Coalescence of the crystallites under hydrothermal conditions (II) —— The morphology and stability energy calculation of cuprite

The coalescence of crystallite under hydrothermal conditions was discussed in our previous paper[1]. When the solute concentration exceeds the supersaturation, the nucleation and growth process take place. The initial crystallites are only several nanometers. They have high surface-to-volume ratio, high index surfaces, and therefore have high surface energy. As the hydrothermal reactions proceed in the alkaline medium, the crystallite surfaces are apt to absorb polar solvate ions such as OH-,…     

The growth units and hydrothermal preparation of lead tungstate (PbWO4) crystallites

The crystal structure of lead tungstate (PbWO4) can be regarded as ordered combination of the tungsten oxide tetrahedrons (WO4) and lead ions (Pb2 ). According to the growth unit model, the growth units of lead tungstate are the aggregations of the tungsten oxide tetrahedrons and lead cations with various geometry configurations. It is suggested that the favorable growth units of lead tungstate crystal are pyramidal, tetragonal prism and quadrangular units corresponding to geometric orientations of the simple forms of the crystal. Under low restricted growth conditions, the growth form of lead tungstate crystallites is the aggregation of the geometric configurations of these favorable growth units. The above conclusions are completely confirmed by the experiment on hydrothermal preparation of lead tungstate crystallites.     

The formation of titania polymorphs under hydrothermal condition

The formation process of crystal polymorphs of titania under hydrothermal condition is studied. According to the experimental results and theoretic analysis, the formation process of crystal polymorphs can be described as a unit process. It includes the formation of growth units, the formation of nuclei through the polymerization of growth unit, and the growth of crystallites. The influence of the environmental phase and growth conditions on the formation of polymorphs is reflected in the changes of the structures of growth units. For example, when changing the pH of the reaction medium, the structure of growth unit with the highest stable energy in the hydrothermal system changes. Then different titania polymorphs can be prepared. The absorption, movement, crystallization or desorption of the growth unit are related to crystalline structure. On the other hand, the formation of crystal inner defects is related to the disturbance of the crystallizing process.     

Hydrothermal preparation and crystal habit of X-zeolite powder

The preparation of X-zeolite powder was investigatedin hydrothermal system, the crystal growth process of X-zeolite in hydrothermal condition was characterized by means of X-ray diffraction, scanning electron microscope and infrared ray. The results show that X-zeolite powder with uniform granularity and intact crystal shape can be obtained in hydrothermal system of acid-treated stellerite-NaOH-NaAl(OH)4-H2O; the crystallite size is in the range of 2 - 3μm. The best reaction time of hydrothermal preparation is 6 h. The formation phases of X-zeolite crystal are as follows: dissolution of feedstocks → formation of [SiO4]4- and [AlO4]5- tetrahedron, many-membered ring,β cage → formation of crystal nucleus and nano-particle → aggregation growth of nano-particle → coalescence growth of crystallite. The crystal habits of X-zeolite are intimately related with crystallization orientation ofβ cage in crystal and with its coupling stability on every crystal face family.     

Formation mechanism of barium titanate nanocrystals under hydrothermal conditions

Growth units and the crystallization habit of BaTiO₃ nanocrystals have been investigated. It has been proposed that the growth units of BaTiO₃ were surface hydroxylated Ti(OH)₆²⁻ octahedra. The relationship between crystal morphology and the variation of the current intensity in the solution has been obtained through the measurement of the OH⁻ in the solution and the hydrothermal experiment with superimposed direct electric field. Based on the computation of the stability energy of the growth units, the relationship between the crystallized morphology of crystallites and the most favorable growth units under different conditions has been derived. It has been found that there is structure similarity between anatase (TiO₂) and BaTiO₃ from the crystal chemistry viewpoint, so they are soluble in each other, which can serve as a reasonable explanation for the abnormal phenomenon of the retention of cubic substable phase at room temperature. Project supported by the National Natural Science Foundation of China.     

Formation mechanism of barium titanate nanocrystalis under hydrothermal conditions

Growth units and the crystallization habit of BaTiO3 nanocrystals have been investigated. It has been proposed that the growth units of BaTiO3 were surface hydroxylated Ti(OH)62- octahedra. The relationship between crystal morphology and the variation of the current intensity in the solution has been obtained through the measurement of the OH in the solution and the hydrothermal experiment with superimposed direct electric field. Based on the computation of the stability energy of the growth units, the relationship between the crystallized morphology of crystallites and the most favorable growth units under different conditions has been derived. It has been found that there is structure similarity between anatase (TiO2) and BaTiO3 from the crystal chemistry viewpoint, so they are soluble in each other, which can serve as a reasonable explanation for the abnormal phenomenon of the retention of cubic substable phase at room temperature.     

