Fabrication of calcined hierarchical porous hollow silicate micro-size spheres via double emulsion process

Silicate (7 to 12 μm) microspheres with porous shell were prepared via modified double emulsion (water₁/oil/water₂) method mediated with N₂ pressure filtration and calcination to completely remove the organic components. With the addition of sodium polymethacrylate (Na-PA) into the aqueous solution of water₁/oil/water₂ emulsion system then calcined, led to the formation of stable hierarchical macroporous (surface area: 42.94 m²/g) from mesoporous (surface area: 259.2 m²/g) shell wall of silicate hollow microspheres.     

Fabrication of hollow silver spheres by MPTMS-functionalized hollow silica spheres as templates

In this study, we provide a strategy to prepare the hollow silver spheres by accumulating the silver nanoparticles on the surface of 3-mercaptopropyltrimethoxysilane (MPTMS)-functionalized silica as templates, which was accomplished by the chemisorption between silver nanoparticles and thiol groups. Then, the resulting hollow silver spheres were obtained through the chemical wet etching process with 10 M HF solution. In conventional method, the fabrication of hollow silver spheres from core-shell spheres was not easy due to the difficulties in retaining the shell structures during core removal. The method in this paper could overcome this limitation. The major focus of study is on understanding the mechanism of formation of the hollow silver spheres through the self-assembly behavior by chemisorption between silver nanoparticles and thiol groups. The silver-coated silica and hollow silver spheres were characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution TEM (HR-TEM), and X-ray photoelectron spectroscopy (XPS).     

Preparation of mono-dispersed carbonaceous spheres via a hydrothermal process

Mono-dispersed carbonaceous spheres (CS) with a narrow size distribution were synthesized via hydrothermal treatment of glucose. The effects of hydrothermal temperature and time, glucose concentration and pH value of solution were investigated in detail. Structures and surface properties of as-prepared products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Induced coupled plasma emission spectroscopy (ICP), thermogravimetric analysis/differential scanning calorimetry (TG/DSC), Nitrogen adsorption/desorption and Fourier transformed infrared spectroscopy (FTIR). The results showed that the production yield of CS increased from 2.1 to 32% with increasing the temperature from 160 to 180 °C, and the average size increased from 0.23 to 0.95 μm with extending the hydrothermal time from 8 to 16 h. pH value of the starting solution showed an evident effect on the morphology of CS via affecting the decomposition products of glucose. CS could be obtained when the pH value of starting solution was less than 12, but further increasing the pH value to 13–14 led to the formation of lumpy aggregations of carbon rather than spherical CS. The CS prepared under pH 6 and 9 showed good adsorption capacity for Methylene blue (MB), which was attributed to their relatively high specific surface area.     

磷掺杂中空碳球的制备及其电容性能EI北大核心CSCD

以酚醛预聚体和苯乙烯为原料通过水热法一步合成中空聚合物球(HPS),再以三氯化磷为反应剂通过傅-克反应对HPS处理得到含磷交联聚合物,经高温炭化和KOH活化制备磷掺杂中空碳球(AP-HCS)。采用FT-IR,TG,SEM,TEM,Raman,BET,XPS等手段对含磷聚合物和碳材料的组成、结构与形貌进行表征,测试碳材料在1 mol/L H2SO4介质中的电容性能。结果表明:AP-HCS的比表面积可达2177 m2/g,在1 A/g电流密度下,比电容为288 F/g,5 A/g电流密度下经循环充放电5000次后比电容值仍能保持88.9%,具备良好的电容性能。     

氧化硅空心微球的制备及表面形貌的调控

采用改进的St(o)ber溶胶凝胶法制备聚苯乙烯(PS)/氧化硅(Silica)复合微球,研究了添加油酸对复合微球形貌的影响.微球在经过500℃高温煅烧后,得到氧化硅空心微球.应用HPPS、Zeta电位分析、TEM、SEM、氮气吸附等手段对空心微球进行研究,证实了在包裹过程中油酸与氨水作用生成的油酸铵吸附在聚苯乙烯微球表面,增加模板微球表面电势从而有利于氧化硅粒子在其表面成核生长.此外油酸与硅羟基之间形成氢键增加氧化硅的生长点,增加了氧化硅壳层的密实程度.     

