化学液相沉淀法制备过氧化银及其表征

采用化学液相沉淀工艺制备了过氧化银(AgO)粉体,研究了Na2S2O8用量、反应体系的pH值、反应时间等制备工艺参数对AgO产率的影响,并采用X射线衍射仪(XRD)及扫描电子显微镜(SEM)对制备的AgO粉体进行了表征.结果表明,优选的制备工艺是将AgNO3、Na2S2O8和SDBS的质量比定为1∶4.4∶1,然后在反应体系的温度达到60℃后通过滴加NaOH溶液调整反应体系的pH值为13.00,并维持反应时间30 min.随着AgNO3与SDBS的质量比从2.5升高到20.0,AgO粉末颗粒的形貌从近似的球形转变为球状和片状结构的混合物.     

微波水热条件对氧化锌晶体的形态和粒度的影响

利用微波水热法，以氢氧化锌为前驱物，在反应温度不小于100℃的情况下，成功地制备出氧化锌微晶。研究了水热条件对氧化锌微晶的晶粒大小和形貌的影响。在水热环境下，当反应温度一达到100℃，氧化锌微粒就能快速形成和生长。反应温度在100℃时，延长反应时间(～4h)氧化锌微晶的形貌和晶粒大小均没有受到大的影响；然而，升高反应温度氧化锌微晶的晶粒大小会略微地减小。另一方面，当反应前溶液中的pH值从9增大到12时，氧化锌微晶的形态从不规则的片状颗粒改变到长柱状晶粒。另外，随着溶液中pH值的增加，氧化锌微晶的结晶性变好、粒度变大。合理地解释了反应温度、溶液中的pH值对制得的氧化锌微晶的形态、晶粒粒度的影响。     

制备工艺参数对氟离子和碳酸根复合掺杂纳米羟基磷灰石的影响

通过共沉淀法制备了氟和碳酸根复合掺杂纳米羟基磷灰石(CFHA)。研究了合成温度、掺杂离子浓度和pH值对CFHA形貌、替代类型和替代量的影响。用透射电镜观察合成粉体的形貌,用红外光谱和碳硫仪表征了碳酸根替代的类型和含量,用氟选择电极法测定了样品中的氟含量。结果表明:合成温度、碳酸根掺杂浓度和pH值对CFHA形貌有明显影响。随着合成温度的升高、碳酸根掺杂浓度和pH值的减小,晶粒尺寸和长径比增加;合成粉体中氟和碳酸根含量随掺杂离子浓度的增加而非线性增加,但实际替代量与理论计算值有较大偏差;高pH值有利于碳酸根和氟的替代。     

共沉淀法制备Al2O3-ZrO2复合纳米粉体

以ZrOCl2·8H2O、Al(NO3)3·9H2O、Y(NO3)3为原料,NH4HCO3 (AHC)为络合剂,采用共沉淀法制备Al2 O3-ZrO2复合纳米粉体.利用X射线衍射分析(XRD)、扫描电镜(SEM)、透射电子显微镜(TEM)、激光粒度分析仪等对Al2 O3-ZrO2复合粉体进行测试表征,详细研究了pH和AHC/Zr摩尔比对复合粉体的影响.结果表明,当前驱体的煅烧温度低于1200℃时,只形成t-ZrO2相,当煅烧温度达到1300℃时,α-Al2O3相开始形成;沉淀反应的pH和AHC/Zr摩尔比对Al2O3-ZrO2复合粉体的产率有很大的影响.在pH7、AHC/Zr =4.5:1的条件下制备前驱体,经过1300℃煅烧2h得到两相纯度高,分散性能好,粒度分布窄,平均粒径为0.75 μm的Al2O3-ZrO2复合粉体.     

pH值和烧结温度对溶胶-凝胶方法制备堇青石粉体性能的影响

以正硅酸乙酯、镁盐和铝盐为原料,通过溶胶-凝胶法合成堇青石粉体,通过TGA-DSC、XRD等测试手段,讨论了反应体系pH值和烧结温度对产物晶相和性能的影响.结果表明:体系pH值为2的试样,在900℃时,出现尖晶石相和假蓝宝石相,升温到1000℃的时候,开始有μ-堇青石出现,在1250℃煅烧2h几乎全部转化为α-堇青石,体系pH为7的试样,在900℃时,有μ-堇青石形成,经1250℃煅烧后,β-堇青石相增多,μ-堇青石相和镁铝尖晶石相消失,合成粉体的平均晶粒尺寸随pH值增加呈先减小后增加的趋势,在不同温度煅烧下的压片试样,体系pH值为7的试样收缩最大.     

