扫描电子显微分析仪模拟系统

扫描电子显微分析仪是研究物质微观形貌的大型组合式仪器。扫描电子显微分析仪模拟系统(SSEM)能模拟扫描电子显微分析仪的基本原理、仪器结构、样品制备和操作过程,SSEM是在AppleⅡ微机上采用浮点BASIC语言开发的软件系统,具有较强的交互功能,操作方便灵活。由于采用了计算机图形显示技术,特别是动画技术,因而能形象逼真地模拟扫描电子显微分析仪操作的全过程。

一种提高扫描电子显微镜-能谱空间分辨率的方法

目前,扫描电子显微镜-能谱（SEM-EDS）联用技术在分析测试领域已得到广泛应用,它可对材料和生物样品的微观表面进行形貌观察,并对样品中所选定的微区内进行元素成分定性定量以及元素分布分析。但是,由于元素的特征X射线能量高,在样品中的出射范围较深,能谱的空间分辨率较差,导致在使用传统制样方法时都不可避免地会受到来自叠加样品特征X射线以及基底材料特征X射线的干扰,从而影响最终实验结果。为了克服能谱空间分辨率不足的问题,本文应用薄片法的原理研制了一种新的装置,将纳米厚度的样品分散在装置的碳膜上,进行能谱分析。通过与传统实验的对比,附加新装置后其能谱空间分辨率较以往常规实验提高了2~4倍。

正电子发射计算机断层扫描显像仪屏蔽设计和辐射防护

目的建立正电子发射计算机断层扫描显像仪(PET/CT)的辐射防护和屏蔽设计规范。方法依据国际国内相关规范、标准,通过对日常工作中的PET/CT工作场所的屏蔽设计实例,探讨分析其屏蔽设计要求和辐射防护情况。结果参考美国物理师协会关于PET/CT的防护设计报告,计算得出场所的屏蔽设计要求,提出相关辐射防护措施的建议。结论加强屏蔽设计和辐射防护措施,能有效降低工作人员和公众的受照剂量。

基于FIB加工和SEM-EDS技术联用对共格BCC/B2高熵合金的元素分布表征分析

BCC/B2高熵合金中体心立方结构(body centered cube, BCC)纳米粒子影响其软磁性能和高温力学性能。然而,扫描电子显微镜-能量色散谱仪(scanning electron microscopy-X-ray energy dispersive spectroscopy, SEM-EDS)难以表征BCC纳米粒子的元素分布。本文利用聚焦离子束(focused ion beam, FIB)和SEM-EDS联用,制备BCC/B2高熵合金的纳米尺度薄片,并对其元素分布进行了研究。结果表明,AlCoFeCr高熵合金微观组织是由B2相与共格的BCC相构成,其中BCC粒子约为20~40 nm。对比SEM-EDS对块体试样和FIB制备的纳米尺度的薄片元素分布结果,FIB制备的纳米薄片提高了EDS的分辨率,BCC纳米粒子富集Cr元素,且B2基体相富集Al、Co和Fe元素。电子的加速电压和束流强度影响纳米薄片中BCC纳米粒子元素分布表征结果的准确性,其中30 kV 6.4 nA下元素分布表征结果的准确度最高。

生石膏加固软土的试验研究

为了揭示生石膏加固软土的固化机理和强度增长规律,利用扫描电子显微仪试验及无侧限抗压强度试验从微观上研究了生石膏加固软土的固化效果。研究认为,随着固化剂中生石膏掺量增加,固化土强度先增加后降低,即生石膏的掺入量存在最优值并从理论上推导出固化剂中生石膏最佳掺量的计算公式,通过算例验证了该公式的适用性;分析了生石膏与各种添加剂的相容性。为生石膏应用于软土固化提供了理论基础。

Tribological Performances of Fatty Acyl Amino Acids Used as Green Additives in Lubricating Oil

The friction and wear characteristics of lauroyl glutamine, lauroyl glycine and lauroyl alanine, used as green additives in HVI 350 mineral lubricating oil, were evaluated on a four-ball tribotester. The morphologies and chemical species of the worn surfaces were analyzed by scanning electron microscope （SEM） and X-ray photoelectron spectroscope （XPS）, respectively. The test results indicated that the three fatty acyl amino acids could effectively improve the anti-wear and friction-reducing abilities of the HVI 350 mineral oil. The improvement in anti-wear and friction-reducing abilities of the mineral oil by the related amino acids was mainly ascribed to the formation of a composite boundary lubrication film due to the adsorption of amino acids on the friction surfaces.

