添加稳定剂对反应烧结法合成铁铝尖晶石的影响

以工业氧化铝、氧化铁为原料,石墨为还原剂,高纯镁砂、电熔镁铝尖晶石为Fe2+的稳定剂;按照FeO: Al2O3:C =41.0:59.0:3.0的质量比设计基础配方,在合成体系中分别外加适量的高纯镁砂及镁铝尖晶石;各种原料经过共磨等工序加工后,压制成φ50 mm×50 mm试样,并在非控制气氛下于高温电炉1550℃,5h烧结合成.采用XRD、SEM及EDS等手段对试样进行表征,结果表明:非控制气氛下反应烧结法制备铁铝尖晶石时,引入高纯镁砂与镁铝尖晶石做为稳定剂均能促进Fe2+的稳定及铁铝尖晶石的合成.以高纯镁砂为稳定剂,制备的铁铝尖晶石晶体结构中镁含量相对较高,晶格参数与理论值相差较大,合成产物中还存有少量镁铝尖晶石相及单质铁;以电熔镁铝尖晶石为稳定剂,制备的铁铝尖晶石晶体结构中镁含量相对较低,晶体发育完善,晶格常数更接近理论值,合成产物中存在纯净铁铝尖晶石相.     

四种镁铁铝材料的物相组成与显微结构表征

分别以烧结铁铝尖晶石、电熔铁铝尖晶石、烧结镁铁砂及电熔镁铁砂为铁载体,在控制试样化学组成接近的前提下,按照镁铁铝尖晶石砖生产工艺制备镁铁铝尖晶石砖试样.采用XRD和SEM对试样的物相组成和显微组织结构进行分析表征.结果表明:铁铝尖晶石试样中,存在(Mg,Fe2+)Al2O4复合相,其中铁以Fe2+的形式存在,并产生少量镁铁尖晶石脱溶物;镁铁砂试样中,形成Mg(Fe3+,Al)2O4复合相,铁以Fe3+的形式存在,并产生了AlFe2O4连续固溶体相;烧结铁载体试样的显微结构中存在较多微气孔,电熔铁载体试样显微组织结构致密.     

电熔镁铝尖晶石和轻烧镁粉对合成镁铁铝系复合尖晶石的影响

本文研究电熔镁铝尖晶石和轻烧镁粉对合成镁铁铝复合尖晶石的影响.电熔镁铝尖晶石和轻烧镁粉分别与氢氧化铁、活性氧化铝混合均匀制得φ20 mm×10 mm的试样,在空气气氛烧结条件下,于1550℃×6 h高温烧成.采用XRD、SEM和EDS等手段对烧后试样的物相组成和显微结构进行表征.结果表明:加入电熔镁铝尖晶石的试样中存在刚玉相、赤铁矿、铁铝尖晶石相和镁铁铝复合尖晶石相四种矿物相,镁铁铝复合尖晶石的化学式为Mg796Al15.31Fe0.68O32;加入轻烧镁粉的试样中存在刚玉相、铁铝尖晶石相和镁铁铝复合尖晶石相三种矿物相,镁铁铝复合尖晶石的化学式为Al15.71Mg3.35Fe4.94O32;加入电熔镁铝尖晶石的试样中铁铝尖晶石的晶粒尺寸和镁铁铝复合尖晶石相差无几,加入轻烧镁粉的试样中铁铝尖晶石的晶粒尺寸明显大于镁铁铝复合尖晶石.     

TiO2含量对铁铝尖晶石晶体结构影响的研究

以分析纯氧化铁、氧化铝和二氧化钛为原料,按FeO∶Al2O3质量比为40.8∶59.2配料,并于合成体系中分别引入质量分数为0、1;、3;和5;的二氧化钛.在保护气氛(CO2/CO)下于1550℃煅烧4h合成铁铝尖晶石.用X射线衍射、扫描电子显微镜和能谱对烧后试样进行分析.结果表明:在铁铝尖晶石合成过程中,引入的TiO2参与了铁铝尖晶石的结晶、长大;添加TiO2的铁铝尖晶石衍射峰向小角度偏移,晶格常数增大.TiO2加入量小于1;时,各试样的微观结构都比较均匀,引入的TiO2进入了铁铝尖晶石的晶格,且以复合尖晶石的形式存在;TiO2添加量大于3;时,烧后试样的结晶形貌发生明显变化,铁铝尖晶石发生分解.     

烧结温度对煤系高岭土制备堇青石陶瓷的影响

我国的煤系高岭土具有明显的资源优势,应对其进行充分地研究和合理地应用,以缓和优质高岭土资源枯竭的燃眉之急.以鄂尔多斯煤系高岭土、鄂尔多斯滑石、工业氧化铝为原料,通过反应烧结一步合成堇青石,探讨了堇青石合成温度范围,以拓宽该煤系高岭土的应用范围.通过高温显微镜观察堇青石试样的合成温度范围为1400～1420℃.经1420℃合成的堇青石试样的吸水率为16.11;,显气孔率为28.44;,体积密度为1.77 g/cm3,径向烧成收缩为1.77;,厚度烧成收缩为4.80;,抗折强度为43.56 MPa.镁铝尖晶石是合成堇青石的重要中间产物,适当提高烧结温度可以促进镁铝尖晶石相向堇青石相转变,有利于堇青石晶粒的生长与发育.烧结温度的变化是堇青石晶粒发生变化的原因,同时导致液相量的变化,最终影响堇青石试样显微结构和烧结性能.     