Photocatalytic performance of Gd ion modified titania porous hollow spheres under visible light

In this work, Gd-doped titania hollow spheres were prepared using hydrothermally prepared carbon spheres as template. The prepared samples were characterized by XRD, TEM, SEM, DRS and XPS. The photocatalytic activity of as-prepared hollow titania spheres was determined by degradation of Reactive Brilliant Red dye X-3B (C.I. reactive red 2) under visible light irradiation. The effect of Gd content on the physical structure and photocatalytic properties of doped titania hollow sphere samples was investigated. Results showed that there was an optimal Gd-doped content (4%) for the photocatalytic activity of X-3B degradation.     

Preparation and enhanced photocatalytic performance of Sn ion modified titania hollow spheres

Sn-doped hollow titania spheres were prepared using carbon spheres as template and Sn-doped titania nanoparticles as building blocks. The Sn-doped titania nanoparticles were synthesized under mild condition (low temperature and atmospheric pressure). The prepared hollow spheres were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM) and X-ray photoelectron spectroscopy (XPS). The effects of Sn content on the physical structure and photocatalytic activity of doped hollow titania sphere samples were investigated. It shows that the increasing of Sn content induces the transformation of titania from anatase to rutile phase. Results also showed that there was an optimal Sn-doped content (5%) in our samples for the photocatalytic degradation of Reactive Brilliant Red X-3B (C.I. reactive red 2).     

Preparation of CeO2 hollow spheres via a surfactant-assisted solvothermal route

In this study, CeO₂ hollow spheres were synthesized via a facile surfactant-assisted solvothermal route. The synthesized products were characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, selected area electron diffraction, and N₂ adsorption–desorption. Different solvent species has been demonstrated as the key factor responsible for the controlled morphologies. Furthermore, both the water and the oleic acid were crucial to the formation of CeO₂ hollow spheres. The possible formation mechanism of CeO₂ hollow spheres has been preliminary discussed.     

Synthesis of montmorillonite-chitosan hollow and hierarchical mesoporous spheres with single-template layer-by-layer assembly

In order to develop a facile and precisely controlled approach to synthesize hierarchical mesoporous materials with tailored property, in this work, a novel study was carried out to fabricate montmorillonite-chitosan hollow and hierarchical mesoporous spheres (MMTNS@CS-HMPHS) based on single-template layer-by-layer (LbL) assembly. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), specific surface area analysis and X-ray photoelectron spectroscopy (XPS) analyses were carried out to characterize the morphology and surface properties of MMTNS@CS-HMPHS. Benefitting from the unique lamellar structure of MMTNS, mesoporous channels are formed on the shell of MMTNS@CS hollow spheres, resulting in high surface area. Moreover, the surface functionalization and pore size of MMTNS@CS-HMPHS can be easily tuned, due to the tailored property through LbL assembly method. Besides the unique microstructure, MMTNS@CS-HMPHS also possesses the active sites generated from both MMT and chitosan, which greatly promotes its performance in fields of adsorption, drug delivery and catalyst supports, etc.     

新型多级形貌的硅酸盐空心球的合成

由化学方法制备的氧化硅通常是在较苛刻的条件下制备的,如升高的温度、较高压力和/或强酸性、强碱性媒介,相比之下,在自然界里具有精致形貌的硅藻氧化硅构架在温和周围环境下的水相中就可以形成.本文中我们系统研究了具有相似于硅藻多级形貌的氧化硅空心球的合成,该合成经过一步步骤,采用嵌段高分子EO76PO29EO76基的乳液和廉价硅酸钠溶液为硅源.     

Preparation and characterization of CdS hollow spheres

CdS hollow spherical particles with average diameter of 800 and 850 nm have been prepared using core/shell fabrication method with poly-(styrene-acrylic acid) (PSA) latex particles as template. TEM images show that smoothly coated core/shell composite particles have been fabricated by multicycles of coating in optimum concentration of reactants. CdS hollow spheres were obtained after removing the template by dissolving the polymer in the organic solvent, and the wall thickness is about 40-100 nm.     

反相微乳法制备纳米CdS/SiO2复合颗粒和空心SiO2球

采用TritonX-100/环己烷/正辛醇/水W/O型微乳体系,制备了粒径分布均匀、尺寸在30～50nm范围内的CdS/SiO2复合球,并通过酸处理,得到了相应的空心SiO2球.用TEM、XRD、FTIR、BET等手段对产品进行了表征.研究表明,改变反应物的加入量和反应物的浓度,影响颗粒的尺寸及其空心的大小.     

