Fracture toughness of multiphase TiAl-Nb alloy in situ consolidated by spark plasma sintering

A fine-grained TiAl alloy with a composition of Ti-45Al-5Nb-1.5Cr-0.2W (mole fraction, %) with multiphases was prepared by spark plasma sintering (SPS) and heat-treating at 1 100 °C for 48 h. The relationship among sintering temperature, microstructure and fracture toughness were investigated by X-ray diffractometry (XRD), optical microscopy (OM), scanning electron microscopy (SEM) and mechanical testing. The results show that microstructure of the bulk alloy depends on the sintering temperature strongly, and the main phase TiAl and few phases Ti₃Al and niobium solid solution (Nbss) are observed in the SPS bulk samples. In the heat-treatment condition, the lamellar and Nbss phase can provide significant toughening by plastic strengthening, interface decohension, crack branch and crack bridge mechanisms. The fracture mode of the SPS TiAl composite samples is intergranular rupture and cleavage fracture.     

Effects of annealing on microstructure, mechanical and electrical properties of AlCrCuFeMnTi high entropy alloy

The multi-component A1CrCuFeMnTi high entropy alloy was prepared using a vacuum arc melting process. Serial annealing processes were subsequently performed at 590 ℃, 750 ℃, 955 ℃ and 1 100 ℃ respectively with a holding time of 4 h at each temperature. The effects of annealing on microstructure, mechanical and electrical properties of as-cast alloy were investigated by using differential thermal analysis （DTA）, X-ray diffraction （XRD）, scanning electron microscopy （SEM） and transmission electron microscopy （TEM）. The experimental results show that two C14 hexagonal structures remain unchanged after annealing the as-cast A1CrCuFeMnTi alloy specimens being heated to 1 100℃. Both annealed and as-cast microstructures show typical cast-dendrite morphology and similar elemental segregation. The hardness of alloys declines as the annealing temperature increases while the strength of as-cast alloy improves obviously by the annealing treatment. The electrical conductivities of annealed and as-cast alloys are influenced by the distribution of interdendrite re~ions which is rich in Cu element.     

放电等离子烧结制备碳化钛块材研究

利用放电等离子烧结（SPS）对碳化钛（TiC）/氢化钛（TiH2）混合粉末进行烧结以制备块材。利用X射线衍射（XRD）并结合Rietveld精修法对块材进行定性与结构分析;借助扫描电子显微镜（SEM）对块材断面微观形貌进行观察;测试了块材硬度并探讨SPS技术制备TiC块材的致密化过程与反应机理。结果表明：混合粉末经SPS烧结,获得了高度致密的TiC块材;与传统烧结方法比较,SPS技术更具低温快速性。     

Effect of pre-heating temperature on structural and optical properties of sol-gel derived Zn<Subscript>0.8</Subscript>Cd<Subscript>0.2</Subscript>O thin films

Zn_0.8Cd_0.2O thin films prepared using the spin-coating method were investigated. X-ray diffraction, scanning electron microscopy, and UV-Vis spectrophotometry were employed to illustrate the effects of the pre-heating temperature on the crystalline structure, surface morphology and transmission spectra of Zn_0.8Cd_0.2O thin films. When the thin films were pre-heated at 150 °C, polycrystalline ZnO thin films were obtained. When the thin films were pre-heated at temperatures of 200 °C or higher, preferential growth of ZnO nanocrystals along the c-axis was observed. Transmission spectra showed that thin films with high transmission in the visible light range were prepared and effective bandgap energies of these thin films decreased from 3.19 eV to 3.08 eV when the pre-heating temperature increased from 150 °C to 300 °C.     

Properties of plasma sprayed NiCrAlY+(ZrO2+Y2O3) coating on refractory steel surface

NiCrAlY+(ZrO₂+Y₂O₃) thermal barrier coating was prepared on the surface of refractory steel 1Cr18Ni9Ti with plasma spraying technique. The phases and microstructure of the thermal barrier coating were determined by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The results show that the bonding between thermal barrier coating and substrate is sound. The surface hardness of 1Cr18Ni9Ti reaches up to 1 000 HV, but that of substrate is only 300 HV. The patterns sprayed with CoNiCrAlY+(ZrO₂+Y₂O₃) ceramic coating have a good heat insulation effect at 800 °C for heat insulation temperature difference reaches 54 °C, which increases the operating temperature and service life of refractory steel. Foundation item: Project (5040202140) supported by Scientific Research Common Program of Beijing Municipal Commission of Education     

