氟锆酸盐光纤玻璃中析晶相的电子探针分析

本文利用大视场光学显微镜、扫描电子显微镜配合能量色散谱仪及分光光谱仪对zrF_4-BaF_2-LaF_3-AlF_3-NaF氟化物玻璃中存在的一些微晶颗粒进行了分析,确定为玻璃中不同尺寸的LaF_3晶粒的存在,并对所采用的分析方法的利弊进行了讨论.     

The influence of polarization and filtration of beams on the ED spectrometers sensitivity

The topic under discussion is the influence of X‐ray polarization and filtration, as well as the influence of detectors count rate on sensitivity and detection limits (DLs) in spectrometers with energy dispersion (EDS). Parameters calculation technique for searching optimal analysis conditions has been developed. Typical DLs of elements with medium and high atomic numbers on various spectrometers are given (on wave dispersive spectrometers (WDS), energy dispersive spectrometers (EDS) without polarization and energy‐dispersive polarized‐beam X‐ray spectrometers (EDPXRS). Apparently, EDS variants are preferred for determining elements with Z > 62–65, and EDPXRS spectrometers with concave targets and increased aperture are preferred for determining elements with medium atomic numbers.     

Inter‐laboratory comparison of a WDS–EDS quantitative X‐ray microanalysis of a metallic glass

We conducted an inter‐laboratory study of a metallic glass whose main component is nickel. Two determinations of the mass fractions of the different elements present within the sample were asked to the participants: one at an acceleration voltage of 15 or 20 kV and another one at 5 kV. We compare the mass fractions obtained from wavelength dispersive (WDS) and energy dispersive spectrometries (EDS) and also try to find an influence of the kind of EDS detector and its entrance window, the background subtraction method, the use or not of standards as well as the quantification method. Both means of WDS and EDS mass fractions are close to the reference values. The dispersion of the results was larger at 5 kV than at 15–20 kV owing to the use of the L lines rather than K lines and to the lowest collected intensities. There is an exception with the case of boron because at the lowest voltage, the excitation condition is more favorable for the production of the K line. It appears that the dispersion of the results is larger with EDS than with WDS, but it was not possible to find a correlation between the large dispersion and one of the considered experimental parameters and quantification factors. Thus, one can think that electron microprobes are inherently better for the determination of mass fractions or that the implementation of quantitative analysis must be optimized for some cases, especially in scanning electron microscopes. Copyright © 2014 John Wiley & Sons, Ltd.     

Sliding friction and wear behaviors of surface-coated natural serpentine mineral powders as lubricant additive

This work aims to investigate the friction and wear properties of surface-coated natural serpentine powders (SP) suspended in diesel engine oil using an Optimal SRV oscillating friction and wear tester. The worn surface was characterized by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS). Results indicated that the additives can improve the wear resistance and decrease friction coefficient of carbon steel friction couples. The 0.5 wt% content of serpentine powders is found most efficient in reducing friction and wear at the load of 50 N. The SEM and XPS analysis results demonstrate that a tribofilm forms on the worn surface, which is responsible for the decrease in friction and wear, mainly with iron oxides, silicon oxides, graphite and organic compounds.     

Thickness effect on the evolution of morphology and optical properties of ZnO films

N-Al co-doped ZnO films with various thicknesses were deposited on glass substrates by ultrasonic spray pyrolysis (USP). The crystalline microstructure, morphology, distribution of elements and photoluminescence properties of ZnO films were characterized by X-ray diffraction (XRD), field emission scanning microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS) and photoluminescence (PL) spectroscopy. The XRD and FESEM results show that with the increase of film thickness the grain size increases and the grain shape changes from regular hexagonal sheet-like to wedge-shaped, even pyramidal. The PL spectra illustrate that there is an obvious red-shift for the emission center from ultraviolet to blue region, and the intensities of defects emissions increase with the increase of thickness. In addition, the electrical properties are proved to be strongly affected by film thickness.     

