Pr1-xCexB6阴极材料的原位反应合成及性能研究

本文以CeH2,PrH2纳米粉和B粉为原料,在无氧环境下采用放电等离子原位反应成功制备了单相多元稀土六硼化物Pr1-xCexB6=（x=0．2—0．8）阴极材料．系统研究了掺杂元素Ce对Pr1-xCexB6的物相组成、力学性能及热电子发射性能的影响．结果表明,当烧结温度为1450℃,烧结压强为50MPa时可制得单相的Pr1-xCexB6多晶块体材料并且该系列样品具有良好的力学性能,维氏硬度和抗弯强度最高值分别达到了24．34GPa和226．02MPa,已达到单晶水平．热电子发射性能结果表明,随着Ce掺杂量的增加Pr1-xCexB6的发射电流密度线性增加．当阴极温度为1973K,外加电压为950V时,Pr0．4Ce0．686最大发射电流密度达到47-3A．cm^-2,该值远高于传统热压烧结法制备的发射电流密度．因此,本文该方法制备的Pr1-xCexB6多晶块体具有良好的力学性能和发射性能,作为热阴极材料将会有很好的应用前景．     

LaB6与TaC混合涂层热阴极

研究了一种LaB6与TaC混合涂层热阴极,其发射层通过均匀混合LaB6与TaC粉末得到。比较了该阴极在LaB6与TaC混合比例为1∶1, 2∶1和3∶1下的发射特性,发现混合型LaB6阴极的功函数与多晶LaB6阴极的非常接近,在3∶1的混合比例下,电极的发射电流稳定,得到的电流密度为30 A/cm2。该电极可被应用于需要大电流密度和超大面积阴极的真空电子器件及动态真空电子束设备中。     

机械合金化过程对硫化铋块体热电性能的影响机理

以机械合金化法(MA)结合放电等离子烧结技术(SPS)制备了Bi₂S₃多晶块体热电材料. 研究了MA过程中干磨转速、湿磨时间和湿磨介质对Bi₂S₃多晶热电材料电传输性能的影响. 分析了样品的物相, 观察了显微组织, 测试了电传输性能和热传输性能. 研究表明, 以无水乙醇为湿磨介质时, 随着湿磨时间的延长, 出现了微量Bi₂O₃第二相, 样品的晶粒尺寸减小, 电阻率大幅增加, 功率因子下降. 以丙酮为湿磨介质时, 虽然不存在微氧化反应, 但是由于样品中存在大量孔洞, 导致功率因子降低. 425 r/min 干磨15 h后未湿磨的样品在573 K取得最大的ZT值0.25, 是目前文献报道的最高值.     

纯PCBN高压烧结行为与工艺规律

采用粒度为10μm的纯cBN微粉在不同的高压烧结工艺参数(烧结压力、温度和时间)下制备了纯聚晶立方氮化硼(PCBN)烧结体。利用扫描电镜观察了PCBN烧结体的微结构,并测试了其耐磨性和抗压强度,进而讨论了压力、温度和烧结时间对纯PCBN烧结体性能的影响规律。结果表明:对纯PCBN烧结体性能影响最大的因素是烧结压力,其次是烧结温度和时间;在本实验条件下,当压力为9GPa、温度为1 700℃和烧结时间为240s时,高压烧结得到的纯PCBN烧结体样品性能最优,其磨耗比为10 200,抗压强度为2.52GPa。     

电子束蒸发沉积六硼化镧薄膜的逸出功(英文)

六硼化镧(LaB6)具有电子逸出功低、高熔点和高化学稳定性等优点,是制作热阴极和场发射阴极的理想发射体材料。而且在常规场发射尖锥表面涂敷一层LaB6薄膜能够大幅度提高场发射尖锥的发射能力。为了测量LaB6薄膜的逸出功,采用电子束蒸发技术沉积LaB6薄膜,并对薄膜进行了X射线衍射分析和X射线光电谱分析。通过测量薄膜的热电子发射特性和敷LaB6薄膜的硅尖锥阵列的场致电子发射特性确定了LaB6薄膜的逸出功,与块状LaB6多晶材料的逸出功大体相同,说明电子束蒸发沉积技术适合于制备高纯度、低逸出功的LaB6薄膜。     