8-羟基喹啉金属配合物的制备与提纯

对以8-羟基喹啉为配位体的金属配合物合成过程中几个重要的影响因素进行研究,发现反应溶液的浓度、合成反应的时间、反应体系的pH值、反应温度等因素对8-羟基喹啉金属配合物的产率以及发光性能有很大的影响.结果表明:当8-羟基喹啉乙醇溶液浓度为80 g/L,反应体系pH值为7.14,温度为70 ℃,反应时间为3 h时,Alq3的产率最高;反应体系pH值为10,温度为50 ℃,反应时间为1 h,Liq的产率最高;pH值为8,温度为70 ℃,反应时间为1 h,Znq2的产率最高.     

纳米级锆酸钐的合成工艺研究

采用L9(33)正交试验方案研究了溶液浓度、反应温度和pH值等三因素对共沉淀法制备锆酸钐粉体的影响.采用XRF、SEM等测试手段对纳米级锆酸钐粉的组分和形貌等进行表征,结果发现三因素对纳米级锆酸钐的组分有不同程度的影响:在共沉淀反应中,三因素相互作用,其中溶液浓度是影响其组分的主要因素;随着溶液浓度的升高,其组分差距增大,随着反应温度和pH值的升高,其组分差距表现出先增大后减小的趋势.当溶液浓度为0.6 mol/L、反应温度为50℃、pH值为10时为最佳制粉工艺,并在最佳工艺条件下制得了组分、形貌优良的纳米级锆酸钐粉.     

基于正交实验优化沉淀法制备针状羟基磷灰石

羟基磷灰石(HAP)已在临床得到运用,但其强度低、韧性差、不易成型等缺点依旧制约着其的广泛应用.为制备出理想且能满足临床应用的纳米针状羟基磷灰石,本文在不添加任何分散剂和表面活性剂的条件下以磷酸钠与硝酸钙为原料,氢氧化钠调节pH,使用正交实验设计对沉淀法中针状HAP的制备工艺进行优化.结果表明,反应条件对HAP晶体形貌的影响程度为:温度>滴加速度>pH;当反应pH=9、反应温度为90 ℃和滴加速度为2 mL/min时为其优方案,可制备出性状规则、粒度均匀、结晶度高、趋向于针状的纳米羟基磷灰石粉体.反应温度升高可提高HAP的结晶速度,可增大HAP晶体的大小,使晶形更趋于针状,但温度过高时对长轴的促进作用开始逐渐降低,长径比的增加趋势有所减缓;降低滴加速度,可提高产物结晶程度,有利于针状羟基磷灰石的形成;此外,反应pH值升高虽可加速晶核形成,提高产物的结晶率和产物纯度,但是不利于晶粒长大,且pH过高会减缓形成针状的趋势.     

反应条件对水热合成铁酸钇(YFeO3)微晶的物相、粒径和磁性能的影响

以氧化钇、硝酸和硝酸铁为原料,氢氧化钾为矿化剂,采用水热合成法制备了钙钛矿结构铁酸钇正铁氧体(YFeO3)微晶.研究了水热反应时间、温度和溶液pH值对产物的物相组成、粒径大小和磁性能的影响,研究结果表明,在实验条件所在区间内,随着反应时间的增加和反应温度的升高,产物纯度逐渐变高.合成纯相YFeO3需要在一定的溶液pH值范围内.随溶液pH值的降低,产物颗粒的粒径变小,粒径分布变窄,并且晶粒的磁化强度增大.最佳的合成条件是pH值为9.5,温度为260℃,反应时间为60h.     

pH值及烧结温度对制备β-TCP粉体的影响

为了研究反应体系的pH值、烧结温度对磷酸钙粉体物相和形貌的影响,采用氢氧化钙和磷酸为原料,氨水为pH调节剂,通过化学共沉淀法制备磷酸钙前驱体.并通过在不同温度下进行烧结,制得β-TCP粉体.用X射线衍射(XRD)、红外光谱(FT-IR)、扫描电镜(SEM),对制备的磷酸钙进行表征和分析.结果表明:pH值为7、烧结温度1100 ℃情况下可得到较纯的β-TCP粉体.     

On the inhomogeneity of the transition surface layer of the solid core of the earth

Different geophysical data and conclusions of theoretical models, which can give information about the behavior of the solid and liquid cores of the Earth as well as about the existence of a transition layer as a temperature-hysteresis region at a relatively weak first-order phase transition, are compared. It is concluded that liquid inclusions inevitably exist in this region; these inclusions are involved (due to the complex convective processes occurring in the liquid core) in the transport of light materials from some areas of the solid-core surface. The porosity and permeability of the transition layer determine the seismic acoustic inhomogeneities in these areas, which contact the convective flows in the liquid core. In particular, this explains the well-known ??east-west?? effect. Obviously, the model of the crystalline core is not the only possible alternative for a model of a core with a metallic glasslike structure.     