Formation of titania composite coatings on carbon steel by plasma electrolytic oxidation

Titania composite coatings were prepared on carbon steel by plasma electrolytic oxidation in silicate electrolyte and aluminate electrolyte with titania powers doping in the electrolytes. The microstructure of the coatings was characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). The properties of the coatings including bond strength, thickness, thermal shock resistance and corrosion resistance varying with the quantities of titania powers in the electrolytes were studied. Investigation results revealed that the coating obtained in silicate electrolyte was composed of anatase-TiO₂, rutile-TiO₂ crystal phases and some Fe, Si, P elements; coating obtained in aluminate electrolyte consisted of anatase-TiO₂, Al₂TiO₅ and some Fe, P elements. Coatings obtained in two types of electrolytes show porous and rough surface. With increasing the concentration of titania powers in the electrolytes, the coating surface first became more compact and less porous and then became more porous and coarse. The bond strength and thickness were not strongly affected by concentration of titania powers in electrolytes. The valves were 23 MPa and for 66 μm for coatings obtained in aluminate electrolyte, and 21 MPa and 35 μm for coatings obtained in silicate electrolyte. Coatings obtained in silicate electrolyte showed a little better thermal shock resistance than those obtained in aluminate electrolyte and the best coatings were obtained with middle concentration of titania powers in the electrolytes. All coated samples showed better corrosion resistance than the substrate in 3.5 wt% NaCl solution. The best coatings were also obtained with middle concentration of titania powers doping in both electrolytes whose corrosion current density was decreased by 2 orders of magnitude compared with the substrate.     

One-dimensional and quasi-one-dimensional ZnO nanostructures prepared by spray-pyrolysis-assisted thermal evaporation

One-dimensional (1D) and quasi-1D ZnO nanostructures have been fabricated by a kind of new spray-pyrolysis-assisted thermal evaporation method. Pure ZnO powder serves as an evaporation source. Thus-obtained products have been characterized by X-ray diffraction (XRD) analysis, scanning electron microscope (SEM) equipped with energy dispersive X-ray spectroscopy (EDS), transmission electron microscope (TEM). The room temperature photoluminescence spectrum of these ZnO nanostructures is presented. The results show that as-grown ZnO nanomaterials have a hexagonal wurtzite crystalline structure. Besides nanosaws, nanobelts and nanowires, complex ZnO nanotrees have also been observed in synthesized products. The study provides a new simple route to construct 1D and quasi-1D ZnO nanomaterials, which can probably be extended to fabricate other oxide nanomaterials with high melting point and doped oxide nanomaterials.     

The determination of calcium concentrations in human milk with energy dispersive X-ray fluorescence

This work reports on an alternative method for the determination of element concentrations in human milk. Energy dispersive X-ray fluorescence (EDXRF) spectrometer with an annular Am²⁴¹ and Fe⁵⁵ sources was applied for the analysis of human milk samples. A sample preparation method suitable for the EDXRF analysis was described. The results were presented in Table 1. Energy dispersive X-ray fluorescence technique has been successfully used for the determination of calcium and other elements in human milk. For this reason, the experimental approach and the analytical method used in this study appear adequate for the purpose and can therefore be exploited for similar investigations.     

On the possibility of elemental analysis of solid crystals by the X-ray diffraction method

A new method of elemental analysis of solid crystals by the X-ray diffraction method is proposed. The possibility of application of this method to multicomponent polymorphic systems (including a wide range of elements being analyzed and quantitative determination of their mass concentrations without using an external or internal standard) is demonstrated for natural aluminum silicate and titanium oxide samples as examples.     