A Facile Route for Synthesis of LiFePO_4/C Cathode Material with Nano-sized Primary Particles

A facile and practical route was introduced to prepare LiFePO4/C cathode material with nano-sized primary particles and excellent electrochemical performance. LiH2PO4 was synthesized by using H3PO4 and LiOH as raw materials. Then, as-prepared LiH2PO4, reduced iron powder andα-D-glucose were ball-milled, dried and sin-tered to prepare LiFePO4/C. X-ray diffractometry was used to characterize LiH2PO4, ball-milled product and LiFePO4/C. Differential scanning calorimeter-thermo gravimetric analysis was applied to investigate possible reac-tions in sintering and find suitable temperature for LiFePO4 formation. Scanning electron microscopy was em-ployed for the morphology of LiFePO4/C. As-prepared LiH2PO4 is characterized to be in P21cn（33） space group, which reacts with reduced iron powder to form Li3PO4, Fe3（PO4）2 and H2 in ball-milling and sintering. The appro-priate temperature for LiFePO4/C synthesis is 541.3-976.7 ℃. LiFePO4/C prepared at 700 ℃ presents nano-sized primary particles forming aggregates. Charge-discharge examination indicates that as-prepared LiFePO4/C displays appreciable discharge capacities of 145 and 131 mA·h·g^-1 at 0.1 and 1 C respectively and excellent discharge ca-pacity retention.

Microstructure and dielectric properties of Ca-Al-B-Si-O glass/Al_2O_3 composites with various alkali oxides contents

The effects of alkali oxides （Na2O and K2O addition on both the sintering behavior and dielectric properties of Ca-AI-B-Si-O glass/Al2O3 composites were investigated by Fourier transform infrared spectroscopy （FTIR）, differential scanning calorimeter （DSC）, X-ray diffractometry （XRD） and scanning electron microscopy （SEM）. The results show that the increasing amount of alkali oxides in the glass causes the decrease of [SiO4], which results in the decrease of the continuity of glass network, and leads to the decrease of the softening temperature Tf of the samples and the increasing trend of crystallization. And that deduces corresponding rise of densification, dielectric constant, dielectric loss of the low temperature co-fired ceramic （LTCC） materials and the decrease of its thermal conductivity. By contrast, the borosilicate glass/A1203 composites with 1.5% （mass fraction） alkali oxides sintered at 875 ℃ for 30 rain exhibit better properties of a bulk density of 2.79 g/cm3, a porosity of 0.48%, a 2 value of 2.28 W/（m.K）, a er value of 7.82 and a tand value of 9.1 × 10-4 （measured at 10 MHz）.

Experimental research on electromagnetic continuous casting high-speed steel composite roll

A high speed steel composite roll billet was fabricated, which is regular in shape, smooth in surface, slight in trace, compact in internal structure, free of slag inclusion, shrinkage cavity, cracks and other flaws, and good in macro quality of junction surface using a vertical continuous casting machine. The interface zone microstructure of bimetallic in billet of high speed steel composite roll was analyzed by metallurgical microscope(OM), X-ray diffractmeter(XRD), scanning electron microscopy(SEM) and energy-dispersive X-ray analysis(EDS). The results indicate that the microstructure of roll billet is composed of chilled solidified layer, dendrite zone, interfacial zone of bimetal and core material zone. The microstructure of outer shell material is composed of martensite + bainite + residual austenite + some small labyrinth-shape, small-short lath-shape, or dollop-shape eutectic carbides. The microstructure of core material is slice-shape pearlite and a little ferrite along boundary of cells. The interface region microstructure of bimetallic composite roll consists of diffusion region, chilled solidified layer and columnar grain region.

