超细羰基铁粉的EELS谱和微衍射分析

最近,由于在雷达吸波材料(RAM)中的应用,直径为5到50纳米的超细羰基铁粉(UFCIP)受到越来越多的重视(1,2)。本工作在JEOL-2000FX分析电子显微镜上,利用电子能量损失谱(EELS)和微衍射等方法观察和分析了直径为5～30nm超细羰基铁粉。发现绝大部分超细铁粉由α-Fe中心核和Fe_3O_4外壳组成,其中部分超细粉完全被氧化,形成空心的γ-Fe_2O_3。图1a.显示了一些空心的UFCIP微粒,图1b是这种空心微粒的微衍射花样,微束直径约为6nm。微衍射花样表明这些微粒由多晶的γ-Fe_2O_3组成。在空心微粒中没有发现α-Fe的衍射花样。

人天然牙的高分辨X线微区衍射分析

通过使用X线微区衍射法直接对人天然牙表面正常牙釉质、牙本质及龋坏组织三个测量点进行检测,以测试X’pert Pro型衍射仪对人天然牙正常和早期龋损组织晶体结构改变的检测能力。结果显示,牙磷灰石由多种物相构成,是一种生物混晶,主要物相为羟基磷灰石,龋坏组织中可能有新物相的形成。从正常牙釉质到牙本质再到龋坏组织,晶体a轴逐渐增大,c轴基本不变。晶体晶胞参数计算结果:正常牙釉a=9.550,c=6.883;正常牙本质a=9.554,c=6.883;龋坏组织a=9.558,c=6.884。晶粒尺寸计算结果:正常牙釉质D002=27.600nm;正常牙本质D002=16.561 nm;龋坏组织D002=13.163 nm。结晶性:正常牙釉质>正常牙本质>龋坏组织。结果表明采用新型高分辨X线衍射仪可以非常方便地对牙齿进行X线衍射微区分析。

NaOH表面处理前后人牙釉质和牙本质的高分辨微区衍射研究

目的:评价去蛋白处理对牙面微观结构和晶体学性能的影响。方法:选取因正畸治疗所需拔除的健康前磨牙1颗,在流水冷却下用慢速锯沿牙长轴制备剖面。借助微区衍射分析和扫描电镜检测,比较经10%NaOH溶液在40℃水浴条件下处理2 h前后样本的变化。结果:天然牙釉质不同区域的衍射谱线之间差异明显;但化学处理后,牙釉质衍射谱线间的差异减小,且牙面粗糙度增加。结论:去蛋白处理能够有效去除牙面所含的有机成分,且对牙面有机物含量较高的区域的微结构及晶体学性能改变显著。

Reservoir characteristics of Donghe well No.1 in Tarim Basin

Based on the techniques of X-ray diffraction analysis, identification of the thin sections of core cast, phys- ical analysis and scanning electron microscopy analysis, this paper studied the reservoir characteristics of the Carboniferous strata in Donghe well No.1 of Tarim region. The results show that the reservoir lithology is mainly the fine-grained quartz sandstone with ferrocalcite and pyrite, mud cement-based, the permeability concentrated in 5-40 × 10-3 μm2, a small part of the high permeability up to 150-327 ×10-3 μm2 and porosity ranged from 10% to 20%. The most part of the reservoirs is low perme- ability with a small part of the layer in moderate-high permeability. The types of reservoir space include intergranular pores, intra particle-molding pores, micro-pores and cracks, which mainly are intergranular pores with the pore diameter of 15-200 μm, 95.5μm on average. And the types of the throats are comolex with the main tvne of constricted l：hroats in this area and large contribution to the permeability.

