X-射线粉晶衍射谱图的计算机模拟

编写了一个FORTRAN程序 ,用于从单晶结构计算粉晶X射线衍射数据 ,并进一步用ORIGIN软件绘制出粉晶衍射图谱。选择了 13个代表性经典化合物进行计算 ,结果与粉晶卡片上的实验数据相当一致。本文模拟方法 ,既可弥补粉晶标准图谱缺乏的不足 。

生、煅石膏的粉晶X-射线衍射分析

目的:建立生、煅石膏粉晶XRD鉴定分析方法。方法:应用粉晶XRD分析方法,对石膏、煅石膏等进行粉晶XRD指纹图谱分析及特征标记峰鉴别。结果:对16种生石膏样品、5种煅石膏样品含石膏制剂清咽六味散进行粉晶XRD分析鉴定,获得了石膏、煅石膏粉晶XRD指纹图谱及特征标记峰值。结论:生、煅石膏具有完全不同粉晶XRD指纹图谱,粉晶XRD法可用于石膏、煅石膏以及含石膏的中药成方散剂的鉴定。

岩矿在火驱条件下的物理化学变化

利用一维火烧油层驱油物理模拟试验装置,研究火驱温度与时间对岩矿物理化学的影响。研究表明:火驱之后,薄片中岩石颜色变浅,矿物出现裂缝,泥质有机质有烧失现象,加大了孔隙度;通过X-射线粉晶衍射试验可知岩石组分基本不变,但随着火驱温度与时间的增加,高岭石会向蒙脱石及伊利石转变。

滑石中石棉的鉴定方法研究

如何鉴定出滑石中含有的微量石棉,多年来一直困扰着分析界的人士。笔者经过多年的实践和大量资料的积累,以透射偏光显微镜观察和X-射线粉晶衍射为主要方法,以油浸法为辅助方法,对滑石中含有的各种微量石棉,进行快速准确的鉴定。本文列出了各种石棉的X-射线粉晶衍射特征数据。并以滑石中含有的透闪石石棉为例,详细论述了这一鉴定方法的科学性及合理性。若样品为块状岩石,则需要先在偏光显微镜下观察,再进行X射线粉晶衍射进一步验证。若样品为粉末状,则需要先进行X射线粉晶衍射分析,再进行油浸薄片观察。

合成碲金矿及其热液蚀变实验研究初探

通过实验合成出了碲金矿 ,并对其进行了 2 0 0℃、80℃温度下不同 p H溶液中的蚀变实验。对碲金矿及蚀变产物分别进行了 X-射线粉晶衍射、矿相显微镜鉴定及电子探针和光电子能谱分析。实验结果表明 ,在中性、偏酸性和碱性溶液的实验条件下碲金矿基本保持稳定 ,而在碱性稀溶液实验条件下可观测到少量含 Fe、 Te、 Au新相的生成及碲金矿表面氧化态碲的明显增加。

新疆萨尔托海铬铁矿中“绿泥石壳”的研究

萨尔托海铬铁矿的成因一直存在争议,通过研究其特有的"绿泥石壳"可知其矿床成因。采用光、薄片的镜下鉴定、X-射线粉晶衍射和电子探针分析,可知矿区围岩主要为蛇纹石,而"绿泥石壳"和矿石中的脉石矿物空间上互相过渡,二者矿物成分完全相同,为淡斜绿泥石。围岩蛇纹石中未见淡斜绿泥石,"绿泥石壳"中也未见蛇纹石残留,说明"绿泥石壳"与矿石中的脉石矿物成因相同,为成矿晚期残余矿浆直接沉淀结晶生成,非蛇纹石经绿泥石化蚀变生成。证明矿床为晚期岩浆熔离式矿床。

