微波水热法制备六方片状CdS团簇

采用微波水热法,以氯化镉(CdCl2·H2O)和硫代乙酰胺(CH3CSNH2)为镉源和硫源,制备了具有六方片状结构的CdS微晶。利用X射线衍射仪(XRD)、场发射扫描电子显微镜(FE-SEM)、EDS、透射电子显微镜(TEM)和高分辨透射电子显微镜(HRTEM)等对样品的物相、形貌和元素组分进行了分析,并采用紫外吸收光谱表征其光学性能。结果表明:以CH3CSNH2为硫源合成的CdS微晶具有六方片状团簇的特殊形貌,通过与相同条件下以Na2S2O3·5H2O为硫源合成CdS晶的FE-SEM照片对比发现,CH3CSNH2在此特殊形貌的制备过程中起到了重要作用。通过紫外吸收光谱得出,样品的禁带宽度为3.82 eV,蓝移量达到了1.37 eV。     

一维Sm2O3纳米晶的可控合成及其光学性能研究

以有机碱二乙烯三胺(EDTA)为碱源,Sm(NO3)3·6H2O为钐源,在不同模板剂辅助条件下采用水热-热处理相结合的方法进行Sm2O3纳米晶的可控合成.利用X-射线衍射仪(XRD)、扫描电子显微镜(SEM)和Lambda 950分光光度计分别对产物的物相、形貌和光学性能进行表征,并研究了未添加模板剂和分别以六亚甲基四胺(HMTA)、聚乙烯吡咯烷酮(PVP)和十六烷基三甲基溴化铵(CTAB)为模板剂条件下对产物的物相、形貌及光学性能的影响.结果表明:以HMTA为模板剂条件下得到了长条状结构的Sm2O3纳米晶,未添加模板剂和分别以PVP和CTAB为模板剂条件下得到了尺寸可控的棒状结构的Sm2O3纳米晶.不同模板剂会影响产物的微观结构及尺寸,进而对其光学性能产生有较大的影响,其中以HMTA为模板剂时所得长条状结构的Sm2O3纳米晶的禁带宽度较小为4.775 eV.     

水热法生长立方MgO微晶研究

以尿素与Mg(NO3)2·6H2O在不同的反应温度和不同物质的量配比条件下,制备出前驱体Mg5(OH)2(CO3)4·4H2O/MgCO3,经煅烧得到立方MgO微晶粉末.利用X射线衍射仪(XRD)和扫描电子显微镜(SEM)对所制得产物的晶相和形貌进行了表征.结果表明:当尿素和Mg(NO3)2·6H2O物质的量的比为2∶1时,在160℃的水热反应条件下,制备出立方MgO前驱体微晶,在1000℃煅烧2h后能够获得晶型完整、形貌规则、粒径约为5μm的MgO立方微晶.     

结构导向剂对Cu2O微晶的形貌及光催化性能的影响

以抗坏血酸和甲酸为还原剂,Cu( NO3)2为铜源制备了Cu2O微晶,并借助X射线衍射(XRD)和场发射扫描电子显微镜( FE-SEM)对样品的物相组成和形貌进行了表征,同时以罗丹明B为模型污染物,探讨了Cu2O微晶的形貌对光催化活性的影响.结果表明,在室温条件下以抗坏血酸为结构导向剂可获得八面体Cu2O微晶;而以甲酸为还原剂,160℃水热反应可获得Cu2O球形微晶.光催化降解实验表明,所得Cu2O微晶对罗丹名B有一定的光催化活性,且催化剂的形貌对其活性有很大影响,八面体Cu2O微晶(111)活性晶面外露较多,因而具有较高的光催化活性.     

枝状Ni2P微晶的制备、表征及其光催化性能研究

以硫酸镍(NiSO4·7H2O)为镍源,尿素为pH调节剂,采用表面活性剂辅助的水热法成功制备出了枝状Ni2P微晶.X-射线粉末衍射(XRD)、场发射扫描电子显微镜(FESEM)和紫外-可见分光光度计(UV-Vis)对所得产物进行表征.结果表明,所得产物为纯六方相的磷化镍(Ni2P),其形貌为有明显主干和高度有序分支的树枝状结构.其中,表面活性剂(SDBS)在枝状Ni2P微晶的整个生长过程中起到模板作用.对所得产品光催化性能研究发现,枝状Ni2P微晶能够很好地光催化降解亚甲基蓝溶液,降解率较高.     

