氯氧化铋晶体的制备及其表征研究

采用铋盐转化水解法制备了四方相氯氧化铋晶体,研究反应温度、水解反应用水量以及反应液滴加顺序对产物粒径、产率及表面形貌的影响.结果表明,最佳反应条件为Bi(NO3)3·5H2O与HCl摩尔比为1∶5,反应温度为25～30℃,反应液滴加顺序为A→B,用水量为35 mL.该条件下制备出片状氯氧化铋晶体颗粒粒径0.5～2 μm,产物分散性良好.利用马尔文激光粒径分析仪、X射线衍射仪(XRD)、热场发射扫描电子显微镜(SEM)对氯氧化铋的粒度分布、晶面结构和微观形貌分析可知,所制备的氯氧化铋粒径分布符合正态分布曲线,且纯度高无任何杂质,反应液滴加顺序对产物形貌影响较大.     

微胶囊模板法TiO2微球的制备及表征

以钛酸丁酯为原料、硝酸为催化剂,通过水解-胶溶法制备了TiO2溶胶.以TiO2溶胶为内水相、环己烷为油相,制备了稳定的W/O型乳状液.在此基础上,以聚乙烯醇水溶液为外水相在W/O/W复相乳液体系中制备了TiO2溶胶微胶囊,经500℃煅烧除去有机物模板可得TiO2微球.利用SEM、FT-IR、TG/DTG等表征手段,重点考察了外水相中表面活性剂的使用对TiO2微球形貌的影响.结果表明,外水相中添加表面活性剂OP-10时所制备微胶囊的球形完整性、分散性和囊壁包覆完整性均较好,经煅烧后可得到球形完整、分散良好、粒径均匀且平均粒径在6μm左右的TiO2微球.XRD分析表明所得TiO2微球呈单一锐钛矿型、晶粒的平均尺寸约为6.5 nm.     

二氧化钛纳米晶囊泡微乳液在聚氨酯涂饰体系中的应用

以钛酸丁酯为原料,十六烷基三甲基溴化铵与十二烷基苯磺酸钠自组装形成的囊泡为微反应器,制备了二氧化钛纳米晶囊泡微乳液.将二氧化钛纳米晶囊泡微乳液与水性阳离子聚氨酯复配,得到聚氨酯/TiO2囊泡微乳液(UPC/TVM)复合皮革涂饰剂,采用TEM、马尔文粒径分析和紫外漫反射等方法,研究了TiO2囊泡微乳液和聚氨酯配比对涂饰剂分散、成膜、涂饰性能的影响.研究结果表明,TiO2囊泡微乳液与聚氨酯形成均一的微乳液,粒径尺寸在80 nm左右.TiO2囊泡微乳液的加入,使得UPC/TVM3膜与UPC膜相比,抗张强度、断裂伸长率和吸水性都有所提高并出现明显的抗紫外效果.UPC/TVM复合皮革涂饰剂应用实验结果表明涂层的抗水性提高,耐折性能没有改变.     

反相微乳液法制备CdS/ZnS纳米晶及其表征

用反相微乳液法制备了CdS纳米粒子,以ZnS对其表面进行包裹,得到了核壳结构的CdS/ZnS纳米晶.采用X射线衍射(XRD)、透射电镜(TEM)表征其结构、粒度和形貌,紫外-可见吸收光谱(UV-VIS)、光致发光光谱(PL)表征其光学特性.制得的CdS纳米微粒近似呈球形,直径约3.6nm;包裹以后颗粒仍为球形,粒径约10nm,以XRD、UV-VIS和PL证实了CdS/ZnS核壳结构的实现.文章还研究了不同Zn/Cd的摩尔比对CdS/ZnS纳米微粒光学性能的影响,UV-VIS谱表明随着壳层厚度的增加CdS/ZnS纳米晶的吸收带边有轻微的红移;PL谱表明壳层ZnS的包覆可减少CdS纳米微粒的表面缺陷,带边直接复合发光几率增大,且具有合适的壳层厚度时,CdS核层的发光效率有较大提高.     

溶胶-凝胶法制备氧化铝陶瓷球的研究

采用溶胶-凝胶法结合乳液微封装技术,以异丙醇铝为原料,稀硝酸为胶溶剂制备了粒径为毫米级的α-Al2O3球,并通过TG-DSC、IR、SEM、X射线衍射等分析手段对样品进行了表征.研究了形成稳定透明溶胶反应体系的条件、固化温度对α-Al2O3球粒径的控制以及煅烧温度对氧化铝球的晶型的影响,并揭示了其成球机理.结果表明:澄清透明的稳定氧化铝溶胶形成条件是:异丙醇铝:水:硝酸的物质的量比为1:100:0.25,水解温度为85℃;氧化铝球的粒径随固化温度的升高而增大;在1200℃保温5h可以得到结晶度好的α-Al2O3球.所制备的α-Al2O3球表面光滑,粒径在0.5 ～1.5 mm之间,球形度大于98.3;.     

