Novel and facile method for the preparation of monodispersed titania hollow spheres

The fabrication of monodispersed hollow spheres in varying sizes and shapes is very interesting and has a lot of potential applications. This paper provides a very simple route to preparing hollow titania spheres using polystyrene (PS) as a template. In this approach, the titania shells were first formed and the PS cores were dissolved subsequently, even synchronously, in the same medium; neither an additional dissolution nor a calcination process was needed to remove the PS cores. Transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, and Barret-Emmet-Teller measurements were used to characterize the monodispersed hollow titania spheres. A possible formation mechanism of the hollow spheres was proposed.     

A novel method for the fabrication of monodisperse hollow silica spheres

In this paper, we report a novel method for the fabrication of small monodisperse hollow silica spheres. In this approach, when silica shells were coated on polystyrene particles by the sol-gel method, the polystyrene cores were dissolved subsequently, even synchronously, in the same medium to form monodisperse hollow spheres. Neither additional dissolution nor a calcination process was needed to remove the polystyrene cores. Transmission electron microscopy, scanning electron microscopy, and porosity measurements were used to characterize the monodisperse hollow silica spheres.     

水相一步合成锐钛矿型二氧化钛空心球

报道了水相一步直接合成晶体TiO2空心球的方法. 以水溶性的过氧化钛配合物(peroxo-titanium complex, PTC)为前驱体、聚苯乙烯(polystyrene, PS)球为模板, 在水溶液体系中可直接制备得到锐钛矿型纳米TiO2空心球. 与传统的模板法相比, 模板的包覆、去除及TiO2壳层的晶化等步骤在水相中可一步完成. 利用透射电子显微镜(TEM)、扫描电子显微镜(SEM)、X射线衍射仪(XRD)及热重分析仪(TGA)对所合成的纳米TiO2空心球进行了表征, 同时推断了可能的反应机理.     

Au纳米粒子负载的ZnO空心球复合材料的光生电荷转移行为及光催化活性

通过简单的两步法合成了不同负载量的Au/ZnO空心球。采用扫描电子显微镜(SEM),X射线衍射(XRD),X射线光电子能谱(XPS)及紫外-可见漫反射光谱(UV-Vis DRS)对样品的形貌、结构、组成和晶相等进行一系列的表征。以罗丹明B (RhB)为目标降解物,探究了Au/ZnO空心球的光催化活性。结果表明,适量Au修饰的ZnO光催化剂在混合光下20 min内对RhB的降解率达到73%。利用表面光电压谱(SPS)和瞬态光电压(TPV)技术,探讨了Au修饰后对ZnO光诱导电荷转移行为与光催化性能之间的关系。结果表明,混合光照下Au/ZnO空心球光降解性能的提高主要归因于作为电子受体的Au纳米粒子与ZnO之间形成的强的电子相互作用。适量Au纳米粒子的负载能够提高ZnO空心球中光生载流子的分离效率,相应地延长载流子的传输时间,增加光生电荷的寿命,从而促进其光催化活性的提高。     

ZnO-based hollow microspheres with mesoporous shells: Polyoxometalate-assisted fabrication, growth mechanism and photocatalytic properties

With the assistance of Keggin-type polyoxometalate, ZnO hollow microspheres with mesoporous shells were synthesized via a simple solvothermal approach without any templates and surfactants. The observations of morphology and structure performed by field emission scanning electronic microscopy and transmission electron microscopy indicated that the shells of the ZnO hollow spheres were built from nanosheets which were composed of nanoparticles. The transformation of structure and composition of samples were investigated by X-ray diffraction, X-ray photoelectron spectrometry and fourier transform infrared absorption spectroscopy. The formation mechanism of the hollow spheres is proposed based on time-dependent experimental results. The ZnO hollow microspheres exhibited a high photocatalytic activity for decolorization of Rhodamine B under ultraviolet irradiation.     

