Electro-static discharge method of zone location for paper chromatographs

This paper presents an entirely new application of static discharge current for the localization of zones or spots on paper chromatographs Electroscope and neon-tube methods of location are described Both methods can be carried out by the same instrument, which is inexpensive to construct, takes up little space, and is portable Used in conjunction with Blake's titrimeter quantitative measurements are made     

The Effect of Microwave Sintering on the Microstructure and Properties of Calcium Phosphate Ceramic

Despite good ability to improved biological affinity and activity of calcium phosphate (CP) ceramic to the surrounding host tissue when implanted, CP ceramic is capable to encourage direct bond with bone as their chemical compositions are similar to the mineral phase of bone. However, the low mechanical property of CP ceramic restricts use in load-bearing applications. Therefore, the primary aim of this study was to fabricate dense CP ceramic via used of microwave sintering analyze the microstructure and mechanical properties comparison to conventional ceramic sintering. The sintered specimens were characterized by their surface microstructure, density measurement and hardness test. The result demonstrated that the density and hardness values of sintered CP ceramic specimens by microwave sintering were higher than conventional sintering. The microstructures of CP ceramic microwave sintered specimens show also better microstructures (analyzed by FESEM technique), with fines grain size and the present of apatite layer growth on the surface when examined with SBF solution. It can be concluded that the microwave sintering enhanced better microstructure and mechanical properties of CP ceramic.     

Combined use of lattice source interferences and divergent beam X-ray interferences to investigate the microstructure of ion-bombarded Cu-Sn-diffusion zones

Diffusion processes and phase formations as well as the crystallographic structure of microelectronic contact zones decisively influence the electrical and mechanical properties of electronic components. Using various physical methods in the same analysis area, such as lattice source interferences and divergent beam X-ray interferences, optical microscopy and SEM, electron probe microanalysis and the ion beam slope cutting method, profound statements about the microstructure can be made. A Kossel camera and an additional divergent beam X-ray device were built and installed in a Scanning Electron Microscope (SEM) CamScan CS 44. X-ray interferences in the microrange of selected areas were taken using both systems, providing information on the crystallographic orientation and the real structure of the specimens. The interference techniques were tested using single-crystal and ion-bombarded polycrystalline copper. In addition, applying the mentioned methods, the diffusion generated intermetallic compounds Cu₃Sn, Cu₆Sn₅ and Cu₄₁Sn₁₁ were investigated using ion-bombarded Cu-Sn/Pb model samples.     

Surface remelting of 316 L + 434 L sintered steel: microstructure and corrosion resistance

This study presents arc surface remelting of three types of sintered stainless steels carried out in order to constitute a homogeneous microstructure in the surface layer which is free from open and interconnected porosity. The main aim of this treatment was to improve functional properties of the sinters analysed, especially their resistance to pitting corrosion. The sinters were obtained from powders of 316 L and 434 L steels. The PM austenitic-ferritic stainless steels are used mainly in the automotive industry, but their general application is still limited due to relatively poor corrosion properties when compared to casts or wrought components. This study used the gas tungsten arc welding (GTAW) process as a method of economical surface treatment. The effect of surface treatment was evaluated based on macro- and microstructural observations, energy-dispersive X-ray spectroscopy (EDX) analysis, X-ray phase analysis, measurements of surface roughness and electrochemical examinations. It was found that a cellular or mixed cellular and dendritic structure was formed in the remelted zone of the sinters after remelting. X-ray analysis demonstrated that application of remelting contributes to formation of the austenitic phase in the surface layer. The corrosion resistance of the remelted surface layers was evaluated using polarization tests in 0.5 M NaCl solution. It was found that arc surface remelted layers exhibit much better anticorrosive properties than sinters without surface treatment. Microstructural observations of the surface of specimens after electrochemical tests showed only a few single pits in the remelted layer, while the surface of initial sinters was much more corroded.     

