A Hybrid Angular/Energy Dispersive Method to Improve Some Characteristics of Laboratory X-Ray Diffraction

The Energy Dispersive X-ray Diffraction, generally referred as EDXD, has shown to be a valid alternative to the conventional Angular Dispersive X-ray Diffraction, the ADXD. EDXD exhibits several advantages to its AD counterpart, mainly related to the properties of the polychromatic X-ray beam utilized for diffracting, such as higher signal intensities, a wider accessible region of the reciprocal space, a greater transparency of samples, and a parallel data collection of the q-points in the diffraction pattern acquisition. However, the main drawback of poly-chromaticity lays in the fact that the quantities that modulate the scattered intensity in a diffraction measurement depend on the energy. These quantities are the primary X-ray beam spectrum, polarization, and X-ray absorption, the last producing by far the most critical effect because it rapidly changes as a function of energy. Therefore, a detailed knowledge of the energy dependence of all these quantities is required in EDXD in order to process the data correctly and prevent systematic errors. The difficulty in handling the energy-dependent factors complicates the experimental procedure and may make the measurements unreliable. In the present paper, a hybrid method between the ED and AD X-ray Diffraction is proposed to maintain the advantages of the polychromatic nature of the radiation utilized in EDXD, while preventing the problems produced by the energy-dependent quantities.

Energy-dispersive X-ray Spectroscopy for the Quantitative Analysis of Pyrite Thin Specimens

To explore ways to improve the accuracy of quantitative analysis of samples in the micrometer to nanometer range of magnitudes,we adopted analytical transmission electron microscopy(AEM/EDS)for qualitative and quantitative analysis of pyrite materials.Additionally,the k factor of pyrite is calculated experimentally.To develop an appropriate non-standard quantitative analysis model for pyrite materials,the experimentally calculated k factor is compared with that estimated from the non-standard quantitative analytical model of the instrument software.The experimental findings demonstrate that the EDS attached to a TEM can be employed for precise quantitative analysis of micro-and nanoscale regions of pyrite materials.Furthermore,it serves as a reference for improving the results of the EDS quantitative analysis of other sulfides.

Phase Identification Using Series of Selected Area Diffraction Patterns and Energy Dispersive Spectrometry within TEM

Transmission electron microscopy (TEM) is a very powerful technique for materials characteriza-tion, providing information relating to morphology, composition, and crystal structure. Selected area diffraction patterns (SADPs) are crystallographic data that can be obtained using a TEM in-strument. Conventional identification through SADP/TEM is tricky and tedious, thereby increasing the difficulty of phase identification. To establish a procedure for phase identification of known and unknown phases, in this study we examined two samples: one, a known phase, was Si with alignment;the other, unknown, was the TixOy phase at the 96.4Au-3Ni-0.6Ti interlayer/ yttria-stabilized zirconia (YSZ) interface of a steel/96.4Au-3Ni-0.6Ti interlayer/YSZ joint. The procedures for phase identification of the known and unknown phases are described herein using a series of SADPs and energy dispersive spectrometry within TEM that would be useful for general researchers.

Determination of Element Levels of Lagoon from Townships near Cocody City Abidjan Côte D’Ivoire Using Energy Dispersive X-Ray Fluorescence

Eight water bottles from Ebrie lagoon with pollution potency were studied using nuclear chemistry technique and Energy dispersive X-ray fluorescence. This pollution is characterized by pH and conductivity parameters, concentrations average in mg/L of metals such Fe (0.731), Mn (0.345), Cr (0.070), Cu (0.014) and concentrations of nutrients known to be pollutants and toxic for living or-ganisms. These heavy metals are dangerous to the lives, the local inhabitants and also a threat to aquatic life since this water is essential for the economical town, Abidjan. According to the Manganese concentration average (0.345 mg) values that higher than WHO (0.05 mg) value, the main likely source of pollu-tants is anthropogenic, industrial and agricultural. This study also shows the use of materials and lubricants near the lagoon that pollute this water.