Micromorphological Aspects of Two Forest Soils Development Derived from Igneous Rocks in Lahijan, Iran

In order to characterize various micromorphologic properties of two forest soils derived from different parent rocks in Lahijan, and use the data collected from micromorphological analysis to interpret dominant pedogenic processes. Two representative soil pedons, granite （P1） and andesitic basalt （P2） were selected in a mountain landform with northwest aspect. Samples for thin section preparation were taken from each horizon by Kubiena boxes or clods. Micromorphological analysis of soils derived from these two soil pedons in eastern part of Lahijan （northern Iran） were conducted based on the physicochemical and mineralogical data. Micromorphological properties were characterized using a polarized light microscope under plain and cross light. Thin section study indicated that the nature of the parent material clearly affected the content of clay formation. It also showed that clay accumulation in the Bt horizons was not only due to clay illuviation （argillan）, but that strong in situ weathering of primary minerals also contributed to the enrichment of clay in soils derived from andesitic basalt. Comparing the results of clay mineralogy obtained from X-ray diffraction （XRD） with microscopic studies revealed that birefringence fabric （b-fabric） of the groundmass was partly striated due to smectitic minerals in soil of andesitic basalt （Hapludalf）, whereas speckled birefringence fabric was dominant in soil of granite （Udorthent） because of the absence of these minerals. We speculate that pores of skeletal fragments or microcracks in P1 were a place for illuvial clay protection. However, the main factor for flluvial clay film disruption （striation anddeformation） was biological activity （faunal turbation and root pressure） in P1 and expandable minerals and faunal turbation in P2.

Effects of Eu_2O_3 doping on microstructural and electronic properties of ZnO Bi_2O_3-based varistor ceramics prepared by high-energy ball milling

ZnO-Bi2O3-based varistor ceramics doped with EU2O3 in a range from 0 to 0.4% were obtained by high-energy ball milling and fired at 900-1000 ℃ for 2 h. XRD and SEM were applied to determine the phases and microstructure of the varistor ceramics. A DC parameter instrument was applied to investigate the electronic properties and V-I characteristics. The XRD analysis of Eu2O3-doped ZnO-Bi2O3-based varistor ceramics shows that the ZnO, Eu-containing Bi-rich, Zn7Sb2O12-type spinel and Zn2Bi3Sb3O14-type which is the pyrochlore phase are present. With increasing Eu2O3 content, the average size of ZnO grain firstly decreases and then increases. The grain boundary defect model was particularly used to explain the excellent nonlinearity of ZnO-Bi2O3-based varistor ceramics with the addition of0.1% Eu2O3 and sintered at 950 ℃.

Sedimentary characteristics and depositional model of a Paleocene-Eocene salt lake in the Jiangling Depression,China

We studied the sedimentary characteristics of a Paleocene-Eocene salt lake in the Jiangling Depression through field core observation,thin section identification,scanning electron microscopy,and X-ray diffraction analysis.On the basis of sedimentary characteristics we have summarized the petrological and mineralogical characteristics of the salt lake and proposed 9 types of grade IV salt rhythms.The deposition shows a desalting to salting order of halite-argillaceous-mudstone-mud dolostonemud anhydrock-glauberite-halite.The relationship among grade IV rhythms,water salinity and climate fluctuations was analyzed.Based on the analysis of the relationship between boron content and mudstone color and by combining the mineralogy and sedimentary environment characteristics,we propose that the early and late Paleocene Shashi Formation in the Jiangling Depression was a paleolacustrine depositional environment with a high salt content,which is a representation of the shallow water salt lake depositional model.The middle Paleocene Shashi Formation and the early Eocene Xingouzui Formation were salt and brackish sedimentary environments with low salt content in a deep paleolake,which represents a deep salt lake depositional model.

Droplet spraying of aluminum on magnesium

An A1 coating on Mg substrate was achieved by droplet spraying treatment. The microstructure was studied by electron probe microanalysis （EPMA） and X-ray diffraction （XRD）. The coating layer is composed of AI phase and exhibits superior corrosion resistance. The formation of the coating is mainly attributed to the obstruction of expansion of the transition zone by primarily solidified Mg]7All2 during rapid cooling, and the diffusion is restricted in a thin layer. These results show that droplet spraying is a promising way to protect magnesium by using corrosion-resistant materials available now.

