球磨对碳化硼粒度及游离碳的影响

主要研究球磨因素对碳化硼粒度分布的影响,并考察游离碳含量随球磨时间的变化规律.实验结果表明：随着球磨时间增加,碳化硼粒径分布曲线向粒径小的方向移动,当球磨时间达到60 h,粉体粒径细化程度减缓,继续球磨可进一步提高超细颗粒含量;当球磨时间达到一定程度,不同的球料比对粉体粒径分布曲线影响较小;游离碳含量随着球磨时间增加而提高,在20～40 h碳含量增加显著,之后增加缓慢;SEM电镜显示球磨前后粉体显微形貌发生显著变化;XRD分析显示球磨60 h后粉体中出现很强的游离碳衍射峰.     

Synthesis of nanocrystalline NiCrC alloy feedstock powders for thermal spraying by cryogenic ball milling

Nanocrystalline NiCrC alloy powders with a qualified particle size distribution for thermal spraying were synthesized us-ing the cryogenic ball milling (cryomilling) method.The morphology,microstructure,size distribution,and phase transformation of the powders were characterized by scanning electron microscopy (SEM),laser scattering for particle size analysis,X-ray diffraction (XRD),and transmission electron microscopy (TEM).After cryomilling for 20 h,the average grain size of the as-milled powders ap-proached a constant value of 30 nm by XRD measurement.The average particle size slightly increased from 17.5 to 20.3 μm during the 20-h milling.About 90vo1% of the powders satisfied the requirement for thermal spraying with the particle dimension of 10-50 grn,and most of the powders exhibited spherical morphology,which were expected to have good fluidity during thermal spraying.The Cr2O3 phase formed during the cryomilling process as revealed in the XRD spectra,which was expected to enhance the thermal stability of the as-milled powders during the followed thermal spraying or other heat treatment.     

球磨法制备Si-C-N/Ni纳米粉

以Si-C-N纳米粉和Ni微粉为原料,利用高能球磨法制备Ni包覆Si-C-N纳米粉.Si-C-N纳米粉由原始的灰色转为包覆后的深黑色,Ni除包覆在Si-C-N纳米粉体表面,部分还在复合粉体之间形成了粉体之间的镶嵌和塑性连接.实验结果表明:球磨时间是影响包覆粉体粒度的重要条件,在10h内,球磨时间长,粉体粒径小,最小粒径约为100nm.球磨时,液相载体正己醇的加入改善了复合粉体分散性,并且纳米粉体保持了一定的非晶性质.     

热处理工艺参数对T12钢碳化物球化的影响

用正交试验法研究了奥氏体化温度、保温时间、等温温度3个热处理工艺参数对T12钢碳化物球化的影响,以碳化物的粒化程度和硬度值为目标,通过极差分析和方差分析得出:奥氏体化温度是影响T12钢碳化物球化的最主要因素,保温时间和等温温度是次要影响因素;在755℃保温1 min后以690℃等温的热处理工艺为T12钢较优球化退火工艺。利用较优球化退火工艺处理后的试样得到了碳化物细小均匀的球状珠光体组织。     

热处理工艺参数对T12钢碳化物球化的影响

用正交试验法研究了奥氏体化温度、保温时间、等温温度3个热处理工艺参数对T12钢碳化物球化的影响,以碳化物的粒化程度和硬度值为目标,通过极差分析和方差分析得出：奥氏体化温度是影响T12钢碳化物球化的最主要因素,保温时间和等温温度是次要影响因素;在755℃保温1min后以690℃等温的热处理工艺为T12钢较优球化退火工艺。利用较优球化退火工艺处理后的试样得到了碳化物细小均匀的球状珠光体组织。     

