失活加氢精制催化剂中硫铁相的高分辨透射电镜研究

利用高分辨透射电镜(HRTEM)结合X射线能谱仪(EDS)和选区电子衍射(SAED)分析,对运转后的加氢精制催化剂中含有的微量未知相的化学组成、晶体结构进行了研究.通过X射线能谱仪确定该未知相主要成分为硫和铁.根据选区电子衍射结果,该硫铁相为单晶结构.采用样品倾转的方法,获得3幅不同取向的选区电子衍射图,根据衍射谱中衍射斑点对应的晶体学信息及3幅电子衍射图取向间的夹角关系,确定该硫铁化合物属于正交晶系的硫化亚铁,分子式为Fe0.91S.该催化剂应用于高温高压下的加氢环境中,其中原料油中的酸性物质,尤其是环烷酸对加氢设备材质的腐蚀是导致硫铁化合物相形成的主要原因,并由此探讨了硫铁化合物相的形成机制.     

快速凝固TiAl基合金稀土相显微组织的研究

利用两种不同的快速凝固方法对TiAl-RE合金中稀土相的显微组织进行了研究并与铸态组织进行对比,选择的快速凝固方法为溶体旋转法（MS）和锤钻法（HA）,试验结果表明,随着材料冷却速度的变化稀土相的显微组织发生了很大的变化,由铸态完全分布于晶粒边界之上过渡到锤砧法极细的层片和弥散分布的颗粒组织,选区电子衍射结果表明,稀土相的衍射斑点与AlCe金属间化合物一致。     

用TEM分析溅射法制备Ag超微粒的空间分布

用透射电镜对在氩气中电离溅射沉积于碳膜上的Ag超微粒进行了直接研究。通过明场象和电子衍射观察分析发现,在溅射入射角为60°时,经不同的出射角收集,形成的超微粒的粒径、粒径分布、形态和物相结构各有不同。     

电子衍射径向分布函数测定稀土顺1,4聚丁二烯的原子间距分布

本文用电子衍射径向分布函数测定了稀土顺1,4聚丁二烯的原子间距分布。从电子衍射实验强度曲线的傅里叶变换得到的RDF曲线上,具有二个分子内峰和三个分子间峰。说明在熔点以上,处于非晶态的顺1,4聚丁二烯中不同程度的存在分子链间的局部有序性。     

超细Mo-Co-K催化剂的制备及其选区电子衍射表征

采用类凝胶-超临界流体干燥法制备了超细Mo-Co-K催化剂,并运用TEM和选区电子衍射技术对制得的催化剂进行了表征.结果表明,制得的催化剂由属于超细粒子范畴的片状微晶和球状小颗粒组成,进一步经选区电子衍射技术分析,前者归属为MoO3物相,后者归属为CoMoO4物相.     

Gd5Si2Ge2相的线状缺陷

使用X射线粉末衍射(XRD)表征了电弧炉熔炼的Gd5Si2Ge2.2合金的相组成,结果表明Gd5Si2Ge2.2合金主要由Gd5Si2Ge2相和GdGe相构成。扫描电镜(SEM)分析表明,Gd5Si2Ge2晶粒内部有大量规则分布的线状特征;透射电镜(TEM)研究发现了Gd5Si2Ge2相的基体上存在两种不同形态的线条组织,选区电子衍射证明两种不同形态的线条组织既非第二相也非孪晶;根据高温原位金相观察的结果推测,该线状组织是在液-固相变过程中形成的。     

顺1,4及反1,4聚丁二烯共混及共聚物结晶形态结构研究

本文用电镜、电子衍射及DSC等研究了顺1,4PB及反1,4PB的共混及共聚物的形态结构。观察了室温下两相结构分布随组分变化的规律及反1,4PB含量对顺1,4PB低温结晶、片层厚度和球晶大小的影响。进一步讨论了这两种不能形成类质同象结构物质结晶的相互影响。     

移动床热煤气脱硫气固反应过程模拟——Ⅱ-错流移动床非催化气固反应过程模拟

基于前文错流移动床反应器模型方程,模拟计算并分析了该类反应器中气、固相流动对热煤气脱硫等非催化气固反应过程的影响。研究表明,床层在床深方向按反应速率的快慢可分为粗脱区和精脱区,在颗粒流动方向上气相浓度差异较大,并主要体现在粗脱区内,床层出口处颗粒转化率呈现较大分布,反应器内气固交错流动、气相浓度和颗粒转化率共同作用（ 于气固反应速率） 等因素是造成过程特征的主要因素。因此反应器优化应满足对两相流动的优化,将粗脱区设置成错流移动床而精脱区设置成固定床,并使粗脱区内颗粒流速沿气流方向逐渐减小,以减小出口颗粒转化率的分布并提高颗粒利用率,同时沿颗粒流动方向应逐渐减小过床气流体积分率以利于床内气固反应速率的均一分布。由此指出对该类床型其底部渐缩下料段和过床气流对床内颗粒流动的影响以及床层结构及颗粒流动对过床气流分布的影响研究的必要性。     

