激光快速烧结合成A(WO4)2(A=Zr2+,Hf2+)的特性研究

利用二氧化碳激光快速凝固技术合成了负热膨胀材料ZrW2O8和HfW2 O8,Raman光谱和X射线衍射分析表明激光烧结合成的ZrW2 O8为正交相,压应力的大小估计在0.4～0.5 GPa之间,激光烧结合成的HfW2 O8,主要为立方晶系,含有极少量的正交系,压应力的大小估计在0.6 GPa左右,这是由于样品在快速凝固的过程中受到了压应力造成的.由于压应力的影响,二氧化碳激光快速凝固技术更适合HfW2O8的制备和合成.     

Factors influencing particle agglomeration during solid-state sintering

Discrete element method(DEM) is used to studythe factors affecting agglomeration in three-dimensionalcopper particle systems during solid-state sintering.A newparameter is proposed to characterize agglomeration.Theeffects of a series of factors are studied,including particlesize,size distribution,inter-particle tangential viscosity,temperature,initial density and initial distribution of particleson agglomeration.We find that the systems with smallerparticles,broader particle size distribution,smaller viscosity,higher sintering temperature and smaller initial densityhave stronger particle agglomeration and different distributions of particles induce different agglomerations.This studyshould be very useful for understanding the phenomenon ofagglomeration and the micro-structural evolution during sintering and guiding sintering routes to avoid detrimental agglomeration.     

铝素坯烧结过程微结构演化的实时观测

为实现对金属粉末压坯烧结过程的实时观测,从而验证现有的相关理论,本文利用同步辐射CT(SR-CT)技术,对铝压制陶瓷坯体的固相烧结过程进行实时投影成像;应用滤波反投影算法和数字图像处理技术,得到了陶瓷坯体在整个固相烧结过程中内部微结构演化的三维重建图像,实现了对铝压制陶瓷坯体整个固相烧结过程的无损原位观测,得到了样品由烧结中期进入烧结后期的完整的演化过程图像。通过重建图像,清晰观测了样品的固相烧结过程:在烧结前、中期(烧结时间t<180min、温度T<600℃),烧结颈形成并随烧结时间生长;由烧结中期开始进入后期时(烧结时间t≥180min、温度T≥600℃),样品内部结构演化加剧,气孔由相互连通演化为相互孤立并球化。进一步在实验图像的基础上分析了二面角等烧结特征的变化情况,得到烧结颈尺寸与时间对数有较好的线性关系,并可根据曲线分辨中期、后期。统计了样品在不同烧结时间的孔隙率,得到了孔隙率随烧结时间和烧结时间对数的变化曲线;分析了样品在不同烧结阶段的致密化特点,得到了烧结中期孔隙率和时间对数的线性关系。实验结果验证了现有的烧结理论,并为进一步完善烧结理论以及建立扩散和本构模型提供了高质量的实验数据。     

Enhancement in age hardenability of sintered Ti–5Fe alloy by Zr addition processed by pulsed electric current sintering

The age-hardenable Ti–5Fe–5Zr (wt. %, 5Zr) alloy has been consolidated by pulsed electric current sintering, following a β solution treatment, and the results are compared with a Ti–5Fe (0Zr) alloy. The precipitation sequence measured at 640°C ageing is β?+?athermal ω?→?β?+?isothermal ω?→?β?+?α. At the peak hardness isothermal ω phase forms at 20?s of ageing. The Zr addition retards the precipitation kinetics of the α phase; as a result, the α phase nucleates at latest at 300?s ageing in the overaged state. Fe is partitioned into β, while it is depleted from the α phases. There is Zr enrichment near the α/β interface when the α phase precipitates due to a solute drag effect; the growth rate of the α phase in the 5Zr alloy is significantly reduced compared with that in the 0Zr alloy.     

Suppression of charge ordering and thermal hysteresis of electronic transport and magnetisation in La0.5Ca0.5Mn1−xNixO3

A series of polycrystalline La_0.5Ca_0.5Mn_1?xNi_xO₃ (x = 0.00, 0.025, 0.050, 0.075, 0.100 and 0.125) was synthesised using solid state reaction. Measurements in a cooling and warming cycle between 300 and 80 K were carried out to study the Ni-doping effects on the electrical resistivity, thermopower and magnetisation of single-phase La_0.5Ca_0.5Mn_1?xNi_xO₃. Partial substitution of Ni for Mn leads to the suppression of charge ordering state, the evidence of which is shown by the dramatic decrease in electrical resistivity and thermal hysteresis width in electrical resistivity, thermopower and magnetisation. However, the magnitude of both electrical resistivity and thermopower increases with increasing Ni content. This can be attributed to an increase in the Mn⁴⁺ concentration, which favours the antiferromagnetic state and leads to a gradual disappearance of ferromagnetic double exchange interaction. Besides, the metal–nonmetal transition temperature decreases with increasing Ni content until x = 0.075, which might arise from increased electron–phonon coupling due to less ordered spins at temperatures above ferromagnetic transition. For samples with x greater than 0.075, no metal–nonmetal transition is observed due to the suppression of double exchange mechanism.     