Optimization of High-Gravity Chelated Iron Process for Removing H_2S Based on Response Surface Methodology

By using a mixture of N2 and H2S as the simulated APG(associated petroleum gas), the desulfurization experiment was performed in a cross-flow rotating packed bed(RPB) based on the chelated iron oxidation-reduction method. In order to determine the operating conditions of the system, the effects of the concentration of Fe3+ ions(ranging from 0.1 to 0.2 mol/L), the liquid-gas volume ratio(ranging from 15 to 25 L/m3) and the high gravity factor(ranging from 36 to 126) on the removal of H2 S were studied by means of the Box-Behnken design(BBD) under response surface methodology(RSM). The overall results have demonstrated that the BBD with an experimental design can be used effectively in the optimization of the desulfurization process. The optimal conditions based on both individualized and combined responses(at a Fe3+ ion concentration of 0.16 mol/L, a liquid-gas volume ratio of 20.67 L/m3 and a high gravity factor of 87) were found. Under this optimum condition, the desulfurization efficiency could reach 98.81% when the H2 S concentration was 7 g/m3 in APG. In this work, the sulfur product was analyzed by X-ray diffraction(XRD), scanning electron microscopy(SEM) and the energy dispersive X-ray spectrometer(EDX). The results of analysis show that the sulfur is made of the high-purity orthorhombic crystals, which are advantageous to environmental conservation.

Nanocrystalline Mg and Mg alloy powders by hydriding-dehydriding processing

The process of mechanically assisted hydriding and subsequent thermal dehydriding was proposed to produce nanocrystalline Mg and Mg alloy powders using pure Mg and Mg-5.5%Zn-0.6%Zr(mass fraction)(ZK60 Mg) alloy as the starting materal.The hydriding was achieved by room-temperature reaction milling in hydrogen.The dehydriding was carried out by vacuum annealing of the as-milled powders.The microstructure and morphology of both the as-milled and subsequently dehydrided powders were characterized by X-ray diffraction analysis(XRD) ,transmission electron microscopy(TEM) ,and scanning electron microscopy(SEM) ,respectively.The results show that,by reaction milling in hydrogen,both Mg and ZK60 Mg alloy can be fully hydrided to form nanocrystalline MgH2 with an average grain size of 10 nm.After subsequent thermal dehydriding at 300℃,the MgH2 can be turned into Mg again,and the newly formed Mg grains are nanocrystallines,with an average grain size of 25 nm.

Effects of yttrium on microstructure and mechanical properties of Mg-Zn-Cu-Zr alloys

The effects of yttrium addition on microstructure and mechanical properties of as-cast Mg-6Zn-3Cu-0.6Zr-xY(x=0,0.5, 1.0,1.5 and 2.0,mass fraction,%)(ZCK630+xY for short in this study)alloys were investigated by means of OM,XRD and SEM. The results show that the average grain size of Mg-Zn-Cu-Zr magnesium alloy is effectively reduced(from 57μm to 39μm)by Y addition.The analysis of XRD indicates the existence of I-phase(Mg3Zn6Y)and W-phase(Mg3Zn3Y2)in ZCK630 alloys with Y addition.The ultimate tensile strength of ZCK630 alloys is significantly deteriorated with increasing Y addition,which is possibly related to the continuous networks of intergranular phases and the increase of W-phase.

Meso-structure and fracture mechanism of mudstone at high temperature

The meso-structure mineral composition and fracture mechanism of uniaxial compressed mudstone samples at high temperature were analyzed by XRD and scanning electron microscopy. The effect of tem- perature on mudstone composition and fracture mechanism were studied from a meso-structural per- spective, and the relationship between meso-structure and macro-mechanical characteristics at high temperature was revealed. The findings demonstrated that the fluctuation in diffraction intensity of kao- linite in the mudstone caused the fluctuation in its mechanical properties. The overall structure under- went a phase change around 600℃, which led to the sudden change in the mechanical properties of mudstone samples. When the temperature reached 600 ℃, the crystalline state worsened and kaolinite disappeared; however, some illite was produced, indicating that the chemical reaction of the structure and sudden drop of bearing capacity of the mudstone. Mudst0ne fracturing at high temperature involves mainly intergranular and transgranular fractures, which are typical in micro-brittle tensile failure. Con- sidering the macro-fracture characteristics of mudstone, the results suggested that macro-fracture under external force corresoonds to the meso-fracture.