Synthesis of refractory cordierite from calcined bauxite, talcum and quartz

A cordierite was synthesized from calcined bauxite, talcum, and quartz. The properties and microstructure of the cordierite sintered samples were characterized by Archimedes’ method, thermal dilatometry, X-ray diffraction (XRD), scanning electron microscopy (SEM), and so on. The experimental results showed that calcined bauxite could broaden the range of synthesizing temperature from 1300 °C to 1420 °C and get pure cordierite. The bulk density and linear thermal expansion coeffi cient of the sample synthesized at 1420 °C for 2 h were 1.97 g·cm^?3 and 2.1×10^?6 °C^?1, respectively. The XRD analysis showed that the major crystalline phase was α-cordierite with almost no glassy matters, the SEM images illustrated a small vent hole and the size were 5–100 μm, the well-grown hexagonal and granular cordierite grains had the sizes distributed among 0.1–8 μm, and providing high mechanical strength and lower linear thermal expansion coeffi cient.     

Eu2Zr2O7纳米晶的硬脂酸法制备

以硝酸锆和硝酸铕作为原材料,硬脂酸作为溶剂和分散剂,通过硬脂酸燃烧法制备了具有立方晶系的萤石型Eu2Zr2O7纳米晶.通过热重和红外光谱对其反应过程进行跟踪.产物经X-射线粉末衍射、透射电镜、高分辨电子显微镜、能谱以及荧光光谱进行了表征.热处理温度对产物的形成有较大的影响,在800℃单一相的Eu2Zr2O7纳米晶已完全形成.所制得的纳米晶由平均粒径为5~20 nm的球状粒子组成.从透射电镜上（222）面的晶面距分别为0.307 nm,与理论值一致.实验检测到Eu2Zr2O7具有较强的荧光性质.     

ZnFe_2O_4纳米粒子的制备及其磁性能

以乙酰丙酮铁和乙酰丙酮锌为原料、三甘醇为溶剂,采用一步法制备ZnFe2O4纳米粒子。通过透射电子显微镜(TEM)、X-射线粉末衍射仪(XRD)和磁性能测量系统(MPMS)等表征手段对ZnFe2O4纳米粒子进行了表征。结果表明,所制备的ZnFe2O4纳米粒子平均粒径约为6 nm,尺寸均匀,水溶性良好,在室温条件下呈现超顺磁性。     

Sol-gel preparation and characterization of Co_3O_4 nanocrystals

A new citrate acid-hydrazine sol-gel route for preparation of Co3O4 nanoparticles has been developed. Co3O4 nanoparticles with different particle-sizes and morphology were prepared at different heat-treatment temperatures and the pure cubic nanocrystals of Co3O4 were obtained at 600℃. The synthesis process was monitored by infrared spectroscopy (IR), thermal gravimetric and differential thermal analysis (TG-DTA). The structure and morphology of Co3O4 nanocrystals were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and X-ray-photoelectron spectroscopy (XPS). The infrared absorption bands blue-shifted with particle size decreasing, which could be attributed to increasing surface effect. XPS results showed that predominant species at surface layers of Co3O4 nanocrystals are octahedral Co (Ⅲ).     

Thermal fatigue behavior of 441 ferritic stainless steel in air and synthetic automotive exhaust gas

The thermal fatigue behavior of 441 ferritic stainless steel was investigated in air and synthetic automotive exhaust gas by the cyclic tests under 100°C–800°C and 900°C conditions. After the fracture failure, the microstructure, oxide film, and precipitated phases were analyzed using optical microscopy, X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. In both atmospheres, increasing the maximum temperature from 800°C to 900°C results in lower strength and fatigue life and higher elongation and grain size. At the same maximum temperature, the thermal fatigue life of the specimen is lower in the synthetic exhaust gas than in the air. Both the higher maximum temperature and the synthetic exhaust gas facilitate fatigue failure. The failure mechanism is discussed according to the grain size, thermal stress, high-temperature oxidation rate, and the precipitation of secondary phases. Some precipitated carbides play an important role in the rapid fatigue failure of specimens in the synthetic exhaust gas.