Microstructure and microwave dielectric properties of lead borosilicate glass ceramics with Al_2O_3

The effects of Al2O3 addition on both the sintering behavior and microwave dielectric properties of PbO-B203-SiO2 glass ceramics were investigated by Fourier transform infrared spectroscope （FTIR）, differential thermal analysis （DTA）, X-ray diffraction （XRD） and scanning electron microscopy （SEM）. The results show that with the increase of Al2O3 content the bands assigned to [SiO4] nearly disappear. Aluminum replaces silicon in the glass network, which is helpful for the formation of boron-oxygen rings. The increase of the transition temperature Tg and softening temperature Tf of PbO-B2O3-SiO2 glass ceramics leads to the increase of liquid phase precipitation temperature and promotes the structure stability in the glasses, and consequently contributes to the decreasing trend of crystallization. Densification and dielectric constants increase with the increase of Al2O3 content, but the dielectric loss is worsened. By contrast, the 3% （mass fraction） Al2O3-doped glass ceramics sintered at 725℃ have better properties of density p=2.72 g/cm3, dielectric constant Er=6.78, dielectric loss tan8=2.6×10^-3 （measured at 9.8 GHz）, which suggest that the glass ceramics can be applied in multilayer microwave devices requiring low sintering temperatures.

Process mineralogy of copper-nickel sulphide flotation by a cyclonic-static micro-bubble flotation column

In our study we investigated a refractory copper-nickel sulfide ore separation by using a cyclonic-static micro-bubble flotation column (FCSMC). The process mineralogy of the main products was studied. Using a scanning electron microscope-energy dispersive system (SEM-EDS) and an X-ray spectrometer the mineral category and content of samples were analyzed. By using a mineral liberation analyzer (MLA) the mineral liberation characteristics were revealed. It is shown that in roughing feed the monomers liberation degree of nickel pyrite and chalcopyrite take up 84.11% and 88.82%, respectively. In tailings, the lost nickel pyrite and chalcopyrite are mainly monomers. Therefore, strengthening the micro-fine particle recovery capacity is the key to increase recovery.

Synthesis of Li_2Fe_(0.9)Mn_(0.1)SiO_4/C composites using glucose as carbon source

Li2Fe0.9Mn0.1SiO4/C composites were synthesized by using X-ray diffractometry （XRD）, scanning electron microscopy （SEM） glucose as carbon source. The samples were characterized by and electrochemical measurements. All Li2Fe0.9Mn0.1SiO4/C composites are of the similar crystal structure. With increasing the carbon content in the range of 5%-20% （mass fraction）, the diffraction peaks in XRD patterns broaden and the particle sizes and the tap density of samples decrease. The Li2Fe0.9Mn0.1SiO4/C composites with carbon content of 14.12% show excellent electrochemical performances with an initial discharge capacity of 154.7 mA.h/g at C/16 rate, and the capacity retention remains 92.2% after 30 cycles.

Electrochemical performance of Ti^(4+)-doped LiFePO_4 synthesized by co-precipitation and post-sintering method

Ti4+-mixed FePO4·xH2O precursor was prepared by co-precipitation method,with which Ti4+ cations were added in the process of preparing FePO4·xH2O to pursue an effective and homogenous doping way.Ti4+-doped LiFePO4 was prepared by an ambient-reduction and post-sintering method using the as-prepared precursor,Li2CO3 and oxalic acid as raw materials.The samples were characterized by scanning electron microscopy (SEM),X-ray diffractometry (XRD),electrochemical impedance spectroscopy (EIS),and electrochemical charge/discharge test.Effects of Ti4+-doping and sintering temperature on the physical and electrochemical performance of LiFePO4 powders were investigated.It is noted that Ti4+-doping can improve the electrochemical performance of LiFePO4 remarkably.The Ti4+-doped sample sintered at 600 ℃ delivers an initial discharge capacity of 150,130 and 125 mA·h/g with 0.1C,1C and 2C rates,respectively,without fading after 40 cycles.