Getting and X-ray Diffraction Analysis of the Microsphere Catalyst U, Nd on the Basis Fly Ash of Thermal Power Plants

To study the physical and chemical properties of aluminosilicate microsphere catalyst by impregnation and calcination us was first obtained aluminosilicate microsphere catalyst U, Nd for petrochemical processes. The method of X-ray structure has been studied for the microsphere catalyst U, Nd.

Effect of precipitation on internal friction of AZ91 magnesium alloy

The effect of precipitation on the internal friction(IF)of AZ91 magnesium alloy was investigated by using X-ray diffraction(XRD)analysis,scanning electron microscope(SEM)observation,and dynamic mechanical analysis(DMA).Six different states of alloy were prepared by applying different heat treatment processes:as-cast,in-complete solid solution,complete solid solution,micro-precipitation,continuous precipitation and continuous-discontinuous precipitation.It was found that the internal friction of in-completely solid-solutionized,completely solid-solutionized and micro-precipitated specimens showed a similar characteristic,and the grain boundary relaxation is completed depressed due to the Al atoms supersaturated in theα-Mg solution.However,a thermal relaxation internal friction peak was observed for continuously precipitated and continuously-discontinuously precipitated specimens at around 438 K and frequency of about 1 Hz,which was attributed to the grain boundaries relaxation.Furthermore,it was found that the relaxation of theβ-Mg17Al12/α-Mg phase interfaces should give its contribution to the background internal friction in the as-cast,continuously precipitated and continuously-discontinuously precipitated specimens.

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.

Characteristics and genesis of clay minerals in the northern margin of the Qaidam Basin

In order to develop appropriate reservoir protection measures in the northern margin of the Qaidam Basin and improve its oil and gas recovery efficiency,characteristics of clay minerals from eleven clay rock samples from the northern margin of the Qaidam Basin were investigated using X-ray diffraction analysis,the Scanning Electron Microscope（SEM）and energy spectrum analysis.Clay mineral composition and distribution characteristics of the main hydrocarbon reservoirs,i.e.,from the Jurassic and Paleogene-Neogene,were explored.We analyzed the main factors which affected these attributes.The results show that the major clay minerals in the northern margin are chlorite,kaolinite,illite,smectite and illite/smectite inter-stratified minerals.Illite is the most widely spread clay mineral in this area. Chlorite is mainly found in the entire Neogene and in shallow horizons of the Paleogene.Smectite is enriched in the shallow Paleogene-Neogene.There are large amounts of kaolinite and illite/smectite inter-stratified minerals in the Jurassic.The major factors affecting the different development of clay minerals in the region are properties of parent rocks,paleoclimate and paleowater media conditions, diagenesis transformation,tectonic and terrain conditions.

Microstructural evaluation of Hastelloy-X transient liquid phase bonded joints:Effects of filler metal thickness and holding time

Transient liquid phase(TLP)bonding was investigated in Hastelloy-X samples with different filler metal thicknesses(20,35,50,65,and 100μm)and holding time(5,20,80,320,and 640 min)to obtain optimum bonding parameters.Microstructural evaluations using electron probe microanalysis(EPMA)and electron backscattered diffraction(EBSD)show that the central eutectic phases present in the athermally solidified zone(ASZ)are Ni_(3)B,Ni_(2)Si,and CrB,and the precipitates formed in the diffusion-affected zone(DAZ)are MoB,CrB_(2),and Mo_(2)B_(5).According to the results,decreasing the filler thickness as well as increasing the holding time helps realize the completion of isothermal solidification and reduction in the density of precipitates in the DAZ,leading to a joint with more uniform properties.Diffusion of boron and silicon to longer distances with increasing holding time causes the removal of Cr-rich borides in the DAZ and the formation of Mo-rich silicide at the joint interface.Decrease in hardness of ASZ and DAZ due to the elimination of brittle phases in these zones during long holding time causes more uniform hardness distribution in the joint area.The best results are obtained for the sample joined with the 35μm-thick filler metal for 640 min holding time.

Properties of CNTs/MoSi2 composites prepared by spark plasma sintering

Molybdenum disilicide(MoSi_2) based composites with various contents of carbon nanotubes(CNTs) were fabricated by spark plasma sintering(SPS) in vacuum under a pressure of 25 MPa.The composites obtained under a sintering temperature of 1500 °C and time of 10 min exhibited optimum mechanical properties at room temperature in terms of fracture toughness and transverse rupture strength.MoSi_2 based composite with 6.0% CNTs(volume fraction) had the highest fracture toughness,transverse rupture strength and hardness,which were improved by about 25.7%,51.5% and 24.4% respectively,as compared with pure MoSi_2.A Mo_(4.8)Si_3C_(0.6) phase was detected in CNTs/MoSi_2 composites by both X-ray diffraction(XRD) method and microstructure analysis with scanning electron microscopy(SEM).It is believed that the fine grains and well dispersed small Mo_(4.8)Si_3C_(0.6) particles had led to a higher hardness and strength of CNTs/MoSi_2 composites because of their particle pullout,crack deflection and micro-bridging effects.

Synthesis and Structural Characterization of Sm-Sr Nickelates

The main purpose of this work was to obtain Sm-Sr nickelates nanoparticles with Ruddelsden-Popper type structures obtained by a simple process such as gelatin synthesis. The powders were calcinated at 900 ℃ and characterized by X-ray diffraction, thermogravimetric analysis, scanning electron microscopy and high-resolution transmission electron microscopy techniques. The effect of chemical substitution of the Sm^3＋ by Sr^2＋ ions on the structural properties of the powders was studied. The Rietveld＇s method was successfully applied for determination of the quantitative phase analysis of the powders and revealed that the main phase of the powders for different strontium content is of Ruddelsden-Popper type structure. A symmetry change from orthorhombic to tetragonal is observed as increasing strontium.

Preparation High-Temperature Behavior of Conversion Coating of Alumina Film on FeCrAI （Ce） Stainless Steel

FeCrAI （Ce） stainless steel was functionalized by a conversion treatment in order to allow alumina by diffusion coatings with strong interfacial bonding. The very porous conversion coating produced in a pack aluminization technique had excellent adhesion and was conductive enough to permit conditions favorable for the precipitation of alumina oxyhydroxide during aluminum diffusion coatings. In this work, the bed was prepared as a mixture of A1, NH4C1 and A1203. In the high-activity bed were heat-treated at 1,173 K in an atmosphere made up of team with subsequent air-cooling. The effect of the bed content on the coating was examined. With the high-activity, the desired Fe2Al5 was formed as the outermost coating layer. The coating presented chemical composition gradients suitable for strong adhesion. The improvement of the thermal oxidation behaviour was studied at 1,373 K. Two different aqueous environments, which are （1） NaC1 and （2） H2SO4, are employed for using the technique of potentiodynamic polarization curve. The obtained experimental electrochemical parameters （Ecorr, Jcorr etc,） were used to compare the corrosion resistance of the tested steel state complemented by MEB （electronic scanning microscopy） in combination with dispersive analysis X in energy （EDS） or X ray diffraction indicated that the elements concentration maximum was located in the vicinity of the interface especially in the FeCrAI （Ce） coated by spherical A1203 powder. These results an discussed in terms of an addition effect on the development of the microstructure of oxide films.