     

Preparation and characterization of nanocomposite MgFe<Subscript>2</Subscript>O<Subscript>4</Subscript>/SiO<Subscript>2</Subscript>

Nanocomposites MgFe₂O₄/SiO₂ were successfully synthesized by the sol-gel method in the presence of N, N-dimethylformamide (DMF). The formation of pure MgFe₂O₄ was confirmed by powder X-ray diffraction (XRD) and electron diffraction. The structural evolution of MgFe₂O₄ nanocrystals was followed by powder X-ray diffraction and IR absorption spectroscopy. The formation of spinel structure of MgFe₂O₄ started at 800 °C, and completed at 900 °C. The transmission electron microscopy (TEM) measurements suggest that the particle sizes increase with the increasing annealing temperature, and the mean particle sizes of the spherical samples annealed at 800 °C, 900 °C and 1 050 °C are ca. 3 nm, 8 nm and 11 nm, respectively. Magnetization measurements at room temperature and 78 K indicate superparamagnetic nature of these MgFe₂O₄ nanocrystals. Funded by the National Natural Science Foundation of China(No. 30771676), the Natural Science Foundation of Jiangsu Province (No. BK20081842), and the Foundation of Nanjing Bureau of Personal for the Returned Overseas Chinese Excellent Scholars     

Synthesis of carbon nanotubes using Cu-Cr-O as catalyst by chemical vapor deposition

A novel powder catalyst Cu-Cr-O applied to the synthesis of carbon nanotubes(CNTs) was developed, which was prepared via ammonia precipitation method. Techniques of thermo-gravimetric/ differential scanning calorimeter(TG-DSC), X-ray diffraction(XRD) as well as scanning electron microscopy(SEM) and transmission electron microscopy(TEM) have been employed to characterize the thermal decomposition procedure, crystal phase and micro structural morphologies of the as-synthesized materials, respectively. The results show that carbon nanotubes are successfully synthesized using Cu-Cr-O as catalyst when the precursors are calcined at 400, 500, 600, and 700 ℃. The results indicate that the calcination of the Cu-Cr-O catalyst at 600 ℃ is an effective method to get MWCNT with few nano-tube defects or amorphous carbons.     

Low-temperature sintering of FeCuCo based pre-alloyed powder for diamond bits

We studied the effects of sintering temperature on FeCuCo based pre-alloyed powder for diamond bits.The FeCuCo composite was fabricated by co-precipitation method.With the addition of tungsten carbide(WC),sintering under different temperatures was investigated.Mechanical properties of the FeCuCo based matrix were systematically studied.The structure of the composite was evaluated by X-ray diffraction(XRD) and scanning electron microscope(SEM) was used to analyze the surface of the powder and matrix.The suitable sintering temperature was determined through differential scanning calorimeter(DSC).Micro drilling experiments were performed,and 820 ℃ was identified to be the ideal sintering temperature,at which the matrix shows the best mechanical properties and drilling performance.     

Spark Plasma Sintering Preperties of Ultrafine Ti （ C, N）-based Cermet

Ultrafine Ti( C, N)-based cermet was sintered by SPS from 1050℃ to 1450℃ and its sintering properties, such as porosity, mechanical properties and phase transformation , were investigated by optical microscopy ( OM ), scanning electron microscopy (SEM), X-ray diffraction ( XRD ), and differential scanning calorimeter (OSC). It is found that the spark plasma sintering properties of Ti ( C, N )-based cermet differ from those of conventional vacuum sintering. The liquid phase appearance is at least lower by 150℃ than that in vacuum sintering. The porosity decreases sharply belove 1200℃ and reaches minimum at 1200℃ , and afterwards it almost keeps invariable and no longer increases. SPS remarkably accelerates the phase transformation of Ti ( C, N )-based cermet and it has a powerful ability to remorse oxides in Ti( C, N)-based cermets. Above 1350℃, denitrification occurred. Fresh graphite phase formed above 1 430℃ . Both the porosity and graphite are responsible for the poor TRS.     

Effect of TiO2 addition on zirconia-mullite composites fabricated by in-situ controlled crystallization of Si-Al-Zr-O amorphous bulk

Zirconia-mullite composite ceramics were fabricated by in-situ controlled crystallization of Si-Al-Zr-O amorphous bulk.The effects of TiO2 addition on the fabrication of zirconia-mullite composites were investigated.The ultra-fine zirconia-mullite composite ceramics were prepared from the amorphous bulk treated at 980 °C for nucleation and 1 140 °C for crystallization.The phase transformation of the ceramics was examined using differential scanning calorimetry (DSC) and X-ray diffractometry (XRD).The micros...     

Preparation of IrO_2 MnO_2 coating anodes and their application in NaClO production

To improve the durability as well as to reduce the cost of anodes, the IrO2 MnO2 composite coating anodes for NaClO production were prepared by thermal decomposition. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and X-ray diffraction analysis (XRD) were carried out to investigate the morphologies, element distribution, and microstructure. The anodic polarization curves were employed to study the effect of sintering temperature on the Cl2 evolution reaction (CER) of the electrodes. The accelerated life tests (ALT) and electrochemical impedance spectroscopy measurement (EIS) were utilized to investigate the stability. The rules of NaClO production were also studied by the static electrolysis experiment. The results indicate that sintering temperature has a significant influence on the CER properties as well as the ALT values of the electrodes. The electrode prepared at 400°C has the best CER properties and the longest ALT value.     