On the role of the porous shell of the solid core of the earth in the anomalous heat and mass flow to the mantle

The model of the pressure-induced first-order phase transition of a metal melt to the metallicglass state considers a thermodynamically nonequilibrium porous near-surface shell of the solid core of the Earth, which contacts cyclonic vortices in the liquid core. Anomalous flows of heat and light-material mass to the mantle from the solid core at these contact points are calculated. These anomalous flows are shown to be comparable with the observed ones under the assumption of a rapid increase in the melt viscosity at pressures of 1–10 Mbar, which is characteristic of a solid core. In this case, the porous layer permeability may be very low.     

Features of the magnetic state of the layered Fe-V nanostructure of the superconductor-ferromagnet type

The magnetic state of the V(39 nm)/20 [V(3 nm)/Fe(3 nm)] nanostructure has been investigated by polarized neutron reflectometry in the temperature range from 1.6 to 30 K in magnetic fields from 0.2 to 15 kOe. The data obtained indicate that the superconductivity of vanadium layers may affect magnetic ordering both over the depth of the structure and in its plane.     

Study of the influence of the rare-earth elements on the properties of lead iodide

Lead iodide (PbI₂) shows excellent electronic properties for detection of ionizing radiation. We report the introduction of rare-earth elements and other elements as admixtures during synthesis to study their influence on the quality of single crystals. Synthesized material as well as single crystals have been characterized by measurements of electrical resistivity and low-temperature photo luminescence and index of refraction. The structural quality with respect to polytypes was analysed by electron back scatter diffraction. Makyoh topography was applied for surface studies.     

Influence of the Crystal Structure of the Nucleus on the Morphology of t-ZnO Tetrapods

Crystallography Reports - A new approach to simulating the morphology of hierarchical nanocrystals has been proposed on the example of ZnO nanotetrapods. Within this approach, twinning is...     

Effect of the temperature on the TMOS sono-hydrolysis and a study of the structure of the resulting aged sonogels

The effect of temperature on the oxalic acid catalyzed sono-hydrolysis of tetramethoxysilane (TMOS) was studied by means of a heat flux calorimetric method. The activation energy of the process was measured as (24.5 ± 0.8) kJ/mol in the temperature range between 10 and 50 °C. The structural characteristics of the resulting sonogels, after long period of aging in saturated conditions, were studied by means of small angle X-ray scattering. The structure can be described as formed by ∼2.7 nm mean size mass fractal-like aggregates (clusters) of primary silica particles of ∼0.3 nm mean size, all imbibed in a liquid phase. The average mass fractal dimension of the clusters was found to be 2.58. The primary particle density was estimated as 2.23 g/cm³, in good agreement with the value frequently quoted for fused silica. The volume fraction of the clusters in the saturated sonogels was estimated as about 28%. The moment in which the meniscus of the liquid phase penetrates into the clusters under rapid evaporation process has been detected by an inflection in the first derivative of the curve of weight loss in a simple thermogravimetric test.     

Ordering of cations in the voids of the anionic framework of the crystal structure of catapleiite

The pseudohexagonal crystal structure of the mineral catapleiite Na_1.5Ca_0.2[ZrSi₃(O,OH)₉] · 2(H₂O,F) from the Zhil’naya Valley in the central part of the Khibiny alkaline massif (Kola Peninsula, Russia) is studied by X-ray diffraction (XCalibur-S diffractometer, R = 0.0346): a = 20.100(4), b = 25.673(5), and c = 14.822(3) Å; space group Fdd2, Z = 32, and ρ_calcd = 2.76 g/cm³. Fluorine atoms substituting part of H₂O molecules in open channels of the crystal structure have been found for the first time in the catapleiite composition by microprobe analysis. The pattern of distribution of Na and Ca atoms over the voids of the mixed anionic framework consisting of Zr-octahedra and three-membered rings of Si-tetrahedra accounts for the pronounced pseudoperiodicity along the a and c axes of the pseudohexagonal unit cell and for the lowering of crystal symmetry to the orthorhombic one. It is shown that part of the hydrogen atoms of water molecules is statistically disordered; their distribution correlates with the pattern of the population of large eight-vertex polyhedra by Na and Ca atoms.     

Investigations of the Chemical Composition of the Metal Finds from the Levadki Necropolis

Crystallography Reports - Copper-based alloy items of the III century A.D., found in Burial no. 182 of the Late-Scythian Levadki necropolis in the submountain Crimea, have been investigated. The...     

Computer Modelling of the Light Propagation through the Complex Anisotropy Systems - the way of a Determination of the Optical Parameters of the Liquid Crystal Displays

A mathematical and numerical method for an analysis of a liquid crystal displays (LCD) has been presented. The assumptions of the calculations of a light propagation through the display are shown. The real conditions of a work of these displays have been taken into account. Basing of this mathematical model a computer program for a numerical modelling of the optical parameters of LC displays working in real conditions has been worked out. This program makes possible to obtain the most important parameters of a display such as: contrast ratio, luminance in on- and off-state, spectral characteristics of light and its colour coordinates in these both states. The results obtained from this program have been verified experimentally. Very high conformity of these results has been obtained.