多晶Li3+xV1-xTxO4(T=Ge,Si)离子导电性能的改善

本文用阻抗谱方法研究了Li_3+xV_1-xT_xO₄(T=Si,Ge)多晶的离子导电性,发现一些工艺条件如成型压强、烧结时间和烧结程序对电导率有很大影响。注意分析了这些影响的物理起因。最佳工艺条件是:在大约8t/cm²压强下成型样品。在1000℃连续烧结5至6天,烧结过程中,应尽量避免温度波动。在此条件下制备的Li_3.5V_0.5Ge_0.5关键词：     

高压烧结对n型PbTe基材料热电性能的影响

 采用高压烧结技术制备了按偏离化学计量比配制的PbTe基热电材料（Pb_0.55Te_0.45），重点研究了烧结压力对材料热电性能的影响。研究结果表明：高压烧结过程能有效降低材料中的晶格缺陷，从而显著改变样品中的载流子浓度及其迁移率。与未经烧结的常压熔融样品相比，高压烧结样品的Seebeck系数得到大幅提高，电导率略有降低，室温热导率降低了50%，所以高压烧结样品的品质因子得到较大提高。当烧结压力为2 GPa时，所得样品在700 K时其品质因子达到0.59，相比未经烧结的常压熔融样品提高了150%。     

一种新型红色荧光粉CaAl12O19： Eu,Mn的制备及发光性能

固相法制备了碱土金属铝酸盐荧光粉CaAl₁₂O₁₉ : Eu,Mn,测试了样品的XRD及激发与发射光谱,对样品的结构及其发光性能进行了分析,并且考察了灼烧温度及Eu³⁺的浓度对样品发光性能的影响,对Eu³⁺的作用机理进行了探讨。 该荧光粉能被波长短于550 nm的蓝绿光以及紫外和近紫外光激发,其发射光谱峰值在590,615,645,657 nm,其中前两个为Eu³⁺的特征发射,后两个为Mn⁴⁺的²E-⁴ A₂跃迁发射。该荧光粉的最佳烧结温度与时间分别为1 550 ℃和4 h,Eu³⁺的最佳掺杂摩尔分数为0.11%左右。     

多晶Li_(3+x)V_(1-x)T_xO_4(T=Ge,Si)离子导电性能的改善

本文用阻抗谱方法研究了Li_(3+x)V_(1-x)T_xO_4(T=Si,Ge)多晶的离子导电性,发现一些工艺条件如成型压强、烧结时间和烧结程序对电导率有很大影响。注意分析了这些影响的物理起因。最佳工艺条件是:在大约8t/cm~2压强下成型样品。在1000℃连续烧结5至6天,烧结过程中,应尽量避免温度波动。在此条件下制备的Li_(3.5)V_(0.5)Ge_(0.5)O_4和Li_(3.3)V_(0.7)Si_(0.3)O_4多晶样品在25℃的离子电导率分别为2.2×10~(-5)Q~(-1)cm~(-1)和1.9×10~(-5)Q~(-1)cm~(-1)。     

共沉淀法制备纳米多晶La2／3Sr1／3MnO3及其低场磁电阻性质

利用共沉淀法制备了纳米多晶La2/3Sr1/3MnO3粉体,并研究了相应烧结陶瓷的相结构、显微形貌、电性质以及磁电阻效应.样品中存在高密的晶界,对电子的疏运过程产生明显的散射作用,从而使得样品具有较大的电阻值,并且只有当烧结温度大于800℃时才出现金属绝缘体温度相变.样品的磁电阻是低场磁电阻效应,源于晶界处电子的自旋极化隧穿.烧结温度越低的样品,其磁电阻越大.     

Effects of process parameters on electrical properties of n-type Bi2Te3 prepared by mechanical alloying and spark plasma sintering

n-Type Bi₂Te₃ thermoelectric materials were prepared by spark plasma sintering (SPS) using mechanically alloyed powders. Seebeck coefficient and electrical conductivity of the resultant materials were measured, with emphasis on the effects of sintering process parameters on the electrical properties. The power factor was improved from 1.5 to 1.6 mW/mK² when the SPS pressure was increased from 20 to 50 MPa at 623 K, and was further increased to 2.1 mW/mK² under 50 MPa by raising the SPS temperature from 623 to 673 K. The maximum power factor was obtained for the sample sintered under optimized SPS process parameters, in which the sintering temperature and the sintering pressure are 673 K and 50 MPa, respectively.     