Template growth mechanism of spherical Ni（OH）2

The microstructures and growth process characteristics precipitation-crystallization method were investigated by SEM, TEM of spherical Ni（OH）2 particles synthesized by the aqueous and XRD, and their growth mechanism was discussed. With the reaction beginning and continuing, amorphous Ni（OH）2 nano-crystallites grow up to spherical micron-particles with radially arranged crystallites. The nucleation, crystallization and re-crystallization led by Ostwald ripening simultaneously take place through the whole growth processes. With the course from reversible aggregation to irreversible agglomeration, the Ni（OH）2 particles tend to grow according to the template growth model： the growth on the crystallite templates stretching in the radius directions is free and quick, while the growth rate for crystallites in other directions is confined due to lower monomers concentration and tends to dissolve So it is only the radially arranged crystallites that predominate in the particle and lead to characteristic microstructures.     

二氧化锡(SnO2)纳米颗粒的水热合成及表征

采用柠檬酸钠辅助水热技术合成单分散的二氧化锡（SnO2）纳米颗粒,用X射线衍射（XRD）、场发射扫描电镜（FESEM）、紫外/可见光谱等手段对其结构、形态和光吸收性能进行了表征,XRD和FESEM结果表明该产物是正方结构的SnO2纳米颗粒,直径约为60 nm,并用吸收光谱估计了禁带宽度（约3.6eV）.     

不同晶体结构的BiVO4的制备及其可见光催化性能

采用水热的方法,通过调控pH值,制备了具有不同晶型和晶体形貌的BiVO4晶体．利用XRD、SEM、XPS和UV—VIS对样品进行了表征．结果表明,在pH值等于1时,生成的是2—5μm的单斜白钨矿结构的BiVO4四方块;pH值等于7时生成的是0．2—1μm的单斜白钨矿结构的BiVO4纳米片;pH值等于12时,得到的是1—10μm的单斜四面体结构的BiVO4纳米带．可见光降解酸性橙II的催化活性测试表明,白钨矿结构的BiVO4的活性高于单斜四面体结构的BiVO4;而pH值等于7制备的BiVO4则表现了最高的催化活性．     

Formation of zirconia polymorphs under hydrothermal conditions

Using zirconium oxychloride solution as precursor, monoclinic zirconia crystallites with narrow distribution of nanosize were obtained in the hydrothermal reaction. However, when the reaction was in weak acidic medium or base medium, whether directly using the colloidal precipitate prepared from zirconium salt solutions with base solution as precursor added, or using the precipitate after filtrating, washing and drying treatments as precursor, the product of the hydro-thermal reaction was the mixture of both monoclinic and tetragonal polymorphs. As the pH of the medium rises, the content of tetragonal phase in the product, the morphologies and size of the crystallites all change. There are three types of formation mechanisms under hydrothermal condition, which can be called as saturation-precipitation mechanism in homogeneous solution, dissolution-crystallization mechanism and in-situ crystallization mechanism, respectively. The formation mechanism of crystallites varies with different hydrothermal condi     

磷酸燃料电池催化剂在运行中的形态变化

运用电化学方法测定了Pt/C催化剂在磷酸中不同时效阶段的电化学活性面积,同时采用XRD/TEM分析了Pt/C催化剂在时效过程中尺寸的变化,并运用分光光度法测量电极所在的磷酸中铂的含量,考察了铂/碳电极在不同情况下的溶解情况.结果表明:催化剂在时效过程中,随着时间的增加电化学活性面积逐渐减小,而Pt/C催化剂的粒径随着时间的增加逐渐增加;在开路电位下,催化剂的溶解量随时间的增加而增大,而催化剂在阴极极化下不发生溶解.分析讨论了碳载铂颗粒的增大机理和不同状态下铂的溶解机理.     

钨酸盐发光材料MWO_4:Eu~(3+)(M=Ca,Sr)的制备及表征

采用共沉淀法合成了CaWO4:Eu3+和SrWO4:Eu3+荧光粉体.利用荧光光谱仪测定了样品的光谱特性,结果表明,其主要激发波长为393nm和464nm,以393nm为激发波长说明样品能被近紫外光有效激发,并在614nm产生红色荧光;采用XRD分析其物相及晶体结构,发现生成的发光材料的晶型为四方晶系,晶粒均在纳米级,且在焙烧温度为400℃时生成的样品不含杂质,晶粒尺寸较小;扫描电镜显示400℃焙烧温度下生成的发光材料的样品颗粒大小在100~300nm之间,焙烧温度升高时,SrWO4:Eu3+的抗烧结能力弱,样品出现团聚,生成的样品颗粒变大.     

Preparation of ITO nano-powders by hydrothermal-calcining process

1 INTRODUCTIONSn-doped In2O3(ITO) is one kind of n-typesemiconductor material[1].It has excellent electro-optical properties , such as electrical conductivityand high transparency under visible light[2],andiswidely used in electronic , transparent electrode ,solar cells and electro-irradiance , especially inscreen display[3 ,4].Recently nearly half of the met-al indium has been used to prepare ITO materialsin the developed countries[5], such as Japan, A-merica ,France and so on.So the…     

水热法KTP晶体形貌及成因

利用双圈接触测角仪、双圈反射测角仪、微分干涉显微镜等测试手段,对不同条件下水热法生长的KTP晶体的宏观形态及各族晶面的微观形貌特征进行了观察和描述.测试了水热法KTP晶体的成分、结构.水热法生长的KTP晶体的宏观形态与晶体生长溶液的过饱和度及籽晶的切向、形态、悬挂方式有关:低过饱和度时,晶体中易出现高指数晶面,随着溶液过饱和度的增大,高指数晶面逐渐消失.各族晶面的微观形貌主要受控于晶体的内部结构.     

