超声波-溶胶-凝胶自蔓延法制备纳米氧化铝粉体

超声空化作用已经被证明是制备纳米粉体有效技术,可以防止团聚体生成。本文以柠檬酸为络合剂,在超声波中制得溶胶,用凝胶自蔓延法合成出了纳米Al2O3粉体。通过X射线衍射仪(XRD)、扫描电镜(SEM)和透射电镜(TEM)分析,探讨了不同比例金属离子与柠檬酸对纳米粉体的形成和粉末晶粒尺寸大小的影响。研究结果表明,超声空化可以减少团聚,金属离子与柠檬酸比例为0.6∶1干凝胶在600℃燃烧,保温60 min,可以得到团聚少、颗粒尺寸为20～30 nm的纳米Al2O3粉体。     

废旧电池溶胶-凝胶法制备Mn-Zn铁氧体的研究

以硝酸溶解废旧碱性锌锰电池所得的溶液为原料,用溶胶-凝胶法制备出了具有尖晶石结构的Mn-Zn铁氧体.借助于XRD、IR和SEM技术,对制备过程进行跟踪检测并对纳米晶铁氧体的晶体形貌进行表征.研究表明:制备Mn-Zn铁氧体的适宜条件为:金属离子和柠檬酸的比例为1:1(mol),pH=5.0,干凝胶煅烧时间为2h,煅烧温度为650℃;所得产物基本为球形,具有粒径小,分散均匀的特点.     

纳米高近红外反射颜料制备工艺研究

采用柠檬酸溶胶-凝胶法制备了纳米高近红外反射颜料,研究了Fe/Cr摩尔比、水解温度、溶液金属离子浓度、pH值、煅烧温度等因素对凝胶时间及试样性能的影响.结果表明,在Fe/Cr摩尔比为0.50,水解温度70℃,溶液金属离子浓度为2.5～3.5 mol/L,pH =3 ～4,煅烧温度为900℃保温60 min的条件下,制备颜料的主晶相为Cr1.3Fe0.7O3,近红外波段范围内(700～2500 nm)其平均反射率可达到77.58;,晶粒尺寸在50～ 200 nm之间.     

溶胶-凝胶法制备Y_(3-x)Ce_xAl_5O_(12)纳米粉体的研究

以Y(NO3)3.6H2O、Ce(NO3)3.6H2O、Al(NO3)3.9H2O、柠檬酸为主要原料,以聚乙二醇作为分散剂,采用溶胶-凝胶法合成了纳米级YAG∶Ce3+粉体。研究了煅烧温度、溶液中金属离子浓度、溶液pH值及Ce3+掺杂量等因素对制备纳米YAG∶Ce3+粉体的颗粒尺寸、颗粒形貌、物相的影响。结果表明:当溶液pH为=4.0、金属离子浓度为0.50 mol/L、煅烧温度为1000℃时,可以制备出具有良好的分散性,平均粒径在30 nm的粉体。     

自蔓延燃烧法合成CoFe2O4与红外辐射性能研究

采用溶胶凝胶自蔓延燃烧法制备了具有高红外辐射性能的钴铁氧体CoFe2O4.利用TG-DSC、FTIR、XRD、SEM以及比表面积、红外发射率测试等对干凝胶、自蔓延燃烧粉末及烧成产物进行了表征,研究了柠檬酸与总金属离子的摩尔比对所合成CoFe2O4粉体红外辐射性能的影响.结果表明,柠檬酸加入量影响干凝胶的自蔓延燃烧特性,进而影响烧成产物产物的结晶度、晶粒尺寸、形貌、比表面积以及红外辐射性能.当柠檬酸与总金属离子摩尔比为1:1时,CoFe2O4粉体结晶度好、晶粒尺寸小,烧成产物结构疏松,比表面积大(26.34 m2/g),红外辐射率高(红外法向全发射率高达0.87).     

自蔓延燃烧法制备ZrO2纳米粉体

以氧氯化锆为原料,采用一种低温而且快速的溶胶凝胶自蔓延燃烧法制备了纳米ZrO2粉体颗粒,通过X射线衍射仪(XRD)和透射电镜(TEM)分析探讨了柠檬酸与金属离子的物质的量比和杂质离子NH;和Cl-的存在对ZrO2粉体颗粒的形成和粉末晶粒尺寸大小的影响.本次试验成功的制备了粒径为30～90 nm的近球形ZrO2纳米颗粒,试验结果表明,NH4+和Cl-两种离子的存在阻碍了ZrO2粉体长大形成更大的颗粒,柠檬酸与金属离子的物质的量比例越大,燃烧产生的瞬间高温越容易使ZrO2粉体颗粒长大.     