燃煤含铁矿物的迁移转化特性研究

采用场发射扫描电镜结合X射线能谱分析仪(FSEM-EDX)系统研究了燃煤电站静电除尘器下各电场飞灰中磁珠的显微结构和化学组成,并利用热力学软件FACT计算预测了煤中含铁矿物的迁移转化过程．结果表明,外在含铁矿物在燃煤过程中易直接氧化形成结晶程度较好的铁氧化物相;内在含铁矿物与其他矿物在高温下熔合形成含Fe、Al、 Si的复杂的玻璃相,煤中含铁矿物的赋存特征、反应温度和气氛是影响含铁矿物迁移转化的主要因素。燃煤过程中Fe2 中间产物的形成以及Fe-O-S共熔体在炉内的长时间停留是结渣形成的重要原因。     

Elemental analysis of trace elements in fly ash sample of Yata?an thermal power plants using EDXRF

Fly ash samples collected by means of an electrostatic precipitator from the lignite-fired Yata?an Power Plants of the located in Turkey was analysed using X-ray fluorescence technique. Five trace elements, namely Nd, Ba, Sr, Mo and As were quantified using XRF. These concentration values can be helpful in developing a environmental pollution abatement approach for various applications of fly ash such as cement manufacture, wastewater treatment, lightweight contraction aggregate, ceramic production, and secondary source in recovery of valuable elements. Present results compared with results of the Kemerkoy thermal power plants [?ahin Y, Karabulut A, Budak G. A practical method for the analysis of overlepped peaks in energy dispersive X-ray spectra. Appl Spectrosc Rev 1996;31:333-45].     

Semi-empirical determination of Kα1,2, Kβ1,3, and Kβ2,4 X-ray natural line widths for various elements between 29 ≤ Z ≤ 74 at 123.6 keV

Abstract

In this study, K_α1,2, K_β1,3, and K_β2,4 X-ray natural line widths for various elements were determined semi-empirically at 123.6?keV by using K shell fluorescence yields obtained from energy dispersive X-ray fluorescence measurements. The obtained results contribute to a database for the development of new theoretical models of atomic structure, radiation shielding materials, and designing new technological devices related to the structural analysis of materials. The obtained results were compared with the literature, while new fitting polynomials for the studied parameters were acquired. The results showed that the natural linewidths of K X-ray lines fit fourth-order polynomials except for K_β2,4.     

西南印度洋超慢速扩张脊海底热液硫化物中金银矿物的富集特征及富集机制研究

通过电感耦合等离子体光谱仪(ICP-AES)以及扫描电镜等手段对超慢速扩张的西南印度洋中脊热液区的3个硫化物样品的金银含量及其赋存状态进行了研究。通过ICP-AES测定金银含量,结果发现3个样品均有Au和Ag富集的现象。通过能谱-扫描电镜联用(SEM/EDS),在三个样品中发现了大量的金银矿物。其中S27-4中,主要以不规则粒状的银金矿和自然金的形式赋存于硫化物中或者晶粒之间,而S35-22中,则发现了大量的银矿物和部分银金矿。能谱分析表明银矿物中常伴随有一定量的卤族元素,推测以卤化银的形式存在,银金矿除了以粒间金赋存还可以呈乳滴状被吸附在黄铁矿表面或者晶棱上,推测与黄铁矿表面缺陷有关。S35-17样品中银金矿是唯一被发现的矿物相,以包体金、吸附金和间隙金形式赋存。由于不同样品中,银金矿的摩尔比有所不同,指示形成环境有所不同。研究结果表明,S27-4的成矿流体中,Ag主要以AgCl-₂络合物迁移,Au经历了以AuCl-₂络合物到AuHS0络合物为主的转变,指示了其温度从中高温到中低温的变化过程,说明了传导冷却在这个变化过程中有重要作用。S35-22中金银矿物的形成也具有类似的富集机制,但S35-22中卤化银的形成显示了早期高温高氯度的流体环境。而黑烟囱样品S35-17中银金矿的形成则与热液流体与海水的混合作用有密切关系。     

Synthesis of aligned GaN nanorods on Si (111) by molecular beam epitaxy

Straight and well-aligned GaN nanorods have been successfully synthesized by molecular beam epitaxy (MBE) method. The GaN nanorods have been characterized by field-emission scanning electron microscopy (FE-SEM) equipped with energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). SEM images show that GaN nanorods are constituted with two parts of which shapes are different from each other. The upper part of the nanorod is very thin and its lower part is relatively thick. The XRD and EDS analysis have identified that the nanorods are pure hexagonal GaN with single crystalline wurtzite structure. The TEM images indicate that the nanorods are well crystallized and nearly free from defects. The XRD, HRTEM, and SAED pattern reveal that the growth direction of GaN nanorods is 〈0001〉. The photoluminescence (PL) spectra indicate the good emission property for the nanorods. Finally, we have demonstrated about the two-step growth of the nanorods. PACS 81.07.Bc; 81.05.Ea; 81.15.Hi     

