水热法合成羟基磷灰石的微分析研究

以CaCO3和CaHPO4·2H2O为前驱体,采用水热法制备了羟基磷灰石(HAP)晶体,利用X射线衍射(XRD)、扫描电镜(SEM)及X射线能谱分析仪(EDS)系统研究了pH值、水热温度、反应时间、Ca2+浓度等条件对合成HAP晶体微结构及晶体生长的影响,同时对其生长机理进行了探讨.结果表明:随着水热合成温度的升高、时间的延长、Ca2浓度的增加,晶体发育越完整,HAP晶体的长径比呈增大趋势;体系的pH值对HAP晶体的生长有较大的影响,随着pH值的增加HAP晶粒的大小、长径比减小趋势明显;在水热温度为200℃,pH值=10,时间8h的条件下,可得到结晶度高、晶形完整清晰,端面尺寸在50～ 70 nm,生长极性明显的六方柱状的一维n-HAP晶体.EDS分析结果证实合成的HAP平均钙磷比约为1.70左右,同理论值比较相符.点分析研究表明晶体端面的钙磷比比平均的略高,钙磷比约为1.75,从而证明了Ca2+的浓度直接影响着HAP晶体的极性生长.     

柠檬酸钾对尿石患者和正常人尿液凝胶中草酸钙晶体生长的影响

采用扫描电子显微镜(SEM)和X射线衍射(XRD)方法,比较研究了防石药物柠檬酸钾(K3cit)在尿石患者尿液和正常人尿液制备的凝胶中对草酸钙(CaOxa)晶体生长的影响.没有加入K3cit时,CaOxa晶体均以一水草酸钙(COM)为主要晶相,加入K3cit后,不但COM晶体变得圆钝,比表面积减小,而且诱导了二水草酸钙(COD)生成.随着K3cit浓度从0.10增加到0.20 mol/L,在正常人尿液凝胶中COD晶体的百分含量从20;增加到45;,而在CaOxa结石患者尿液凝胶中,不但COD含量从10;增加到25;,而且K3cit可诱导草酸钙成核,从而产生大量的小尺寸草酸钙晶体,这有利于阻止草酸钙晶体变大形成尿石.本结果可为临床上治疗CaOxa结石提供启示.     

聚乙二醇分子量对其分散多壁碳纳米管能力的影响

本文研究了聚乙二醇(PEG)分子量对其分散多壁碳纳米管(MWNTs)能力的影响。PEG解团聚的能力与分子量的关系不是单调递增的,而是先降低后增加,存在一个最低点,这与其解团聚路线有关。PEG分散的MWNTs对时间和电解质的稳定性都随着分子量的增加而增加,但是对温度的稳定性却随着分子量的增加而减小。     

海带硫酸多糖防止草酸钙结石形成的体外模拟

采用扫描电子显微镜、X射线衍射法和红外光谱在草酸钙(CaOxa)结石患者尿液中研究了从海带中提取的硫酸多糖(LSPS)的防石作用.结果表明,LSPS可以抑制一水草酸钙(COM)的成核和聚集,并诱导二水草酸钙(COD)晶体形成.随着ESPS浓度从0增加到0.005, 0.02和0.20 mg/ml,COD的百分含量从0分别增加到22;, 55;和100;.这些结果表明LSPS是抑制CaOxa结石形成的一种潜在药物.     

Ca^2＋对KDP晶体的光损伤阈值的影响

Ca2 是KDP原料中一种常见的杂质离子,这种杂质不仅会影响晶体的生长过程,而且会加重晶体的光散射.通过传统降温法和点籽晶快速生长法生长不同Ca2 掺杂浓度的KDP晶体样品,对样品进行激光损伤实验,结果表明,Ca2 的存在降低了KDP晶体的光损伤阈值,其原因主要在于Ca2 掺杂导致晶体内部缺陷增多,内应力增加以及晶体中的散射颗粒密度增大使晶体光吸收加重.     