中空TiO_2微球的制备及对聚丙烯酸酯薄膜性能的影响

采用阳离子聚苯乙烯微球作为模板,钛酸四丁酯为钛源,氨水为催化剂,制备了中空TiO_2微球.采用X射线衍射、扫描电镜及比表面测定仪对其形貌和结构进行了表征,并考察了模板粒径、钛源用量以及催化剂用量对中空TiO_2微球形貌的影响.通过物理共混法将其引入至聚丙烯酸酯乳液中并成膜,研究了复合薄膜的保温性能、抗紫外性能及力学性能.结果表明,锐钛矿相中空TiO_2微球模板粒径、钛源用量以及催化剂用量影响中空TiO_2微球的空心尺寸、壁厚及壳层致密性.中空TiO_2微球可显著提升聚丙烯酸酯薄膜的保温性能、抗紫外性能和力学性能.采用不同粒径的模板制备的中空TiO_2微球对复合薄膜的各项性能均有影响,其中模板粒径为140 nm时复合薄膜性能最优,光反射率提升63%,导热系数降低27%,且在波长小于360 nm范围内,紫外透过率几乎为0,抗张强度增加100%,断裂伸长率提升62%.     

基于pH响应型微凝胶模板的二氧化锰空心球制备

以pH响应型微凝胶为模板制备出了二氧化锰空心球材料,并利用XRD、TGA、SEM、FT—IR和TEM等手段对其进行了表征．结果表明,通过调节KMn04的用量可以有效控制二氧化锰空心球的球壳厚度．对洗脱后上层清夜中的pH响应型微凝胶进一步研究发现,部分微凝胶呈现出非可逆的膨胀一收缩转变,这一现象主要是由于其内部的交联程度不高造成的．在对表征结果进行分析后提出了空心球结构的形成机理．     

HAP自组装球的简易合成及其光催化增效作用

选择生物协同模板,通过简单的控制组装工艺,制备出结构均一有序的羟基磷灰石(HAP)纳米组装球.该纳米组装球整体尺寸约5-6 μm,球体中心部分尺寸约为2.5-3 μm.通过X射线粉末衍射(XRD)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)、傅里叶变换红外(FT-IR)光谱、比表面积(BET)测试等手段对产物形貌、结构和比表面积进行了表征.产物作为催化剂载体,对氧化锌催化降解罗丹明B (RhB)的催化效率提高了125%,催化剂回收率提高了23.1%,有效降低了催化剂的用量,在有机物降解领域具有潜在的应用价值.同时还对产物的控制生成过程和催化增效机理做了初步探讨.     

Double template electrosynthesis of ZnO nanodot array

This communication describes the preparation of highly-ordered nanodot arrays of ZnO, a technologically important material, by the double template approach developed by Bartlett and co-workers. Colloidal polystyrene spheres were used as the primary template, and electrodeposited polypyrrole was used as the secondary template in this study. The ZnO nanodot arrays were prepared on a polycrystalline Au substrate by electrodeposition using the pyrrole secondary template after making it insulating by potentiodynamically deactivating it. The ZnO nanodot array was characterized by scanning electron microscopy, energy-dispersive X-ray analyses, and laser Raman spectroscopy.     

ZnO/In2O3复合空心球的制备及其光电催化葡萄糖降解性能

通过葡萄糖协助的水热以及随后的退火处理两步法成功制备了系列ZnO/In₂O₃复合空心球. X射线衍射谱(XRD)表明, 经500 ℃退火制得的ZnO/In₂O₃复合空心球中ZnO以非晶态存在, 但是随着退火温度的提高, 其逐渐转变为纤锌矿结构. 场发射扫描电子显微镜(FE-SEM)和透射显微镜(TEM)结果表明, ZnO/In₂O₃复合材料具有空心球结构, 复合纳米颗粒之间结合紧密. 将ZnO/In₂O₃复合空心球组装成薄膜光电极, 研究了其光电催化降解葡萄糖的性能. 结果表明, 700 ℃退火处理的ZnO/In₂O₃复合空心球薄膜电极可产生最高的光致电流密度. 通过光致发光光谱(PL)发现, 与ZnO或In₂O₃空心球相比, ZnO/In₂O₃复合空心球的发光强度猝灭效果明显. 这是由于复合材料中晶界处产生的p-n结电场, 降低了光生电子-空穴对的复合几率, 从而使更多的光生电子可迁移到电极表面.     

