Ammonium mediated hydrothermal synthesis of nanostructured hematite (α-Fe2O3) particles

Uniform α-Fe₂O₃ particles of different shapes have been synthesized through hydrothermal process. The additives, the type of Fe(III) salts and reaction conditions in hydrothermal process were thoroughly investigated. The crystalline structure and morphology of the as-synthesized powder have been characterized by using X-ray powder diffraction, scanning electron microscopy and field emission scanning electron microscopy. Rod and ellipsoidal-shaped α-Fe₂O₃ were obtained with ferric chloride as a precursor, while only irregular-shaped particles were synthesized by using ferric nitrate as precursors in the absence of NH₄OH. Direct transformation of micro-rod hematite to ellipsoidal particles with FeCl₃ as precursor was also observed by adding NH₄OH. It is shown that the nanorod was formed through presumed directional aggregation of rapidly formed nucleus, while the formation of ellipsoidal hematite particles may undergo a nucleation–aggregation–dissolution–recrystallization process in the presence of ammonium.     

Structure of polyphenylsilsesquioxane particles prepared by two-step acid-base catalyzed sol-gel process and formation of hollow particles

Spherical polyphenylsilsesquioxane (PhSiO(3/2)) particles, one of the inorganic-organic hybrid materials, were synthesized by a two-step acid-base catalyzed sol-gel process, and hollow particles were successfully prepared by washing the as-prepared particles with organic solvents. It was found that the inside and outside parts of the as-prepared particles were composed of PhSi03/2 species with relatively low and high molecular weight, respectively, i.e., the PhSiO(3/2) particles had a kind of "core-shell" structure. Because the core portion in the as-prepared particles was soluble in ethanol and tetrahydrofuran, hollow particles were obtained through washing the as-prepared PhSiO(3/2) particles with ethanol or tetrahydrofuran. Furthermore, the molecular weight of the as-prepared particles was varied by the concentration of phenyltriethoxysilane used as a starting alkoxide. As a result of the variation of the molecular weight, the hollow PhSiO(3/2) particles with different stabilities against organic solvents were formed.     

纳米CaCO3/SiO2复合粒子的原位有机杂化及其应用研究

采用含有纳米碳酸钙的硅酸钠水性悬浮液在酸性物质的作用下，硅酸盐发生水解－缩合反应生成溶胶从而沉积在纳米碳酸钙粒子表面的溶胶沉积法，制备出具有核－壳结构的纳米碳酸钙／二氧化硅复合粒子；在体系中引入适当的亲油性诱导剂和有机改性剂，对复合粒子进行原位有机杂化并探索了其应用性能。     

核壳椭球微粒的吸波特性分析

基于离散偶极子近似方法，分析了核壳椭球微粒的电磁波吸收特性，给出了在电磁波波长与微粒粒径不同比例情形下，核壳椭球结构微粒的外壳厚度的变化对电磁波散射和吸收特性的影响，并讨论了椭球微粒形状变化（趋于针形）对吸波效果的影响。     

Color effects of uniform colloidal particles of different morphologies packed into films

The experimentally determined chromaticities and reflectance spectra of films consisting of uniform ellipsoidal or spherical colloidal hematite particles are compared with calculated values and are found to be in good agreement. The theoretical treatment of the light-scattering problem involves the Mie theory for the spheres and the T-matrix method for the ellipsoids. The reflectance spectra for the pigment films are calculated through the use of the Kubelka-Munk analysis.     

直流碳弧法制备碳包覆铁纳米颗粒机理研究

采用直流碳弧等离子体法成功制备了碳包覆铁纳米颗粒,利用透射电子显微镜和高分辨透射电子显微镜、X射线衍射、X射线能谱仪对样品的形貌、物相结构、化学成分和粒度进行表征分析,并对碳包覆纳米金属颗粒的形成机理进行初步探讨。结果表明:直流碳弧等离子体技术制备的碳包覆纳米金属颗粒具有明显的铁核(bcc-Fe)/碳壳(石墨层片)包覆结构,颗粒大多呈球形和椭球形,粒径分布在20~60nm范围,平均粒径为44nm,铁粒子外碳层的厚度为5~8nm。碳包覆铁纳米铁颗粒是通过颗粒内部固态形式的碳自行扩散至颗粒表面和颗粒外部气态形式的碳沉积到颗粒表面形成的。     