利用SEM图和XRD指纹图谱鉴别矿物类中药生石膏与玄精石

目的:采用性状鉴别、理化鉴别等传统方法结合扫描电子显微镜(SEM)及粉晶X-射线衍射(XRD)等现代分析技术,对矿物类中药生石膏和玄精石进行系统鉴别。方法:采集生石膏和玄精石样品,记录原药材及其粉末性状特点,进行理化鉴别,确定样品真伪及品种。在上述基础上,采集各药材样品SEM显微图,对比生石膏与玄精石各显微图之间的差异,总结两者SEM鉴别特征;同时采集各样品粉末的XRD图谱,分别计算并绘制生石膏与玄精石的XRD平均图谱,确定共有指纹峰,并对共有指纹峰相对强度数据分别进行相似度评价、聚类分析和主成分分析(PCA),验证生石膏与玄精石的XRD共有指纹峰用于两者鉴别的可行性。结果:生石膏和玄精石碎屑的SEM特征具有差异,玄精石均呈疏松层片状堆叠,细小碎屑均成沙粒状;而生石膏呈紧密聚合的长纤维状,且细小碎屑或粉末具碎裂状纤维特征。生石膏和玄精石粉末的XRD图谱峰位相似,但玄精石各峰相对生石膏各峰略左移,相同峰位衍射峰的相对强度存在差异。相似度评价显示生石膏与玄精石明显分离,聚类分析及主成分分析均可将两者准确区分。结论:SEM和XRD技术均可准确鉴别生石膏和玄精石及其粉末,传统鉴别方法结合SEM和XRD分析技术能够为生石膏和玄精石及其粉末的快速鉴别和质量控制提供快速准确的新方法。

XRD法定量分析蒙脱石含量及影响因素研究

本文以大量试验数据为基础,总结了生产实践中用XRD法精确定量蒙脱石含量的方法及影响因素。试验证明:人工处理、结晶程度会导致蒙脱石第一主峰发生变形,不能作为定量的依据,而0.448nm处的特征峰可以作为定量的重要依据;样品加工时,温湿度可以使蒙脱石第一主峰d值发生变化,但d_((001))值可以恢复。

Effect of ZrO_2 Crystalline Phase on the Performance of Ni-B/ZrO_2 Catalyst for the CO Selective Methanation

Amorphous Ni-B/ZrO2 catalysts were prepared by coprecipitation-chemical reduction with KBH4 aqueous solution,and various crystalline phase ZrO2(amorphous-ZrO2,tetragonal-ZrO2 and monoclinic-ZrO2) supported Ni-B catalysts were obtained by thermal treatment in 5%H2-N2 stream at different temperature.The effect of ZrO2 polymorphs and the treatment temperature on the catalytic performance for the CO selective methanation were investigated,and the catalysts were characterized by N2 physisorption,Powder X-ray diffraction(XRD), Temperature-Programmed Desorption(CO-TPD and H2-TPD),and Differential Scanning Calorimeter(DSC).The treatment temperature affected strongly the crystalline structure of ZrO2,and the CO methanation activity and selectivity of the Ni-B/ZrO2 catalysts were significantly influenced by the crystalline phase of ZrO2.Of the three forms of ZrO2 polymorphs(amorphou-ZrO2,tetragonal-ZrO2 and monoclinic-ZrO2),the amorphous-ZrO2 supported nickle catalyst showed highest CO methanation activity,attributing in large part to the largest specific surface area and the optimum CO/H2 absorption intensity of the Ni-B/amorphous-ZrO2 catalyst.

Preparation of Luminescent Tb^3＋ Doped CaO Green Phosphor

CaCO3 was chosen as main raw material and Solid State method was used to prepare the sample. The precursor was directly sintered at 1100 ℃ with reducing atmosphere for 3 h to obtain new green CaO：Tb^3＋, Li^＋ Phosphors. The effects of the content of the doping ions Tb^3＋ on the luminescent properties have been studied. The structure, morphology and luminescent properties of the phosphors were characterized by XRD, SEM, UV and PL-PLE spectra respectively. The results showed that the CaO：Tb^3＋, Li^＋ was a single face-centered cubic crystals, the phosphor particle distributed uniformly. The phosphor has a strong absorptive capacity excited by 282 nm ultraviolet ray, and could emit the strong green light with the wavelength of 543 nm （^5D4→^7F5）. The CaO：Tb^3＋, Li^＋ is a new type of green fluorescent material.

