Structural properties of (Mn1-x Fe x )Nb2O6 columbites from X-ray diffraction and IR spectroscopy

A suite of (Mn_1-x Fe _x )Nb₂O₆ (x=0, 0.05, 0.25, 0.50, 0.75, 1) columbite samples has been prepared by solid-state reaction from oxides. X-ray diffraction and spectroscopic investigations have been carried out in order to gain different perspectives on how the solid solution adapts at different length scales to cation mixing. X-ray powder diffraction and powder absorption IR spectroscopy data are presented. The powder diffraction data show that there is no significant excess volume of mixing on the Fe–Mn columbite join. All the unit-cell parameters decrease linearly as a function of increasing Fe content. Substitution of Fe²⁺ for the larger Mn²⁺ cation causes a decrease in the volume of the A polyhedron, which also becomes more regular with respect to both bond-length and edge-length distortion parameters. No significant variation of the B site has been observed. Wavenumber shifts of the IR peaks nearly all vary linearly with composition, consistent with linear variations of the lattice parameters. Line broadening has been quantified by autocorrelation analysis of the IR spectra. This is interpreted as suggesting that there is some element of local strain or positional disorder at the length scale of second or third nearest neighbours around sites occupied by Fe.     

Kinetic study of the dehydroxylation of chrysotile asbestos with temperature by in situ XRPD

 The kinetics of the dehydroxylation of chrysotile was followed in situ at high temperature using real-time conventional and synchrotron powder diffraction (XRPD). This is the first time kinetics parameters have been calculated for the dehydroxylation of chrysotile. The value of the order of the reaction mechanism calculated using the Avrami model indicates that the rate-limiting step of the reaction is a one-dimensional diffusion with an instantaneous nucleation or a deceleratory rate of nucleation of the reaction product. Hence, the rate-limiting step is the one-dimensional diffusion of the water molecules formed in the interlayer region by direct condensation of two hydrogen atoms and an oxygen atom. The calculated apparent activation energy of the reaction in the temperature range 620–750 °C is 184 kJ mol⁻¹. The diffusion path is along the axis of the fibrils forming the fibers. The amorphous or short-range ordered dehydroxylate of chrysotile is extremely unstable because forsterite readily nucleates in the Mg-rich regions. Moreover, it is less stable than the dehydroxylate of kaolinite, the so-called metakaolinite, which forms mullite at about 950 °C. This difference is interpreted in terms of the different nature of the two ions Mg²⁺ and Al³⁺ and their function as glass modifier and glass-forming ion, respectively. Received: 10 April 2002 / Accepted: 7 January 2003 Acknowledgements This work is part of a COFIN project (04 Scienze della Terra, NR 17, 2000) supported by MURST. Dr Dapiaggi is kindly acknowledged for help during the data collection at the Dipartimento di Scienze della Terra, University of Milan.     

斜方辉石的反演畴结构对其衍射效应的影响

斜方辉石内部存在着众多的相邻间呈反演关系的(100)晶畴。这些晶畴的存在使斜方辉石的K为奇数的okl衍射之强度明显减弱,且参与衍射的晶畴的数目越多,其减弱的程度也就越大。这一现象在一定程度上掩盖了斜方辉石P2_(1ca)的真实对称性。与X射线衍射相比,利用电子衍射来研究斜方辉石的空间群类型具有明显的优越性。     

白钨矿的原位高压X射线衍射研究

使用金刚石对顶砧高压装置(DAC)和同步辐射光源,对天然白钨矿进行了原位高压能量色散X射线衍射(EDXD)研究,实验最高压力为16.0 GPa.在实验压力范围内观察到了一次白钨矿结构→钨锰铁矿结构的可逆相变:压力小于5.3 GPa时为白钨矿结构(I4_1/a),在5.3～12.3 GPa压力区间内为白钨矿结构与钨锰铁矿结构(P2/c)并存,大于12.3 GPa时完全相变为钨锰铁矿结构.从键长、配位数和配位多面体角度对白钨矿→钨锰铁矿结构的相变机制进行了解释.     