多晶形γ-CuI晶体的制备与导电性能表征

以粗碘和硫酸铜为原料,水合肼为还原剂,利用液相法和微乳液法合成了不同晶形γ-CuI晶体.采用XRD和SEM研究了液相法和微乳液工艺技术条件对合成γ-CuI微观结构的影响,分析了具有不同微观结构γ-CuI对其导电性能的影响.结果表明,分别以聚乙二醇(PEG-6000)和柠檬酸为表面活性剂,采用液相法常温下500 r/min反应30 min可制备出纳米球形和三角锥形γ-CuI.按CTAB-正戊醇-环己烷-水配比3∶3∶7∶10分别配制硫酸铜和碘化铵微乳液,常温下500 r/min反应2h可制备出六边形薄片状γ-CuI.不同微观形貌和粒径分布对γ-CuI产品电导率具有较大的影响.纳米球形γ-CuI电导率最小,为4.9 Ω·cm.     

金刚石微粉对SiC机械抛光的影响研究

研究了金刚石微粉对碳化硅晶片表面机械抛光质量及去除率的影响.选取粒径均为W0.5～1μm、粒径分布和形貌不同的3种金刚石微粉,配置3种SiC单晶片机械抛光液.通过纳米粒度仪和扫描电镜分别测试了金刚石微粉的粒度分布和微观形貌.使用原子力显微镜测试了SiC晶片机械抛光后表面粗糙度.金刚石微粉的微观形貌越圆滑,粒径分布越集中,抛光后晶片的表面质量越好.金刚石微粉中单个颗粒的表面棱角有利于提高材料去除率.     

固相法合成BaTiO3粉体的水热改性研究

以固相法合成的BaTiO3粉体为前驱物,研究了4种不同水热条件处理后粉体的化学组成、颗粒形貌以及粒度分布的变化.结果表明:加水和加醇两种热处理后,粉体粒径变小,粒度分布范围变宽.经过加碱加盐和加酸加碱加盐处理后的粉体平均粒径增大,而粒度分布范围变窄.通过SEM观察发现,用不同配料方式的水热条件对BaTiO3进行水热处理后,粉体颗粒形貌变得圆整,实现了高温高压下的"整形"作用.     

微乳液法制备二氧化硅包覆ZnS:Mn/CdS纳米晶

采用微乳液法制备核壳结构ZnS:Mn/CdS(～4.5nm)纳米晶,为获得水溶性纳米晶,继续向此微乳液添加硅酸乙酯(TEOS),并使用氨水作为催化剂,通过TEOS水解缩聚反应,在ZnS:Mn/CdS粒子表面生长连续的二氧化硅壳层.采用透射电子显微镜(TEM)、X射线衍射(XRD)、红外光谱(IR)、光致发光谱(PL)对其表面形貌、结构和光学特性进行表征.ZnS:Mn /CdS纳米粒子表面被二氧化硅壳层完全包覆,粒径大小约为10nm左右,粒子均匀性好.由于二氧化硅相无定形且透光性良好,二氧化硅包覆ZnS:Mn/CdS纳米晶的光学特性与未包覆的ZnS:Mn/CdS极其相似.     

陶瓷墙地砖干法制粉造粒过程湿含量数值分析

针对陶瓷墙地砖干法制粉过程粉体颗粒湿含量分布不均匀性问题.采用有限体积法建立干法制粉造粒过程欧拉-欧拉多相流模型,模拟干法造粒过程雾化液滴的分布情况,分析干法造粒过程中粉体颗粒的湿含量均匀性;同时搭建试验平台测试干法造粒粉体颗粒湿含量.数值仿真结果表明:当干法造粒时间为10 s、20 s、30 s时,粉体颗粒分布区域雾化液滴的质量比分布分别在0.08 ～0.09、0.09～0.1、0.11-0.12区域,且20 s时造粒室内雾化液滴分布均匀性均最佳.同时实验与仿真对比表明:当干法造粒时间为10 s、20s、30 s时,造粒室内雾化液滴最大质量比实验测得值为0.086、0.112、0.123,数值模拟值为0.09、0.1、0.12;造粒室内雾化液滴平均质量比实验测得值为0.081、0.102、0.109,数值模拟结果为0.082、0.096、0.118.从局部与整体角度表明数值模拟与实验结果基于吻合,说明数值模拟结果的真实性,为陶瓷墙地砖干法制粉粉体颗粒湿含量均匀性分析提供了可靠的理论依据.     

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.     

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.     

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.     

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.