Composition change and capacitance properties of ruthenium oxide thin film

Ru O2·n H2O film was deposited on tantalum foils by electrodeposition and heat treatment using Ru Cl3·3H2O as precursor.Surface morphology, composition change and cyclic voltammetry from precursor to amorphous and crystalline RuO2·n H2O films were studied by X-ray diffractometer, Fourier transformation infrared spectrometer, differential thermal analyzer, scanning electron microscope and electrochemical analyzer, respectively. The results show that the precursor was transformed gradually from amorphous to crystalline phase with temperature. When heat treated at 300 °C for 2h, RuO2·n H2O electrode surface gains mass of2.5 mg/cm2 with specific capacitance of 782 F/g. Besides, it is found that the specific capacitance of the film decreased by roughly20% with voltage scan rate increasing from 5 to 250 m V/s.

Recovery of high specific area silica and sodium fluoride from sodium hexafluorosilicate

Sodium fluoride and high specific area silica were synthesized by using sodium hexafluorosilicate(Na2Si F6) and sodium carbonate decahydrate(Na2CO3·10H2O). The influencing factors of react temperature, contact time, sodium dodecyl sulfate(SDS) and molar ratio of Na2 Si F6 to Na2CO3·10H2O were investigated. The optimum process involves the reaction of 0.075 mol Na2 Si F6 and 150 m L, 0.225 mol Na2CO3·10H2O(molar ratio of 1:3) at 85 °C for 90 min, and 2.0×10-3 mol sodium dodecyl sulfate(SDS) as additive. The results show that the purities of Si O2 and Na F at extraction yields of 96.5% and 98.0% are 91.0% and 98.6%, respectively. The obtained Si O2 were characterized by X-ray diffraction(XRD), scanning electron microscope(SEM), Fourier transform infrared ray(FTIR), differential scanning calorimetry and thermogravimetric analysis(DSC-TGA), N2 absorption/desorption(BET) and laser particle size analyzer. The result demonstrates that Si O2 particles have a high BET surface area of 103 m2/g, and a mean grain size of 985 nm.

A Novel γ-Alumina Supported Fe-Mo Bimetallic Catalyst for Reverse Water Gas Shift Reaction

In reverse water gas shift （RWGS） reaction COa is converted to CO which in turn can be used to pro- duce beneficial chemicals such as methanol. In the present study, Mo/AlaO3, Fe/AlaO3 and Fe-Mo/Al2O3 catalysts were synthesised using impregnation method. The structures of catalysts were studied using X-ray diffraction （XRD）, Brunauer-Emmett-Teller （BET） method, inductively coupled plasma atomic emission spectrometer （ICP-AES）, temperature programmed reduction （H2-TPR）, CO chemisorption, energy dispersive X-ray （EDX） and scanning electron microscopy （SEM） techniques. Kinetic properties of all catalysts were investigated in a batch re- actor for RWGS reaction. The results indicated that Mo existence in structure of Fe-Mo/AlzO3 catalyst enhances its activity as compared to Fe/AlaO3. This enhancement is probably due to better Fe dispersion and smaller particle size of Fe species. Stability test of Fe-Mo/AlzO3 catalyst was carried out in a fixed bed reactor and a high CO yield for 60 h of time on stream was demonstrated. Fez（MoO4）3 phase was found in the structures of fresh and used catalysts. TPR results also indicate that Fez（MoO4）3 phase has low reducibility, therefore the Fe2（MoO4）3 phase significantly inhibits the reduction of the remaining Fe oxides in the catalyst, resulted in high stability of Fe-Mo/Al2O3 catalyst. Overall, this study introduces Fe-Mo/Al2O3 as a novel catalyst with high CO yield, almost no by-products and fairly stable for RWGS reaction.