Effect of Heat Treatment on Crystallization of Nd:YAG Ceramics

(Nd0.01 Y0.99 )3 Al5 O12 nano-sized powders were synthesized by low temperature combustion (LCS),using Nd2 O3 ,Y2 O3 ,Al(NO3)3 ·9H 2 O,ammonia water and citric acid as starting materials.The powders were characterized by TG-DTA,XRD,FT-IR,ICP and TEM,respectively.The grain sizes were calculated by the Scherrer’s formula using the full width at half maximum(FWHM)of YAG(420)crystal plane diffraction lines. The study focused on crystallization of ceramics at different heat treatment temperatures.The experimental results show that crystallizing temperature of YAG is 850℃,and the intermediate crystal phase YAP,appearing during heat treatment,transforms to YAG cubic crystal phase at the temperature of 1 050℃.The particle size of the powders synthesized by LCS is nano-sized.With the temperature increasing,the mean grain sizes raise,the stand deviations keep almost at the value of 2.0 and the lattice parameters decrease.The grains mainly grow by grain boundary diffusion.The lattice parameter expansion is caused by an increase of the repulsive dipolar interactions on surfaces of crystallites.     

GCr15钢奥氏体化过程组织转变的动力学模型

根据扩散和相变动力学的基本理论,采用定量金相法研究GCr15钢的奥氏体化过程。分析奥氏体化后未溶碳化物体积分数和颗粒尺寸与奥氏体化加热温度及保温时间之间的关系,建立奥氏体化后剩余碳化物体积分数和碳化物平均粒径的数学模型。计算和分析结果表明：模拟曲线与实验数据基本符合;奥氏体化温度越高,保温时间越长,剩余碳化物体积分数越小,碳化物平均粒径也越小。该模型能够预测一定奥氏体化条件下剩余碳化物体积分数和平均粒径。     

Effects of Solid-State Reaction Synthesis Processing Parameters on Thermoelectric Properties of MgaSi

The Mg2 Si-matrix thermoelectric material was stnthesized by low temperature solid-state renc-tion.This paper studies the effects of holding time and reaction temperatare on the particle size and the properties of the material, and also studies effects of doping elemental Sb, Te and their doping seqence on the properties of the materiol. The result shows that excessirely high temperature and elongated holding time of solid-state reaction are harmful, there is a range of partiele size to ensure optimum properties and the doping sequence of Sb or Te without influencing the properties.     

The flowability of ground powders and the comminuting mechanism of mills

The ground powders with the same particle size distribulion and the sanw mean particle diameter were prepared by five different types of mills. The flowability index (FI) and the particle shape indices, namely. Wadell‘s working sphericity ψw and circularity ψc , of five kinds of test powders were nwasured. The effect of the comminuting mechanisms on the flowability of ground powders was investigated, and the relationship between the flowability of ground powders and the partticle shape indices was analyzed. The experimental restdts show that the ground turn,tiers obtained by collision have irregular particle shapes and smooth surfaces, showing a high flowability. On the other hand, though the particle obtained by grinding is close to a spherical particle, but it has a rugged suttee, and shows a bad flowability. Furthermore, the flowability index is more corrdated with the circularity titan the working sphericity is. This means that the surface roughness is more effective, in determining the flowability of powders than the roundtwss is.     

Fabrication and plasma arc thermal shock resistance of HfB2-based ultra high temperature ceramics

Two hafnium diboride based ceramic matrix composites containing 20% (volume fraction) SiC particle and with or without AlN as sintering additives were fabricated by hot-pressed sintering. The mechanical properties and microstructures of these two composites were tested and the thermal shock resistances were evaluated by plasma arc heater. The results indicate that the composite with AlN as sintering additive has a denser and finer microstructure than composite without sintering additive, and the mechanical properties, thermal shock resistance of the composite with AlN as sintering additive are also higher than those of the composite without AlN. Microstructure analysis on the cross-section of two composites after thermal shock tests indicates that a compact oxidation scale contains HfO₂ and Al₂O₃ liquid phase is found on the surface of composite with AlN, which could fill the voids and cracks of surface and improve the thermal shock resistance of composite.     

