In Situ Treatment of Thermal RF Plasma Processed Nanopowders to Control their Agglomeration and Dispersability

Titanium carbonitride nanoparticles have been produced in an inductively coupled thermal plasma and subsequently modified using a surfactant that has been deposited in situ on their surface in-flight. The surfactant was injected in the reactor while the nanoparticles are still dispersed in the gas phase, allowing the coating of primary particles instead of the corresponding agglomerates. In contrast to naked TiCN nanoparticles, the surfactant coated particles could be readily dispersed in water with a short ultrasonic treatment and built up no large agglomerates as proved by Photon Correlation Spectroscopy measurements. The investigated surfactants seem, however, to undergo a chemical modification and/or a thermal degradation at the surface of the TiCN nanoparticles.     

油酸包覆纳米铝粉/黑索今复合体系的热行为及非等温分解反应动力学

在氮气气氛下,采用油酸(OA)对纳米铝粉(nmAl)进行了表面包覆处理,采用扫描电镜(SEM)、X射线衍射(XRD)和傅里叶变换红外(FTIR)光谱对其形貌和结构进行了表征.用差示扫描量热(DSC)对油酸包覆前后的纳米铝粉与黑索今(RDX)构成的复合体系[nmAl/RDX和(nmAl+OA)/RDX]的热分解反应动力学进行了研究,得到了动力学参数和动力学方程.结果表明,大量油酸以物理吸附的方式吸附在纳米铝粉表面,少量油酸与纳米铝粉表面铝原子发生了化学反应,以化学键合的形式附着在纳米铝粉表面.与nmAl/RDX复合体系相比,(nmAl+OA)/RDX复合体系在不同升温速率下的分解峰峰温都相对降低,分解反应的表观活化能(Ea)和指前因子(A)分别为141.18kJ·mol-1和1012.57s-1,分解反应机理为三维扩散,服从n=1/2的Jander方程,其动力学方程为dα/dt=1013.35(1-α)2/3[1-(1-α)1/3]1/2e-16981.0/T.     

粘土层间距对粘土/环氧树脂插层复合材料热机械性能的影响

研究了混料温度对蒙脱土／环氧树脂复合材料相关性能的影响。用X射线衍射表征了复合材料的层间距，并且在动态热机械分析仪（DMTA）上用不同的模式表征了不同层间距的插层复合材料的性能。测试结果表明，混料温度对蒙脱土／环氧树脂插层复合材料的热机械性能有一定的影响。插层后蒙脱土／环氧树脂的软化温度提高了11℃，弹性模量也有相应的提高。     

The Influence of the Thermal Behaviour of AgGaS2 on the Crystal Growth Process

Differential thermal analysis has been carried out on AgGaS₂ samples in order to investigate the relationship between the superheating of the melt and the supercooling behaviour of the material leading to an improvement of crystal growth conditions. The knowledge gained will be correlated to the crystal growth experiments which had been carried out by using the gradient freezing method.This revised version was published online in November 2005 with corrections to the Cover Date.     

A Study of PbTiO3 Crystallization in Pure and Composite Nanopowders Prepared by the Sol-Gel Technique

Summary.  In this investigation the crystallization of PbTiO₃ upon annealing of pure nanopowders and PbTiO₃–SiO₂ (1:1 v/v) nanocomposite powders prepared by the sol-gel technique was studied. Using X-ray diffraction phase analysis, the start of PbTiO₃ crystallization in pure PbTiO₃ powders was detected at 400°C. Distinct crystallization of PbTiO₃ in PbTiO₃–SiO₂ nanocomposites starts at 700°C, whereas SiO₂ remains amorphous. There are indications that an interface interaction between the PbTiO₃ and the SiO₂ phase plays an important role in hindering the crystallization of PbTiO₃. The particle size (size of coherently scattering regions) was estimated from the broadening of the X-ray diffraction line profiles. The average size of PbTiO₃ nanocrystallites increases with temperature and time of annealing, the influence of temperature being more significant than that of the annealing time. Differential scanning calorimetry confirmed the results of the X-ray diffraction with respect to the start of the crystallization. Laser beam scattering and scanning electron microscopy provided the statistical distribution of the grain size and the morphology of the powder grains, showing that each grain of the powders contains several nanocrystallites (coherently scattering regions). Received October 4, 2001. Accepted (revised) December 14, 2001     