Effects of Ce on microstructure of semi-continuously cast Mg-1.5Zn-0.2Zr magnesium alloy ingots

Mg-1.5Zn-0.2Zr-xCe (x=0, 0.1, 0.3, 0.5, mass fraction, %) alloys were prepared by conventional semi-continuous casting. The effect of rare earth Ce on the microstructure of Mg-1.5Zn-0.2Zr-xCe alloys was studied and the distribution of Ce was analyzed by optical microscopy (OM), X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The results indicate that Ce element exists in the form of Mg12Ce phase and has an obvious refining effect on the microstructure of test alloys. As the Ce content increases, the grain size reduces, the grain boundaries turn thinner, and the distribution of Mg12Ce precipitates becomes more and more dispersed. The Mg-1.5Zn-0.2Zr alloy with 0.3%Ce has the best refinement effect. From center to periphery of the ingot, the amount of granular precipitates in the grain reduces. In longitudinal section of the ingot, some relative long columnar grains appear.

Effects of KMnO_4 on microstructure and corrosion resistance of microarc oxidation coatings on 2024 aluminum alloy

Microarc oxidation （MAO） coatings were prepared on 2024 aluminum alloy in a Na2SiO3-KOH electrolyte with KNinO4 addition varying from 0 to 4 g/L. The microstructure and phases of the coatings were characterized by scanning electron microscopy （SEM） and X-ray diffractometry （XRD）, respectively. The corrosion resistance of MAO coatings was evaluated by electrochemical potentiodynamic polarization in 5% （mass fraction） NaCl solution. The results show that when KMnO4 is added into base electrolyte, the growth speed of oxide coatings is increased obviously. The main phase of oxide coatings is Al2O3, and the contents of MnO2 and MnEA104 phases are increased at the top of oxide coatings with increasing the concentration of KMnO4. The solute elements participate in forming the oxide coatings. When a proper concentration of KMnO4 （2.5 g/L） is added into the base solution, the micropores of the MAO coatings are small and compact, and the corrosion resistance of oxide coatings is increased largely.

Hydroxyapatite Coatings on Titanium Prepared by Electrodeposition in a Modified Simulated Body Fluid

Hydroxyapatite coatings were directly prepared on anodized titanium by electro-deposition method in a modified simulated body fluid.The configuration,structure and bioactivity of the coating were investigated with scanning electron microscopy(SEM),X-ray diffraction analyzer(XRD)and Fourier transform infrared spectros-copy(FTIR)techniques.The results demonstrated that pure and homogeneous hydroxyapatite coating can be obtained without any post-treatment.The prepared coating showed good bioactivity in simulated body fluid(SBF).The time required for a fully covered dense hydroxyapatite coatings was 4 days immersion in SBF.

Protonic and Electronic Conductivities and Hydrogen Permeation of SrCe0.95-xZrxTm0.05O3-δ（0≤x≤0.40） Membrane

Zr-substituted,Tm-doped SrCeO3（SrCe0.95-xZrxTm0.05O3-δ,0≤x≤0.40）were synthesized via citrate complexing method,and the membranes of SrCe0.95-xZrxTm0.05O3-δwere prepared by pressing followed by sintering. X-ray diffraction（XRD）was used to characterize the phase structure of sintered membrane.The microstructure of the sintered membranes was studied by scanning electron microscopy（SEM）.Protonic and electronic conductivities were measured under different circumstance.Hydrogen permeation through the SrCe0.75Zr0.20Tm0.05O3-δmembranes was carried out using gas permeation setup.Hydrogen permeation fluxes（ 2H J）of the SrCe0.75Zr0.20Tm0.05O3-δ membrane reach up to 0.042 ml·min^ -1 ·cm^-2 at H 2 partial pressure of 0.4×10 ^5 Pa at 900°C.The hydrogen permea- tion fluxes（ 2H J）obtained in this paper are slightly lower than that of SrCe0.95Tm0.05O3-δon the same orders,and Zr doping can increase chemical stability of the SrCe0.75Zr0.20Tm0.05O3-δmembranes.