添加剂促进锌铝尖晶石生成机理研究

以氧化铝和氧化锌为原料,采用固相反应法合成锌铝尖晶石,将试样在800～1500℃进行烧结,研究了添加剂对矿物组成和微观结构的影响,采用XRD、SEM和EDS等手段对烧后试样的物相组成和显微结构进行表征.结果表明:在800℃时,空白样的主晶相为氧化锌,次晶相为锌铝尖晶石,添加ZrO2的试样主晶相为锌铝尖晶石,次晶相为氧化锌和氧化锆,添加TiO2的试样,主晶相为锌铝尖晶石,次晶相为钛酸锌,两种添加剂均有促进锌铝尖晶石生成的作用,添加TiO2和ZrO2的试样晶粒尺寸均比空白样大;1500℃时,氧化钛与氧化铝反应生成钛酸铝,当TiO2含量在1;～5;之间时,随着TiO2含量增加,锌铝尖晶石晶粒尺寸增大.     

含Mg2+铁铝尖晶石晶体结构的研究

以分析纯氧化铁(Fe2O3)、分析纯氧化铝(Al2O3)和分析纯氧化镁(MgO)为原料,按照质量比MgO∶ Fe2O3∶Al2O3=0∶44∶56及1∶44∶56进行配料,压制成φ25 mm×30 mm试样.成型后的试样在CO2/CO混合气氛下加热至1600℃并保温6h.采用XRD、SEM、EDS、HRTEM及SAED等手段对烧后试样进行了表征.结果表明:经1600℃高温处理6h后,烧后试样的微观结构均匀,物相为含Mg2+的铁铝尖晶石IV(Mg0.035 Fe0.808Al0.157)∑1.000Ⅵ(Fe0.158Al1.772Mg0.070)∑2.000O∑4.002.引入的氧化镁参与了铁铝尖晶石的合成,并以Mg2的形式进入铁铝尖晶石晶格;Mg2+占据铁铝尖晶石中四面体和八面体的位置,造成铁铝尖晶石晶格常数的变大.     

原位反应烧结制备莫来石-锌铝尖晶石多孔陶瓷研究

以天然高岭土以及活性氧化铝、氧化锌为原料,通过添加天然长石,以石墨为造孔剂,原位反应烧结制备了莫来石-锌铝尖晶石多孔陶瓷.采用XRD、SEM、EDS能谱分析分别确定了试样的物相组成、显微结构与微区化学组成.采用阿基米德排水法与抗压强度测定法测定了试样的孔隙率与抗压强度.结果表明:当原位合成温度为1450～1500℃范围时,试样的物相组成为莫来石与锌铝尖晶石,莫来石呈针状晶须,锌铝尖晶石晶形发育良好,材料的抗压强度增加迅速,为最合适的原位合成温度.长石的加入促进了针状莫来石的形成,促进了材料的烧结,提高了多孔陶瓷的强度.     

添加剂对锌铝尖晶石晶粒尺寸的影响

本文以氧化铝和氧化锌为原料,B2O3、Y2O3、TiO2为添加剂,采用固相反应法合成锌铝尖晶石,将试样在1550℃进行烧结,研究了三种添加剂对矿物组成和微观结构的影响,采用XRD、SEM等手段对烧后试样的物相组成和显微结构进行表征.结果表明:三种添加剂均使显气孔率显著降低,当含量超过1.5;时,显气孔率下降不明显.B2O3进入锌铝尖晶石间隙内形成间隙固溶体;Y2O3与Al2O3发生化学反应生成钇酸铝;当TiO2含量小于1.5;时,TiO2进入锌铝尖晶石晶格内形成置换固溶体,超过1.5;以后,TiO2与Al2O3反应生成钛酸铝.添加Y2O3的试样,生成的钇酸铝在锌铝尖晶石晶间,与空白样相比,晶粒尺寸更均匀;添加B2O3的试样,晶粒尺寸最大;其次是添加TiO2的试样.添加TiO2的试样抗KCl侵蚀性最好.     

镁铝尖晶石-钇铝石榴石复相材料的制备研究

以富铝尖晶石为原料,分别加入Y2O3细粉、Y2O3和α-Al2O3混合粉、钇铝石榴石前驱体,制备尖晶石-钇铝石榴石复相材料.研究了氧化钇的不同引入方式和烧结温度对尖晶石-钇铝石榴石复相材料烧结性能的影响,并通过XRD、SEM等手段对其物相组成和显微结构进行表征.结果表明:向富铝尖晶石中分别加入Y2O3细粉、Y2O3和αt-Al2O3混合粉、钇铝石榴石前驱体,均能制备出尖晶石-钇铝石榴石复相材料;当Y2O3和α-Al2O3混合粉的加入量为6;,经1750℃烧结3h后,所制备的试样的致密化程度较高,体积密度达3.34 g/cm3,显气孔率为8.0;,制备的试样中镁铝尖晶石、钇铝石榴石晶粒发育较好.     

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.