Ultrahard X-ray multifunctional application beamline at the SSRF

The ultrahard X-ray multifunctional application beamline(BL12SW)is a phase-II beamline project at the Shanghai Syn-chrotron Radiation Facility.The primary X-ray techniques used at the beamline are high-energy X-ray diffraction and imaging using white and monochromatic light.The main scientific objectives of ultrahard X-ray beamlines are focused on two research areas.One is the study of the structural properties of Earth’s interior and new materials under extreme high-temperature and high-pressure conditions,and the other is the characterization of materials and processes in near-real service environments.The beamline utilizes a superconducting wiggler as the light source,with two diamond windows and SiC discs to filter out low-energy light(primarily below 30 keV)and a Cu filter assembly to control the thermal load entering the subsequent optical components.The beamline is equipped with dual monochromators.The first was a meridional bending Laue monochromator cooled by liquid nitrogen,achieving a full-energy coverage of 30-162 keV.The second was a sagittal bending Laue monochromator installed in an external building,providing a focused beam in the horizontal direction with an energy range of 60-120 keV.There were four experimental hutches:two large-volume press experimental hutches(LVP1 and LVP2)and two engineering material experimental hutches(ENG1 and ENG2).Each hutch was equipped with various near-real service conditions to satisfy different requirements.For example,LVP1 and LVP2 were equipped with a 200-ton DDIA press and a 2000-ton dual-mode(DDIA and Kawai)press,respectively.ENG1 and ENG2 provide in situ tensile,creep,and fatigue tests as well as high-temperature conditions.Since June 2023,the BL12SW has been in trial operation.It is expected to officially open to users by early 2024.

Alpha-actinin expression at different differentiating time points from temporal lobe cerebral cortex neural stem cells to neuron-like cells using energy dispersive X-ray analysis

BACKGROUND： Alpha-actinin （ a -actinin） plays a key role in neuronal growth cone migration during directional differentiation from neural stem cells （NSCs） to neurons. OBJECTIVE： To detect in situ microdistribution and quantitative expression of a -actinin during directional differentiation of NSCs to neurons in the temporal lobe cerebral cortex of neonatal rats. DESIGN, TIME AND SETTING： Between January 2006 and December 2008, culture and directional differentiation of NSCs were performed at Department of Histology and Embryology, Preclinical Medical College, China Medical University. Immune electron microscopy was performed at Department of Histology and Embryology and Department of Electron Micrology, Preclinical Medical College, China Medical University. Spectrum analysis was performed at Laboratory of Electron Microscopy, Mental Research Institute, Chinese Academy of Sciences. MATERIALS： Basic fibroblast growth factor, epidermal growth factor, brain-derived nerve growth factor, type-1 insulin like growth factor, and a -actinin antibody were provided by Gibco BRL, USA; rabbit-anti-rat nestin monoclonal antibody, rabbit-anti-rat neuron specific enolase polyclonal antibody, and EDAX-9100 energy dispersive X-ray analysis were provided by PHILIPS Company, Netherlands. METHODS： NSCs, following primary and passage culture, were differentiated with serum culture medium （DMEM/F12 ＋ 10% fetal bovine serum ＋ 2 ng/mL brain-derived nerve growth factor ＋ 2 ng/mL type-1 insulin like growth factor）. MAIN OUTCOME MEASURES： Expression of a -actinin in neuron-like cells was quantitatively and qualitatively detected with immunocytochemistry using energy dispersive X-ray analysis. RESULTS： Immunocytochemistry, combined with electron microscopy, indicated that positive α -actinin expression was like a spheroid particle with high electron density. In addition, the expression was gradually concentrated from the nuclear edge to the cytoplasm and expanded into developing neurites, during differentiation of neural stem cells to neurons. Conversely, energy dispersive X-ray analysis indicated that the more mature the neural differentiation was, and the greater the expression of α -actinin. CONCLUSION： The gradual increase of α -actinin expression is related to growth, development, and maturity of differentiated neuron-like cells, in neonatal rat frontal lobe cortex, at different differentiating time points of NSCs to neurons.

Energy Dispersive X-Ray Spectroscopy of the Sohnari Member of Laki Formation from Southern Indus Basin of Pakistan

This study determines the geochemical and depositional environment analysis of the sediments of the Sohnari Member of the Laki Formation, Northern Kirthar Fold Belt of Pakistan. The Energy-Dispersive-X-Ray Spectroscopy (EDS) technique is used for the detection of major elements and the effects of shifting depositional climatic conditions of six representative samples which were acquired from the Sohnari Member of the Laki Formation at Lakhra area, Sindh, Pakistan. The sedimentological studies clarify that the sediments the Sonahri Member are relatively immature and most migrated in clastic mode. The availability of Silica shows that the Member was formed due to biochemical precipitation and detrital mode and was deposited at a fast rate of sediment deposition under the fluvio-deltaic depositional system. This is also deduced that the rapid rate of sediment deposition might be created a reducing atmosphere and allowing for the mineralization of sulphur.