核壳粒子复合材料的等效磁导率

为了预测复合材料的等效磁导率,建立了填充核壳粒子复合材料等效磁导率的物理模型,应用电磁场理论推导了核壳粒子以单一介质球代替的等效方法并推广得到椭球核壳粒子情况.基于平均极化理论和Maxwell-Garnett理论给出了核壳粒子以特定浓度随机分布于复合材料时等效磁导率的预测公式,通过数值计算分析了核壳粒子浓度、结构参数以及磁导率对复合材料等效磁导率的影响.数值计算与实验结果吻合很好,验证了该等效方法用于复合材料电磁特性优化设计的有效性.     

Microstructure of iron particles reduced from silica-coated hematite in hydrogen

Poly- and nearly monocrystalline hematite particles having diameters of around 2 and 0.1 μm, respectively, were prepared by the gel-sol method and coated with a uniform silica layer by the sol-gel method. The core in the silica shell was reduced to iron without agglomerate formation between the particles by using a hydrogen stream. The microstructure and morphology of these cores and the silica layers were examined by high-resolution transmission electron microscopy, and electron and X-ray diffraction analysis. In hematite particles, around 2 μm in diameter, the reduced products were mostly α-Fe, but partially magnetite. In hematite particles, around 0.1 μm in diameter, only α-Fe was observed. Most of the raw hematite and iron particles produced were monocrystalline, and part of core grew hexagonal prism-shaped monocrystalline particles. In the case of the growth of a crystal to a hexagonal prism, a nanometer-scaled space at the interface between the iron crystal core and the silica layer was discovered.     

An aerosol-process for the synthesis of nanostructured molybdenum oxide catalysts by integrated chemical vapour synthesis/chemical vapour deposition at atmospheric pressure

We report the synthesis of composite nanoparticles by an integrated CVS/CVD process at atmospheric pressure. Iron oxide and silica support particles were generated by chemical vapour synthesis (CVS), using Fe(CO)5 and Si(OC2H5)4 and were directly coated in the aerosol state with molybdenum oxide by chemical vapour deposition of Mo(CO)6. Depending on the CVS temperature hematite (600 degrees C) or maghemite (1500 degrees C) iron oxide phases were determined by XRD and FTIR. Core-shell structures with a coating thickness in the lower nm range were obtained for CVD temperatures below 150 degrees C. Complete encapsulation of the core particles and uniform elemental distribution is shown by TEM and EELS measurements. Higher CVD temperatures lead to unwanted homogenous decomposition of the molybdenum precursor. Additional aerosol temperature treatment was used to reach further oxidation and the formation of a mixed oxide shell, indicated by FTIR measurements. The results show the potential of the process for the synthesis of structured core-shell nanoparticles.     

SiO2@TiO2核壳结构及其在高温下的隔热性能表征（英文）

以SiO2@TiO2核壳结构粒子为新型功能填料,采用旋涂方法制得了高温隔热涂层.TEM照片显示通过溶胶-凝胶法,成功在SiO2核上包覆上厚度为50 nm的TiO2壳层.通过自开发的测试设备表征了填料加入前后涂层在1300~1500℃的隔热性能.结果表明:SiO2@TiO2核壳结构粒子加入后,隔热涂层能将从热源辐射出的热流减少50%,在热源温度达1500℃时涂层试样的表背温度差为260℃.加入SiO2@TiO2核壳粒子的涂层在高温下隔热效果明显,是一种很有前景的高温隔热涂层填料.     

Morphology of ultra fine iron particles

Variation in morphology of the silica thin film coated ultra fine goethite particles(length:140 nm, aspect ratio:11/1, surface area:95 m²/g, SiO2/Fe:3.4 wt%) in the process of decomposition and subsequent reduction was examined by means of gas adsorption and electron microscopy. Microporous hematite particles, prepared by decomposition of the silica-coated ultra fine goethite particles at 250°C in vacuo, were subjected to heat-treatment at 700°C in air to form the nonporous hematite particles without degradation of the acicular shape. The highly acicular and nonporous ultra fine iron particles(length:110 nm, aspect ratio:10/1, surface area: 80 m²/g) were obtained as a result of shrinkage of the particles in the reduction process of the nonporous hematite particles at 400°C in hydrogen gas. Coercivity of the ultra fine iron particles was 1660 Oe.     

