Series of resins consisting different amount of silica particles with different sizes and surface properties were prepared as suspended samples under an acoustic levitator. The resulting composites after curing under irradiation have been investigated. Fracture surface morphologies of the resins were compared to those with same composition prepared in a normal gravity field via scanning electron microscopy. The results showed that except for such factors like particle sizes, surface properties, particles concentration, and monomer viscosity, the microgravity state produced by acoustic levitation could also be an element that affects silica particles dispersion in the resins.     

Production of Colourful Pigments Consisting of Amorphous Arrays of Silica Particles

It is desirable to produce colourful pigments that have anti‐fading properties and are environmentally friendly. In this Concept, we describe recently developed pigments that exhibit such characteristics. The pigments consist of amorphous arrays of submicron silica particles, and they exhibit saturated and angle‐independent structural colours. Variously coloured pigments can be produced by changing the size of the particles, and the saturation of the colour can be controlled by incorporating small amounts of black particles. We review a simple analysis that is useful for interpreting the angular independence of the structural colours and discuss the remaining tasks that must be accomplished for the realistic application of these pigments.     

Preparation of Thick Films by Electrophoretic Deposition Using Surface Modified Silica Particles Derived from Sol-Gel Method

Thick films were prepared by the electrophoretic sol-gel deposition of organically modified, sub-micron silica particles. The silica particles were modified with 3-aminopropyltriethoxysilane (APS) and vinyltriethoxysilane (VTES). Smooth and crack-free films ca. 15 m thick were obtained when APS modified silica particles were used for the cathodic electrophoretic deposition. Thick films with decreased open spaces among particles were obtained when silica particles modified with VTES were co-deposited with an organic polymer, polyethylene maleate.     

Synthesis of Nano Silica Particles for Polishing Prepared by Sol–Gel Method

In order to produce an excellent abrasive, a fabrication method for cocoon shaped silica particles has been studied. The particles are prepared from TMOS, water, ammonia and methanol by a sol–gel method. The method is to add the methanol solution of TMOS at a constant supply rate to a mixture of water, ammonia and methanol. Effects of various reaction conditions such as temperatures, supply rates of TMOS, and amounts of TMOS are studied on the diameter and shape of the particles. The diameter and shape are resulted in depending strongly on temperatures. High temperature makes particles with the high aspect ratio and the small diameter. And the mechanism of forming the cocoon shaped particle is also discussed. It is concluded that the primary particles are generated at the beginning stage of reaction and two of them become the cocoon shaped particle. For the polishing efficiency, particles have high polishing efficiency with the diameter between 40 nm and 210 nm. As a result, best diameter of particles for abrasive is 40–100 nm with respect to polishing efficiency and surface finish.     

Synthesis of Microporous Silica Spheres

Spherical microporous silica powders with a narrow size distribution have been prepared by a precipitation technique involving the hydrolysis reaction of a silicon alkoxide in ethanol. The formation of the important microporosity has been investigated following two templating methods: the co-hydrolysis and condensation of two alkoxides, one of which presents porogen function, and the adsorption of an organic compound (glycerol) as the porogen. In both processes, the organic porogen is removed by a simple calcination. In the first method, the addition of more than 20 mol% of the porogen alkoxide, necessary for generating enough microporosity, disturbs completely the condensation process resulting in microporous, nonuniform silica particles of large size distribution. The best result has been obtained with the glycerol method where submicrometer-sized silica spheres with a very narrow size distribution and about 40 vol% porosity have been synthesized. The presence of glycerol during the synthesis considerably affects the precipitation mechanism, resulting in a larger mean particle size. The use of an aggregative growth model has successfully been employed to explain the effect of the porogen during particle formation. The precipitation mechanism of silica involves the aggregation between particles of similar size until a critical size is reached, resulting in a uniform particle size distribution. In the presence of glycerol, it has been shown that a second aggregative growth between still-nucleating primary particles and large particles occurred with increasing reaction time. This second aggregative growth appears at an intermediate stage of the precipitation process and is due to both the precipitation of smaller primary particles and the destabilization of the colloidal stability of the system. This explains why the final particle size reached in this system is larger compared to silica particles synthesized without glycerol and shows how glycerol is incorporated in the silica particles. The synthesis of silica microporous spheres of narrow size distribution, by varying particle size and porosity, should yield a wide range of aqueous silica slurries for particular chemical mechanical polishing applications. Copyright 2000 Academic Press.     

