合肥X射线衍射光束线单色仪中晶体反射曲线的测量

合肥X射线衍射光束线装备了一台以两晶体无色散 ( +n ,-n)排列 ,能量可连续扫描 ,空间位置固定输出为特点的双晶单色仪。选用单晶硅作为分光元件 ,它所对应的不同能量产生的全反射的本征宽度决定了双晶单色仪的分辨率。因此 ,晶体在投入使用之前 ,测量它的本征宽度 ,为单色仪的调试提供依据是非常必要的。介绍了用于合肥X射线衍射光束线单色仪中两块晶体的测量 ,包括测试方法、装置、测量结果和分析。

氢气放电源和X光机X射线源打靶谱的研究

用氢气放电源打靶的方法,测到了系列的谱线.为了鉴别这些谱线,进行了X光机X射线源打靶实验和两种源打靶的对比实验.实验结果表明:在X光机X射线源打靶谱中,除靶材料的特征X射线和两条源谱线外,还存在两种谱线:一种是能量变化的谱线,根据不同衍射角θ和测量角φ的实验结果,及打多晶体靶和非晶体靶的实验事实,表明这种能量变化的谱线是衍射线;另一种是能量恒定不变的谱线.氢气放电源和X光机X射线源打靶谱的对比实验结果表明:两种源打靶谱自洽.这说明和X光机X射线源打靶谱一样,氢气放电源打靶谱中那些能量变化的谱线是衍射线.但两种源打不同材料靶时都出现了同一类能量恒定的未知谱线,这类谱线的来源和特性有待进一步的实验研究.

X射线环面聚焦镜压弯调整与面形测量

长条形柱面镜在一特制机构中压弯成环面镜，用以水平和垂直两个方向上聚焦同步辐射，是Ｘ射线光束线中常用的成像装置。压弯后的镜面精度直接影响成像质量。合肥Ｘ射线衍射光束线上的环面聚焦镜由德国ＺＩＥＳＳ公司生产的柱面镜，配以国内自行研制的压弯机构，最后在法国ＥＳＲＦ对实验室组合、调试和测量。结果可见，压弯半径随载荷增加而减小，三个循环的重复度＜２％，面形误差＜５μｒａｄ。

Introduction of the X-ray diffraction beamline of SSRF

The X-ray diffraction beamline developed at Shanghai Synchrotron Radiation Facility(SSRF)is located at the BL14B1 bending magnet port of the 3.5 Ge V storage ring. The beamline optics is based on a collimating mirror,a sagittally focused double crystal monochromator and a focusing mirror. Photon flux of 4.43 × 1011phs/s at10 ke V is obtained. The primary instrument equipped in the experimental end-station is a Huber 5021 sixcycle diffractometer. BL14B1 is a general purpose X-ray diffraction beamline and focused on material science,condensed matter physics and other relevant fields looking for structural information.

Extraction of nickel from molybdenum leaching residue of metalliferous black shale by segregation roasting and acid leaching

The recovery of nickel from molybdenum leach residue by the process of segregation roasting-sulfuric acid leaching-solvent extraction was investigated. The residue was characterized by microscopic investigations, using X-ray fluorescence spectrometry （XRF） and X-ray diffractometry （XRD） techniques and the residue after segregation roasting was characterized by chemical phase analysis method. A series of experiments were conducted to examine the mass ratio of activated carbon （AC） to the residue, segregation roasting time and temperature, sulfuric acid concentration, liquid-to-solid ratio, leaching time, leaching temperature, addition amount of 30% H2O2, stirring speed （a constant） on the leaching efficiency of nickel. A maximum nickel leaching efficiency of 90.5% is achieved with the mass ratio of AC to the residue of 1：2.5, segregation roasting time of 2 h, segregation roasting temperature of 850 ℃, sulfuric acid concentration of 4.5 mol/L, liquid-to-solid ratio of 6：1, leaching time of 5 h, leaching temperature of 80 ℃, addition of 30% H202 of 0.6 mL for 1 g dry residue. Under these optimized conditions, the average leaching efficiency of nickel is 89.3%. The nickel extraction efficiency in the examined conditions is about 99.6%, and the nickel stripping efficiency in the examined conditions is about 99.2%.

Investigation of Temperature Dependency of Morphological Properties of Thermoplastic Polyurethane using WAXS and SAXS Monitoring

Polyether and polyether/ester based TPU （thermoplastic polyurethanes） were investigated with wide-angle XRD （X-ray diffraction） and SAXS （small angle X-ray scattering）. Furthermore, SAXS measurements were performed in the temperature range of 30 ℃ to 130 ℃. Polyether based polymers exhibit only one broad diffraction signal in a region of 2 θ 15° to 25°. In case of polyurethanes with ether/ester modification, the broad diffraction signal arises with small sharp diffraction signals. SAXS measurements of polymers reveal the size and shape of the crystalline zones of the polymer. Between 30 ℃ and 130 ℃ the size of the crystalline zone changes significantly. The size decreases in most of investigated TPU. In the case of Desmopan 9365D an increase of the particle size was observed.