Synthesis of high pure Ti3AlC2 and Ti2AlC powders from TiH2 powders as Ti source by tube furnace

Titanium aluminum carbide (Ti₃AlC₂ and Ti₂AlC) powders were synthesized from TiH₂ powders instead of Ti powders as Ti source by a tube furnace under argon atmosphere without preliminary dehydrogenation. 95 wt% pure Ti₃AlC₂ powders were synthesized from TiH₂/1.1Al/2TiC at 1 450 °C for 120 min. High-purity Ti₂AlC powders were also prepared from 3TiH₂/1.5Al/C and 2TiH₂/1.5Al/TiC powders at 1 400 °C for 120 min. The as-synthesized samples were porous and easy to be ground into powders. Sn or Si additives in starting materials increased the purity of synthesized Ti₃AlC₂ obviously and expanded the temperature range for the synthesis of Ti₃AlC₂. With Si or Sn as additives, high pure Ti₃AlC₂ was synthesized at 1 200 °C for 60 min from TiH₂/x Si/Al/2TiC and TiH₂/x Sn/Al/2TiC (x = 0.1, 0.2), respectively.     

Enhancement of the hydrogen storage properties of Mg/C nanocomposites prepared by reactive milling with molybdenum

The effect of Mo on the morphology, crystal structure and hydrogen sorption properties of Mg/C composites prepared by reactive milling was studied. Transmission electron microscopic(TEM) observation shows that Mg/C composites prepared with the addition of Mo are of nanoscale with particle size about 20-120 nm after 3 h of milling under 1 MPaH_2. MgH_2 of tetrahedral crystal structure predominates in the materials with the geometric shape of oblique hexagonal prism. From X-ray diffraction(XRD) and hydrogen content studies, Mo and crystallitic carbon have a synergistic effect on promoting the hydrogenation rate in the reactive milling process. From differential scanning calorimetric(DSC) studies, the dehydrogenation peak temperature of the Mg/C materials with Mo is lowered to 299-340 ℃.     

Synthesis and characterization of bismuth-doped tin dioxide nanometer powders

Bismuth-doped tin dioxide nanometer powders were prepared by co-precipitation method using SnCl4 and Bi（NO3）3 as raw materials. The effects of calcining temperature and doping ratio on the particle size, composition, spectrum selectivity of bismuth-doped tin dioxide and the phase transition of Bi-Sn precursor at different temperatures were studied by means of X-ray diffraction, transmission electron microscopy, ultraviolet-visual-near infrared diffuse reflection spectrum and the thermogravimetric-differential scanning calorimetry. The results show that prepared bismuth-doped tin dioxide powders have excellent characteristics with a single-phase tetragonal structure, good dispersibility, good absorbency for ultraviolet ray and average particle size less than 10 nm. The optimum conditions for preparing bismuth-doped tin dioxide nanometer powders are as follows： calcining temperature of 600℃, ratio of bismuth-doped in a range of 0. 10 - 0.30, and Bi-Sn precursor being dispersed by ultrasonic wave and refluxed azeotropic and distillated with mixture of n-butanol and benzene. The mechanism of phase transition of Bi-Sn precursor is that Bi^3＋ enters Sn-vacancy and then forms Sn-O-Bi bond.     

Crystal structure and hydrogen storage behaviors of Mg/MoS<Subscript>2</Subscript> composites from ball milling

The Mg/MoS₂ composites were prepared by ball milling under argon atmosphere, and the effect of MoS₂ on the crystal structure and hydrogen storage properties of Mg was investigated. It is found that 10 wt% of MoS₂ is sufficient to prevent particle aggregation and cold welding during the milling process. The crystallite size of Mg will remain constant at slightly less than 38.8 nm with the milling process due to the size confinement effect of MoS₂. The dehydrogenation temperature of MgH₂ is reduced to 390.4-429.4 °C due to the crystallite size reduction. Through fitting by Johnson-Mehl-Avrami model, it is found that Mg crystal grows by three dimension controlled by interface transformation during the process of MgH₂ decomposition. MoS₂ has a weak catalyst effect on the decomposition of MgH₂ and activation energy of 148.9 kJ/mol is needed for the dehydrogenation process calculated by the Arrhenius equation.     