Er,Yb：(LaLu)2O3透明陶瓷制备及上转换发光性能

采用柠檬酸燃烧法制备Er,Yb：（LaLu）₂O₃陶瓷粉体,用X射线衍射对其进行了物相鉴定,研究表明1 000℃时已经得到纯相的（LaLu）₂O₃。采用冷等静压-真空烧结法制备了Er,Yb：（LaLu）₂O₃和Er：（LaLu）₂O₃陶瓷,对陶瓷的结构和光谱性能进行了详细的研究,研究发现掺杂5% Yb³⁺和10% La³⁺样品的上转换发光强度与未掺Yb³⁺、La³⁺样品相比明显增大,根据上转换光谱显示较强发射峰位于564 nm和661 nm处,对应Er³⁺的⁴S_3/2（²H_11/2）→⁴I_15/2能级跃迁和⁴F_9/2→⁴I_15/2能级跃迁,并讨论了Er³⁺-Yb³⁺的能量传递过程及其上转换发光机制。     

采用快速升温烧结方法生长Tl-1223超导薄膜的研究

报道了在铝酸镧(00l)衬底上生长Tl-1223超导薄膜的快速升温烧结方法以及铊(Tl)源陪烧靶的配比对Tl-1223薄膜晶体结构的影响.扫描电子显微镜观测表明,采用快速升温烧结方法生长的Tl-1223超导薄膜具有致密的晶体结构.X-射线衍射等测试表明,采用合适配比的陪烧靶在氩气环境下可以制备出纯c轴取向的Tl-1223超导薄膜,充氧退火后的薄膜具有较好的电学性能,其临界转变温度T_(c onset)达到116K,临界电流密度达到1.5MA/cm~2(77 K,0 T).实验结果表明,采用这一新的烧结方法制备Tl系超导薄膜具有升降温时间和恒温时间短、生产成本低等特点.     

PEG-6000对Mn-Zn铁氧体纳米粉体烧结特性的影响

利用化学共沉淀回流法制备Mn-Zn铁氧体纳米粉体的过程中,加入适量PEG-6000,试图通过在纳米颗粒表面形成一保护层以起到抑制其团聚的目的.研究结果表明,PEG-6000的加入不仅减小了纳米粒子的尺寸,还有效缓解了它们的团聚.将这些纳米Mn-Zn铁氧体粉体进行成型烧结,材料的起始磁导率随烧结温度的升高呈抛物线规律变化,并于1200 ℃达到最大值.而且添加PEG-6000的样品起始磁导率比未添加的提高了约20;.导致这一变化的原因应归咎于纳米粉体稳定性的改善以及烧结后材料内部组织均匀度的提高和晶粒尺寸的减小.     

凝胶注模成型Al2O3陶瓷的显微结构及力学性能研究

以Al2O3粉为原料,TiO2+MgO为烧结助剂,琼脂糖为单体,聚丙烯酸铵为分散剂,利用凝胶注模及无压烧结工艺制备了Al2O3陶瓷.研究了琼脂糖固化机制、烧结助剂作用机理以及琼脂糖含量对Al2O3陶瓷坯体及烧结体的显微结构及力学性能的影响规律.试验结果表明,琼脂糖利用内部氢键的结合,形成三维网络状结构,将Al2O3粉原位凝固成型.TiO2+MgO烧结助剂使材料实现了液相烧结机制,有利于降低材料的烧结温度及促进致密化进程.随着琼脂糖含量增加,坯体的致密度、坯体及烧结体的抗弯强度均呈先增大后减小趋势.当琼脂糖含量为0.5wt;时,Al2O3陶瓷的抗弯强度达到最大值.     

CeO2掺杂KNN-LiNbO3无铅压电陶瓷的压电与介电性能研究

采用传统固相烧结法制备了0.98K0.5Na0.5NbO3-0.02LiNbO3-xCeO2(0.98KNN-0.02LN+xCeO2)无铅压电陶瓷.研究了不同CeO2掺杂含量(x=0、0.01、0.02、0.03、0.04)对0.98KNN-0.02LN陶瓷显微结构和电学性能的影响.研究结果表明:当CeO2掺杂含量从x=0.00到x=0.01和从x=0.02到x=0.03时,样品出现了正交-四方相转变.当x=0.00和x=0.02时,样品都处于正交与四方两相共存状态.CeO2少量掺杂时Ce4+完全进入晶格,表现为"受主"掺杂的特性;而大量CeO2掺杂时,有杂相的生成,主要起到烧结助剂的作用.样品在1080℃下烧结,当掺杂含量为x=0.02时取得最佳的综合性能:d33=104pC/N,Qm=2201,kp=0.24423,εr=804.2,tanδ=8.748;.