用正电子湮没研究纳米碲化铋的缺陷及其对热导率的影响

利用水热法合成了Bi₂Te₃纳米粉末, 并在300–500 ℃的温度范围内对其进行等离子烧结. X射线衍射测试表明制得的Bi₂Te₃粉末是单相的. 对于300–500 ℃范围内烧结的样品, 扫描电子显微镜观察发现随着烧结温度的升高样品颗粒明显增大, 但是根据X射线衍射峰的宽度计算得到的样品晶粒大小并没有明显的变化. 正电子湮没寿命测试结果表明, 所有的样品中均存在空位型缺陷, 而这些缺陷很可能存在于晶界处. 正电子平均寿命随着烧结温度的升高而单调下降, 说明较高的烧结温度导致了空位型缺陷浓度的降低. 另外, 随着烧结温度从300 ℃升高到500 ℃, 样品的热导率从0.3 W·m^-1·K^-1升高到了2.4 W·m^-1·K^-1, 这表明在纳米Bi₂Te₃中, 空位型缺陷和热导率之间存在着密切的联系.     

ZnO纳米块体材料的制备及其性能的研究

采用连续成型方式压制了纳米ZnO素坯，考察了素坯密度、烧结时间、致密化温度等参数与 成型方式的关系.用场发射扫描电镜表征了烧结体微观组织特征.测定了ZnO纳米块体材料中 硬度随烧结温度的变化规律.结果表明，采用连续成型方式可使素坯密度提高56％、烧结时 间缩短了3h、致密化温度降低200℃.场发射扫描电镜显示烧结体内部密度及颗粒尺寸分布 均匀.硬度测定结果显示ZnO纳米块体材料中显微硬度随烧结温度的变化不是单调的，而是随 烧结温度的升高显微硬度先升高后降低，拐点对应的晶粒尺寸为50—60nm. 关键词： ZnO纳米块体 连续成型 硬度     

高压熔渗生长法制备金刚石聚晶中碳的转化机制研究

在6 GPa和1500 ℃的压力和温度范围内, 利用高压熔渗生长法制备了纯金刚石聚晶, 深入研究了高温高压下金刚石聚晶生长过程中碳的转化机制. 利用光学显微镜、X-射线衍射、场发射扫描电子显微镜检测, 发现在熔渗过程中金刚石层出现了石墨化现象, 在烧结过程中金刚石颗粒表面形貌发生了变化. 根据实验现象分析, 在制备过程中存在三种碳的转化机制: 1)金属熔渗阶段金刚石颗粒表面石墨化产生石墨; 2)产生的石墨在烧结阶段很快转变为填充空隙的金刚石碳; 3)金刚石直接溶解在金属溶液中, 以金刚石形式在颗粒间析出, 填充空隙. 本文研究碳的转化机制为在高温高压金属溶剂法合成金刚石的条件下(6 GPa和1500 ℃的压力和温度范围内)工业批量化制备无添加剂、无空隙的纯金刚石聚晶提供了重要的理论指导.     

Synthesis, thermionic emission and magnetic properties of (NdxGd1-x)B6

Polycrystalline rare-earth hexaborides(NdxGd1-x)B6(x = 0,0.2,0.6,0.8,1) were prepared by the reactive spark plasma sintering(SPS) method using mixed powder of GdH2,NdH2 and B.The effects of Nd doping on the crystal structure,the grain orientation,the thermionic emission and the magnetic properties of the hexaboride were investigated by X-ray diffraction,electron backscattered diffraction and magnetic measurements.It is found that all the samples sintered by the SPS method exhibit high densities(> 95%) and high values of Vickers hardness(2319 kg/mm2).The values are much higher than those obtained in the traditional method.With the increase of Nd content,the thermionic emission current density increases from 11 to 16.30 A/cm2 and the magnetic phase transition temperature increases from 5.85 to 7.95 K.Thus,the SPS technique is a suitable method to synthesize the dense rare-earth hexaborides with excellent properties.     