两段式气流床煤气化炉内气固流动数值模拟研究

建立了两段式气流床煤气化炉内气固两相流动的三维计算流体力学（CFD）模型,将气体视为连续介质,在Euler坐标系下考察气相的运动;将颗粒视为离散体系,在Lagrange坐标系下研究颗粒的运动。利用所建CFD模型对基本设计尺寸和操作条件下的两段式气流床煤气化炉内气固两相流动进行了模拟,给出了两段式气流床煤气化炉内的气固两相流动的规律和颗粒的分布规律。在此基础上,针对不同的结构(喉口直径变化)和不同的操作条件（两段气固进料量变化）进行了一系列的模拟比较。结果表明,喉口直径的变化对于炉内气固两相流动及颗粒分布有重要影响。随着喉口直径减小,喉口附近区域的气相回流增强,颗粒运动轨线变得更加曲折,颗粒分布发生明显变化。两段气固流量的改变可以明显改变炉内气固流动,随着一段反应区的气固流量增加和二段反应区气固流量减小,一段反应区内的气相回流更加显著, 二段反应区气相回流减弱,颗粒螺旋上升运动增强,反应器边壁处颗粒浓度增大,颗粒沉积现象减弱。     

高钆耐热镁合金在高温蠕变过程中的显微组织演变

以时效态Mg-12Gd-3Y-1Sm-0.5Zr (%,质量分数)合金为研究对象,利用蠕变持久试验机在250℃/50 MPa下对合金的蠕变性能进行了测试,并采用TEM研究了合金在250℃/50 MPa下蠕变10, 30 min, 100 h过程中的显微组织和相的演变。结果表明:时效态Mg-12Gd-3Y-1Sm-0.5Zr合金相由α-Mg基体和β′相组成,β′相为纳米析出相,在高温蠕变过程中,晶内析出相明显长大,形貌由黑色椭圆形颗粒向菱形和长条状转变,经对应的选区电子衍射谱标定,相结构未发生变化;晶界上析出相粗化,转化为平衡相β相。本研究为开发高温高强抗蠕变耐热镁合金提供理论基础。     

Evidence for a bound HeH2 halo molecule by diffraction from a transmission grating

The HeH2 van der Waals complex has been identified in a molecular beam produced by a cryogenic (T0=24.7 K) free jet expansion of a 1% H2 mixture in 99% 4He gas. The weakly bound HeH2 complexes in the beam are identified via their first order diffraction angles after passing through a 100 nm period transmission grating. An electron impact mass spectrometer analysis of the diffraction patterns is used to discriminate against ion fragments of the constituent gas clusters.     

The determination of the populations of vibrational levels of molecules from electron diffraction data

The application of modern gas-phase electron diffraction for directly determining the populations of vibrational levels is demonstrated for the molecule I₂. It is concluded that, under the conditions of the conventional electron diffraction experiment, a thermal equilibrium can reliably be assumed for a gas jet but at a temperature which can be markedly lower than that of the nozzle. The diffraction results favour a Boltzmann distribution of molecules over the vibrational states.     

In situ x-ray diffraction measurements of the capillary fountain jet produced via ultrasonic atomization

In situ x-ray diffraction measurements were carried out for investigating the liquid structure in the ultrasonic fountain jet to consider the mechanism of the "ultrasonic ethanol separation" reported by Sato et al. [J. Chem. Phys. 114, 2382 (2001)]. For pure liquids (water and ethanol), it was found that the high frequency ultrasound does not affect the liquid structure microscopically. For the 20 mol % ethanol-water mixture, the estimated ethanol mole fraction in the ultrasonic fountain jet by using the position of the main maximum in the x-ray diffraction profile coincided with that in the reservoir. This result suggests that the ethanol separation is not caused by any distorted liquid structure under the ultrasound irradiation and occurs when or after the generation of the liquid droplet mist.     

Possibilities for Energy Pumping in a Radio-Frequency Quadrupole by Shifted Supersonic Gas Jet. Part I: Accelerated and Excited Atom Transmission

Generation of an ion beam and its transmission into a mass analyzer is one of central problems in mass spectrometry. The use of a narrowly directed supersonic gas jet has a number of advantages in comparison with other sampling methods. The aim of this work was to confirm the declared earlier properties of the jet formed at the outlet of a cylindrical channel when the free path length of gaseous atoms at the beginning of the channel is comparable with the channel diameter. The paper describes the ability of such a supersonic jet to conserve an additional energy of jet gas atoms. A significant influence of the temperature of the gas flow on the yield of cyclohexane fragment ions was found, cyclohexane being an admixture in the noble gas jet passing through an electron ionization ion source. A possibility of obtaining a flow of metastable electronically excited atoms inside the jet is also shown. The results of the work confirm the availability of the supersonic gas jet for the design of a high efficiency ion source inside the radio-frequency quadrupole at the input of the mass analyzer.     