The Aqueous Dispersions of Bicontinuous Cubic Phases Formed by Precursor Method

The morphologies and the microstructures of the dispersed particles of the cubic phase, which were formed by precursor method, were studied. The freeze-fracture TEM clearly showed that the aqueous dispersed particles have irregular cubic shapes. X-ray diffraction technique has been utilized to study the microstructure of the particles and it was found that these particles still retained the cubic character. The sizes of the particles were measured by dynamic light scattering, and the results showed that the sizes of the dispersed particles were between 200 ~ 400 nm under different conditions.

Remarks on the Erroneous Dispersion Surfaces From a Pair of a Hyperbolic Branch and An Elliptical Arc of the Intersected Two Laue Spheres Based on the Usual Crude Approximation

In almost all previous works, the hyperbolic dispersion surfaces of the central proper quadrics have been crudely derived from the degree of reduction from the bi-quadratic equation by use of some roughly indefinable approximate relations. Moreover, neglecting the high symmetry of the hyperbola, both the branches have been approximated on the asymmetric surfaces composed of a pair of a branch of the hyperbola and a vertex of the ellipse without the presentation of reasonable evidence. Based upon the same dispersion surfaces equation, a new original gapless dispersion surfaces could be rigorously introduced without crude omission of even a term in the bi-quadratic equation based upon usual analogy with the extended band theory of solid as the close approximation to the truth.

Effect of wire-arc directed energy deposition on the microstructural formation and age-hardening response of the Mg-9Al-1Zn(AZ91)alloy

In recent years,wire-arc directed energy deposition(wa DED),which is also commonly known as wire-arc additive manufacturing(WAAM),has emerged as a promising new fabrication technique for magnesium alloys.The major reason for this is the possibility of producing parts with a complex geometry as well as a fine-grained microstructure.While the process has been shown to be applicable for Mg-Al-Zn alloys,there is still a lack of knowledge in terms of the influence of the WAAM process on the age-hardening response.Consequently,this study deals with the aging response of a WAAM AZ91 alloy.In order to fully understand the mechanisms during aging,first,the as-built condition was analyzed by means of high-energy X-ray diffraction(HEXRD)and scanning electron microscopy.These investigations revealed a finegrained,equiaxed microstructure with adjacent areas of alternating Al content.Subsequently,the difference between single-and double-step aging as well as conventional and direct aging was studied on the as-built WAAM AZ91 alloy for the first time.The aging response during the various heat treatments was monitored via in situ HEXRD experiments.Corroborating electron microscopy and hardness studies were conducted.The results showed that the application of a double-step aging heat treatment at 325℃with pre-aging at 250℃slightly improves the mechanical properties when compared to the single-step heat treatment at 325℃.However,the hardness decreases considerably after the pre-aging step.Thus,aging at lower temperatures is preferable within the investigated temperature range of 250-325℃.Moreover,no significant difference between the conventionally aged and directly aged samples was found.Lastly,the specimens showed enhanced precipitation kinetics during aging as compared to cast samples.This could be attributed to a higher amount of nucleation sites and the particular temperature profile of the solution heat treatment.

馆藏汉代瓦当表面可溶盐的化学组成分析

采用离子色谱仪(IC),扫描电子显微镜-能谱仪(SEM-EDS),X射线衍射仪(XRD)和傅里叶变化显微红外光谱仪(FTIR)等现代分析仪器,对陕西历史博物馆馆藏的汉代瓦当表面可溶盐进行了鉴定,并分析了相关的化学组成。结果表明,瓦当表面可溶盐含有石膏(Ca SO_(4)·2H_(2)O)和有机酸钙盐[Ca_(3)(CH_(3)COO)_(3)Cl(NO_(3))_(2)·6H_(2)O]等成分。

Establishment of Energy Dispersive X-ray Diffraction Experimental System With Synchrotron Radiation Under High Pressure

Because the interactions between molecules and atoms in mediums can be dramatically changed by compression, high pressure studies on materials can provide much information on fundamental properties including phase transition and

The development,performances and applications of the monochromatic X-rays facilities in(0.218–301)keV at NIM,China

