水热种分法制备低密度薄水铝石及其表征

以硫酸铝和尿素水热沉淀合成的低密度薄水铝石为晶种,采用水热种分过饱和铝酸钠溶液的方法成功地制备了低密度薄水铝石,结合ICP-AES、XRD和SEM等分析和表征手段,着重考察了单相、低密度薄水铝石的析出条件及其对产物晶体结构和形貌的影响.研究表明,100℃下种分48h或187℃下种分3h都可以得到单相、低密度薄水铝石,但种分条件对产物的形貌影响不大.上述低密度薄水铝石的水热种分法合成不仅丰富了传统三水铝石种分过饱和铝酸钠溶液过程的研究,也提供了一种低密度薄水铝石的制备方法.     

水热处理和尿素改性对三水铝石微观结构的影响

以尿素为改性剂,用水热处理方法对三水铝石进行了改性处理。结果表明,尿素的加入量和水热处理时间对产物微观结构有显著的影响,当尿素与三水铝石的摩尔比小于6∶1时,水热处理24 h的产物为片状薄水铝石;当摩尔比超过8∶1时,产物为板条组装的球形碱式碳酸铝铵.纯相碱式碳酸铝铵的形成与水热处理的时间有关,随处理时间的延长,氢氧化铝经历了由三水铝石到薄水铝石与碱式碳酸铝铵混相结构再到纯相碱式碳酸铝铵的演变过程,期间发生由块体到片状再到片组装块体的微观形貌变化,最后演变为板条组装球形结构。     

水热法制备花状γ-AlOOH

以十八水合硫酸铝和尿素为原料,十六烷基三甲基溴化铵(CTAB)和酒石酸钠为表面活性剂,在165℃水热条件下反应3h,制备花状γ-AlOOH结构。采用扫描电镜(SEM)、热重分析和X射线衍射(XRD)对样品进行表征。实验结果表明,采用水热法可以得到长度、厚度均匀的γ-AlOOH纳米片组装成的花状γ-AlOOH。     

多相氢氧化铝向薄水铝石相转变过程的微观结构研究

以铝直接水解法所得氢氧化铝粉为原料,经水热处理获得了纯相的薄水铝石粉体。研究了水热反应温度对产物γ-AlOOH晶体结构及微观形貌的影响,并利用XRD、SEM、TEM、HRTEM、粒度分布和TG-DSC对样品的物相、微观形貌及晶相转变过程进行分析表征。结果表明,水热温度对于制备纯相薄水铝石发挥重要作用,且有利于优化合成条件。随着水热温度的升高,物质结构转变动力也随之增强,可实现由多相氢氧化铝向纯薄水铝石相转变。利用CASTEP软件分别对薄水铝石、拜耳石及诺耳石体系进行几何优化,计算各体系的总能量。证实在同一计算精度下,薄水铝石的总能量最低,说明该体系最稳定。     

无模板合成海胆状薄水铝石超结构及其形成机理

在乙醇-水溶液体系中,在无模板剂的情况下,水热合成由纳米棒自组装成的独特海胆状薄水铝石(AlOOH)超结构.采用XRD、SEM、TEM和SAED对其物相结构和形貌进行了分析,讨论了铝盐前驱体、醇水比例和反应温度对产物形貌的影响.研究结果表明:当铝盐前驱体为AlCl3.6H2O,醇水体积比为1:2,反应温度为200℃时,得到形貌规则、分散均匀的三维海胆状薄水铝石超结构,该海胆状超结构是由直径60~80nm的纳米棒自组装而成,海胆球直径为6~10μm,选区电子衍射表明该海胆状薄水铝石的多晶本质.在薄水铝石海胆状超结构的形成过程中,定向附着机制起到关键性作用.     

溶剂热处理对氢氧化铝微观形貌分化作用

采用水、异丙醇及二者不同比例混合液为介质,通过140℃下溶剂热处理方法对种分法获得的氢氧化铝粉体进行处理,研究了溶剂类型、热处理时间对产物微观形貌的影响.研究结果表明,当以水为介质时,可以实现三维材料向二维材料的分化,即产物由块体三水铝石分化为片状薄水铝石;当介质中有醇存在时,产物由块体向叶片组合的薄水铝石相花型结构分化.     

PVP对溶剂热合成FeS2(Pyrite)的形貌控制研究

采用溶剂热合成技术,以FeSO4和(NH2)2CS为反应前驱物,在聚乙烯吡略烷酮(PVP)作表面活性剂的醇-水体系中获得了晶粒完整的FeS2(Pyrite)粉体.借助X射线衍射(XRD)和透射电镜(TEM)对合成样品的晶相组成、分散性、形貌进行了分析与表征,结果表明,以PVP为表面活性剂可以显著提高产物的分散性,适当调节PVP的用量可以有效调控FeS2晶体的大小与形貌.     

表面活性剂对水热合成Bi2Te3纳米结构形貌的影响

以Bi(NO3)3·5H2O和TeO2为原料,KBH4为还原剂并外加适量表面活性剂,在180℃保温48h水热合成出Bi2Te3纳米粉末.采用X射线衍射分析了产物的相结构和成分.采用透射电镜观察了产物的形貌,结合产物的形貌与表面活性剂的特性讨论了不同表面活性剂对水热合成Bi2Te3形貌的影响,分析了不同纳米结构的形成机制.     