The convective heat transfer analysis of the casson nanofluid jet flow under the influence of the movement of gyrotactic microorganisms

Jet flows provide an effective mode of energy transfer or mass transfer in industrial applications. When compared to traditional cooling through convection, jet flows have high heat and mass transfer coefficients. Further, the devices equipped with jet flow provides efficient use of fluid and also offers enhanced heat and mass transfer rates. Hence in this study, the jet flow of Casson nanofluid containing gyrotactic microorganisms that stabilises the nanoparticle suspension is discussed. To control the fluid from outside external magnetic field is imposed. The model with these characteristics are useful in the appliances like coolants in automobiles, nuclear reactors, micro-manufacturing, metallurgical process etc. Such a model is created by employing PDE, which are then transformed into a system of ODE. The DTM is employed to obtain the solution to system of equations, and the results are interpreted using graphs. It is perceived that the velocity of the nanofluid flow is decreased because of the increased yield stress created by the greater values of the Casson parameter. As a result, the temperature profile is found to be increasing. Meanwhile, it is observed that for increased value of chemical reaction parameter diminishes the nanoparticle concentration. The motile density is found to decrease for increase in the Peclet number and the bioconvection Schmidt number. Further, the thermophoresis improves the temperature and concentration profile of the nanofluid.     

Continuous Synthesis of Hydrogenated Graphene in Thermal Plasma

A single-stage catalyst free synthesis of hydrogenated graphene was studied in the process of methane conversion in a helium plasma jet created by a plasma torch at the power up to 45 kW and the pressure of 710 Torr. The synthesis products were studied by the methods of scanning and transmission electron microscopy, thermal analysis, Raman spectroscopy, X-ray photoelectron spectroscopy, and X-ray diffraction analysis.     

喷气燃料中悬浮物的分离和分析

通过过滤分离出喷气燃料中的悬浮物,并用正己烷和二氯甲烷提取,利用扫描电镜、X射线能潜仪、X射线衍射仪、红外光谱仪和气相色谱-质谱仪分析悬浮物的组成;得出喷气燃料的悬浮物中同时含有烃类物质．极性成分和小粒径颗粒物。实验结果为进一步研究喷气燃料中的悬浮物来源和机理奠定了基础。     

常压高频放电等离子体炬改进制备CO2/CH4重整用Ni/MgO催化剂

比较了常规法、等离子体炬法和等离子体炬辅助焙烧法制得的Ni/MgO催化剂上CO2/CH4重整反应性能差异,并利用X射线衍射、透射电镜、X射线光电子能谱和CO2程序升温表面反应等技术对反应前后催化剂进行了表征,结果表明,采用等离子体炬辅助焙烧法制备的催化剂上Ni晶粒粒径小,分散度较高,低温活性和抗积炭性能较高;在常压,7...     

Measuring electrostatic potential profiles across amorphous intergranular films by electron diffraction.

Amorphous 1-2-nm-wide intergranular films in ceramics dictate many of their properties. The detailed investigation of structure and chemistry of these films pushes the limits of today's transmission electron microscopy. We report on the reconstruction of the one-dimensional potential profile across the film from an experimentally acquired tilt series of energy-filtered electron diffraction patterns. Along with the potential profile, the specimen thickness, film orientation with respect to the grain lattice and specimen surface, and the absolute specimen orientation with respect to the laboratory frame of reference are retrieved.     

Design of novel order mesostructured superacid catalyst from rice husk for the conversion of linseed oil to methyl esters

A novel ordered mesoporous catalyst was prepared from rice husk (MRH catalyst) through condensation–evaporation method in alkaline media. The process used cetyltrimethylammonium bromide (CTAB) as a structure-directing agent (template) and sulfonated biochar obtained from partial rice husk carbonization (SBRH) as precursor. Various parameters such as temperature and CTAB/SBRH mass ratios were investigated to improve the mesoporous structure. The chosen catalyst was based on its degree of order of the mesoporous channels, and its activity was also tested in the methanolysis of linseed oil to methyl esters which was considered as a valuable blending composition for commercial jet fuels. The results showed that the temperature and CTAB/SBRH mass ratio should be of 70 °C and 0.3/1, respectively. The catalyst samples were characterized by many techniques including X-ray diffraction (XRD), infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and ammonia-temperature programmed desorption (NH₃-TPD). The methyl ester composition of the as-synthesized biofuel was determined using gas chromatography supported by mass spectroscopy detector (GC–MS). The results of the characterizations showed that the catalyst possessed superacidic sites (NH₃-TPD) caused by –SO₃H groups (confirmed by FT-IR analysis) and ordered mesoporous structure (XRD). The mesoporous channel distribution was also observed by TEM images. The methanolysis yield reached 93.5% (calculated through GC–MS analysis) at mild conditions with high purity of methyl ester products strongly proving the catalyst activity and selectivity.