柠檬酸凝胶燃烧法制备Nd∶YAGG多晶粉体

采用柠檬酸凝胶燃烧法制备了Nd∶YAGG多晶粉体.将Nd2O3,Ga2O3,Y2O3和Al(NO3)3分别用稀硝酸溶解后,与柠檬酸溶液均匀混合并于100℃加热4h,可以得到棕黄色凝胶,凝胶自燃可获得干凝胶.干凝胶分别在500℃、700℃和900℃下进行煅烧获得Nd∶ YAGG多晶粉体.红外光谱测试表明NO、OH等在900℃已被分解完全;扫描电镜观察发现煅烧后的Nd∶ YAGG多晶粉体是由规则的球状颗粒组成,粒径约为30 nm;XRD测试表明900℃为Nd∶ YAGG多晶粉体的最佳煅烧温度;荧光光谱分析发现Nd∶ YAGG多晶粉体具有较好的荧光性能,荧光发射的最强峰位于1064.54 nm处,属于Nd3+的4F3/2-4I11/2能级跃迁.     

凝胶燃烧制备中温固体电解质La0.9Sr0.1Ga0.8Mg0.2O3-δ

本文采用凝胶燃烧法制备La0.9Sr0.1Ga0.8Mg0.2O3-δ固体电解质(LSGM),讨论了溶液浓度、pH值、柠檬酸的加入量、加热温度等工艺条件对成胶的影响,X射线衍射分析表明,凝胶经1400℃煅烧10h制备得到单相粉体,制备的粉体颗粒尺寸平均为150nm.     

燃烧剂对低温燃烧合成Pr-CeO2粉体结构与性能的影响

以乙酸铵和柠檬酸为燃烧剂,Ce(NO3)3·6H2O和Pr6O11为主要原料,采用低温燃烧法(LCS)制备了Ce0.95Pr0.5O2纳米晶粉体.用DSC、XRD、SEM及色度测试等手段研究了Ce0.95Pr0.5O2纳米晶微粒前驱体的着火温度、产物晶体结构、晶体形貌及色度.结果表明:乙酸铵和柠檬酸作为燃烧剂的反应前驱体着火温度分别在250℃和300℃左右.两种燃烧产物均为单一的萤石型固溶体.与柠檬酸相比,乙酸铵作为燃烧剂得到的燃烧产物结晶程度更完善、Pr离子进入CeO2晶格的含量更多、呈色更好,且颗粒的团聚程度变小.根据Scherrer公式计算,用两种燃烧剂制备产物的平均晶粒尺寸分别为20～30 nm和10～15 nm,为纳米晶颗粒.最后得到Ce0.95Pr0.5O2粉体的颗粒尺寸则在200～300 nm之间.乙酸铵与硝酸铈的最佳摩尔配比为2:1,柠檬酸与硝酸铈的最佳摩尔配比为3:1.     

溶胶-凝胶法制备Nd_(1.85)Ce_(0.15)CuO_(4-δ)先驱体及粉体（英文）

以柠檬酸为螯合剂,采用一种简单的溶胶-凝胶法,成功的合成了蓝色透明的Nd-Ce-Cu-O体系的凝胶,保证了各元素在分子级别的均匀混合。采用红外光谱仪、热分析和XRD对实验过程和产物进行了分析。结果表明,对干凝胶及粉体的分析结果显示金属离子与柠檬酸螯合形成金属-柠檬酸螯合物,这些螯合物又通过酯化反应相互聚合成胶体粒子。干凝胶在30～600℃的温度区间内有五个失重过程。在600℃下已经合成了Nd1.85Ce0.15CuO4-δ粉体,该合成温度远低于固相法,此外通过谢勒公式计算得在600℃、700℃和1000℃下煅烧获得的粉体的平均粒径分别是18.2nm,31.1 nm和60.5 nm。     

Modelling of mechanism of agglomeration of KCl crystallization

The article presents an analysis into agglomeration during KCl vacuum crystallization. The theoretical and experimental investigations into the mechanism of agglomeration during mass crystallization result in an extension of the growth phenomena within the known model equations. The basis for this is essentially constituted by the collision model concepts of the theory of floculation in disperse systems. The parameters derived from the microprocess analysis (energy dissipation, content of solids, growth rate of individual grains) lead to model equations which are confirmed by laboratory and test trials.     