莫来石抗氧化外涂层的制备及抗氧化性能

以莫来石粉体(3Al2O3·2SiO2)为原料,采用水热电泳沉积法在C/C-SiC复合材料表面制备了莫来石外涂层。借助XRD和SEM等对涂层的晶相组成和显微结构进行了表征。研究了水热沉积电压对莫来石外涂层相组成、形貌及高温抗氧化性能的影响。结果表明:外涂层主要由莫来石晶相组成。当沉积电压控制在120~180 V范围内时,莫来石外涂层的致密程度、厚度及抗氧化性能随着沉积电压的升高而提高。当沉积电压达到210 V时,制备的外涂层出现疏松、裂纹等缺陷,抗氧化性能减弱。抗氧化测试表明与包埋法制备的SiC-C/C涂层试样相比,莫来石-SiC-C/C涂层试样的抗氧化性能明显提高。当沉积电压为180 V时,制备的复合涂层试样可在1500℃的空气气氛下有效保护C/C复合材料164 h,其失重仅为1.75%。     

Study on microstructure and corrosion resistance of Ti-doped nickel-based alloy coatings

Journal of Solid State Electrochemistry - The Ti-doped nickel-based alloy coating was prepared by plasma melting, and its microstructure was investigated by optical microscopy (OM) and X-ray...     

Thermogravimetry of ternary cement blends

This study reports the microstructure characteristic and compressive strength of multi-blended cement under different curing methods. Fly ash, ground bottom ash, and undensified silica fume were used to replace part of cement at 50 % by mass. Mortar and paste specimens were cured in air at ambient temperature, water at 25, 40, and 60 °C and sealed with plastic sheeting for 28 days. In addition, these specimens were cured in an autoclave for 6, 9, and 12 h. Results indicated that the compressive strength of multi-blended mixes containing silica fume 10 % by mass cured with plastic sealed and cured in water at 25 and 40 °C was similar to or higher than the corresponding Portland cement control at 28 day. Moreover, the mixes containing silica fume 10 % by mass cured in water at 60 °C had higher compressive strength than Portland cement control. X-ray diffraction and thermogravimetry results confirmed that there was increased pozzolanic reaction with increasing silica fume content which relates to the increasing in strength. For autoclaved curing, the compressive strength of multi-blended cement specimens with silica fume (total of 50 % replacement) was noticeably higher than control Portland cement mix and was highest when autoclaving time was 9 h. X-ray diffraction results showed the pattern of 0.9, 1.1, and 1.4 nm tobermorite crystalline phases as the main product of this curing. Thermogravimetry results showed dehydration of 1.4 nm tobermorite and 1.1 nm tobermorite at about 80–90 and 135–150 °C, respectively. Tobermorite (also shown by scanning electron microscope) thereby as a result lead to significant compressive strength improvement in the short time of autoclaved curing.     

Corrosion behavior of Mg,AZ31, and AZ91 alloys in dilute NaCl solutions

Corrosion behavior of extruded Mg, extruded AZ31 alloy, and cast AZ91 alloy was investigated by electrochemical measurements in dilute NaCl solutions. Corrosion products and passivation films were analyzed by X-ray diffraction and X-ray photoelectron spectroscopy. All specimens exhibit the corrosion and passivation zones in dilute NaCl solutions. The aluminum content and alloy microstructure influence the corrosion and passivation processes. AZ91 alloy shows the broadest passivation zone followed by AZ31 alloy and Mg. AZ91 alloy reveals a highest corrosion resistance, and preferential attack is located at the primary Mg phase. Its relatively fine β-phase (Mg₁₇Al₁₂) network and Al₂O₃/Al(OH)₃ compounds produced on the passivation film are the main factors which limit the corrosion progress as compared with AZ31 alloy and Mg. The thick passivation product on AZ31 alloy is the key factor which restricts the corrosion attack in dilute solutions.     