白云鄂博天然钕独居石的振动光谱研究(英文)

Raman, infrared and energy dispersive X-ray spectra of monazites have been measured and discussed. The result shows that the mineral is enriched in cerium, lanthanum,neodymium and praseodymium (Ce＞La＞Nd＞Pr)， The monazites have marked spectral characteristics, especially their v1, V3 Raman bands and v1, v4 infrared absorption bands. The characteristics can distinguish between monazite and other phosphate minerals. In addition, based on EDS and infrared absorption spectra, a small amount of fluoro-carbonate is found in the monazites.     

Microstructures and properties of plasma sprayed FeAl/CeO2/ZrO2 nano-composite coating

Commercial FeAl powders and ZrO₂ nano-particles as well as CeO₂ additive were reconstituted into a novel multi-compositional feedstock powders via spray drying. The resulting feedstock powders were used to deposit FeAl/CeO₂/ZrO₂ nano-composite coating by plasma spraying on 1Cr18Ni9Ti stainless steel. An X-ray diffractometer (XRD), a scanning electron microscope equipped with an energy dispersive spectrometer (SEM/EDS), and a field emission scanning electron microscope equipped with an energy dispersive spectrometer (FESEM/EDS) were employed to characterize the microstructure of the as-prepared feedstock powders and nano-composite coating. At the same time, the mechanical properties and friction and wear behavior of the nano-composite coating and pure FeAl coating were comparatively evaluated by using a Vickers microindentation tester and ball-on-disk sliding wear tribotester, respectively. And the wear mechanisms for the two types of coatings are discussed in terms of their microstructure and mechanical properties. Results indicate that the nano-composite coating has a much higher hardness and fracture toughness as well as drastically increased wear resistance than pure FeAl coating, which could be mainly attributed to the reinforcing effect of ZrO₂ nano-particles and partially attributed to the refining effect of CeO₂ in the nano-composite coating.     

波长与能量色散复合式X射线荧光光谱仪特性研究及矿区土壤分析

波长与能量色散(WD-ED)复合式X射线荧光(XRF)光谱仪是一型国际上新近研发的XRF光谱仪。该研究比较了此型光谱仪的特性,建立了联用分析方法,并用不确定度对所建方法进行了评估,证明WD-EDXRF复合型光谱仪及其所建分析方法可用于土壤样品中主、次、痕量元素定量测定,并兼具了WD和ED各自的优点。研究表明：(1)对土壤质量和生态环境评价中具有重要意义的Mg,Al,P和K等元素,因WDXRF对轻元素具有更高灵敏度,故采用该型光谱仪和所建方法,可弥补单一采用ED方法的不足,从而为土壤质量和生态环境评价提供了更为灵敏和准确可靠的分析技术手段;(2)在本方法实验条件下,采用WDXRF测定,主元素Na₂O,MgO,Al₂O₃,P₂O₅,K₂O的检出限优于EDXRF,而SiO₂, SO₃, CaO, MnO, Fe₂O₃则是由EDXRF测定的检出限更优。对于谱线重叠较严重的微量元素,多数情况下WDXRF的检出限更低;(3)对主元素而言,总体上K及其原子序数之前的轻元素WDXRF准确度更好,Ca及其之后的元素EDXRF准确度更好。然而,由WDXRF和EDXRF获得的准确度也与样品相关,在某些情况下,EDXRF测定K的准确度会更好。微量元素和重叠干扰比较大的元素,采用分辨率好的WDXRF可获得更好的准确度;对于受其他元素谱线重叠影响较小的元素,EDXRF给出的结果准确度更好;(4)选用添加石蜡粘结剂的粉末压片法,利用该方法制成的地质样品粉末压片结实、无脱落,未观察到掉渣、掉粉现象,且分析准确度和精密度良好;(5)利用所建立的WD-EDXRF方法测定了采自集中开采矿区和附近河流及河漫滩沉积物,揭示矿区表层土含有较高浓度的Cu,Pb和Zn,可为找矿提供指示信息;(6)进行了矿区周边农田土壤分析,获得了元素分布趋势图,揭示矿集区附近农田土壤Pb和As等浓度较高,需要采取必要的生态与环境保护措施,以减小和避免对于人类健康的潜在影响。     