Preparation of microsized single-crystalline Co_3O_4 by high-temperature hydrolysis

Microsized single-crystalline Co3O4 has been synthesized by high-temperature hydrolysis of CoCD2H20 at 600℃. The samples were characterized by powder X-ray diffraction （XRD）, scanning electron microscopy （SEM） and transmission electron microscopy （TEM）. The results reveal that the as-prepared powders are microsized single-crystalline CO3O4 with cubic spinel structure. An increase in the high-temperature hydrolysis time results in the evolution of particle shapes from cube to quasi-sphere, and then to octahedron. The effect of NaCl additive on the surface morphologies of Co3O4 particles was experimentally investigated. The results indicate that the NaCl additive acts as an inert disperse phase in the high-temperature hydrolysis, and prevents the aggregation of Co3O4 particles effectively.

Synthesis of polycrystalline γ-AlON powders by novel wet chemical processing

The synthesis of polycrystalline aluminum oxynitride （AlON） powders was investigated by the carbothermal reduction and ni- tridation （CRN） of amorphous precursor obtained by wet chemical processing. Co-precipitation processing was employed to achieve amorphous precursor from AI（NO3）3 solution dispersed by nanosized carbon particles, which was composed of AI（OH）3 and C particles homogeneously. The effects of the content of carbon black, pH value, and calcination temperature on formation of A1ON phase were investigated by means of XRD, SEM and TEM, respectively. It was found that single phase AION powder could be synthesized when the resultant precursors were calcined at 1750℃ for 2 hours under flowing N2. Un- der optimal additional content of C （5.6wt%）, the resultant A1ON powders exhibited the primary particle size of about 1-3 μm with a specific surface area of 3.2 m2/g, which were superior to that of carbothermal reduction of immediate mixture of γ-A1203/C powders.

Syntheses, structures and magnetic properties of three Co(Ⅱ)coordination architectures based on a flexible multidentate carboxylate ligand and different N-donor ligands

Three new cobalt complexes, {[Co5（tci）2（bimb）3（μ3-O）2（H2O）2]·3DMF·4H2O}n（1）, {[Co3（tci）2（bib）]·2DMF·2H2O}n （2） and {[Co（Htci）（bpea）0.5]-H2O}n （3） （H3tci = tris（2-carboxyethyl）isocyanurate, bimb = 4,4＇-bis（imidazol-l-yl）biphenyl, bib = 1,4-bis（imidazol-l-yl）benzene, bpea = 1,2-bis（4-pyridyl）ethane, DMF = N,N＇-dimethylformamide）, have been successfully synthesized through the assembly of Co（If） ions, H3tci and different N-donor ligands, respectively. All complexes were structurally characterized by single crystal X-ray diffraction, elemental analyses, IR spectra, thermogravimetric （TG） analyses and X-ray powder diffraction （XRPD）. Complex 1 exhibits a 3D three-fold parallel interpenetrated 3D · 3D structure with （65.8） CdSO4 topology. Complex 2 is built from [Co3（μ/2-Ocarboxyl）2（CO2）4] clusters and linear bib ligands, displaying a two-fold par- allel interpenetrated （3,8）-connected （4^3）2（4^6.6^18·8^4） topology, while complex 3 is a 3D pillar-layered structure involving an in- finite -Co-（μ2-Ocarboxyl）（CO2）-Co-chain. The diverse structures of the three complexes indicate that the skeletons of different N-donor ligands play an important role in the assembly of such different frameworks. In addition, magnetic investigation indi- cates that besides spin-orbit coupling of Co（II） ions, there exist antiferromagnetic exchange interactions in Co5 and Co3 clus- ters of 1 and 2, respectively.

Enhancement of gas-framework interaction in a metal–organic framework by cavity modification

Originated from the pore space segmentation modification of a reported metal-organic framework （MOF） （NOTT-125）, a new porous MOF ZnX was obtained and characterized by single-crystal X-ray diffraction, elemental analysis, X-ray powder diffraction and TGA. The ZnX exhibits remarkable selective CO2 adsorption property compared with that of the NOTT-125, which should be attributed to the enhanced gas-framework interactions induced by the fragmented pore space in ZnX.