Synthesis and characterization of fine lithium niobate powders by sol‐ gel method

Lithium niobate (LN) nanocrystal powders were prepared by low‐temperature sol‐gel method. Dihydrate lithium acetate as lithium source, and niobium chloride as niobium source were used as starting materials. The gel and powders were characterized by thermogravimetry and differential scanning calorimetry (TG/DSC), X‐ray diffraction (XRD), transmission electronmicroscopy (TEM) and Fourier transform infrared (FTIR) spectra. The results show that when the gel was heat‐treated at 600°C, the fine LN nanocrystals with the size of 40‐60 nm were obtained, and the size of the powders become larger with the heat‐treated temperature increasing. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

热注法合成CuInSe2纳米晶的性能研究

以氯化亚铜(CuCl)、氯化铟(InCl3·4H2O)作为金属源,溶解在三辛基膦(TOP)中的Se粉作硒源,利用油胺(OLA)作为配体、十八烯作为溶剂,采用热注入法合成出了CuInSe2纳米晶(NCs),研究了反应温度对产物的影响.采用X射线衍射仪(XRD)、透射电子显微镜(TEM)、能谱仪(EDS)和紫外-可见分光光度计(UV-Vis)等测试手段对CuInSe2纳米晶的晶体结构、形貌、化学组分和光学性能进行了表征.实验结果表明:通过调控反应温度合成了具有不同形貌的黄铜矿结构的CuInSe2纳米晶,纳米晶的形貌由三角形或四边形向球形演化,其晶粒平均尺寸为3.71~13.65 nm,其光学带隙Eg在1.75~1.50 eV之间变化.所得到的产物在有机溶剂甲苯中分散性良好,这样的"墨水"溶液在后期制备薄膜太阳能电池更有利.     

Effect of ferric ions on the morphology and size of magnetite nanocrystals synthesized by ultrasonic irradiation

Two‐dimensional plate‐like Fe₃O₄ nanocrystals and nanoparticles could be synthesized by a simple one‐step sonochemical method through ultrasonic irradiation in reverse co‐precipitation solution at low temperature. This technique provided a facile and rapid way to prepare Fe₃O₄nanocrystals with different morphology and size. Magnetite nanoplates were synthesized with only ferrous salt adding into alkali solution, and adding ferric ions with low molar ratio in the metal salts solution would lead to the formation of very small magnetite nanoparticles (∼10 nm). The size of as‐prepared magnetite nanoparticles increased with increasing reaction temperature and showed narrow size distribution, the standard deviation less than 2 nm. This investigation indicated that ferric ions had significant influence on the morphology of Fe₃O₄ nanocrystals. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Relationship between morphology and structure of shape‐controlled CeO2 nanocrystals synthesized by microwave‐assisted hydrothermal method

The influence of synthesis conditions on morphology and structure of CeO₂ nanocrystals prepared by microwave‐assisted hydrothermal method were studied by XRD, TEM, Raman spectroscopy and photoluminescence measurements. Decisive effect of the OH^‐/Ce³⁺ molar ratio in the reaction mixture on the size and shape of CeO₂ nanocrystals was established and explained. Rise of the concentration of OH^‐ groups at the surface of growing CeO₂ nanocrystals promotes shape transformation from irregular (spheroidal) to cube and enables oriented attachment mode of particle growth. I was found that the unit cell parameter and intensity of Ce³⁺ defect related band in the luminescence and Raman spectra in ceria nanoparticles increase as follows: irregular shape nanocrystals < large cube < small primary cube shape particles. The reason is growing contribution of total subsurface volume under {100} faces, exposed by ceria nanocubes, where enhanced concentration of Ce³⁺ and oxygen vacancies occur.     

Synthesis and structural analysis of angled Te nanocrystals

In this paper, a new direct method to prepare angled Te nanocrystals (NCs) in the isotropic thiol‐ligand system from the transformation of MA‐stabilized CdTe nanoparticles (NPs) induced by the post‐addition of L‐cysteine was presented, without removing aforehand the protective shell of organic stabilizer. Besides nanorods, angled Te nanocrystals, including nanocheckmarks, X‐shaped, nanomoths, y‐shaped, and so on, also were obtained. By means of high‐resolution transmission electron microscopy (HRTEM), selected‐area electron diffraction (SAED) and powder X‐ray diffractometry (XRD), we further investigated intensively the internal crystal structure of angled Te NCs and the growth direction of the arms in this study. The experimental results obtained show that the preferential growth direction of either arms in nanocheckmarks is along the [001] direction of trigonal Te, and the corresponding contact plane should be (112) of hexagonal lattice. In the meantime, these results also confirm that L‐cysteine not only can be used as the stabilizer for the synthesis of aqueous CdTe NPs as reported previously, but also can act as a strong complexing agent like EDTA, inducing the decomposition of CdTe NPs, i.e. the transformation from CdTe NPs to Te nanocrystals. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

