二次加热法制备单分散性CoFe2O4纳米晶及其磁性研究

本文分别以CoCl2·6H2O,FeCl3·6H2O,NaOH为原料,利用N(CH3)4OH (四甲基氢氧化铵)作为改性剂,对CoFe2O4纳米颗粒进行原位表面改性,采用二次加热法,制备单分散性CoFe2O4纳米晶.利用透射电子显微镜(TEM)、X射线衍射仪(XRD)、能量散射分析仪(EDS)和振动样品磁强计等测试手段对样品的形貌,粒径,结构,以及磁学性能等进行了表征.结果表明,单分散性CoFe2O4纳米晶仍具有较大的饱和磁化强度和矫顽力.     

凝胶模板燃烧法制备铝酸镁纳米晶

以Al(NO3)3 · 9H2O、Mg(NO3)2 · 6H2O为原料,明胶为模板分散剂,采用凝胶模板燃烧法成功制备MgAl2O4纳米晶,利用TG-DTA、FT-IR、XRD、SEM、TEM和激光粒度分析仪对样品的结构和性能进行了表征.结果表明: 该方法能明显降低MgAl2O4的合成温度,最佳制备条件为硝酸盐与明胶质量比为6.29、650 ℃热处理2 h,所得产物粒子形状基本为球形,直径约为20 nm,颗粒分散较均匀,晶化良好,属单一尖晶石相.     

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。     

离子液体[Bmim]BF4辅助制备超顺磁性Fe3O4纳米粒子

以七水硫酸亚铁(FeSO4·7H2O)与六水三氯化铁(FeCl3·6H2O)为原料,离子液体1-丁基-3-甲基咪唑四氟硼酸盐([Bmim] BF4)为添加剂,70℃下反应2h制备了Fe3O4纳米粒子.通过X射线衍射仪(XRD)、傅里叶红外光谱(FT-IR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)以及热重分析(TG)等方法对样品的结构和形貌进行表征,并测试了所合成样品的磁性能.实验结果表明:离子液体辅助制备的Fe3O4纳米粒子形貌较为均一,呈近似球状,平均直径约为14 nm,产品在室温下表现出超顺磁性,饱和磁化强度为60.66 emu/g.利用密度泛函理论(DFT)计算模拟了Fe3O4分别与离子液体和水相互作用的电子结构,发现离子液体通过阴离子的桥联,更易吸附在Fe3O4晶粒表面.     

双金属NiCoP的制备、表征及其性能研究

采用溶剂热法成功地制备出特定组成和形貌的NiCoP微晶.产物的物相和纯度利用X射线粉末衍射仪进行表征,结果表明,所得到的产物为纯六方相的NiCoP结构,并且结晶度很高;产物的形貌和尺寸利用扫描电子显微镜进行表征,结果显示,该产物是由平均直径为1 ～2 μm的实心球组成.为了得到最佳的制备条件,我们还进行了一系列的溶剂、温度和时间条件实验.此外,我们对产物进行了吸附性能的研究.实验结果表明,所制备的产物NiCoP实心球对一些有机染料表现出了较好的吸附性能,如甲基橙,孔雀石绿.     

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.     

可见光响应型ZnO/Bi2O3复相光催化剂的制备及其性能研究

以Zn(Ac) 2·2H2O和Bi( NO3)3·5H2O为主要原料,采用溶胶-凝胶法成功制备了可见光响应型的高效复相ZnO/Bi2O3催化剂.利用X射线衍射(XRD)、扫描电镜(SEM)对样品进行了表征,并以甲基橙为目标污染物,测试样品的光催化性能,研究了初始合成条件、光源等对样品光催化性能的影响.实验结果表明:在nZn∶nBi为1∶1,浓度为0.05 mol/L条件下制得的凝胶,经600℃煅烧2h后,样品呈现六方纤锌矿结构的氧化锌晶相并伴有单斜α-Bi2O3、三斜ω-Bi2O3晶相.在16 W紫外灯、500W卤素灯照射下,2.5h后,甲基橙的脱色率为95.73;,68.36;,而经太阳光照射2.5h,甲基橙的脱色率分别为53.8;,但将其继续置于阳台上24h,脱色率可达97.6;.在16 W紫外灯的辐照下,样品重复使用6次,甲基橙的脱色率仍在90;以上,表明催化剂具有较高的重复使用率.     

水热法镧掺杂铁酸锌的制备及表征

以FeCl3·6H2O、La(NO3)3·6H2O和Zn(Ac)2为原料,通过水热法制备ZnLa0.2Fe1.8O4纳米颗粒.主要探讨水热反应时间和pH,并通过X射线仪(XRD)、扫描电子显微镜(SEM)和振动磁强计(VSM)等仪器对材料的结构及磁学性能进行了研究,结果表明:水热反应温度180℃,反应8 h,pH值为10时,制备出ZnLa0.2 Fe1.8 O4样品具有完整尖晶石结构且无中间产物产生,水热保温时间的延长对ZnLa0.2Fe1.8O4饱和磁强度(Ms)影响不大.     

不同钙源种类对CaTi2O5粒子的光催化性能影响

采用溶剂热法制备了CaTi2O5微纳结构.用X射线衍射(XRD)、扫描电子显微镜(SEM)和比表面积分析仪(BET)对样品进行了表征,并用紫外-可见吸收光度计分析样品对光的吸收特性,研究不同钙源种类对CaTi2O5样品的物相、微观形貌及光催化性能的影响.结果表明:CaTi2O5样品更有利于降解甲基橙溶液.钙源为CaCl2所制备的CaTi2O5样品的结晶度高、颗粒大小均匀,具有低的反射率和高的吸收率,高的比表面积(112.34 m2·g-1),因此样品呈现出较高的光催化性能.     

高分散镁铝层状双氢氧化物的煅烧改性及其对甲基橙的吸附性能研究

以Mg(NO3)2·6H2O为镁源,Al(NO3)3·9H2O为铝源,采用水热法制备了高分散的镁铝层状双氢氧化物MgAl-LDH,并高温煅烧生成MgAl-LDO.利用场发射扫描电子显微镜(FE-SEM)、X射线衍射(XRD)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FTIR)、X射线光电子分析(XPS)、氮气吸附-脱附法对产物进行表征分析,并且探讨了其吸附机理.结果 表明,2种产物的吸附过程对比于Langmuir吸附模型基本一致,其中MgAl-LDO的比表面积更大,吸附性能更好,对甲基橙的最大吸附量可达925.9 mg·g-1.吸附机制包括化学作用、氢键、静电作用和表面络合作用.     

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.