General sacrificial template method for the synthesis of cadmium chalcogenide hollow structures

Semiconductor CdX (X=Te, Se, S) hollow structures have been successfully prepared by using Cd(OH)Cl precursors as a sacrificial template. The hollow structures can be hollow spheres or tubes by controlling the shape of the sacrificial template. The products were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and energy-dispersive spectrometry. The obtained results showed that the hollow structures had complementary shapes and sizes of the original sacrificial templates. This is a general method for the synthesis of cadmium chalcogenide hollow structures, and the method is simpler and more practical than direct synthesis of certain hollow structures, which further widens the avenue to using those materials that have been synthesized with various shapes to fabricate specific hollow structures.     

PAMAM树形分子为模板低温制备纳米硫化锌空心球

Hollow ZnS spheres have been prepared in the presence of generation 3.5 poly (amidoamine) dendrimers with surface ester groups (G3.5-COOCH3 PAMAM dendrimer) as synthetic matrix template. The products obtained were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and UV-Vis absorption. TEM studies show that the hollow spheres with diameters ranging from 80 to 100 nm are prepared. The range of wall thickness was estimated to be about 20～30 nm. It was found that the concentration of PAMAM dendrimer had a significant influence on the formation of hollow ZnS spheres. The possible formation mechanism of the hollow spherical structure is also discussed.     

SnO2 hollow spheres:Polymer bead-templated hydrothermal synthesis and their electrochemical properties for lithium storage

SnO2 hollow spheres have been synthesized via a facile hydrothermal method using sulfonated polystyrene beads as a template followed by a calcination process in air.X-ray diffraction,scanning electron microscopy,and transmission electron microscopy show that the as-obtained SnO2 hollow spheres have a wall thickness of about 50 nm,and consist of nanosized SnO2 particles with a mean diameter of about 15 nm.Electrochemical measurements indicate that the SnO2 hollow spheres exhibit improved electrochemical performance in terms of specific capacity and rate capability in comparison with commercial SnO2 when used as anode materials for lithium-ion batteries.The enhanced performance may be attributed to the spherical and hollow structure,as well as the building blocks of SnO2 nanoparticles.     

反应性模板法合成硫化银中空球-银纳米粒子异质结构

以Cu₂S中空球为反应性模板, 通过在水溶液中与银离子的阳离子交换和氧化还原反应制备了大小均匀的Ag₂S中空球-Ag纳米粒子异质结构, 即Ag₂S-Ag异质中空球. 该异质结构中每个Ag₂S中空球的直径约为600 nm, 壁厚约20–30 nm, 其表面均附着一个Ag纳米粒子. 采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射(XRD)和能量色散X射线谱(EDS)对所得Ag₂S-Ag异质中空球的结构和组成进行了表征. 若以CuS中空球为反应性模板, 在相似转化条件下则主要得到不含Ag粒子的Ag₂S中空球. 该结果表明, Cu₂S中的Cu(I)的还原性在Ag₂S-Ag异质中空球的形成中发挥了重要作用. 通过对所制备的Ag₂S-Ag异质中空球进行二次生长, 还可以得到Ag₂S中空球的半球表面均被Ag膜所包覆的Ag₂S-Ag异质中空球.     

Urchin-like double-shelled Pd–PdO/ZnO hollow sphere as an efficient catalyst for the Suzuki-Miyaura reaction

In recent years, the modi?cation of metal oxides with noble metals to decrease the loading amount of expense of noble metal catalyst and amend the stability of nanocatalyst in chemical reactions has attracted signi?cant attention. Here in this study, the urchin-like double-shelled Pd–PdO/ZnO hollow sphere is successfully prepared by using a simple hydrothermal method and carbon sphere as a hard template. The structure of the catalyst was confirmed by using field-emission scanning electron microscopy, transmission electron microscopy, X-ray powder diffraction, energy-dispersive X-ray spectroscope, and BET. The total amount of palladium particles on ZnO was determined by induced coupled plasma analysis. The prepared catalyst gave high catalytic activity for the Suzuki reaction of aryl halides to afford biphenyls under milder conditions. Furthermore, the stability and reusability of catalyst were investigated, and all of the data proved that urchin-like double-shelled Pd–PdO/ZnO hollow sphere could be recycled five times without marked loss of activity.     