Structure of the organic crystallite unit in coal as determined by X-ray diffraction

X-ray diffraction （XRD） was used to study the structure of the organic crystallite unit （La, Lo doo2） in coals collected from Henan and Shanxi Provinces. XRD patterns of coal were collected in a step-scan mode （0.1 °/step） over an angular range of 2-90° （20）, allowing 8 s at each step. The structure of the crystallite unit was determined from the Scherrer equation and peak parameters deduced from whole pattern fitting. The results show that the structure of the crystallite unit in coal is mainly controlled by the coal rank. As the coal rank increases the average diameter of a coal crystallite unit （La） increases, the interlayer spacing （doo2） decreases slightly, and the average height of a coal crystallite unit （Lc） increases at first but then decreases. A new diffraction peak from the crystallite unit in coal was found at a low scattering angle in the XRD pattern （2-10~）. This suggests a structure with an inter-layer spacing from 1.9 to 2.8 nm exists in coal crystallites.

Simulation of X-ray Diffraction Line Broadening Caused by Stress Gradients and Determination of Stress Distribution by Fourier Analysis

Different physical, mechanical and chemical processes, such as： ion implantation, oxidation, nitridation and others create on the surface of materials residual stress state, characterized by high level and strong gradient. X-ray diffraction method widely used for stress measurements has some difficulties in interpretation of experimental data, when the depth of X-ray penetration is compared with thickness of surface layer where inhomogeneous stress distribution is localized. Early it has been shown by authors that diffraction line broadening occurs when analyzed surface is characterized by strong gradient. The interest to study the diffraction line broadening is connected to the possibility of obtaining information about parameters of surface stress distribution. In the present paper the convolution and deconvolution concepts of Fourier analysis were applied to study X ray diffraction line broadening caused by surface stress gradients. Developed methodology allows determining of stress distribution in superficial layers of materials.

Influence of Mineral Admixtures on Essential Properties of Ternary Cement Blends

Two CaCO3-based materials （limestone and clamshells） and steel slag were used as mineral admixtures in cement to produce ternary blends and their influences on hydration and portlandite formation were analyzed. Additionally, mechanical properties were determined. These properties were determined using X-ray diffraction and scanning electron microscopic/energy dispersive X-ray analytical techniques as well as applying methods specified by EN （European Standards） and ASTM （American Standards for Testing and Materials）. The portlandite （Ca（OH）E） content was considerably reduced from 36.9% of reference cement to between 13.79% and 15.5%. With the water demand and setting times of the cements containing up to 10%, admixtures did not change significantly. The mechanical tests results showed that ternary blends produced 2-day strengths higher than that specified by EN 197-1 and that blends containing up to 20% admixtures can be used to produce both Class 32.5N and 42.5N cements.

Synthesis and Crystal Structure of a Novel Polymer Copper(Ⅱ) Complex

A novel chain complex was synthesized and its crystal structure has been deter- mined by X-ray diffraction technique. It was found that the local coordination geometry around Cu(Ⅱ) is a distorted tetrahedron and C14H9CuNO3CH3OH is bridged by the carboxylate oxygen atom to form an infinite one-dimensional linear chain. The hydrogen bond exists between O(1) and solvate molecule O(4). The crystal belongs to monoclinic, space group P21 with a = 9.6650(19), b = 7.1280(14), c = 9.925(2) ? b = 98.39(3)? V = 676.4(2) 3, Z = 2, F(000) = 342 and m(MoK? = 1.629 mm-1 .

Structure-Property Relations in xWO3-0.31P2O5-0.31B2O3-（0.38-x）Cs2O （0.01 ≤ x ≤0.28） Glasses by IR, UV and EPR Spectroscopic Studies

Glasses in the series of xWO3-0.31P2O5-0.31B2O3-（0.38-x）Cs2O （0.01 ≤ x ≤0.28） （G1-G4： x= 0.01, 0.1, 0.19, 0.28） were prepared by sol-gel method. Glassy phase in the samples were ascertained by powder X-ray diffraction pattern. Differential scanning calorimetry （DSC） traces of the samples show glass transition temperature Tg, in the range 247-253 ℃. IR spectra at 300 K of G1-G4 show the presence of [WO6], [WO4], [PO4]^3-, [PO3]^2-, [BO4]^＋, [BO3] units in the glass matrix. Observed electron paramagnetic resonance （EPR） lineshapes show two signals with very different intensities which are associated with W^5＋ （5d^1） and Mo^5＋ （4d^1） （impurity） paramagnetic sites. Signal with values ofg factors in the range 1.68 〈 g⊥ 〈 1.72 and 1.58 〈 gⅡ 〈 1.62 are due to W^5＋ ions present in axially distorted octahedral symmetry. The optical absorption spectra show that the W^5＋ ions have pyramidal coordination, involving a tungstyl ion WO^3＋ （C4v symmetry）. EPR and optical studies suggest the existence of blocks of octahedra linked by tungsten clusters.