One‐pot fabrication of large‐scale ordered NiTe nanosheets and its application in lithium‐ion batteries

Large‐scale sheet‐like nickel telluride (NiTe) nanocrystals in situ grown on nickel foam with three‐dimensional network structure were successfully synthesized by reacting elemental nickel with tellurium powder. The reaction was conducted via a facile solvothermal method in a mixed solvent composed of 1 mL ethylenediamine and 15 mL ethylene glycol at 170°C for 24 h. The growth process and the possible formation mechanism were discussed based on the intermediate products obtained at different reaction stages including different reaction times and temperatures. When the as‐synthesized NiTe nanosheets were employed as anode materials for lithium‐ion batteries, this work enriches the electrode materials for energy materials, and can serve as a good reference for the fabrication of desired materials.     

Nanocrystallization of Insoluble Copper(I) Complex and Formation Mechanism

We have successfully fabricated insoluble copper(I) complex [Cu(μ-I)dppet]₂ nanocrystals by developing the heterogeneous reaction process between rod-like nanocrystals of dppet ligand prepared in advance and added acetonitrile solution of copper(I) halide. During this reaction process, the shape of dppet ligand nanocrystals was dramatically changed from rod-like to spherical. Probably, the complexation reaction and subsequent nanocrystallization would proceed on or near swollen surface of dppet nanocrystals in acetonitrile droplet as restricted reaction field.     

A novel thermolysis method of colloidal protein precursors to prepare hydroxyapatite nanocrystals

A novel thermolysis method of colloidal protein precursors is introduced to prepare hydroxyapatite (HAP) nanocrystals. The colloidal protein precursors are sonochemically synthesized from saturated Ca(OH)₂ aqueous solution, Ca(H₂PO₄)₂ aqueous solution and bovine serum albumin (BSA) molecules. The colloidal protein precursors are amorphous and composed of 15‐90 nm near spherical calcium phosphate nanoparticles and BSA molecules. The particle size analysis shows the volume particle size distribution is from 9.0 nm to 222.6 nm and the volume‐averaged particle size is 45.8 nm. During the calcination procedure BSA molecules are burningly removed and the HAP nanocrystals can be obtained at 500 °C. The effects of BSA concentration on the properties of samples are discussed. Results show that BSA combustion can promote the transformation of crystalline HAP from amorphous material. Moreover, the increase of BSA concentration reduces the crystalline sizes of HAP crystals and the crystallinity of product. With BSA concentration of 5 g/L, the obtained HAP nanocrystals are mainly 25∼100 nm similar spherical nanoparticles besides some 40∼70 nm×75∼150 nm short rod‐like crystals. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Malic acid assisted precursor route to hierarchical structured nickel oxide

A novel malic acid assisted precursor route to prepare NiO materials with novel hierarchical structures has been investigated in this work. The Ni‐based precursors can be synthesized by a malic acid‐assisted hydrothermal route, which have been characterized by powder X‐ray diffraction (XRD), field‐emission scanning electron microscopy (FE‐SEM), thermogravimetric analysis (TGA). NiO materials can be prepared via the thermal treatment of the precursor in ambient atmosphere. The XRD, SEM, Energy dispersive X‐ray spectroscopy (EDS) and UV‐Vis spectroscopy of the NiO materials were also examined. The effects of the reaction conditions, such as the reaction temperature, the quantity of the raw materials on the morphologies of the precursors were discussed, which indicates that it is an effective method to synthesize NiO materials with different hierarchical structures. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

High‐performance gas‐sensing properties of octahedral NiO crystals prepared via one‐step controllable synthesis route

Octahedrally shaped NiO powders have been synthesized via a one‐step composite‐hydroxide‐mediated method without any surfactant. The synthesized materials are characterized by XRD, EDS, TEM and FESEM techniques. Each particle exhibited a nearly perfect octahedron shape with sharp edges and corners as well as smooth surfaces. The octahedral NiO particles performed better gas‐sensitivity toward ethanol than that of NiO nanopowders, which was attributed to the exposed ｛111｝ facets of octahedron. The result was confirmed by the first‐principle calculation which indicated that the (111) facet was more active than (100) and (110) facet.     