In2O3/ZrO2-TiO2空心球复合材料的制备与光解水制氢性能

以聚苯乙烯(PS)胶球为模板, 通过一步法结合煅烧后处理制备了空心球复合材料In₂O₃/ZrO₂-TiO₂. 采用X射线衍射(XRD)、 X射线光电子能谱(XPS)、 扫描电子显微镜(SEM)、 紫外-可见漫反射吸收光谱(UV-Vis DRS)和氮气吸附-脱附等测试手段对复合材料的结构、 组成和形貌进行了表征. 结果表明, In₂O₃/ZrO₂-TiO₂复合材料的晶型结构以锐钛矿型TiO₂为主, 同时存在少量含有Ti—O—Zr键的混合氧化物. 该复合材料经聚苯乙烯模板处理后呈现空心球状结构, 球壁由纳米粒子堆积而成. In₂O₃/ZrO₂-TiO₂空心球复合材料的比表面积较大(66.92 m²/g), 且In₂O₃与ZrO₂-TiO₂复合后光吸收发生了红移. 对该复合材料光解水制氢性能的研究结果表明, 空心球状In₂O₃/ZrO₂-TiO₂具有较好的产氢效果(56.7 μmol/g, 8 h), 明显高于P25、 ZrO₂、 空心球状ZrO₂-TiO₂及粉末状In₂O₃/ZrO₂-TiO₂.     

自催化还原制备微米和纳米级空心镍球的研究

提出了一种新型的制备超细空心金属镍粉的方法.通过FESEM,TEM和XRD衍射对该制备方法进行了研究,并考察了有关工艺参数对产物粒径和粒度分布的影响.研究认为,通过在胶核表面发生自催化还原反应,形成金属镍壳,同时胶核发生自分解,最后可得到空心金属镍球.控制反应物浓度和NaOH的配比可得到粒径均匀的镍球;通过调整这两个参数可得到粒度在微米或纳米尺度的空心镍球.     

水热沉淀法制备掺铁二氧化钛中空球及其光催化性能

 以碳球为模板剂, 采用水热沉淀法制备了不同配比掺 Fe 的 TiO2 (Fe-TiO2) 中空球, 并运用 X 射线粉末衍射、扫描电子显微镜、元素分析能谱、红外光谱和热重等方法对其进行了表征. 结果表明, 中空球为锐钛矿相, 大小为 0.5~3.20 ?m, 壳层厚度为 30~60 nm, 比表面积为 150~300 m2/g. 随着 Fe 掺杂量的增加, 中空球在可见光区的吸收强度逐渐增加. 光催化降解实验表明, 掺 Fe 后, TiO2 中空球的可见光催化活性升高, 其中 0.5% Fe-TiO2 在 80 min 内降解亚甲基蓝超过 75%. 同时还讨论了光催化机制.     

以手性两亲小分子自组装体为模板制备介孔二氧化硅空心球

合成了手性阳离子型两亲性小分子化合物,利用圆二色谱分析了其在水中形成的自组装体的结构;以该化合物的自组装体为模板,在正丙醇和氨水的混合溶剂中制备得到了介孔二氧化硅空心球;利用扫描电镜、透射电镜、X射线衍射仪以及氮气吸附-脱附试验装置分析了二氧化硅空心球的形貌及孔结构.结果表明,两亲性小分子在水中形成的自组装体呈现手性堆积;合成的介孔二氧化硅空心球的直径约为600~800nm,壁厚约为100~150nm,其孔道垂直于球的表面,孔径约为3.0nm,比表面积约为306m2·g-1.正丙醇作为模板控制二氧化硅空心球的空腔尺寸和形貌,而两亲性小分子的自组装体作为模板控制放射状孔道的形貌和尺寸.     

A facile method of synthesis of asymmetric hollow silica spheres

This paper presents a "one-step" method to synthesize asymmetric hollow silica spheres. In this method, when positively charged polystyrene particles were blended with mercaptopropyltriethoxysilane and stirred at 50 °C in alkaline ethanol/water medium for a period of time, Janus or lobed asymmetric hollow silica spheres could be directly obtained, just changing the ratio of ethanol to water in the reaction medium. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were used to characterize the morphology and topography of the asymmetric hollow silica spheres. The formation mechanism was described in detail.