Space scientific exploration is rapidly becoming the primary battlefield for humankind to explore the universe.Countries worldwide have launched numerous space exploration satellites.Accurate calibration of the detectors on the ground is a crucial element for space science satellites to obtain observational results.For the purpose of providing calibration for various satellite-borne detectors,multiple monochromatic X-rays facilities have been built at the National Institute of Metrology,P.R.China(NIM).These facilities mainly pertain to grating diffraction and Bragg diffraction,and the energy range of the produced monochromatic X-rays is 0.218–301 ke V.These facilities have a high performance in terms of energy stability,monochromaticity,and flux stability.The monochromaticity was greater than 3.0%.The energy stability of the facility is 0.02%at 25 ke V over 8 h,and the flux stability was within 1.0%at 25 ke V over 8 h.Calibration experiments on the properties of satellite-borne detectors,such as energy linearity,energy resolution,detection efficiency,and temperature response,can be conducted at the facilities.Thus far,the calibration of two satellites has been completed by the authors,and the work on three other satellites is in progress.This study will contribute to the advancement of X-ray astronomy the development of Chinese space science.

Goss Texture Evolution of Grain Oriented Silicon Steel by High-Energy X-ray Diffraction

High energy synchrotron diffraction offers great potential to study the recrystallization kinetics of metallic materials. To study the formation of Goss texture （{ [10}（001）） of grain oriented （GO） silicon steel during secondary recrystallization process, an in situ experiment using hi gh energy X-ray diffraction was designed. The results showed that the secondary recrystallization began when the heating temperature was 1,494 K, and the grains grew rapidly above this temperature. With an increase in annealing temperature, the large grains with 7 orientation [〈111〉//normal direction] formed and gradually occupied the dominant position. As the annealing temperature increased even further, the grains with Goss orientation to a very large size by devouring the 7 orientation grains that formed in the early annealing stage. A single crystal with a Goss orientation was observed in the GO silicon steel when the annealing temperature was 1,540 K.

Production and Characterization of Nano Structured Silicon Carbide by High Energy Ball Milling

The article has been retracted due to the investigation of complaints received against it. The Editorial Board found that substantial portions of the text came from other published paper. Comparing with the paper published in International Journal of Engineering, Science and Technology Vol. 3, No. 4, 2011, pp. 82-88 (www.ijest-ng.com), these two papers have the same contents before Figure 7 and the author added Fig. 8, 9, 10 on the 2012 paper. The scientific community takes a very strong view on this matter, and the Journal of Minerals and Materials Characterization and Engineering (JMMCE) treats all unethical behavior seriously. This paper published in Vol.11 No.5, 529-541, 2012 has been removed from this site.

X-Ray and Mössbauer Study of Magnetic Black Sand from Mayotte Island

Natural magnetic black sands are known from several sites often located in areas of volcanic origin. Their elemental and mineral composition provides information on the geology of their territory and depends on several factors occurred during their formation. A sample of black sand was collected on the seashore of the island of Mayotte in the Indian Ocean and its magnetic part was investigated by means of energy dispersive X-ray spectroscopy (EDS), powder X-ray diffraction (XRD), and MÖssbauer spectroscopy at room temperature. The mineral composition is dominantly magnetite, in good agreement with samples collected in other sites of volcanic origin. Contrary to pure magnetite, a relevant fraction of Ti was detected by EDS. The 16% Ti and 1% Mn content increase the magnetite lattice parameter to 8.4312 (25) Å. The broadening of XRD lines pointed towards a significant degree of disorder. This was confirmed by MÖssbauer spectroscopy and is attributed to the presence of Ti replacing Fe in the magnetite lattice. The presence of Ti modifies the local magnetic field on the Fe sites, leading to a broader and more complex MÖssbauer transmission spectrum with respect to the one of pure magnetite. To study the effect of temperature, samples were heated for 12 hours to 600°C and 800°C in argon and to 1000°C in air. Annealing in argon did not improve the crystallinity while annealing in air caused a complete decomposition of magnetite into hematite and pseudobrookite.

Mossbauer,X-Ray and Magnetic Studies of Black Sand from the Italian Mediterranean Sea

The study of natural magnetic sands is instrumental to investigate the geological aspects of their formation and of the origin of their territory. In particular, Mossbauer spectroscopy provides unique information on their iron content and on the oxidation state of iron in their mineral composition. The Italian coast on the Mediterranean Sea near Rome is known for the presence of highly magnetic black sands of volcanic origin. A study of the room temperature Mossbauer spectrum, powder X-ray diffraction, energy dispersive X-ray spectroscopy, and magnetic measurements of a sample of black magnetic sand collected on the seashore of the town of Ladispoli is performed. This study reveals magnetite as main constituent with iron in both tetrahedral and octahedral sites. Minor constituents are the iron minerals hematite and ilmenite, the iron containing minerals diopsite, gossular, and allanite, as well as ubiquitous sanidine, quartz, and calcite.