Relationship of Morphological Types of Dynamic Forms of Crystals

Crystallography Reports - The relationship of morphological spectra (sets of data on the morphological types of real polyhedral crystals and their probabilities under current physicochemical...     

Velocities of Disappearance and Lifetime of Faces of Growing Crystals

The formulae for absolute R_disap and relative R velocities of disappearance and lifetime τ of faces of growing crystals have been derived for stationary growth. It was shown that the quantities are determined by the relative growth velocity R_A/R_critA of the vanishing face A with respect to the critical growth velocity R_critA and by the geometry of a crystal expressed by the trigonometric functions of interfacial angles β and γ formed between face A and the adjacent faces. R increases and τ decreases with the increase in R_A/R_critA to certain limiting values. The calculations have been verified and illustrated by the experimental results for triclinic potassium bichromate (KBC) crystals. Results enable ones to predict values of velocities of disappearance and lifetimes of undesirable, supplementary faces of any real crystal.     

Development of Pauling's concepts of geometric characteristics of atoms

The evolution of the geometric characteristics introduced by Pauling and their dependence on the specific features of the structure and chemical bonds have been considered. The values of the covalent and van der Waals radii are given as well as their relationships and mutual transitions.     

Comparative analysis of two methods of calculation of the orientation of domain walls in ferroelastics

Two types of domain-wall equations are analyzed: the equations derived by the Sapriel method and the equations obtained by interface matching of the thermal-expansion tensor. It is shown that, for W-type domain walls, these methods yield the same equations. For W′-type domain walls, the equations obtained by different methods coincide for proper ferroelastics and differ for improper ferroelastics.     

Dependence of the parameters of equations of viscous flow on chemical composition of silicate melts

The temperature dependence of viscosity of silicate melts is discussed in the framework of the Avramov–Milchev (AM) equation. The composition is described by means of two parameters: the molar fraction, x, and the “lubricant fraction”, l. The molar fraction is the sum of the molar parts x_i of all oxides dissolved in SiO₂, the molar fraction of the latter being 1 ? x. It is shown that, with sufficient precision, two of the parameters of the AM equation can be presented as unique functions of the molar fraction. On the other hand, x is not sufficient to determine properly the reference temperature T_r , at which viscosity is η_r = 10¹³ [dPa.s]. Therefore, additional parameter, “lubricant fraction” l, is introduced. For each of the components, l_i is a product of molar part x_i and a specific dimensionless coefficient 0 ≤ k_i ≤ 1 accounting for the specific contribution of this component to the increased mobility of the system. It is demonstrated that, for l > 0, the reference temperature is related to the “lubricant fraction” l through the reference temperature T_r,SiO2 of pure SiO₂.     

A review of measurement of thermophysical properties of silicon melt

Measurements of thermophysical properties of Si melt and supplementary study of X-ray scattering/diffraction by the authors' group were reviewed. The values obtained differed variously from those of literature. Density was 2–3% larger, surface tension 20–30% smaller, viscosity up to 40% larger, electrical conductivity 8% smaller, spectral emissivity more or less in good agreement with literature values, and thermal diffusivity a few percent larger. An anomalous density jump was found near the melting point. Surface tension and viscosity also showed anomaly. A strange time-dependent change of density was observed over 3 h after melting. X-ray analyses suggested a slight change in local atom ordering, but showed no sign of cluster formation. An addition of 0.1 at% gallium caused the density jump to disappear, while that of boron caused no change. An EXAFS study of the former melt indicated a strong interaction between Ga and Si atoms as if molecules of GaSi₃ existed. The implications of the measured properties are a possibility of soft-turbulence in an Si melt in a relatively large crucible, a more complicated manner of intake of oxygen depleted molten Si from the free surface region to underneath the growing crystal, and a relaxation of the melt after melting arising from trapped gas species.     

Generation of crystal structures of heteromolecular compounds by the method of discrete modeling of packings

Within the method of discrete modeling of packings, an algorithm of generation of possible crystal structures of heteromolecular compounds containing two or three molecules in the primitive unit cell, one of which has an arbitrary shape and the other (two others) has a shape close to spherical, is proposed. On the basis of this algorithm, a software package for personal computers is developed. This package has been approved for a number of compounds, investigated previously by X-ray diffraction analysis. The results of generation of structures of five compounds—four organic salts (with one or two spherical anions) and one solvate—are represented.