Morphology of iron fine particles

The process of formation of iron fine particles from goethite microcrystals was investigated by means of powder X-ray diffraction, gas adsorption, and electron microscopy. In the first process, microporous hematite particles were prepared by decomposing goethite particles. The pores formed in hematite particles were slit-shaped (width : 0.9 nm). In the second process, microporous hematite particles were reduced at 250-350°C under the flow of hydrogen gas, and the reduction degree R (%) was determined. In the sample of R=8%, mesopores of 4 - 8 nm were formed by aggregation of slit-shaped micropores, but the skeleton of acicular particles was not significantly altered. With the progress in reduction, a number of crystallites were formed in the parent particles together with growth of pore size. In the sample of R=72%, the crystallites were separated from the parent particles. Finally, the separated crystallites sintered to give granular iron particles having low coercivity of 375 Oe. It was found that alumina or silica gel coated on the surface of goethite particles was remarkably effective for preventing the separation and sintering of crystallites formed in the parent particles. The silica-coated iron fine particles consisting of the crystallites which were as large as single domain particles showed excellent acicular shape and high coercivity of 1600 - 1700 Oe.     

核壳乳液聚合乳胶粒形态理论研究进展

综述了核壳乳液聚合乳胶粒形态的理论研究进展，重点评述乳胶粒形态的热力学相关理论与演化动力学相关理论，认为乳胶粒热力学性质决定其平衡形态，演化动力学主要决定具体反应条件下的乳胶粒形态，聚合物的性质和相互之间的化学作用和物理作用影响乳胶粒形态。具体条件下的核壳乳胶粒形态是由热力学、动力学、聚合物性质和相互之间的作用共同决定的。     

不同结构聚合物核壳粒子对环氧树脂的增韧改性

传统环氧树脂的增韧改性方法往往达不到理想的效果。核壳粒子与环氧树脂混合,能减小内应力,获得显著的增韧效果,且不改变热变形温度。文中采用微皂核壳乳液的聚合方法合成了不同的核壳粒子,并对这些核壳粒子增韧环氧树脂体系的力学性能进行试验研究、理论分析和数值计算。用力学强度、动态力学分析等表征手段对核壳粒子的结构和改性环氧树脂体系的增韧机理进行了探讨。结果发现,改善核、壳之间或者核壳粒子壳层同环氧树脂之间的相容性和界面粘合力,核层能更好地将能量充分耗散,改性体系的冲击强度得以进一步提高。     

Thermal formation mechanism and size control of spherical hematite nanoparticles

Hematite nanoparticles were prepared by a FeCl₂ solution. The whole thermal formation mechanism as well as the size and dispersity control of hematite nanoparticles was studied. It has been found that goethite nanoparticles were firstly produced through the mix and oxidation of 0.5 M ferrous salt and 2.1 M bicarbonate and then hematite nanoparticles were obtained directly by thermal transformation of the goethite samples. At higher temperatures, nanopores were observed in the goethite nanocrystals and then merged into slits due to the high water pressure in the nanopores. The morphology of hematite particles with regular texture was changed due to recrystallization and then spherical nanoparticles were formed in the end. The particle size and dispersity of hematite nanoparticles could be controlled by different charging rates. From the second particle size distribution diagrams measured by the laser dynamic scatter method, not only the hematite particle size became small but also the dispersity of hematite nanoparticles was improved as the charging rate increased.     

Self-doped conducting core-shell poly(styrene/pyrrole) nanoparticles via two-stage shot-growth

Self-doped conducting core-shell poly(styrene/pyrrole) (poly(St/Py)) nanoparticles were successfully prepared by a one-pot synthetic route in both Fe(3+)-catalyzed oxidative polymerization and emulsifier-free emulsion polymerization. Modified two-stage shot-growth method was introduced to obtain higher doping level of the self-doped conducting core-shell poly(St/Py) nanoparticles. The particle size and core-shell morphology of the resulting particles before and after two-stage shot-growth were investigated by SEM and TEM analyses. Surface charge density of the particles highly increased after two-stage shot-growth and was measured by zeta-potential analysis. The self-doped core-shell nanoparticles showed a high conductivity after two-stage shot-growth.     