Characteristics of Self-Healing Microcapsules for Cementitious Composites

Urea formaldehyde/epoxy resin microcapsules were prepared by an in situ polymerization method and the effect of emulsifier on the syntheses process of the microcapsules was discussed. The surface morphology of the microcapsules was observed by optical microscopy and scanning electron microscopy(SEM). Chemical structure was characterized by Fourier transform infrared spectroscopy(FTIR). Thermal stability was obtained using simultaneous thermal analysis(STA). The microcapsules were composed of urea-formaldehyde resin shell and epoxy resin core. Emulsifier played an important role in the polymerization process when the core material was packed by pre-polymer, so the effects of different emulsifiers(OP-10, SDS and SDBS) were discussed respectively. Results showed that the particle size of the microcapsules was uniform when SDBS as an emulsifier. Microcapsules showed good thermal stability below 240 ℃ and the initial decomposition temperature of the microcapsules was 265 ℃. The core materials released after microcapsules rupturing, which could be proven by the images of SEM. When implanted in cementitious composites, complete shape of microcapsules and good interface between microcapsules and cement specimen substrate could also be observed.     

Synthesis of n-alkane mixture microcapsule and its application in low-temperature protective fabric

We investigated synthesis and characterization of melamine-urea-formaldehyde(MUF) microcapsules containing n-alkane mixture as phase change core material for thermal energy storage and low-temperature protection. The phase change microcapsules(microPCMs) were prepared by an in situ polymerization using sodium dodecyl sulfate(SDS) and polyvinyl alcohol(PVA) as emulsifiers. Surface morphology, particle size, chemical structure, and thermal properties of microPCMs were, respectively, characterized by using scanning electron microscopy(SEM), field emission scanning electron microscopy(FESEM), Fourier transform infrared spectroscopy(FT-IR), differential scanning calorimetry(DSC), and thermal gravimetric analysis(TGA). Low-temperature resistance performances were measured at-15,-30,-45, and-60 ℃ after microPCMs were coated on a cotton fabric by foaming technology. The results showed that spherical microPCMs had 4.4 μm diameter and 100 nm wall thickness. The melting and freezing temperatures and the latent heats of the microPCMs were determined as 28.9 and 29.6 ℃ as well as 110.0 and 115.7 J/g, respectively. Encapsulation of n-alkane mixture achieved 84.9 %. TGA analysis indicated that the microPCMs had good chemical stability below 250 ℃. The results showed that the microencapsulated n-alkane mixture had good energy storage potential. After the addition of 10 % microPCMs, low-temperature resistance duration was prolonged by 126.9%, 145.5%, 128.6%, and 87.5% in environment of-15,-30,-45 and-60 ℃, respectively as compared to pure fabric. Based on the results, phase change microcapsule plays an effective role in lowtemperature protection field for the human body.     

基于PVP模板剂水热法制备TiO_2纳米管

以聚乙稀吡咯烷酮(PVP)为模板剂,钛酸四正丁酯为钛源,水热法制备TiO2纳米管.分别采用X射线粉末衍射仪(XRD)、红外光谱仪(FT-IR)、透射电子显微镜(TEM)和比表面积孔径分析仪对产物的晶相、结构、形貌、比表面积和孔径分布进行了表征.考察了所制备TiO2纳米管的水热稳定性和热稳定性.结果表明:用PVP为模板剂能制得高比表面积的TiO2纳米管,其管径约在6～8 nm之间.所制备的TiO2纳米管,100℃水热处理7 d,500℃焙烧3 h后,TiO2纳米管的结构没有被破坏,说明制备出了具有较高的热稳定性和水热稳定性的TiO2纳米管.     

Preparation of Superfine-Cemented Carbide by Spark Plasma Sintering

92WC-8Co puwder mixture with superfine-tungsten carbide was respectively sintered by spark plasma sintering（ SPS ） and sintering isostutic pressure （SIP）. Complete dense samples with 200 nm WC grains and 94.2HRA hardness were prepared by spark plasma sintering at 1 150 ℃ and under 4.5 kN for 5 minutes. SIP was carried out at 1 400 ℃ for 30 minutes with a result of 300-400 nm WC grains and 93 HRA hardness. The results show that sintering temperature is greatly decreased by SPS, sintering time is largely shortened and WC grain growth is effectively retarded. Micropores and drawb（wks in superfine-cemented carbide made by SPS are greatly declined, which is very useful to improving nwehanical properties.