钒酸铜空心纳米结构的制备及电化学性能

以CuSO4·5H2O和NH4VO3为原料,聚苯乙烯(PS)微球为模板,采用模板法制备了具有空心结构Cu3V2O7(OH)2·2H2O材料.采用X射线衍射(XRD)和场发射扫描电子显微镜(FE-SEM)对不同结构的Cu3V2O7(OH)2·2H2O的组成和形貌进行了表征.实验发现通过控制反应温度及反应体系的pH值可实现对Cu3V2O7(OH)2·2 H2O材料微观结构及形貌的良好控制.电化学性能测试表明:不同结构的Cu3V2O7 (OH)2·2H2O材料其放电性能存在着明显的差异,具有蜂窝状结构的Cu3V2O7 (OH)2·2H2O展现出较高的放电比容量,25℃条件下其首次放电容量可达到489 mAh/g.     

微波水热时间对CuS微晶形貌及光学性能的影响

采用微波水热法,以Cu(NO3)2·3H2O和SC(NH2)2为原料,在无模板剂的条件下,对靛铜矿CuS微晶进行了形貌的可控制备.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和紫外可见吸收光谱(UV-vis)分别对产物的物相,形貌和光学性能进行了表征.结果表明:微波水热条件下,反应温度为150℃时,反应时间仅为5 min即可得到CuS微晶,随着反应时间的延长,产物的结晶性逐渐提高,同时其形貌由纳米片形成的花球形逐渐转变为卷曲的棒状结构.所制备的CuS微晶具有较强的可见光吸收特性,同块体材料相比有明显的红移,其光学禁带宽度显著降低.此外,伴随产物形貌随时间的变化,其禁带宽度也发生相应改变,表明通过改变微波加热时间(10 ～40min),可对所得产物的光学性质进行控制.     

葡萄糖的加入量对C/Bi2WO6微晶的结构及可见光催化性能的影响

以葡萄糖(C6H12O6),分析纯硝酸铋(Bi(NO3)3·5H2O)和钨酸钠(Na2 WO4·2H2O)为原料,在简单的微波水热-煅烧条件下成功制备了形貌可控的交叉薄片状C/Bi2 WO6微晶.研究了反应体系中前驱物的不同摩尔比对产物的结构形貌以及光催化性能的影响.采用X-射线衍射仪(XRD)、EDS能谱分析、扫描电子显微镜(SEM),Perkin Elmer Larnbda 950型紫外可见漫反射光谱仪和康塔公司NOVA 2200e型表面空隙度分析仪分别对产物的结构、形貌,光学性能以及氮吸附-脱附等温线进行表征.结果表明:当前驱物葡萄糖,硝酸铋和钨酸钠的摩尔比为1∶10∶5时,合成了形貌可控且具有较好可见光催化性能的C/Bi2WO6微晶,其禁带宽度为3.055 eV,在可见光照射240 min后对罗丹明B的降解效率可达到94.8;.     

不同镉源制备铜锌锡硫电池缓冲层的研究

目前制备CZTS薄膜太阳电池的缓冲层绝大多数采用硫酸镉作为镉源.本文将主要介绍用醋酸镉((Ch3COO)2Cd)、氯化镉(CdCl2)和硝酸镉(Cd(NO3)2)和硫酸镉(CdSO4)四种不同的镉源制备硫化镉薄膜.通过X射线衍射仪(XRD)、扫描电子显微镜(SEM)和紫外可见分光光度计对硫化镉薄膜的结构、表面形貌和光学性能进行分析研究.分析结果表明以硝酸镉为镉源制备的硫化镉薄膜最适合作为缓冲层使用.将不同镉源制备的硫化镉薄膜作为CZTS薄膜电池的缓冲层,制备出的电池效率分别为:1.83;((Ch3COO)2Cd)、2.89;(CdCl2)、3.4;(Cd(NO3)2)、3.19;(CdSO4).     

水热法制备蝴蝶结形貌的CeO2粉体

以Ce(NO3)3·6H2O为铈源,L-半胱氨酸为表面活性剂,NaOH为碱源通过水热法制备了前驱体Ce2O(CO3)2·xH2O,经煅烧后得到了蝴蝶结形貌的CeO2粉体,采用X射线衍射仪(XRD)和扫描电子显微镜(SEM)对所制得产物的晶相和形貌进行了表征,并分析了不同反应条件对产物形貌的影响.结果表明:水热反应温度180℃反应24h制备出蝴蝶结形CeO2的前驱体,经400℃煅烧1h,获得长约14 μm,两端呈分叉多枝结构的CeO2粉体;随着反应时间的延长,产物经历了由椭球形向蝴蝶结形的转变.     

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...     

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.     

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.