Synthesis and characterization of Cu2ZnSnSe4 nanocrystals prepared by one pot route

Quaternary compound Cu₂ZnSnSe₄ (CZTSe) is one of the most promising absorber layer materials for thin film solar cells. In present work, the CZTSe nanocrystals were successfully synthesized via one pot route, and the influences of reaction temperature on the structural, compositional, morphological and optical properties of as‐synthesized CZTSe nanocrystals were investigated in detail via X‐ray powder diffraction (XRD), energy dispersive X‐ray spectrometry (EDS), transmission electron microscopy (TEM) and UV‐Vis spectrophotometry, respectively. The characterization results of as‐synthesized nanocrystals, under optimal synthesis condition (250 °C, 1 h), indicated that the nanocrystals was monodispersed with polycrystalline, the size was in the range of 10–15 nm, and the band gap energy was around 1.44 eV which is very closed to the best band gap energy for the solar cell. All results suggested that the as‐synthesized CZTSe nanocrystals were good light absorber layer material for thin film solar cell.     

Synthesis of zeolite ZSM‐5: Effect of emulsifiers

Zeolite ZSM‐5 has been synthesized in presence of various emulsifiers. Influence of types and proportions of cationic, anionic and non‐ionic emulsifier has been studied. Cationic emulsifier, cetyl trimethyl ammonium bromide resulted in an amorphous phase, whereas anionic emuisifier, sodium lauryl sulphate afforded crystalline phase, identified as magadiite. Non‐ionic emulsifiers, 1,2,3‐benzotriazole and sorbital mono‐stearate led to the formation of pure crystalline ZSM‐5 phase. Emulsifier concentration was found to affect the process of crystallization, and the crystal size and morphology of ZSM‐5. Emulsifier necessitated higher crystallization temperature and/or longer hydrothermal period. ZSM‐5 crystallization was observed to proceed through magadiite phase formation. In case of benzotriazole, unusual stacked square platelet type morphology and with sorbital monostearate, very small crystals were observed.     

Effect of growth temperature on the structure and optical properties of ZnO nanorod arrays grown on ITO substrate

ZnO nanorod arrays have been successfully prepared on ITO substrate by a chemical‐bath deposition method at different growth temperatures. The influence of the growth temperature on the morphology and microstructure of the ZnO nanorods was investigated by scanning electron microscopy (SEM) and X‐ray diffraction (XRD). The results showed that the diameter of the ZnO nanorods decreased and the size of the nanocrystals increased with increasing growth temperature. Optical absorption measurements showed the absorption band edge has shifted to a lower‐energy region due to the quantum size effect. Green emission and UV emission bands were observed and they are found to be temperature dependent, which indicates that the deep‐level emission and band‐edge emission of ZnO nanorods is closely related to the rod diameter, and the related mechanism is discussed.     

An X‐ray powder diffraction study of the microstructural evolution on heating 3:2 and 2:1 mullite single‐phase gels

Single‐phase gels with compositions 3Al₂O₃·2SiO₂ and 2Al₂O₃·SiO₂ were prepared by gelling mixtures of aluminium nitrate and tetraethylorthosilicate. Gels were fast heated at different temperatures between 900°C and 1600°C. The phase transformation and microstructural changes of both mullite precursor gels over the temperature range were followed by X‐ray powder diffraction (XRD), lattice parameter determination (LP), and scanning and transmission electron microscopies (SEM and TEM). The distribution of crystallite sizes and strains were determined by linewidth refinements of X‐ray diffraction patterns using the integral breadth method of Langford and the Warren‐Averbach analysis. XRD of both heated gels showed the formation of crystalline mullite single phase. Some amount of glassy phase coexisted with mullites at low temperatures, i. e. below 900°C. The compositional range of mullites formed on heating gels at temperatures between 900°C and 1600°C was dependent on the starting nominal composition of gels. SEM and TEM micrographs of both heated gels below 1200°C showed the formation of small, discrete, prismatic, well‐shaped nanocrystals in a very ordered arrangement. The size of these nanocrystals was dependant on the nominal composition of gels and increased on rising the heating temperature of gel precursors. The microstructural features obtained from linewidth refinement results of X‐ray diffraction patterns also allowed to suggest the formation of prismatic a little elongated nanocrystals at temperatures below 1200°C. Microstrain values were small and only displayed a relatively significant value for mullites processed at 900°C. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Optical and electrical properties of lithium doped nickel oxide films deposited by spray pyrolysis onto alumina substrates

Non-doped and lithium doped nickel oxide crystalline films have been prepared onto quartz and crystalline alumina substrates at high substrate temperature (600 °C) by the pneumatic spray pyrolysis process using nickel and lithium acetates as source materials. The structure of all the deposited films was the crystalline cubic phase related to NiO, although this crystalline structure was a little bit stressed for the films with higher lithium concentration. The grain size had values between 60 and 70 nm, almost independently of doping concentration. The non-doped and lithium doped films have an energy band gap of the order of 3.6 eV. Hot point probe results show that all deposited films have a p-type semiconductor behavior. From current–voltage measurements it was observed that the electrical resistivity decreases as the lithium concentration increases, indicating that the doping action of lithium is carried out. The electrical resistivity changed from 10⁶ Ω cm for the non-doped films up to 10² Ω cm for the films prepared with the highest doping concentration.     