Crystal Orientation Mapping Applied to the Y-TZP/WC Composite

 Crystal orientation measurements made by electron backscattered diffraction (EBSD) in the scanning electron microscope (SEM) and microscopic observations provided the basis for a quantitative investigation of microstructure in an yttria stabilised, tetragonal zirconia-based (Y-TZP) composite. Automatic crystal orientation mapping (ACOM) in a SEM can be preferable to transmission electron microscopy (TEM) for microstructural characterisation, since no sample thinning is required, extensive crystal data is already available, and the analysis area is greatly increased. A composite with a 20 vol.% tungsten carbide (WC) content was chosen since it revealed crystal relationships between the matrix and carbide phase already established by TEM analysis. However, this composite was difficult to investigate in the EBSD/ SEM since it is non-conductive, the Y-TZP grain size is of the order of the system resolution, and the sample surface, though carefully prepared, reveals a distinctive microtopography. In this paper, some useful solutions to these problems are discussed and the resulting data, which confirm crystal correlations previously established by TEM analysis, are presented.     

热处理对TiO2纳米管结构相变的影响

TiO₂纳米管为无定形结构,焙烧后则由无定形转变为锐钛矿型,纳米管的管状结构被破坏,晶型转变是TiO₂纳米管的管状结构破坏的根本原因.经热处理,原来的TiO₂纳米管部分转变为长棒状的金红石型晶柱结构,而原料TiO₂在较大温度范围内焙烧均未出现长棒状晶柱结构;TiO₂由A→R的相变温差很大,TiO₂纳米管的A→R相变温度比原料约低350℃;合成的TiO₂纳米管的比表面积和孔体积很大.     

Exploring the Microstructure of YBCO Nanopowders

High temperature superconductor YBa2Cu3O7-π (YBCO) nanopowders were successfully prepared by a citrate pyrolysis technique. The phase formation and microstructure of the nanopowders were studied. The microstructure analysis shows that the obtained YBCO powders have very fine grains with a size around several tens of nanomaters. The suoerfine morphology reveals that the thermal agglomeration of the particles decreases with decreasing the annealing temperature and shortening the annealing time. In addition, the complete phase formation of YBCO depends upon the annealing temperature and the annealing time as well. So far, these nanopowders have been used to fabricate the melt-textured YBCO bulk materials.     

A Study of PbTiO3 Crystallization in Pure and Composite Nanopowders Prepared by the Sol-Gel Technique

 In this investigation the crystallization of PbTiO₃ upon annealing of pure nanopowders and PbTiO₃–SiO₂ (1:1 v/v) nanocomposite powders prepared by the sol-gel technique was studied. Using X-ray diffraction phase analysis, the start of PbTiO₃ crystallization in pure PbTiO₃ powders was detected at 400°C. Distinct crystallization of PbTiO₃ in PbTiO₃–SiO₂ nanocomposites starts at 700°C, whereas SiO₂ remains amorphous. There are indications that an interface interaction between the PbTiO₃ and the SiO₂ phase plays an important role in hindering the crystallization of PbTiO₃. The particle size (size of coherently scattering regions) was estimated from the broadening of the X-ray diffraction line profiles. The average size of PbTiO₃ nanocrystallites increases with temperature and time of annealing, the influence of temperature being more significant than that of the annealing time. Differential scanning calorimetry confirmed the results of the X-ray diffraction with respect to the start of the crystallization. Laser beam scattering and scanning electron microscopy provided the statistical distribution of the grain size and the morphology of the powder grains, showing that each grain of the powders contains several nanocrystallites (coherently scattering regions).     

添加提钒尾渣对膨胀石墨/石蜡复合相变材料稳定性和导电性的影响

以不同膨胀石墨(EG-300、EG-350和EG-400)为支撑材料,石蜡(PW)为相变主材,提钒尾渣(VT)为导电强化剂,采用熔融共混法制备复合相变材料,并对复合材料的稳定性和导电性进行测试分析.结果表明,进行60次热循环,EG/PW复合材料质量损失率小于0.03％,VT/EG/PW复合材料质量损失率小于0.08％,...     