共沉淀法制备Tb_3Sc_2Al_3O_(12)纳米粉体的研究

采用共沉淀法制备TSAG纳米粉体,确定粉体制备的最佳工艺条件。以NH_4HCO_3为沉淀剂,通过反滴定法获得了TSAG前驱体,通过TG-DSC,XRD,FTIR和SEM测试手段对不同温度和不同保温时间下煅烧的粉体进行了表征。结果表明:前驱体在800℃时为非晶态,在800℃~900℃之间形成中间晶相TbScO_3和TbAlO_3,1200℃下煅烧6h得到TSAG粉体,所得到的TSAG纳米粉体纯度高、粒径分布均匀,晶粒尺寸约50nm。     

Preparation of Fe-Al Intermetallie /TiC-Al2O3 Ceramie Composites from llmenite by SHS

Fe-Al intermetallic/TiC-Al2O3 ceramic composites were successfully prepared by selfpropagating high-temperature synthesis （SHS） from natural ilmenite, aluminium and carbon as the raw materials. The effects of carbon sources, preheating time and heat treatment temperature on synthesis process and products were investigated in detail, and the reaction process of the FeTiO3-Al-C system was also discussed. It is shown that the temperature and velocity of the combustion wave are higher when graphite is used as the carbon source, which can reflect the effect of the carbon source structure on the combustion synthesis; Prolonging the preheating time or heat treatment temperature is beneficial to the formation of the ordered intermetallics; The temperature and velocity of the combustion wave are improved, but the disordered alloys are difficult to eliminate with the preheating time prolonged. The compound powders mainly containing ordered Fe3Al intermetallic can be prepared through heat treatment at 750 ℃.     

Molten Salt Synthesis of Ba（ Mgl／3Nb2／3 ）O3 Powder

The single-phrase Ba(Mgl/3Nb2/3)O3(BMN) powder was saccessfully prepared by the KCImolten salt synthesis(MSS) method. The temperature for single-phase BMN powders by MSS was about 400℃ lower than that by the solid-phase method. The average particle size (APS) was about 0.91,u.m at 900℃ and increased with increasing synhesis temperature. Based on the APS, the activation energy for particle growth in theMSS, whose value was 64. 1kJmol^-1.was attained. The sinterability of the powder prepared by MSS method wasbetter than that pretared by solid-phase method.     

Effects of mechanical activation on the structural changes and microstructural characteristics of the components of ferruginous quartzite beneficiation tailings

The effects of mechanical activation in a planetary mill on the structural changes and microstructural characteristics of the components of ferruginous quartzite beneficiation tailings generated by wet magnetic separation process were studied using X-ray and laser diffraction methods. The results revealed the relationship between variations in the mean particle size of activated powders and the milling time. The crystallite size, microstrain, lattice parameters and unit cell volumes were determined for different milling times in powder samples of quartz, hematite, dolomite, and magnetite from the beneficiation tailings. The main trends in the variation of the crystallite size of quartz, hematite, dolomite, and magnetite as a function mean particle size of powder samples were revealed. Changes in the particle shape as a function of the activation time was also investigated.     

Phase transformation of nano-grained W(Co, C) composite powder and its phase constitute

1 INTRODUCTION Nano-grained WC-Co cemented carbides with high toughness and high hardness have drawn extensive attention of hard metal industry[1?2]. There are two key processes for the fabrication of this high performance alloy[3?4]. One is the preparation of nanometer WC-Co composite powders, the other is the effective control of grain growth during sintering. At present, great technical breakthrough has been achieved in the preparation of nanometer powders. The typical methods of na…     

机械合金化制备碳化钛纳米粉体的合成机理研究

本研究中,以金属钛（Ti）粉与环己烷为原料,利用机械合金化制备了碳化钛（TiC）纳米粉体。利用X射线衍射并结合Rietveld精修对球磨产物进行定性与定量分析;借助透射电子显微镜对产物进行形貌与元素以及结晶性进行分析;对球磨过程中TiC的合成机理进行了研究。结果表明,球磨产物中主相为TiC,另有少量残留的氢化钛（TiH2）与Ti;所制备TiC粉体易于团聚、颗粒度均匀、结晶性良好;TiC合成机理属于扩散型机制。