碱土金属离子对ZnO极性生长的影响

本文采用水热法,以3mol/L KOH为矿化剂,填充度35%,温度430℃,通过添加适量比例的MgCl2.7H2O和CaO,合成了非极性生长的ZnO晶体。当Mg2 :Zn2 =2%和Ca2 :Zn2 =2~3%时,晶体c轴方向生长速度明显减弱,{0001}方向的极性生长得到控制,所合成的晶体大面积显露正极面 c{0001},同时显露负极面-c{1001-}、正锥面 p{101-1}、负锥面-p{101-1-}和柱面m{101-0}。X光能谱(EDS)没有检测到晶体中含有碱土金属离子。     

Al^3＋：KTP晶体生长及其相关性质研究

采用高温溶液法生长不同掺质浓度的Al3 :KTP晶体,以等离子体发射光谱法测定晶体中Al3 的含量,并计算出Al3 在相应生长体系中的分配系数.采用X射线粉末衍射和粉末倍频法分别测定了所生长晶体的晶胞参数和倍频效应,结果表明随着晶体中掺质浓度的增加,晶胞参数逐渐减小,而倍频效应呈现略微增强的趋势.     

GdCOB晶体的坩埚下降法生长

本文报道了非线性光学晶体Ca4GdO(BO3)3(GdCOB)的垂直Bridgman法生长.已获得直径25mm的高质量单晶.生长界面处的纵向温度梯度维持在30～40℃/cm,生长速度0.2～0.8mm/h.GdCOB晶体为二维成核的层状生长机制,易出现(111)及(20)解理面.讨论了影响生长的因素.保证原料配比准确和混料充分,减小温度波动和测温误差等是成功生长GdCOB晶体的重要因素.     

Li/Nb比变化对Ce：Fe：LiNbO3晶体的光折变性能的影响

在LiNbO3晶体中掺进0.1wt?O2和0.03wt?2O3以Czochralski技术生长不同Li/Nb比(0.94、1.20、1.40)Ce:Fe:LiNbO3晶体,其中Li/Nb=1.40的Ce:Fe:LiNbO3晶体是化学计量比.测试了不同Li/Nb比Ce:Fe:LiNbO3晶体抗光损伤能力,得到随着Li/Nb比的增加,晶体的抗光损伤能力增加.研究了晶体抗光损伤能力增强的机理.随着Li/Nb比的增加,晶体的响应速度和光折变灵敏度增加.测试不同Li/Nb比Ce:Fe:LiNbO3晶体位相共轭效应,利用产生的位相共轭光波消除图像的位相共轭畸变.利用Li/Nb=1.40的Ce:Fe:LiNbO3晶体做记录介质,Li/Nb=1.20的Ce:Fe:LiNbO3晶体作位相共轭镜进行全息关联存储实验.实验结果表明,存储系统具有实时处理,成像质量好,信噪比高和可反复使用的优点.     

微下拉法生长炉研制及其在BGSO混晶生长上的应用

基于垂直凝固原理设计并研制了适合中低温晶体生长的微下拉法生长炉.采用该生长设备成功生长出不同掺杂浓度的锗硅酸铋纤维晶体,讨论了工艺参数以及掺杂浓度对晶体生长的影响,所得纤维晶体的最大长度达到195 mm.测试了晶体XRD和发射光谱.结果表明,随着SiO2含量增加,Bi4(Ge1-xSix)3O12单晶的晶胞参数随着Si含量增加而减小,而Si掺杂使晶体主发射峰轻微地向短波方向移动.     

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...     

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.     

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.     

Investigation of the Mechanism of Influence of Stress Corrosion on the Development of Macroplastic Instabilities of Aluminum–Magnesium Alloy

Crystallography Reports - Macroscopic jumps of plastic deformation (few percent in amplitude) on creep curves of aluminum–magnesium alloy, caused by a local effect of concentrated solution of...     

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.     

Mechanism of thermal expansion of structural modifications of zinc pyrovanadate

Crystal chemical characteristics of the α and β modifications of Zn₂V₂O₇ are calculated based on in situ high-temperature X-ray measurements. The expansion of the structure is found to be strongly anisotropic up to the negative volumetric thermal expansion of the α-Zn₂V₂O₇ unit cell in the temperature range of 300–600°С, α _V =–17.94 × 10^–6 1/K. The transformations of the “hard” and “soft” sublattices with an increase temperature and at the phase transition are considered in detail. It is shown that the negative volumetric thermal expansion of α-Zn₂V₂O₇ is due to the degeneracy of the zigzag-like shape of zinc–oxygen columns at constant distances between their vertices.     

A SAXS study of kinetics of aggregation of silica sols

SAXS in situ experiments on the evolution of TMOS solutions during hydrolysis and polycondensation lead to power laws with scaling exponents ≈ 2. It is suggested that this could be the result of the polydispersity of the samples and that only an apparent fractal dimension can be obtained in this way. Kinetic studies tend to indicate that agglomeration in the sol is the result of a diffusion-controlled process.