Characterization of laser sealed coatings of yttria partially stabilized zirconia

The present paper reports an experimental investigation based on X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), and wavelength dispersive spectroscopy (WDS) analyses of phases formed after laser sealing of plasma sprayed coatings of 8.5 wt% yttria partially stabilized zirconia (YPSZ). X-ray diffraction and X-ray step-scanning analyses showed that the plasma sprayed and sealed coatings consisted mainly of t′ phase with a very small amount of monoclinic phase (m phase) in the plasma sprayed coatings. It was also found that the small amounts of m and cubic phases (c phase) present in the sealed coatings were dependent on laser processing specific energies (specific energy is equal to laser power/traverse speed x beam diameter). It was also found that rhombohedral (r) phase formed after laser sealing of coatings at higher specific energies. A direct relationship between c/a ratio of transformable tetragonal phase (t phase) produced by thermal treatment of sealed coatings and nontransformable tetragonal phase (t′ phase) and the amount of Yttria was obtained. A new equation was derived, which describes the relationship between Yttria concentration and the c/a ratio of tetragonal phases (t or t′).     

Improved biological performance of low modulus Ti-24Nb-4Zr-7.9Sn implants due to surface modification by anodic oxidation

Dental implants are usually made from commercially pure titanium or titanium alloys. The purpose of this study was to evaluate the influence of surface treatment to low modulus Ti-24Nb-4Zr-7.9Sn (TNZS) on cell and bone responses. The TNZS alloy samples were modified using anodic oxidation (AD). Surface oxide properties were characterized by using various surface analytic techniques, involving scanning electron microscopy (SEM) equipped with energy dispersive spectrometer (EDS), X-ray diffractometry (XRD) and surface profilometer. During the AD treatment, porous titanium oxide layer was formed and Ca ions were incorporated into the oxide layer. The viability and morphology of osteoblasts on Ca-incorporated TNZS were studied. The bone responses of Ca-incorporated TNZS were evaluated by pull-out tests and morphological analysis after implantation in rabbit tibiae. The non-treated Ti and TNZS samples were used as the control. Significant increases in cell viability and pull-out forces (p < 0.05) were observed for Ca-incorporated TNZS implants compared with those for the control groups. Porous structures supplied positive guidance cues for osteoblasts to attach. The enhanced cell and bone responses to Ca-incorporated TNZS implants could be explained by the surface chemistry and microtopography.     

In-depth micro-spectrochemical analysis of archaeological Egyptian pottery shards

Old Egyptian pottery samples have been in-depth microchemically analyzed using laser induced breakdown spectroscopy (LIBS), energy dispersive X-ray (EDX), and X-ray diffraction (XRD) techniques. Samples from two different ancient Islamic eras, Mamluk (1250–1517 AD), Fatimid (969–1169 AD) in addition to samples from the Roman period (30 BC–395 AD) were investigated. LIBS provided the analytical data necessary to study in micrometric steps the depth profiling of various elements in each sample. Common elements such as silicon, calcium, and aluminum relevant to the originally manufactured and processed clay, showed up in all the investigated samples. EDX and XRD techniques that have been used in the present work provided important chemical insight about the structure of the samples. The obtained analytical results demonstrated the possibility of using LIBS technique in performing in situ spectrochemical analysis of archaeological pottery. This leads to fast in-depth spatial characterization of the samples in the micron range with nearly invisible surface destructive effects. There is no doubt that this can help in restoration and conservation of such precious objects.