NaYbF4纳米晶浓度调节方法研究

本文采用热分解法制备了NaYbF₄纳米晶.通过TEM图像对NaYbF₄纳米晶的尺寸进行表征.根据Beer-Lambert理论建立了NaYbF₄纳米晶浓度与其光吸收度间的关系.提出了NaYbF₄纳米晶浓度调节方法,利用NaYbF₄纳米晶中Yb³⁺的吸收光谱确定溶液中NaYbF₄纳米晶的浓度,并给出了纳米晶浓度调节公式.为了检验这种浓度调节方法,对五批次NaYbF₄纳米晶样品的浓度进行调节,发现浓度调节方法非常可靠.并对调整后的浓度进行多次测量,检验此调节方法的误差,最大误差在9;.     

氧化镍纳米晶体的制备及其过程分析

为了开发一种新型纳米氧化镍催化剂,能有效地应用于生物质气化过程中去除焦油,本文采用均匀沉淀法成功地制备了纳米氧化镍晶体,并利用TGA、FTIR、XRD、BET、YEM等分析手段对前驱体和产品的性能进行了表征.同时,对前驱体的分解过程进行了全面的分析.分析结果表明前驱体是水合碱式碳酸镍,其分子式为NiCO3·Ni(OH)2·nH2O,它能在360℃下完全分解转化为纳米NiO,同时煅烧条件对合成纳米NiO的晶体粒径影响很大.实验证实所得纳米NiO颗粒呈球形,分散性好,纯度较高,属立方晶系结构,平均粒径约为7.5nm,其BET表面积为187.98m2/g,这显示纳米NiO晶体具有作为高效催化材料的应用可行性.     

柠檬酸法制备固体氧化物燃料电池阳极材料Ni/SDC

采用硝酸盐-柠檬酸法合成出不同NiO含量的NiO/Ce_(0.8)Sm_(0.2)O_(1.9)(NiO/SDC)复合粉体,借助差热热重、XRD等对粉体的形成条件和相组成等进行了分析,并对粉体的比表面、粒度等进行了测定.由NiO/SDC粉体制备出固体氧化物燃料电池Ni/SDC金属陶瓷阳极材料,并对其微结构及相关性能进行了测试分析.结果表明:硝酸盐-柠檬酸法可以在较低的温度下合成出高比表面积的NiO/SDC粉体.制备的Ni/SDC阳极材料具有均匀细小的晶粒度和孔隙,以及高的电导率.1350 ℃烧结含55;NiO的NiO/SDC烧结体还原后所得Ni/SDC试样的孔隙率和电导率(700 ℃,H_2中)分别为38;和1825 S·m~(-1).     

Hydrothermal synthesis of ultralong single‐crystalline α‐Ni(OH)2 nanobelts and corresponding porous NiO nanobelts

Ultralong α‐Ni(OH)₂ nanobelts with uniform size have been prepared on large scale via a facile template‐free hydrothermal method. The as‐prepared nanobelts were single crystals, with several tens of microns in length and about 100 nm in width. For the whole process, a novel nucleation–aggregation–dissolution–seed‐directed growth mechanism was proposed based on the experimental results. The roles of aqueous ammonia and hydrothermal temperature were also discussed. Furthermore, porous NiO nanobelts were obtained by annealing the as‐prepared Ni(OH)₂ nanobelts. This facile, template‐free, and low cost method might feasibly be scaled up for industrial production. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis via an organic molten salt solvent route and characterization of PbS nanocrystals

In this paper, four petals flowers‐like and quasi sphere‐like PbS nanostructures were successfully synthesized by an environment friendly organic molten salt solvent (OMSS) route at 200 °C, with different sulfur sources, e.g. thiourea and sodium thiosulfate, respectively. The as‐synthesized products were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), UV–vis absorption spectrum and photoluminescence (PL) spectrum, respectively. It was shown that four petals flowers‐like and quasi sphere‐like PbS nanocrystals were formed. It was also demonstrated that the morphologies of PbS nanocrystals were significantly influenced by different sulfur sources. The ultraviolet‐visible absorption peaks of PbS nanocrystals exhibited a large blue‐shift and the luminescence spectra had strong and broad emission bands centered at 488 nm and 492 nm. The possible formation mechanisms of the PbS nanostructures were discussed. The organic molten salt solvent (OMSS) method is preferable for synthesizing high‐quality PbS nanocrystals. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)