还原热处理条件对Pt-Fe/C 合金催化剂性能的影响

采用脉冲微波辅助化学还原-含氢气体热处理法制备了质子交换膜燃料电池(PEMFC)用Pt-Fe/C合金催化剂.通过电感耦合等离子体(ICP)检测了金属元素含量,用透射电镜(TEM)、X射线衍射(XRD)和X射线光电子能谱(XPS)等技术对催化剂的微观结构和形貌进行了表征,并利用循环伏安(CV)法评价了催化剂催化氧还原性能.结果表明,脉冲微波辅助化学还原法是一种快速制备粒径较小、分布均匀的Pt-Fe/C催化剂的有效方法,含氢气体热处理对提高催化剂活性有重要作用.还原热处理温度和时间对催化剂活性也有很大影响.经过500°C还原热处理后的催化剂活性比还原热处理之前的催化剂性能有很大提高.TEM和XRD结果显示,Pt-Fe/C-500-3h的纳米粒子均匀地分散在碳载体上,平均粒径为1.8nm,500°C下热处理3h的催化剂有最大的电化学表面积(ESA),为55.14m2·g-1.     

微波水热时间对C/C复合材料结构和抗氧化性能的影响

以磷酸、B4C和Al2O3为原料,采用一种新的微波水热法对C/C复合材料基体进行了抗氧化改性,重点研究了微波水热时间对改性试样物相组成、微观结构和抗氧化性能的影响。采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、能量色散谱仪(EDS)及X射线光电子能谱(XPS)对改性后试样进行了表征。结果表明:改性后复合材料表面覆盖了一层由熔融态的HPO3、B2O3和结晶的Al(PO3)3、微量B4C粒子组成的涂层。经60~120 min的微波水热改性,复合材料的抗氧化性能随着微波水热处理时间的延长而改善,达到一定程度后,其变化不再明显。微波水热处理100 min后的试样抗氧化性能最佳,在600℃静态空气气氛下氧化16 h后,氧化失重仅为9.5×10-4 g.cm-2,氧化失重速率维持在4.46×10-5 g.cm-2.h-1的极低水平。     

Microstructural Exploration of the High Capacitance in RuO_2-ZrO_2 Coating

A high capacitance RuO₂-ZrO₂ coating was prepared by thermal decomposition method.Extended X-ray absorption fine structure(EXAFS),X-ray diffraction(XRD),high-resolution transmission electron microscope(HRTEM)and ab initio calculations were applied to understand the role of the microstructure in the acquisition of high specific capacitance of RuO₂-based oxides.The results show that the RuO₂-ZrO₂ oxide prepared at critical crystallization temperature can be considered to be quasi-amorphous or microcrystalline(A short-range ordered crystal structure can be seen from the TEM image,but no diffraction peaks can be seen from the XRD diffraction patterns).And this RuO₂-ZrO₂ was identified as a solid solution with high solid solubility.It referred to herein as a quasi-amorphous solid solution.Such a special microstructure was conducive for"synergistic catalysis"owing to the cationic interaction and thus could gain high"active site density"and high"active surface",thus developing high specific capacitance.     

Liquid crystalline side chain-coil diblock copolymers by living free radical polymerization

A series of LC-coil diblock copolymers was prepared using living radical polymerization. The resulting polymers were shown to possess a smectic mesophase and a lamellar microstructure by X-ray diffraction. The microstructure slowly develops on annealing as suggested by DSC studies.     

Design of nanostructured ceria-based solid electrolytes for development of IT-SOFC

A considerable interest has been shown in the application of doped ceria (CeO₂) compounds for “intermediate” (300–500 °C) temperature operation of solid oxide fuel cells. The microdomains with ordered structure of oxygen vacancy were observed in the microstructure of the M-doped CeO₂-sintered bodies (where M: Gd, Y, and Dy). We have previously shown that the conductivity of doped CeO₂-sintered bodies was lower when the sintered body contained large microdomains within grains. As a consequence of this observation, we have examined the grain size dependence and dopant content on conductivity in specimens where we adjust the microdomain size and a degree of oxygen vacancy ordering in the microdomains by controlling the microstructure. The microdomain size control in Dy-doped CeO₂ specimens was obtained by combining pulsed electric current sintering and conventional sintering. Using these techniques, we were able to improve the conductivity in Dy-doped CeO₂ specimens to a point where it became comparable to that of the more conventional Gd-doped CeO₂ specimens. It is concluded that by combining ultimate high-resolution analysis of these nanostructures with the adjusting processing route design, it is possible to further develop these materials in CeO₂-doped fuel cell application.     