Synthesis of hollow spheres with mesoporous silica nanoparticles shell

Hollow spheres with mesoporous silica nanoparticles shell were synthesized with the use of cetyltrimethylammonium bromide (CTAB) and polystyrene (PS) hollow spheres as dual templates. The key to this study is that the uneven surface of the template provides nucleation sites for mesoporous nanoparticles, resulting in the formation of hollow spheres with mesoporous silica nanoparticles shell. The final products with hierarchical mesopores can be obtained through a simple one-step approach.     

二氧化硅/MeFe_2O_4中空复合微球的制备、结构及其磁性能

采用磺酸基团官能化中空二氧化硅微球为模板,通过化学共沉淀法,将尖晶石铁氧体(MeFe2O4)包覆在中空二氧化硅微球表面,制备出二氧化硅/MeFe2O4中空复合微球。利用TEM、XRD和样品振动磁强计对中空复合微球的形貌、结构和磁性能进行表征。实验结果表明,通过调节三价铁盐与二价金属离子之间的比例可以将尖晶石铁氧体的粒径范围控制在15nm以下。所制备的复合中空微球具有优良的软磁性。当金属离子总浓度为0.10mol/L时,复合微球的饱和磁化强度可达9.75Am2/kg。     

Theoretical and experimental studies on molecular spectra of the silica hollow spheres

The IR and UV spectra of the silica hollow spheres (SHSs) have been investigated using semi-empirical PM3 method. The calculated results have been compared with those from experiments. A cluster model of porous silica containing up to 36 SiO₄ has been proposed to characterize the fine structure of the SHSs. Effects of model size on the spectra have been discussed. The theoretical IR absorption peaks caused by OSiO vibration have matched the experimental response well. The UV absorption has been observed to move to larger wavelengths as the number of cluster and the number of configuration interaction (CI) increase. The PM3 calculations can assist greatly in analyzing the structure and molecular spectra of complicated materials with special morphologies.     

氧化锌空心球的制备及其气敏性能研究

以新制的碳球为模板在溶液相中制备了氧化锌空心球,并制成气敏元件,进行了气敏性能测试。结果表明,氧化锌空心球气敏元件对乙醇、丙酮和三乙胺有很好的敏感性。尤其是对三乙胺和乙醇分别在175℃和400℃表现出高的灵敏度和快的响应特性。     

Sol-gel synthesis, microstructure and adsorption properties of hollow silica spheres

Spherical colloidal particles with a hollow interior and a mesoporous shell are particularly useful for drug delivery and release because such spheres combine the unique properties of hollow interior (for storing the drug) with mesoporous shell (for controlled release). Hollow silica spheres (HSS) with a mesoporous shell were prepared via a sol-gel process in the presence of dual templates polystyrene spheres and cetyltrimethylammonium bromide for creating the hollow core and mesopore shell. The effect of the ratio of silica precursor over polystyrene spheres on particle morphology and pore structure of the HSS was investigated. The adsorption kinetics of methyl blue on the HSS was evaluated and correlated with the mesoporous shell structure.     

Fabrication of hollow silica spheres in an ionic liquid microemulsion

Hollow silica spheres have been successfully synthesized by using the ionic liquid microemulsion droplets as the template. The morphology and microstructures of the silica spheres were investigated by scanning electron microscopy (SEM), high-resolution transmission electron microscope (HRTEM), and Nitrogen adsorption-desorption measurements. The obtained images showed that the average size of the silica spheres was almost between 150 and 300 nm. The Nitrogen adsorption-desorption investigation on the silica spheres indicated the amorphous structure on the interface. Both of these two results provide us new insights into this novel template and hollow silica spheres were for the first time prepared free of additional acid and alkali conditions. The possible mechanism for the formation of silica spheres has been put forward and discussed in details.     

Synthesis of hollow silica spheres SBA-16 with large-pore diameter

Hollow silica SBA-16 spheres with cubic ordered mesoporous shells were synthesized by an emulsion-templating method, using Pluronic F127 as a structure-directing agent, tetraethyl orthosilicateas as a silica source and heptane as a cosolvent in the presence of NH₄F. The size of these spheres is in the range of 10 to 30 μm. The shell is about 700 nm thick and consists of large pores, ~ 9 nm in diameter, arranged in a cubic order. After calcination, the spheres maintain their mesoporosity and show a high surface area of 822 m²/g. The formation mechanism of the silica hollow spheres is discussed.