水热法和溶胶-凝胶法制备Mn_(0.8)Zn_(0.2)Fe_2O_4纳米磁性粒子及其结构表征

通过水热法和Sol-Gel法制备了Mn0.8Zn0.2Fe2O4纳米磁性粒子,利用X射线衍射(XRD)、扫描电镜(TEM)以及ICP元素分析对Mn0.8Zn0.2Fe2O4纳米粒子的晶型和形貌进行了表征,讨论了反应方法和反应条件对纳米粒度和结构的影响。结果表明,水热法和Sol-Gel法制备的纳米粒子均为尖晶石型结构,但前者纯度很高,平均粒径为11 nm,而后者含有氧化物杂相,平均粒径为45 nm,通过对比显示出水热法在此反应中的优越性。     

高反式聚异戊二烯(TPI)单链或寡链晶体形貌

配制 TPI/甲苯极稀溶液 (质量分数为 1 0 - 4%～ 1 0 - 2 % ) ,用喷雾法、漏斗富集法、生物展开法制备 TPI单链或寡链粒子试样 ,分别采用不同结晶温度及结晶时间。用透射电镜观察样品微观形貌 ,发现 TPI单链或寡链呈现多样的微观结晶形态 ,主要有 :尺寸为几十纳米的微晶粒子、几十至几百纳米的寡链单晶及在非晶衬底上的结晶小粒子等。实验发现 TPI寡链单晶较微晶小粒子更耐电子辐照。     

镁锌铁氧体粉末的水热法合成及其矫顽力机理

采用水热法合成名义成分为Mg1-xZnxFe2O4(x=0,0.2,0.4,0.6和0.8)的铁氧体粉末样品,采用X射线衍射仪、扫描电镜和振动样品磁强计等对其结构和矫顽力机理进行研究。结果表明:Zn含量增加有利于(Mg,Zn)Fe2O4铁氧体的成相,晶格常数也随着x的增加而增加;与x=0的样品相比,普通软磁材料矫顽力较大,其他样品的矫顽力呈现典型的软磁铁氧体值,且随着x的增大矫顽力呈逐渐减小的趋势,这与晶粒大小有密切关系;样品中微米级的大颗粒是纳米级小晶粒的聚集体。     

One-pot synthesis of hollow octahedral Cu2O nanostructures at room temperature

Homogeneous hollow Cu2O octahedral nanostructures have been fabricated by a facile one-pot reduction reaction at room temperature. The microscope analysis revealed that the edges of as-prepared hollow structures were around 200 nm with a wall thickness of about 20 nm. To investigate the influence factors and formation mechanism of the hollow octahedral structure, samples subjected to different reaction conditions were studies. The results showed that the morphology and structures of Cu2O particles were greatly affected by the concentration of pH value of the reaction environment and the reaction time. Ostwald ripening process is proposed to explain the growth mechanism of the hollow octahedral nanostructures.     

四方晶相HfO_2在(100)和(001)方向上光学特性的理论计算

文章采用基于密度泛函理论(DFT)框架下广义梯度近似平面波超软赝势法,计算了四方晶相Hf0_2的电子结构.经带隙校正后,计算了四方晶相Hf0_2在(100)和(001)方向上的光学线性响应函数随光子能量的变化关系,包括复介电函数、复折射率、吸收光谱以及反射光谱.计算结果表明四方晶相Hf0_2在(100)和(001)方向上具有明显的光学各向异性,并且具有从紫外到红外的透明区域.文中计算结果与其它文献报道的计算结果及实验值都吻合较好,由此说明采用密度泛函理论的广义梯度近似来计算HfO_2材料的光学特性是可信的.     

Morphologies of hydroxyapatite nanoparticles adjusted by organic additives in hydrothermal synthesis

Properties of hydroxyapatite (HA, Ca₁₀(PO₄)₆(OH)₂), including bioactivity, biocompatibility, solubility and adsorption could be tailored over wide ranges by the control of particle composition, particle size and morphology. In order to satisfy various applications, well-crystallized pure HA nanoparticles were synthesized at moderate temperatures by hydrothermal synthesis, and HA nanoparticles with different lengths were obtained by adding organic additives. X-ray diffractometry (XRD) and Fourier transform infrared (FTIR) spectrometry were used to characterize these nanoparticles, and the morphologies of the HA particles were observed by transmission electron microscopy (TEM). The results demonstrate that shorter rod-like HA particles can be prepared by adding cetyltrimethylammonium bromide (CTAB), as the additive of CTAB can block the HA crystal growth along with c-axis. And whisker HA particles are obtained by adding ethylenediamine tetraacetic acid (EDTA), since EDTA may have effect on the dissolution-reprecipitation process of HA.