Effects of precipitant on microstructure and luminescent properties of Lu2O3:Eu3+ nanopowders and ceramics

Nanocrystalline Lu(2)O(3):Eu(3+) was prepared by co-precipitation method using ammonium hydrogen carbonate and ammonium oxalic acid as precipitants, respectively. The crystal structure and morphology were analyzed by means of XRD and TEM. The resultant powders were sintered into transparent ceramics in vacuum and then in nitrogen without any additive. The surface morphology of the unpolished sintered specimens was characterized using SEM. The effect of different precipitants on microstructure of the nanopowders and transparency of the ceramics are compared. The excitation and emission spectra of Lu(2)O(3):Eu(3+) powders and ceramics were measured at room temperature by using synchrotron radiation as the light source. The fluorescence decay times of all specimens were analyzed. Luminescence of the ceramics decays faster than the corresponding nanopowders.     

Microstructure development in mixes of calcium aluminate cement with silica fume or fly ash

The most widely identified degradation process suffered by calcium aluminate cement (CAC) is the so-called conversion of hexagonal calcium aluminate hydrate to cubic form. This conversion is usually followed by an increase in porosity determined by the different densities of these hydrates and the subsequent loss of strength. Mixes of calcium aluminate cement (CAC) and silica fume (SF) or fly ash (FA) represent an interesting alternative for the stabilization of CAC hydrates, which might be attributed to a microstructure based mainly on aluminosilicates. This paper deals with the microstructure of cement pastes fabricated with mixtures CAC-SF and CAC-FA and its evolution over time. Thermal analysis (DTA/TG), X-ray diffraction (XRD) and mid-infrared spectroscopy (FTIR) have been used to assess the microstructure of these formulations.     

三维多枝雪花状银粉的制备及催化性能

室温下,以聚乙烯醇为保护剂,采用抗坏血酸还原硝酸银,于水相中一步合成出三维多枝雪花状银粉。结合X射线粉末衍射（XRD）、扫描电子显微镜（SEM）等结构表征手段,对三维多枝雪花状银粉的微观结构进行详细分析,在此基础上提出其可能的形成机理。此外,三维多枝雪花状银粉在4-硝基苯酚催化加氢反应中还表现出优异的催化活性。     

添加钴对HD制备NdFeB永磁体矫顽力的影响

采用X射线衍射分析(XRD)和BH测试仪分别研究了添加Co对HD制备的NdFeB永磁体微结构和磁性能的影响规律。微结构研究表明,添加Co前后的永磁体都由主要的四方相Nd2Fe14B(P42/mnm)和微量的富Nd相构成;但添加Co明显改变了永磁体的取向特性和磁性能;Horta法计算表明Co掺杂降低了Nd(FeCo)B永磁体的(004),(006)和(008)晶面的极密度因子;室温下磁性能测试表明,添加Co后永磁体矫顽力有了明显提升,从2038 kA.m-1提升到2162 kA.m-1,提高了接近124 kA.m-1;Kronm櫣ller-Plot行为研究表明两合金的矫顽力机理均为磁畴成核机制,由于Co添加同时增大了微磁参数αk和Neff,这增加磁畴反转需要的磁场能,从而提高了矫顽力。     

In situ anomalous small angle X-ray scattering and absorption on an operating rechargeable lithium ion battery cell

We have employed anomalous small angle X-ray scattering (ASAXS) and X-ray absorption in situ on an operating lithium ion battery cell with LiMn₂O₄ as the positive electrode material. Manganese K-edge absorption spectra and scattering patterns were recorded at various stages of charge between 3.8 and 4.5 V. The shift of the manganese absorption K-edge was observed as a function of the charge of the electrode. Clear changes in the microstructure of the spinel at the 4 V plateau was observed even during the first charging cycle.