介孔结构纳米TbxZr1-xO2-δ复合氧化物的合成及表征

采用以聚乙二醇(PEG)为表面活性剂的水热法合成了不同Tb/Zr比的TbxZr1-xO2-δ复合氧化物,并用以十六烷基三甲基溴化铵(CTAB)为表面活性剂的共沉淀法合成了Tb0.6Zr0.4O2-δ,将其作为不同方法的比较。利用XRD、TG-DTA、HRTEM、SAED和N2吸附-脱附对样品的物相结构、高温热稳定性、样品形貌、晶粒大小及孔结构进行表征。结果表明,当n(Tb)/n(Zr)≥0.6时样品呈现出氧化铽的立方晶体结构,合成的Tb0.6Zr0.4O2-PEG的表面形貌为不规则的类球状纳米粒子,粒径为5nm左右,产物的孔径主要集中在7.2nm左右。HRTEM图中明显显示出其晶体中的(111)及(200)晶面。TG-DTA曲线显示温度高于500℃时失重不明显,表明焙烧后的铽锆固溶体具有良好的热稳定性。     

二氧化钛纳米材料的制备与形貌控制

以草酸钛钾和双氧水为反应物,高纯水为溶剂,在不使用任何表面活性剂的条件下,采用一种简单的水热法制备了形貌可控的二氧化钛纳米材料.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)对所得产物的晶体结构和形貌进行了表征.测试结果表明所得产物为金红石相二氧化钛纳米带状花,通过改变混合溶液的搅拌时间和水热反应时间,可以实现对反应体系中气泡模板和产物形貌的调控,进而制得二氧化钛纳米棒状花.这种制备二氧化钛纳米带状花和二氧化钛纳米棒状花的简单方法,将为二氧化钛纳米材料的形貌和性能调控提供依据.     

EDTA辅助水热法制备不同形貌的氟化镁钠

以氟化钠、六水合氯化镁为主要原料, EDTA (乙二胺四乙酸二钠盐)为辅助剂, 通过水热法制备出不同形貌的氟化镁钠。考察了溶液pH、反应温度、时间和络合剂对产物形貌和物相的影响, 并对其形成机理进行了探讨。采用扫描电镜(SEM)、X射线衍射(XRD)和傅里叶变换红外光谱(FT-IR)等手段对产物形貌和物相进行了表征。结果表明: 在该反应体系中, EDTA既作为原料提供钠离子, 又作为络合剂与镁离子形成络合物; 反应温度、pH和络合剂对产物的形貌和物相有较大影响; 所得产物结晶度高, 有表面光滑的微米立方体晶体和纳米粒子聚集的微米空心球颗粒, 粒径均在1~3 μm之间。     

Fabrication and luminescence of CdWO4 particles by a hydrothermal process

CdWO₄ particles were synthesized by a hydrothermal process with or without surfactant. The particles have a pure monoclinic phase with the wolframite structure. CdWO₄ particles show different morphologies with the assistant of different surfactants. Nanoparticles were obtained when there is no the addition of surfactant. Cetyltrimethyl ammonium bromide and sodium dodecyl benzenesulfonate play the key roles in the formation of nanorods and microspheres, respectively. CdWO₄ particles with different morphologies have an emission peak in the blue wavelength range. The emission intensity of microspheres is higher than that of nanoparticles and nanorods. The results show that cetyltrimethyl ammonium bromide and sodium dodecyl benzenesulfonate alter the shape and size of resulting CdWO₄ crystals.     

Controlled Preparation and Formation Mechanism of Hydroxyapatite Nanoparticles under Different Hydrothermal Conditions

Hydroxyapatite(HAP) nanoparticles with uniform morphologies and controllable size were synthesized successfully by molecular template hydrothermal approach.The organic alcohols including ethanol,glycol,glycerol and butanol were used as templates to regulate the nucleation and crystal growth.The synthesized powders were characterized by X-ray diffraction,Fourier infrared spectrum and transmission electron microscopy.The results showed that the obtained HAP particles were uniform rod-like crystals,and the template molecular structures had significant effect on the morphology and size of HAP particles.The template molecules with longer hydrophobic groups resulted in longer particle length and larger aspect ratio.Compared with the concentration of template molecules,the template molecular structure showed larger influence on controlling the HAP morphology and size.Furthermore,the formation mechanism of these rod-like HAP particles prepared by alkyl alcohol templates was discussed.Moreover,hydrothermal treatment temperature and time could be also used for controlled preparation of HAP nanoparticles.     

Effect of particle morphology on the photocatalytic activity of BiFeO3 microcrystallites

Pure BiFeO₃ (BFO) microcrystallites with different morphologies were synthesized by a controlled hydrothermal process. The crystal structure, morphology and photocatalytic property of BFO microcrystallites were investigated. The results and analysis revealed that the OH^? concentration intensely affected the morphology, dimension and phase purity of BFO. Furthermore, it was found that the smallest and coarse BFO particles exhibited the lowest photocatalytic efficiency, which suggested that the particle morphology, especially defects intensely influence the photocatalytic activity of BFO, other than the particle size.     