热处理对聚乙烯／炭黑导电复合体系形态结构及PTC特性的影响

借助ＷＡＸＤ、ＳＡＸＤ和ＤＳＣ等手段研究了炭黑与聚乙烯复合体系在不同热处理条件下的结晶行为及聚集态结构的大尺寸效应对ＰＴＣ特性的影响。由此提出，不仅结晶度大小，而且聚集大尺寸效应性能对ＰＴＣ行性有重要影响的新观点。     

稀土复合弹性材料的抗热氧化作用

利用稀土醇盐与ＰＳＢＲ橡胶乳液进行反应获得含稀土复合弹性材料进行抗热氧化研究,发现这种复弹性在热氧化后力学性能的保持率比参照样品有明显的提高,热重量试验表明含稀土复合弹性材料的热分解温度大幅度上升,经过氧化机制,认为抗热氧化效率的原因主要是稀土元素具有中止自动化链式反应的作用以及形成的络合结构有阻碍氧化的立体效应。     

The Influence of Mechanical Milling and Subsequent Calcination on the Formation of Lithium Ferrites

The influence of ball milling and subsequent calcination of a 2.5:1 molar mixture of α-Fe₂O₃ and Li₂CO₃ on the formation of lithium ferrites has been investigated. Premilling was found to considerably lower the temperature at which the lithium ferrites LiFeO₂ and LiFe₅O₈ are formed. A β-to-α phase transition in LiFe₅O₈ was found to take place on cooling from ca. 1000°C depending on the milling history and cooling regime.     

还原热处理对铈锆铝复合氧化物性能的影响

采用共沉淀法制备铈锆铝复合氧化物(CeO2-ZrO2-Al2O3,CZA)和铈锆复合氧化物(CeO2-ZrO2,CZ),将样品分别在空气和10%H2/Ar气氛下进行热处理,利用X射线粉末衍射(XRD)、O2脉冲吸附、H2程序升温还原(H2-TPR)等手段研究了复合氧化物的结构及性能.结果表明:CZA样品经950℃还原热处理后出现CeAlO3晶相,热处理温度越高,越有利于CeAlO3物相生成.CZA储氧量(OSC)随着还原热处理温度升高逐渐增大,至900℃达到1270.3μmo·lg-1;温度继续升高,OSC减小,1100℃还原热处理后CZA的OSC仅为23.2μmo·lg-1.研究发现还原热处理中形成CeAlO3,其显著影响CZA样品的储氧性能和还原性能.     

二元-三元羧酸镧复合热稳定剂的制备和应用

以常见的二元羧酸和三元羧酸以及硝酸镧为原料,制备了一系列二元-三元羧酸镧复合热稳定剂产品。通过刚果红试纸法和转矩流变仪法对产品的性能进行了表征,结果表明,己二酸-柠檬酸镧和癸二酸-氨三乙酸镧对PVC的热稳定性最好,动态热稳定时间分别为1 080 s和1 188 s。用五因素三水平正交试验优选出两组较优配方,对PVC的静态热稳定时间分别可达93 min和85 min。     

Thermal decomposition of native cellulose: Influence on crystallite size

The thermal degradation behavior of crystalline cellulose has been investigated using thermogravimetry, differential thermal analysis, and derivative thermogravimetry in a nitrogen atmosphere. Three cellulose samples, Halocynthia, cotton, and commercial microcrystalline cellulose Funacel, were used in this study to analyze the influence on crystallite size. They all belongs to cellulose I_β type and those crystallite sizes calculated from the X-ray diffractometry profiles by Scherrer equation were very different in the order Halocynthia > cotton > Funacel. The thermal decomposition of cellulose shifted to higher temperatures with increasing crystallite size. However, activation energies for the thermal degradation were the almost the same among the samples: 159-166 kJ mol⁻¹. These results indicated that the crystal structure does not affect the activation energy of the thermal degradation but the crystallite size affects the thermal degradation temperature.     

AgSt/AgBr复合物的制备及其热行为研究

分别以溴化钠(NaBr)为溴源、硬脂酸银(AgSt)为底物,用原位法合成了复合物AgSt/AgBr.利用红外光谱(FTIR)、扫描电子显微镜(SEM)、X射线衍射(XRD)与热重-差示扫描量热(TG-DSC)技术对复合物的结构、尺寸、形貌、晶型以及热行为进行了表征.结果表明,1)复合物由底物AgSt与尺寸为30—50nm的外延立方体AgBr粒子构成;2)AgSt/AgBr复合物在较低的温度下出现两个新的吸热相变峰,分别对应于97.8℃和108.8℃;3)AgSt/AgBr复合物的起始分解温度较AgSt也有所降低.