原子转移自由基聚合(ATRP)在二氧化硅表面接枝中的应用

ATRP方法是在二氧化硅(SiO2)表面接枝聚合物的一种有效方法.通过硅烷偶联剂把ATRP引发剂键接到SiO2表面,然后进行表面ATRP聚合,可以在SiO2表面接枝各种均聚物、嵌段共聚物、超支化聚合物.聚合可以在有机溶剂或水中进行.把ATRP方法同其它聚合方法如氮氧稳定自由基聚合或开环聚合相结合,可以在SiO2表面接枝复杂结构的聚合物如V型嵌段共聚物、梳型共聚物等.SiO2表面ATRP聚合可以通过外加引发剂或外加二价铜来实现聚合可控.     

Preparation of Spherical Hydrous Silica Oxide Particles under Acidic Condition via Sol-Gel Processing

Preparation of spherical hydrous silica oxide particles via sol-gel processing was rarely reported. In this study, spherical silica particles were obtained in TEOS/AcOEt/AcOH 50% aq. system. The combination of AcOEt and AcOH 50% aq. widened the spherical particle-forming region. Their size ranged from some ten micrometers to some hundreds micrometers. Hydrophilic molecules or powders like Rhodamine 6G and phosphorescent powders were encapsulated in the spherical particles.     

由硅溶胶生长单分散颗粒的研究

针对现行单分散二氧化硅颗粒制备方法的粒径预见性差、步骤繁琐、收率低等问题，研究了一种用硅溶胶作为种子，在氨、水和乙醇的混合溶液中通过水解正硅酸乙酯（ＴＥＯＳ）生长出单分散颗粒的简便方法。该方法仅在初始的悬浮液中滴加ＴＥＯＳ即可使种子正常生长，无须补充氨水以修正体系浓度的变化。最终的分散相浓度可达１０％（质量分数）。可选择生长的粒径范围在１微米以内并可精确控制。所得颗粒粒径分布偏差于Ｓｔｏｂｅｒ方法     

Silica Coating on Colloidal Maghemite Particles

Maghemite colloidal particles are coated with a silica layer using a silicon alkoxide as silica precursor. The coating process is studied by electrophoresis, quasi-elastic light scattering, nitrogen adsorption, and infrared spectrometry analyses. The conditions of complete coverage of the iron oxide particles by silica and the nature of the maghemite–silica interface are discussed.     

Advances in the Interfacial Assembly of Mesoporous Silica on Magnetite Particles

Interfacing magnetic particles with ordered mesoporous materials is an effective direction for the development of functional porous composite materials with rationally designed core–shell structures. Owing to the combined properties of magnetic nanoparticles and mesoporous silica (high surface area, large pore volume, porosity, and biocompatibility), core–shell magnetic mesoporous silica materials have generated tremendous interest in various disciplines, including chemistry, materials, bioengineering, and biomedicine. Interfacial assembly strategies enable the rational construction of magnetic mesoporous silica materials with well‐defined core–shell structure, morphology, pore parameters, and surface wettability, which can decisively influence their physical and chemical properties and thus improve their application performance. This Minireview summarizes recent progress in the synthesis of core–shell magnetic mesoporous silica and the adjustment of key parameters, including pore size, morphology, and pore orientation.     

Spherical Polyolefin Particles from Olefin Polymerization in the Confined Geometry of Porous Hollow Silica Particles

Porous hollow silica particles (HSPs) are presented as new templates to control the product morphology in metallocene‐catalyzed olefin polymerization. By selectively immobilizing catalysts inside the micrometer‐sized porous hollow silica particles, the high hydraulic forces resulting from polymer growth within the confined geometries of the HSPs cause its supporting shell to break up from the inside. As the shape of the support is replicated during olefin polymerization, perfectly spherical product particles with very narrow size distribution can be achieved by using HSPs exhibiting a monomodal size distribution. Furthermore, the size of the obtained product particles can be controlled not only by the polymerization time but also by the size of the support material.