柔性可拉伸硅橡胶@多壁碳纳米管/硅橡胶可穿戴应变传感纤维

基于核-壳结构设计,采用简便、低成本的浸涂-固化法制得柔性、可拉伸、高灵敏且稳定的聚二甲基硅氧烷硅橡胶@多壁碳纳米管/聚二甲基硅氧烷硅橡胶(PDMS@MWCNTs/PDMS)压阻式应变传感纤维。通过FTIR、XRD、TG、TEM对硅烷偶联剂改性多壁碳纳米管(MWCNTs-KH570)的化学结构、热稳定性和微观形貌进行了分析,深入研究了核-壳结构与MWCNTs-KH570质量分数对PDMS@MWCNTs/PDMS复合纤维导电性能、传感性能及力学性能的影响规律与机制。结果表明:羟基化MWCNTs(MWCNTs—OH)表面接枝KH570使其在壳层PDMS基体中具有良好的分散性和界面相互作用;核-壳结构的设计使PDMS@MWCNTs/PDMS复合纤维在低填充下具有高电导率和传感性能;PDMS@MWCNTs/PDMS复合纤维的导电性能与传感性能随着MWCNTs-KH570质量分数增加而提高,且在人体关节运动监测中表现出良好的可重复性和工作稳定性。      

Controllable synthesis and characterization of novel copper-carbon core-shell structured nanoparticles

A facile hydrothermal method was developed for preparing copper-carbon core-shell structured particles through a reaction at 160 °C in which glucose, copper sulfate pentahydrate and cetyltrimethylammonium bromide were used as starting materials. The original copper-carbon core-shell structured particles obtained were sized of 100-250 nm. The thickness of carbonaceous shells was controlled ranging from 25 to 100 nm by adjusting the hydrothermal duration time and the concentrations of glucose in the process. Products were characterized with transmission electron microscopy, X-ray diffraction, energy dispersive spectroscopy, Fourier transform infrared spectroscopy. Since no toxic materials were involved in the preparation, particles with stable carbonaceous framework and reactive surface also showed promising applications in medicine, electronics, sensors, lubricant, etc.     

氧化石墨烯核-壳杂化粒子/硅橡胶介电弹性体复合材料的制备与性能

采用阳离子聚电解质聚二烯丙基二甲基氯化铵(PDDA)改性SiO₂, 再通过静电自组装制备了SiO₂-PDDA-氧化石墨烯(GO)核-壳杂化粒子。采用溶液共混法将SiO₂-PDDA-GO引入到高温硫化硅橡胶(SR)中, 制备了SiO₂-PDDA-GO/SR介电弹性体复合材料。结果表明:该方法能实现GO在SiO₂表面大面积的包覆, 解决了GO容易自聚集的问题, 且PDDA具有还原GO的作用, 无需再对GO核-壳杂化粒子/SR复合材料进行原位热还原, 简化了实验方案, 节能环保。SiO₂-PDDA-GO填充量为60wt% 时, 在100 Hz频率下, SiO₂-PDDA-GO/SR介电弹性体复合材料的介电常数为21.53, 是SR的11.6倍, 介电损耗保持较低值, 同时, 复合材料的模量保持在较低水平。在电场强度为2.48 kV/mm时, 60wt%的SiO₂-PDDA-GO/SR介电弹性体复合材料横向电致形变在同一电场强度下与SR相比增加了15倍。      

Development of Cu particles and Cu core-shell particles reinforced Al composite

Copper particles were incorporated and retained in elemental state in an aluminium matrix by friction stir processing thereby producing a non-equilibrium particulate composite. The processed Al–Cu_p composite exhibited improved strength with significantly high ductility. The composite was stable up to a temperature of more than 300°C. Thermal exposure at 350°C for more than 10 min led to diffusion of Cu atoms into the Al matrix forming a core-shell type structure in the Cu particles and thus producing an Al–Cu core-shell composite. The shell consists of multiple layers, the thickness of which was controllable.