Novel Thermally-Accessible Structural Changes of Chiral and Some Related Cu（ll） Complexes

A mononuclear chiral copper（ll） complex, [Cu（RRchxn）2（C（CN）3）2]＇H20 （RRchxn = （1R, 2R）-diaminocyclohexane） （RRchxnH）, and its deuterated compound, [Cu（RRchxn）2（C（CN）3）z].D20 （RRchxnD）, and their isomers, [Cu（trchxn）2（C（CN）3）2]＇H20 （trchxn = trans-l,2-diaminocyclohexane） （trchxnH） and [Cu（trchxn）2（C（CN）3）2]＇D20 （trchxnD） have been prepared and characterized by means of 1R （infrared）, electronic, and CD （circular dichroism） spectra, magnetic susceptibility, and variable-temperature X-ray crystallography as single crystals or powder. Interestingly, depending on grain size of samples, RRchxnH exhibits the monoclinic form and the orthorhombic form, which are distinguished by systematic absence and powder XRD （X-ray diffraction） patterns clearly. Although single crystals did not exhibit phase transition, powder XRD patterns of RRchxnH and weakly hydrogen bonded RRchxnD emerged low-temperature phase of monoclinic in the orthorhombic patterns only around 200-220 K. However, as a control, powder XRD patterns of both trchxnH and trchxnD did not exhibit such phase transition clearly.

Crystallographic Parameters and Band Gap of CdSxSe1-x Mixed Crystals

Crystals of CdSxSe1-x alloys have been grown from the vapour phase. Some of the physical properties, such as lattice parameters, crystal structure and x-rays data of CdSxSe1-x alloys were determined using x-ray diffractometry. X-ray diffractometry has shown that CdS-CdSe mixed crystals had the wurtzite structure for all compositions between CdS and CdSe. The lattice parameters （both a and c） were found to show a linear dependence with composition. The dependence of the lattice parameters of a and c on composition can be expressed as： a（x） = 4.165 ＋ 0.16x; c（x） = 6.713 ＋ 0.27x. The variation of band gap with composition was determined for these samples from optical absorption measurements, which showed that the band gap varied smoothly and monotonically, but not linearly over the composition range typical results were found between 2.42-1.74 eV at room temperature.

纳米石墨颗粒粒度的测量与表征

介绍了用负氧平衡炸药在密闭容器内爆轰制备的纳米石墨粉 ;用X射线衍射线线宽法 (谢乐公式 )、透射电镜观察法 (TEM)、激光拉曼散射法、比表面积法和X射线小角散射法等手段 ,对合成的纳米石墨粉颗粒粒度进行了测量 ,结果表明炸药爆轰法制备的纳米石墨粉具有六方石墨结构 ,颗粒呈球形或椭球形 ,分布在4～9nm之间 ,平均粒径为8.7nm ;在5种测量方法中 ,用X射线衍射线线宽法 (谢乐公式 )得到的平均粒径值最小 ,而用其它4种测量方法所得到的粒径值基本一致。

水蒸气对PtSn/ZnAl_2O_4催化剂结构的影响(英文)

利用X-射线衍射研究了经氢还原及还原后又经高温水蒸气处理的PtSn／ZnAl2O4催化剂，结果表明，催化剂的相结构是Sn载量的函数．还原态的Pt／ZnAl2O4催化剂中Pt以金属态存在，Pt／Sn原子比为1：1、1：3及1：10的PtSn／ZnAl2O4催化剂还原后分别生成PtZn、PtSn、尽Sn及Pt物相；高温水蒸气处理对Pt／ZnAl2O4样品的相结构及Pt晶粒尺寸无明显影响，但却使Ptsn／ZnAl2O4催化剂的相结构发生显著变化；对于1：l及1：3的Ptsn／ZnAl2O4，水蒸气使各自还原态中的PtZn、PtSn合金重构为Pt3Sn合金，同时使1：10PtSn／ZnAl2O4的民β-Sn及Pt物相消失，而生成了新的PtSn合金相．

Visible-Light Activities of Erbium Doped BiVO4 Photocatalysts

Er-doped BiVO4 composite photocatalyst was hydrothermal synthesized and characterized by X-ray powder diffraction, scanning electron microscopy, energy-dispersive X-ray Spectroscopy, X-ray photoelectron spectroscopy, and UV-Vis diffuse reflectance spectra techniques. The activity of the catalyst was determined by oxidative decomposition of methyl orange in aqueous solution under visible-light irradiation. X-ray photoelectron spectroscopy and energy-dispersive X-ray Spectroscopy analysis revealed that the doped Er existed in the form of Er2O3. It also showed that the Er doping can enhance the visible-light absorption abilities of catalysts and their visible-light-driven photocatalytic activities in comparison with those of pure BiVO4.