     

一种可精确控制粒径的SiO2微球合成方法

用改进的种子法合成SiO2微球. 微球生长过程中连续缓慢添加正硅酸乙酯,使用动态光散射法实时监控微球粒径的增长过程,调节正硅酸乙酯的添加,实现对粒径的精确控制. 为制备禁带位置位于1000 nm 的光子晶体,合成粒径为446 nm的SiO2微球,微球粒径在4 h内从193 nm 增长到446 nm,远远快于传统种子法,微球粒径与目标粒径偏差为±5 nm. 制得的SiO2微球被组装为光子晶体,其禁带位置恰好位于1000 nm.     

以微凝胶模板合成P(AM-co-DMC)/SiO2杂化粒子

以聚(丙烯酰胺-co-甲基丙烯酰氧乙基三甲基氯化铵)[P(AM-co-DMC)]微凝胶为模板,TMOS为硅前驱体,中性水环境下合成了一系列P(AM-co-DMC)/SiO2有机-无机杂化粒子.对杂化粒子的大小、形态及表面形貌等进行研究,发现微凝胶对杂化粒子的形态和大小起主导作用,SiO2在模板上沉积,即使经过灼烧依然保持模板的形态;TMOS的用量对杂化粒子的性质也有重要影响——用量少时,得到的杂化粒子表面粗糙,增加用量会使表面变得光滑.杂化粒子经过灼烧后,表面会变得更加粗糙.     

Composite Silica Particles Using a Mixture of Organosilane Monomers

Composite silica particles were synthesized by a two-step (acid-base) process in an aqueous solution with a mixture of organoalkoxysilane monomers. The two-step process separates the hydrolysis and condensation procedures to easily control condensation rate. In this study, the silane monomers used were phenyltrimethoxysilane (PTMS), vinyltrimethoxysilane (VTMS), methyltrimethoxysilane (MTMS), and tetraethyl-orthosilicate (TEOS). The physical properties of the resultant composite particles were investigated with the change in the molar ratio of monomers. The size of the particles increased with increasing the molar ratio of R_aSi(OR)₃/R_bSi(OR)₃ or R_aSi(OR)₃/TEOS (R_a: phenyl; R_b: vinyl, methyl).     

Optical Trapping of Titania/Silica Core-Shell Colloidal Particles

Manipulation of colloidal systems via optical trapping techniques requires a refractive index mismatch between particles and solvent which leads to strong interparticle van der Waals interactions. Investigation of the behavior of systems without such strong attractive interactions, however, requires the uncoupling of particle refractive index and particle-particle interactions. To accomplish this, the synthesis of core-shell titania/silica particles has been performed. By index matching a silica shell on a titania core using a mixture of toluene and propanol, the van der Waals interactions between particles can be minimized. Due to the mismatch of the refractive index between the solvent and titania core, however, a strong trapping force can be generated, making optical manipulation feasible. In order to confirm that the silica shell was indeed matched, pure silica particles were synthesized by the method of St?ber (1968) and added to the core-shell system. In these mixed systems of core-shell and pure silica particles in silica-index-matching solvents, only the core-shell particles were trappable. Copyright 2000 Academic Press.     

Synthesis of UV-Cured Silicone Resin/Silica Nanocomposites from UV-Curable Polysilisiquioxane and Methacrylate-Functionalized Silica

A series of silicone resin/silica polymeric nanocomposites with 0–6 wt% silica content, comprising well-distributed silica nanoparticles in silicone resin matrix, have been synthesized from a UV-curable polysilisiquioxane (UV-PSL) and a methacrylate-functionalized silica via UV-curing in the presence of 1-hydroxycyclohexyl phenyl ketone (Irgacure 184) as photoinitiator. To enhance the interfacial interaction, the silica surface was firstly treated with 3-(methacryloxy) propyl trimethoxysilane (MPTS), and its structure was analyzed by FTIR spectrophotometry. The thermal stability of nanocomposites was slightly enhanced with the addition of silica particles. SEM studies indicate that silica particles were dispersed homogenously through the polymer matrix. The physical and mechanical properties such as the thickness, hardness, adhesion, impact strength as well as gloss were examined.