Synthesis of different architectures like stars, multipods, ellipsoids and spikes of zinc oxide by surfactantless precipitation

Zinc oxide with different morphologies like stars, multipods, ellipsoids and spikes was synthesized using zinc nitrate and sodium hydroxide in the absence of surfactants. Seed mediation was found to be essential for the formation of ZnO nanospikes. Synthesized ZnO samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), UV-visible diffuse reflectance spectroscopy (UV-vis-DRS) and energy dispersive analysis by X-rays (EDAX) techniques. The predominant c-axis growth of hexagonal lattice was observed in ZnO anisotropic particles. TEM analysis revealed the formation of two types of ZnO ellipsoid particles. Concentration of the reactants was found to have a role in controlling the morphology of the resulting ZnO. Mechanism of formation of varying morphologies of ZnO particles has been proposed.     

Layered double hydroxide using hydrothermal treatment: morphology evolution,intercalation and release kinetics of diclofenac sodium

The present work demonstrates the possibilities of hydrothermal transformation of Zn-Al layered double hydroxide (LDH) nanostructure by varying the synthetic conditions. The manipulation in washing step before hydrothermal treatment allows control over crystal morphologies, size and stability of their aqueous solutions. We examined the crystal growth process in the presence and the absence of extra ions during hydrothermal treatment and its dependence on the drug (diclofenac sodium (Dic-Na)) loading and release processes. Hexagonal plate-like crystals show sustained release with ～90% of the drug from the matrix in a week, suggesting the applicability of LDH nanohybrids in sustained drug delivery systems. The fits to the release kinetics data indicated the drug release as a diffusion-controlled release process. LDH with rod-like morphology shows excellent colloidal stability in aqueous suspension, as studied by photon correlation spectroscopy.     

Effects of organic additives on the morphology of calcium carbonate particles in the presence of CTAB

In this paper, calcium carbonate particles with unusual morphologies could be easily obtained by a precipitation reaction of sodium carbonate with calcium chloride from mixed solution of organic solvents and water in the presence of cetyltrimethylammonium bromide (CTAB) at 80 °C. The as-prepared products were characterized with scanning electron microscopy and X-ray diffraction. The effects of different organic additives–glycol, glycerine, formaldehyde, acetaldehyde, glycol-methyl ether and glycol-ethylether, on the crystal form and morphology of the as-prepared CaCO₃–were investigated and discussed. The results show that organic additives can have great influence on the forms and morphologies of CaCO₃ at relative high temperature in the presence of CTAB. Various unusual crystal morphologies, such as dendrite-shaped, flower-like, wheatgrass-like, needle-like, whiskers, double-taper-like, etc., can be obtained depending on the experimental conditions. In particular, pure aragonite with unusual morphologies can be produced in the presence of glycol, glycerine, glycol-methyl ether at 80 °C, respectively.     

Fabrication of novel hierarchical ZnO via ultrasonic assisted hydrothermal route and their gas sensing property

Novel hierarchical ZnO nanomaterials with castellated and turriform morphologies were successfully synthesized by ultrasonic assisted hydrothermal route. The morphology and structure of products were characterized by scanning electron microscopy and X-ray diffraction, respectively. The results show that as-prepared castellated ZnO microrods have six-equal axis symmetry features with the length of 2–4 μm and the diameter of about 1 μm, and ZnO with turriform morphology has radical branch structure with the diameter ranging from 500 to 700 nm. It is found that initial alkaline concentration of the solution plays a crucial role in determining two kinds of hierarchical morphologies by etching ZnO crystal during hydrothermal process. A possible formation mechanism of castellated and turriform ZnO microstructures is also proposed. Gas sensing of hierarchical ZnO to different gases was also examined. The result indicates turriform ZnO sensor has fast response properties and excellent selective resolution capability to C₂H₅OH gas.     

Synthesis and hierarchical assembly of CoNi flowery particles

Novel chain-like CoNi hierarchical structures assembled from flowery particles were successfully synthesized via a hydrothermal synthetic route without surfactants or external magnetic fields. The effect of synthetic parameters, including citrate content, NaOH concentration, reaction temperature and time, on the formation and morphologies of the CoNi assemblies were investigated. The experimental results showed that the morphologies of the assemblies could be adjusted by the NaOH concentration and temperature. Compared with the isolated particles, the saturation magnetization of the chain-like assemblies decreased from 132.6 to 114.5 emu g^?1, while the coercivity increased from 84.4 to 260.7 Oe.     

Morphological control of flower-like ZnO nanostructures

Flower-like ZnO nanostructures composed of different building blocks, such as hexagonal pyramids, hexagonal prisms, and cones, have been synthesized on a large scale by a simple hydrothermal method in the absence of surfactants or organic solvents. The effects of the concentration of NaOH, reaction temperature, and reaction time on the morphologies of the resulting products have been investigated. The morphologies and the crystal structures of flower-like ZnO nanostructures were characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM).