Characterization of Average Molecular Structure of Heavy Oil Fractions by ~1H Nuclear Magnetic Resonance and X-ray Diffraction

The chemical structure of heavy oil fractions obtained by liquid-solid adsorption chromatography was character-ized by 1 H nuclear magnetic resonance and X-ray diffraction.The molecular weight and molecular formula of asphaltene molecules were estimated by combining 1 H nuclear magnetic resonance and X-ray diffraction analyses,and were also ob-tained from vapor pressure osmometry and elemental analysis.Heteroatoms,such as S,N,and O atoms,were considered in the construction of average molecular structure of heavy oils.Two important structural parameters were proposed,including the number of alkyl chain substituents to aromatic rings and the number of total rings with heteroatoms.Ultimately,the av-erage molecular structures of polycyclic aromatics,heavy resins and asphaltene molecules were constructed.The number of α-,β-,γ-,and aromatic hydrogen atoms of the constructed average molecular structures fits well with the number of hydro-gen atoms derived from the experimental spectral data.

Fitting Full X-Ray Diffraction Patterns for Quantitative Analysis: A Method for Readily Quantifying Crystalline and Disordered Phases

Fitting of full X-ray diffraction patterns is an effective method for quantifying abundances during X-ray diffraction (XRD) analyses. The method is based on the principal that the observed diffraction pattern is the sum of the individual phases that compose the sample. By adding an internal standard (usually corundum) to both the observed patterns and to those for individual pure phases (standards), all patterns can all be normalized to an equivalent intensity based on the internal standard intensity. Using least-squares refinement, the individual phase proportions are varied until an optimal match is reached. As the fitting of full patterns uses the entire pattern, including background, disordered and amorphous phases are explicitly considered as individual phases, with their individual intensity profiles or “amorphous humps” included in the refinement. The method can be applied not only to samples that contain well-ordered materials, but it is particularly well suited for samples containing amorphous and/or disordered materials. In cases with extremely disordered materials where no crystal structure is available for Rietveld refinement or there is no unique intensity area that can be measured for a traditional RIR analysis, full-pattern fitting may be the best or only way to readily obtain quantitative results. This approach is also applicable in cases where there are several coexisting highly disordered phases. As all phases are considered as discrete individual components, abundances are not constrained to sum to 100%.

X-Ray Diffraction, Electron Paramagnetic Resonance and Optical Absorption Study of Bauxite

The bauxite mineral obtained from Araku, Vishakapatnam district of Andhra Pradesh, India is used in the present work. Structural characterization was performed by X-ray diffraction (XRD). The mineral was found to be gibbsite in phase. The transitional metal ions present were investigated using electron paramagnetic resonance (EPR) and optical absorption spectra. The EPR results suggest that Fe3+ has replaced Al3+ in the unit cell of bauxite. The optical absorption spectrum is due to Fe3+ which indicates that it is in distorted octahedral environment. The near-infrared (NIR) spectrum is due to water fundamentals and combination overtones, which confirm the formula of the compound. The impurities in the mineral are identified using spectroscopic techniques.

Crystallographic Characteristic of Intermetallic Compounds in Al-Si-Mg Casting Alloys Using Electron Backscatter Diffraction

The Al-Si-Mg alloy which can be strengthened by heat treatment is widely applied to the key components of aerospace and aeronautics. Iron-rich intermetallic compounds are well known to be strongly influential on mechanical properties in Al-Si-Mg alloys. But intermetallic compounds in cast Al-Si-Mg alloy intermetallics are often misidentified in previous metallurgical studies. It was described as many different compounds, such as AlFeSi, Al8Fe2Si, Al5（Fe, Mn）3Si2 and so on. For the purpose of solving this problem, the intermetallic compounds in cast Al-Si alloys containing 0.5% Mg were investigated in this study. The iron-rich compounds in Al-Si-Mg casting alloys were characterized by optical microscope（OM）, scanning electron microscope（SEM）, energy dispersive X-ray spectrometer（EDS）, electron backscatter diffraction（EBSD） and X-ray powder diffraction（XRD）. The electron backscatter diffraction patterns were used to assess the crystallographic characteristics of intermetallic compounds. The compound which contains Fe/Mg-rich particles with coarse morphologies was Al8FeMg3Si6 in the alloy by using EBSD. The compound belongs to hexagonal system, space group P6_2m, with the lattice parameter a=0.662 nm, c=0.792 nm. The β-phase is indexed as tetragonal Al3FeSi2, space group I4/mcm, a=0.607 nm and c=0.950 nm. The XRD data indicate that Al8FeMg3Si6 and Al3FeSi2 are present in the microstructure of Al-7Si-Mg alloy, which confirms the identification result of EBSD. The present study identified the iron-rich compound in Al-Si-Mg alloy, which provides a reliable method to identify the intermetallic compounds in short time in Al-Si-Mg alloy. Study results are helpful for identification of complex compounds in alloys.

Measurement of integral diffraction coefficients of crystals on beamline 4B7 of Beijing Synchrotron Radiation Facility

Integral diffraction coefficients of the crystal are the essential data of a crystal spectrometer which is extensively used to measure quantitative x-ray spectra of high temperature plasmas in kilo-electron-volt region. An experimental method has been developed to measure the integral diffraction coefficients of crystals on beamline 4B7 of Beijing Synchrotron Radiation Facility. The integral diffraction coefficients of several crystals including polyethylene terephthalate （PET）, thallium acid phthalate （T1AP） and rubidium acid phthalate （RAP） crystals have been measured in the x-ray energy range 2100-5600 eV and compared with the calculations of the ＇Darwin Prins＇ and the ＇Mosaic＇ models. It is shown that the integral diffraction coefficients of these crystals are between the calculations of the ＇Darwin Prins＇ and the ＇Mosaic＇ models, but more close to the ＇Darwin Prins＇ model calculations.

Microstructural origins of high strength of Al-Si alloy manufactured by laser powder bed fusion:In-situ synchrotron radiation X-ray diffraction approach

The microstructural factors contributing to the high strength of additive-manufactured Al-Si alloys us-ing laser-beam powder bed fusion(PBF-LB)were identified by in-situ synchrotron X-ray diffraction in tensile deformation and transmission electron microscopy.PBF-LB and heat treatment were employed to manufacture Al-12%Si binary alloy specimens with different microstructures.At an early stage of de-formation prior to macroscopic yielding,stress was dominantly partitioned into the α-Al matrix,rather than the Si phase in all specimens.Highly concentrated Si solute(~3%)in the α-Al matrix promoted the dynamic precipitation of nanoscale Si phase during loading,thereby increasing the yield strength.After macroscopic yielding,the partitioned stress in the Si phase monotonically increased in the strain-hardening regime with an increase in the dislocation density in the α-Al matrix.At a later stage of strain hardening,the flow curves of the partitioned stress in the Si phase yielded stress relaxation owing to plastic deformation.Therefore,Si-phase particles localized along the cell walls in the cellular-solidified microstructure play a significant role in dislocation obstacles for strain hardening.Compared with the results of the heat-treated specimens with different microstructural factors,the dominant strengthening factors of PBF-LB manufactured Al-Si alloys were discussed.

In situ observation of the phase transformation kinetics of bismuth during shock release

A time-resolved x-ray diffraction technique is employed to monitor the structural transformation of laser-shocked bismuth.Results reveal a retarded transformation from the shock-induced Bi-Ⅴphase to a metastable Bi-Ⅳphase during the shock release,instead of the thermodynamically stable Bi-Ⅲphase.The emergence of the metastable Bi-Ⅳphase is understood by the competitive interplay between two transformation pathways towards the Bi-Ⅳand Bi-Ⅲ,respectively.The former is more rapid than the latter because the Bi-Ⅴto B-Ⅳtransformation is driven by interaction between the closest atoms while the Bi-Ⅴto B-Ⅲtransformation requires interaction between the second-closest atoms.The nucleation time for the Bi-Ⅴto Bi-Ⅳtransformation is determined to be 5.1±0.9 ns according to a classical nucleation model.This observation demonstrates the importance of the formation of the transient metastable phases,which can change the phase transformation pathway in a dynamic process.

Method for Measuring Residual Stresses Induced by Boring in Internal Surface of Tube and Its Validation with XRD Method

Residual stresses can have a strong effect on the usability of machined parts,and the X-ray diffraction(XRD)measuring equipment,which is commonly used to measure residual stresses,is very expensive.This paper presents a method of measuring the residual stresses induced by boring in the internal surface of a tube with much cheaper equipment.The method,called the strain-based method is mainly based on the strains measured on the external surface of the tube.It is proposed on the basis of the very long tube assumption.The finite element method(FEM)analysis is thus used to validate the length of the tube.Guided by the FEM results,an appropriate length of the tube is chosen,and the residual stresses are obtained from both the strain-based method and the XRD method.Stress profiles obtained from both two methods are compared.The comparison result indicates that the profiles of the two methods agree well with each other.Therefore,it can be concluded that the accuracy of the strain-based method is high enough,and it can be applied to residual stress measurement in practice.

Understanding the influence of petrographic parameters on strength of differently sized shale specimens using XRD and SEM

Ground failure is a major contributor to fatalities in underground mines in the US.Underground coal mines in the Northern Appalachian have weak roof rock composed of shale,which is prone to failure under high horizontal stress.Understanding the relationship among strength,specimen size and rock petrographic parameters is essential for developing an effective ground control plan.Size effect studies have found that rock strength varies with specimen size.This paper attempts to understand this strength variation using three specimen sizes(254-mm,508-mm,and 762-mm).The specimen strength was measured and the major petrographic parameters affecting the strength,namely grain size,grain shape,quartz content,clay content,etc.were analyzed using X-ray diffraction(XRD)and scanning electron microscopy(SEM).The petrographic parameters were then correlated with the strength of the three differently sized specimens.The results showed that 508-mm specimen had the lowest strength.Quartz content of the 508-mm specimen was lower than that of 254-mm and 762-mm specimens.Clay content and average grain size of the 508-mm specimen were higher than those of 254-mm and 762-mm specimens.These results clearly show that grain size,quartz content and clay content contribute to strength variation observed in differently sized shale specimens.

X-Ray Analysis by Williamson-Hall and Size-Strain Plot Methods of ZnO Nanoparticles with Fuel Variation

In this paper, a simple and facile surfactant assisted combustion synthesis is reported for the ZnO nanoparticles. The synthesis of ZnO-NPs has been done with the assistance of non-ionic surfactant TWEEN 80. The effect of fuel variations and comparative study of fuel urea and glycine have been studied by using characterization techniques like X-ray diffraction (XRD), transmission electron microscope (TEM) and particle size analyzer. From XRD, it indicates the presence of hexagonal wurtzite structure for ZnO-NPs. Using X-ray broadening, crystallite sizes and lattice strain on the peak broadening of ZnO-NPs were studied by using Williamson-Hall (W-H) analysis and size-strain plot. Strain, stress and energy density parameters were calculated for the XRD peaks of all the samples using (UDM), uniform stress deformation model (USDM), uniform deformation energy density model (UDEDM) and by the size-strain plot method (SSP). The results of mean particle size showed an inter correlation with W-H analysis, SSP, particle analyzer and TEM results.

Preparation of Organic Semiconductor PTCDA and Studies on Its Crystal Structure and the Absorption Spectrum

Organic semiconductoe 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA) has been synthetized with 1,8-naphthalic anhydride using chemical method.X-ray diffraction spectrum shows that it is monoclinic.Visible absorption spectrum shows that its gap band is 2.2 eV with singlet exciton bandwidth of 0.9 eV.

A combined IR and XRD study of natural well crystalline goethites(α-FeOOH)

Goethite(a-FeOOH)is one of the most abundant minerals on the Earth surface,occurring in temperate,tropical and equatorial climates.Fe in goethite can be substituted by many cations such as Al,Ni for instance.A large amount of research has been conducted on the effect of varying elemental compositions(mainly Al-content)on the spectral features of goethites with most of the studies based on materials synthesized with different elemental ratios.The different elemental ratios,however,may not only affect the composition of the products but also their crystallinity and/or particle size and shape.Both parameters are known to affect results of both X-ray diffraction(XRD)and infrared spectroscopy(IR).These methods are predominantely used to characterize goethites.In the present study,therefore,a significant set of natural goethites was considered in order to investigate the effect of elemental composition on XRD and IR results.The focus was on crystallised samples which had a limited chemical variability but artefacts caused by the presence of admixtures could be excluded in most cases.First of all Rietveld refinement was optimized based on varying different parameters.A fairly good correlation of Rietveld derived crystallite sizes and specific surface area determined by N-adsorption(SSA)was found which proves the importance of considering the crystallite size parameters for Rietveld refinement and at the same times proves the quality of it.Using IR spectroscopy yet published relations of band position and Al-content could be confirmed despite the fact that the range of Al-contents was small.However,the band position of the Fe–O stretching,previously used as proxy for crystallinity assessment,was found to be least variable hence contradicting yet published results.Controversial results were also published for the effect of the Al-content on the position of the asymmetric FeOH stretching band at 450 cm.The goethites investigated in the present study indicate that the crystallite size determines the band position rather than the Al-content which is at least valid for the limited range of Al-contents.The results of the present study indicate that using synthetic sample sets bears the problem that more than one parameter might show systematic differences(e.g.crystallite size in a set of chemically varied goethites).The paper,therefore,provides IR reference data based on a set of natural well crystallised goethites.

Soil Clay Mineralogical Phase Analysis of Ganges Floodplain Soils by XRD and XRF

Soil minerals study is vital in terms of investigating the major soil forming compounds and to find out the fate of minor and trace elements in soils. It is also essential for the soil-plant interaction purpose. To identify soil mineral phases especially clay minerals, X-ray diffraction (XRD) has been a popular technique. The clay mineralogical information of soils in Bangladesh is limited, especially in Ganges flood plain region (Agro Ecological Zone (AEZ) 12 and 13). Therefore, to overcome this limitation, in this study, we performed XRD analysis of <2 mm fractions soil samples of AEX 12 and 13. However, identifying mineralogical phases by XRD in <2 mm fractions soils is not so straight-forward due to many practical problems. We fully matched only two mineralogical phases in all the soil samples which is quartz and potassium-Aluminum-Silicate. However, the full XRD peaks indicate that more minerals are also present, but due to heterogeneity of soils samples, it is difficult to find other minerals phases by only XRD peak of <2 mm fractions. Therefore, to find more information about mineralogical phases, we performed XRF analysis that provides the elemental composition of minerals phase as oxide. XRF analysis indicated the presence of secondary minerals like illite and chlorite. The presence of high percentage Fe oxide not only indicated the iron mineral phase (goethite and ferrihydrite) but also indicated iron rich high charge smectite minerals (beidellite). The presence of iron rich smectite minerals in the Ganges sediments reported in several previous studies. Thus, we concluded that only XRD in <2 mm fractions of soils is not adequate to identify the mineralogical phases of soil samples. Others analyses like XRF, XRD in <2 μm fractions will be necessary to locate an entire image of soil mineralogical phases.

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.

钢渣粉/聚酯纤维沥青混合料水稳定性研究

为了实现钢渣粉在沥青路面中的可持续利用,同时结合河南省冬季冰雪天气下路面的除冰情况,研究了掺有聚酯纤维与钢渣粉沥青混合料的水稳定性。制备4种聚酯纤维掺量(0、0.3%、0.4%、0.5%)AC-13沥青混合料开展复盐(掺量配比为NaCl∶CaCl2∶CH2COONa=1∶1∶2)冻融循环劈裂试验,结果表明聚酯纤维掺量为0.4%时,沥青混合料水稳定最好;在最佳纤维掺量下制备5种替代率(0、25%、50%、75%、100%)钢渣粉沥青混合料,采用冻融劈裂抗拉强度比(freeze-thaw splitting tensile strength ratio,TSR)确定最佳钢渣粉替代率为75%,混合料水稳定性最佳;通过冻融腐蚀因子K评价沥青混合料的抗侵蚀性能,结果表明:聚酯纤维/钢渣粉沥青混合料的抗侵蚀性能最强,聚酯纤维沥青混合料次之,普通石灰岩沥青混合料最弱。通过电镜扫描(scanning electron microscope,SEM)、X射线衍射(X-ray diffraction,XRD)技术探索钢渣粉/聚酯纤维沥青混合料界面黏附作用的改性机理。微观分析表明:掺量为0.4%的聚酯纤维形成的纤维网状结构以及沥青、钢渣粉(75%的替代率)和矿粉三者存在界面能量作用可以很好地改善沥青混合料的水稳定性。

High resolution strain mapping of a single axially heterostructured nanowire using scanning X-ray diffraction

Axially heterostructured nanowires are a promising platform for next generation electronic and optoelectronic devices.Reports based on theoretical modeling have predicted more complex strain distributions and increased critical layer thicknesses than in thin films,due to lateral strain relaxation at the surface,but the understanding of the growth and strain distributions in these complex structures is hampered by the lack of high-resolution characterization techniques.Here,we demonstrate strain mapping of an axially segmented GalnP-lnP 190 nm diameter nanowire heterostructure using scanning X-ray diffraction.We systematically investigate the strain distribution and lattice tilt in three different segment lengths from 45 to 170 nm,obtaining strain maps with about 10^-4 relative strain sensitivity.The experiments were performed using the 90 nm diameter nanofocus at the NanoMAX beamline,taking advantage of the high coherent flux from the first diffraction limited storage ring MAX IV.The experimental results are in good agreement with a full simulation of the experiment based on a three-dimensional(3D)finite element model.The largest segments show a complex profile,where the lateral strain relaxation at the surface leads to a dome-shaped strain distribution from the mismatched interfaces,and a change from tensile to compressive strain within a single segment.The lattice tilt maps show a cross-shaped profile with excellent qualitative and quantitative agreement with the simulations.In contrast,the shortest measured InP segment is almost fully adapted to the surrounding GalnP segments.

炉排式垃圾焚烧炉的结渣特性研究

为了进一步掌握炉排式垃圾焚烧炉的结渣特性和形成机理,选取炉内典型渣块展开研究。通过XRD物相分析、扫描电镜和能谱分析研究炉内结渣特性,并通过化学热力学平衡反应计算与试验结果进行了比较。结果表明,CaO、Al2O3/MgO/ZnO、SiO2等反应生成的钙化合物形成的低熔点共熔物相的存在是灰渣形成的主要原因。渣块内Si和Ca的分布趋势几乎是完全相同,Fe具有局部富集,Na和K对初始层的形成起主要作用。

云母矿粉中游离二氧化硅含量的快速测定

以具有复杂晶体结构、X射线衍射峰与游离二氧化硅衍射峰严重重叠及易择优取向等特点的云母矿粉为研究对象,探讨了利用具有超能探测器的X射线衍射仪在连续扫描模式下收谱以及Rietveld全谱拟合快速测定其中游离二氧化硅含量的可行性。结果表明:与步骤复杂、测试周期长等的传统X射线衍射标准曲线法相比较而言,该方法不仅操作简便、收谱快速而且结果准确性高、重现性好。重现性测定的最大标准偏差为1.39%。实际样品测试也表明此方法是一种简便易行的测定各类粉尘中游离二氧化硅含量的好方法。

白酒糟制备高纯度微晶纤维素工艺优化及其结构表征

白酒糟含有丰富的纤维素和半纤维素组分,是制备食品添加剂微晶纤维素(MCC)的良好原料来源。在硝酸-乙醇法提取酒糟粗纤维的基础上,探索酸法水解制备高纯度酒糟微晶纤维素(GSMCC)的工艺参数并进行结构表征。着重考察盐酸浓度、温度、液固比和时间4个因素对GSMCC纯度和得率的影响,并通过响应面优化法确定最优工艺参数。结果表明,酒糟粗纤维在温度72.3℃,盐酸质量分数7.5%,液固比25∶1(mL/g)的最优条件下水解2 h,可制得纯度92.57%、聚合度276.39的GSMCC,得率高达89.25%;经漂白后纯度略增至93.31%,聚合度降为255.86。扫描电镜(SEM)、傅里叶变换红外光谱(FTIR)和X衍射(XRD)分析发现,GSMCC的微观形貌呈不规则颗粒状,具有典型纤维素的红外光谱特征,纤维素晶型为Ⅰ型,结晶度为67.49%。热重分析(TGA)表明GSMCC热稳定性良好。本试验结果说明利用白酒糟制备食品添加剂微晶纤维素的工艺可行且具有良好结构特性。

弱还原气氛下淮南煤灰矿物质特性研究

对淮南煤在弱还原气氛下的矿物质特性进行实验研究,用X-射线衍射和红外光谱分析不同温度下煤灰矿物组成变化。结果表明:淮南煤中主要晶体矿物有高岭石、石英、方解石、黄铁矿等,高岭石类矿物含量越高,煤灰熔点越高;方解石和黄铁矿含量越高,煤灰熔点越低。煤灰中主要晶体矿物有石英、硬石膏、赤铁矿等,硬石膏和赤铁矿含量越高煤灰熔点越低。随着温度的升高,煤灰中石英、硬石膏、赤铁矿等结晶矿物含量逐渐减少,生成新的矿物质,莫来石的生成是导致淮南煤灰熔点高的主要原因,钙长石起到降低灰熔点的作用。