铝硅酸盐矿物和玻璃中Al的配位与局部结构

利用同步辐射的AlK边X射线吸收近进结构（XANES）谱研究了刚玉和铝硅酸盐矿物（蓝晶石,红柱石,夕线石和钠长石）中Al的配位与局部结构,证明该方法可以作为新的结构探针研究结构未知体系中Al的配位与局部结构。例如,Al的K边XANES谱证明在室温压条件,钠长石玻璃中的Al保持为四面体配位（AlIV）,局部结构与钠长石晶体中的Al相似;尽管硬玉晶体中的Al为八面体配位,但硬玉玻璃中的Al变为四面体配位（AlIV）。而在相同的高温压条件（4．4GPa,1575C）下制备的硬玉-钠长石玻璃系列中,压力引起四面体配位的Al变成五次（Alv）和六次配位（AlVl）,且五次和六次配位Al的比例随玻璃中硬玉含量的增加而增大。     

Geology and geochemistry of Iberian roofing slates

This article analyzes the geochemical and mineralogical composition of the roofing slate deposits of the Iberian Peninsula. Most roofing slate deposits are found on Middle and Upper Ordovician terrains, although there are also deposits in the Ediacaran, Cambrian and Devonian terrains. Samples of slate were taken in most of the active quarries of the Iberian Peninsula, and being analyzed by X-ray Diffraction and Fluorescence. Each lithotect or slate productive formation has its own specific proportions of major and trace elements, being able to differentiate between them by using these relationships. This fact is particularly interesting in geological exploration and prospecting, as it allows knowing exactly the slate lithotect, and also for restoration work in the architectural heritage, due to the ability of identifying the source of the original slate tiles.     

黑海西北部冷泉碳酸盐岩的沉积岩石学特征及氧化还原条件的稀土元素地球化学示踪

黑海西北部罗马尼亚大陆架(水深120m)和乌克兰陆坡(水深190m)发育冷泉碳酸盐岩结壳。XRD测试表明此结壳主要由高镁方解石和文石组成。结壳中与渗漏系统微生物活动有关的凝块和葡萄状文石等特殊的沉积组构非常发育。冷泉碳酸盐岩酸可溶部分(碳酸盐岩相矿物)的稀土元素含量很低(0.068×10-6~2.817×10-6),稀土元素页岩标准化配分模式显示罗马尼亚大陆架冷泉碳酸盐岩具有明显的Ce负异常,乌克兰陆坡冷泉碳酸盐岩具Ce的正异常,表明它们是分别在氧化和还原环境中沉积的。稀土元素和V、Cd和U等微量元素的含量在泥晶中最高,亮晶中最低,可能反映成岩过程对元素含量有控制作用。     

微X射线束荧光扫描成份分析研究：元素二维分布图

经过改进的微X射线扫描分析装置,扩大了测量范围;提高了位移精度;处理数据及绘制二维(平面)元素分布图实现计算机化。测量并绘制出大洋锰结核中多元素平面分布图。     

基于傅里叶变换的频谱分析法在X射线轮胎检测中的应用

子午线轮胎的缺陷检测方法比较多,频谱分析法是基于频域的图像分析方法,其主要功能是获取图像在频域中的纹理特征。傅里叶变换能够将时域的信号分解为频域各频率分量下之和,即分解为各个频率下的谱。然后通过对得到的频谱进行图像处理,判断轮胎有无缺陷。实验证明使用基于傅里叶变换的频谱分析法进行子午线轮胎缺陷检测可以大幅降低工作量,提高轮胎检测效率。     

缺血性脑血管病病变血管的CTA检查价值

目的:探讨缺血性脑血管病病变血管的CTA检查价值。方法:使用Philips Brilliance 16层螺旋CT机,Philips Extended Brilliance TM Workspace或GE AW4.4图像后处理工作站,以MIP、CPR为主,VR为辅,对头颈部动脉进行分析,观察缺血性脑血管病病变血管的形态学改变。结果:102例缺血性脑血管病中有90例发现病变血管(占88.24%),90例中,单纯脑动脉病变57例(占63.33%),单纯颈动脉狭窄、斑块12例(占13.33%),脑动脉及颈动脉联合病变21例(占23.33%)。病变血管的CTA表现:检出的78例脑动脉病变中,24例显示为动脉粥样硬化性改变,38例显示为较明确的局限性血管狭窄,其中6例可见斑块,16例显示为血管闭塞,均在大脑中动脉。检出的33例颈动脉病变中,显示为血管狭窄、斑块形成以及血管壁钙化,均位于颈动脉分叉处及颈内动脉起始部。各种缺血性脑血管病与病变血管的对应关系:48例脑梗死,29例找到责任血管;26例TIA,22例找到病变血管;19例腔隙性脑梗死,16例可见不同程度的颈、脑动脉病变;9例有临床表现而CT和(或)MRI显示正常者,显示脑、颈动脉病变6例。结论:CTA可作为缺血性脑血管病的常规检查方法,用来评价缺血性脑血管病病变血管的形态学改变。