The Mineral Transformation of Huainan Coal Ashes in Reducing Atmospheres

By using the advanced instrumentation of a Computer Controlled Scanning Electron Microscope （CCSEM）, X-ray diffraction （XRD） and X-ray fluorescence （XRF）, the ash composition and the mineral components of six typical Huainan coals of different origins were studied. The transformation of mineral matter at high temperatures was tracked by XRD in reducing conditions. The quartz phase decreased sharply and the anorthite content tended to increase at first and then decreased with increasing temperatures. The formed mullite phase reached a maximum at 1250 ℃ but showed a tendency of slow decline when the temperature was over 1250 ℃. The mullite formed in the heating process was the main reason of the high ash melting temperature of Huainan coals. Differences in peak intensity of mullite and anorthite reflected differences in phase concentration of the quenched slag fractions, which contributed to the differences in ash melting temperatures. The differences in the location of an mnorphous hump maximum indicated differences of glass types which may affect ash melting temperatures. For Huainan coal samples with relatively high ash melting tempera- tures, the intensity of the diffraction lines for mullite under reducing condition is high while for the samples with relatively low ash melting temperature the intensity for anorthite is high.

Development of 3D crystallographic orientation measurement for grain deformation analysis in aluminum alloy

Development of inhomogeneous deformation is an interest matter in material engineering. Synchrotron radiation tomography provides 3D distribution map of local strain in polycrystalline aluminum alloy by tracking microstructural features. To perform further deep analysis on development of inhomogeneous deformation, crystallographic grain orientation is necessary. Three-dimensional X-ray diffraction technique was developed. A new crystallographic orientation measurement method was described in 3D space, utilizing grain boundary tracking （GBT） information.

Reactive Adsorption of Thiophene on ZnNi/Diatomite-Pseudo-Boehmite Adsorbents

The thiophene removal ability of the synthesized ZnNi/diatomite-pseudo-boehmite adsorbent was tested in a lab- scale fixed-bed reaction system. X-ray diffractograms （XRD） were used to characterize the adsorbent samples. The effects of Zn/Ni molar ratio, various model fuels and regeneration patterns on the RADS tests were studied. The adsorption mecha- nism was investigated by XRD and MS analyses. The results indicted that thiophene in the model fuel was first decomposed on the surface Ni of the adsorbent to form Ni3S2 while the hydrocarbon portion of the molecule was released back into the process stream, followed by reduction of Ni3S2 to form H2S in the presence of H2, and then HzS is stored in the adsorbent accompanied by the conversion of ZnO into ZnS.

Preparation and characterization of sulfated TiO_2 with rhodium modification used in esterification reaction and decomposition of methyl orange

A unique Rh/TiO2 solid acid catalyst modified with H2S04 was synthesized and evaluated in the esterification reaction of propylene glycol methyl ether and decomposition of methyl orange （MO） in aqueous phase under halogen lamp irradiation. For this purpose, rhodium （Rh） nanoparticles were loaded on S02-/Ti02 via the photo-deposition method. It was found that S024-/Rh-Ti02 exhibited stronger catalytic activity than S02-/ Ti02. The new catalysts were characterized by X-ray powder diffraction （XRD）, Brunauer-Emmett-Teller （BET）, Transmission electron microscopy （TEM） and high-resolution （HRTEM）, X-ray photoelectron spec- troscopy （XPS） and Fourier Transform infrared spectroscopy （FrlR）. Results from XRD and BET show that S02-/Rh-Ti02 has higher specific surface area and smaller pore size than S02-fri02. The distribution of loaded Rh was found to be uniform with a particle size of 2-4 nm. Data from XPS reveal that Rh primarily exists as Rh~ and Rh3 ＋ in Rh-Ti02 and SO^-/Rh-TiO~. These valence forms of Rh likely contribute to the en- hanced catalytic activity. Furthermore, FT-IR spectra of the catalysts show an abundance of surface hydroxyl groups, which help the formation of hydroxyl radicals and the enhancement of surface acid density. The results show that more acid sites are formed on the sulfated Rh-Ti02, and these acidic sites are largely responsible for improving the catalytic performance. This superior SO]-/Rh-Ti02 catalyst has potential applications in reactions reouirinz efficient acid catalysts, includinz esterification reactions and waste water treatment.