Possible Relevance of the Allende Meteorite Conditions in Prebiotic Chemistry: An Insight into the Chondrules and Organic Compounds

The study of the mineral and organic content of the Allende meteorite is important for our understanding of the molecular evolution of the universe as well as the ancient Earth. Previous studies have characterized the magnetic minerals present in ordinary and carbonaceous chondrites, providing information on the evolution of magnetic fields. The interaction of organic compounds with magnetic minerals is a possible source of chemical diversity, which is crucial for molecular evolution. Carbon compounds in meteorites are of great scientific interest for a variety of reasons, such as their relevance to the origins of chirality in living organisms. This study presents the characterization of organic and mineral compounds in the Allende meteorite. The structural and physicochemical characterization of the Allende meteorite was accomplished through light microscopy, powder X-ray diffraction with complementary Rietveld refinement, Raman and infrared spectroscopy, mass spectrometry, scanning electron microscopy, and atomic force microscopy using magnetic signal methods to determine the complex structure and the interaction of organic compounds with magnetic Ni-Fe minerals. The presence of Liesegang-like patterns of chondrules in fragments of the Allende structure may also be relevant to understanding how the meteorite was formed. Other observations include the presence of magnetic materials and nanorod-like solids with relatively similar sizes as well as the heterogeneous distribution of carbon in chondrules. Signals observed in the Raman and infrared spectra resemble organic compounds such as carbon nanotubes and peptide-like molecules that have been previously reported in other meteorites, making the Mexican Allende meteorite a feasible sample for the study of the early Earth and exoplanetary bodies.

广西桂西地区沉积型铝土矿矿物特征研究

随着中国铝土矿资源日益消耗,高硫铝土矿将成为重要的新型铝土矿资源。中国有大量品位较高的高硫型沉积型铝土矿,但这类矿石由于硫含量高(硫含量>0.7%),严重影响后续提铝工艺流程,因而一直未被工业化利用,在铝土矿资源日益紧缺之时,若能开发利用,对中国铝工业发展具有重要意义。2020—2021年在广西桂西地区自平果—靖西一带铝土矿成矿带新探获得相当量的沉积型铝土矿,该沉积型铝土矿是堆积型铝土矿的矿源层,二者在空间分布上存在重叠,矿石多与黄铁矿密切共生,部分矿段的硫含量高出工业利用允许最高含量的数倍或数十倍,尽管矿石品位较高,但硫含量多在2%~8%,目前该铝土矿矿石性质及工业化技术指标尚不明确。因此,本文以广西桂西地区的沉积型铝土矿为研究对象,采用X射线荧光光谱、偏光显微镜、X射线衍射及扫描电镜-能谱等分析测试技术研究了铝土矿的矿石矿物组成特性,探究了沉积型铝土矿的矿石性质。分析结果表明,该矿石中Al2O3含量为64.21%,S含量为5.13%,属于高硫沉积型铝土矿;矿石中铝矿物主要为一水硬铝石、绿泥石;铁矿物主要有黄铁矿、赤铁矿及褐铁矿;一水硬铝石,其结晶粒度细,呈鲕状集合体形式,表面较光滑;黄铁矿中粗粒、中粒级黄铁矿多以半自形及他形存在,粒径较大。结合本项目组早前对高硫型铝土矿进行的大量试验研究认为,该沉积型铝土矿高硫问题可通过选矿技术方法分离黄铁矿,后续建议通过破碎磨矿手段使矿石矿物单体解离,再辅以合理的选矿药剂制度将黄铁矿浮选分离出来,从而使浮硫后的含铝矿物满足下一步的氧化铝提取入料要求。

煅烧煤系高岭石的相转变

通过X射线衍射分析,红外光谱分析,魔角旋转核磁共振和能量色散等测试手段,研究了煤系高岭石在200～1300℃下煅烧的相转变过程。结果表明:煅烧高岭石的相转变经历了4个阶段:脱羟阶段(≈550℃),偏高岭石阶段(550～850℃),SiO2分凝(850～1100℃)及Al2O3分凝阶段(950～1100℃),莫来石阶段(>1100℃)。550℃时高岭石失去羟基水,转变为半晶态的偏高岭石。偏高岭石莫来石的相转变过程中存在SiO2和Al2O3的分凝。能量色散分析证实了分凝Al2O3的存在。950℃的新生相是γAl2O3而不是AlSi尖晶石。莫来石是由偏高岭石分凝形成的SiO2和Al2O3反应而形成的。