Quick preparation and thermal transport properties of nanostructured β-FeSi2 bulk material

This paper reports that the nanostructured β-FeSi2 bulk materials are prepared by a new synthesis process by combining melt spinning(MS) and subsequent spark plasma sintering(SPS).It investigates the influence of linear speed of the rolling copper wheel,injection pressure and SPS regime on microstructure and phase composition of the rapidly solidified ribbons after MS and bulk production respectively,and discusses the effects of the microstructure on thermal transport properties.There are two crystalline phases(α-Fe2Si5 and ε-FeSi) in the rapidly solidified ribbons;the crystal grains become smaller when the cooling rate increases(the 20 nm minimum crystal of ε-FeSi is obtained).Having been sintered for 1 min above 1123 K and annealed for 5 min at 923 K,the single-phase nanostructured βFeSi2 bulk materials with 200-500 nm grain size and 98% relative density are obtained.The microstructure of β-FeSi2 has great effect on thermal transport properties.With decreasing sintering temperature,the grain size decreases,the thermal conductivity of β-FeSi2 is reduced remarkably.The thermal conductivity of β-FeSi2 decreases notably(reduced 72% at room temperature) in comparison with the β-FeSi2 prepared by traditional casting method.     

正交试验法优化金刚石复合片合成工艺

 通过正交试验法,以磨耗比、电阻、完整性、硬度为指标,设计了金刚石复合片的合成工艺。正交试验可以减少合成工艺试验次数,优化合成工艺。试验结果表明,较合理的烧结工艺为：合成压力5.5 GPa,升温速度为200 ℃/min,保温时间16 min,冷却时间14 min,烧结温度1 350 ℃。从压力、温度和时间等因素的影响方面讨论了金刚石复合片的性能。认为：适当地提高温度有利于提高磨耗比及硬度;延长加热时间有利于性能均匀性的提高;延长冷却时间可减少残余热应力。     

Optimization of intergrain connection in high-temperature superconductor Bi_2Sr_2CaCu_2O_x

A modified spark plasma sintering(SPS) technique was developed for the fabrication of Bi2Sr2 Ca Cu2Ox(Bi-2212)superconducting bulks with better intergrain connections. The influences of the modified SPS process on the microstructures, intergrain connections, and related superconducting properties were systematically analyzed. The modified SPS process can not only increase the final density of the bulk samples but also enhance the texture structures. Clean grain boundaries were obtained instead of the intergrain amorphous layers. Therefore the intergranular properties were obviously improved. Due to the better intergrain connections and the stronger flux pinning properties, the critical current densities of the Bi-2212 bulks obtained via the modified SPS process were greatly increased. The obtained improvements imply the possibility for the modified SPS technique to be used for enhancing the superconducting properties of the Bi-2212 tapes.     

The influence of sintering conditions on the phase purity of bulk EuTiO3 and Eu0.5Ba0.5TiO3 ceramics

EuTiO₃ and Eu_0.5Ba_0.5TiO₃ ceramics were synthesized using mechanochemical activation of oxide precursors and then calcined. The uniaxially as well as isostatically pressed samples were sintered in different kinds of reducing atmospheres, namely Ar?+?(7–10)%H₂, respectively, 99.99%H₂ in the case of pressureless sintering or in vacuum (enriched by CO vapors) in the case of pressure-assisted spark plasma sintering (SPS). The samples prepared by SPS contained the pyrochlore phase as the second phase. In contrast with SPS, pressureless sintered samples were phase pure, although thermodynamics calculations showed that CO atmosphere in SPS is more reducing than pure hydrogen. This is explained by short sintering times in SPS that do not allow establishment of the thermodynamic equilibrium. The proper choice of sintering temperature, time, and atmosphere enabled preparation of dense and phase pure samples of Eu _x Ba_{1? x} TiO₃ ceramics suitable for the evaluation of “true” physical properties (e.g., infrared reflectivity), or for experimental confirmation of specific functionalities proposed from theory.     

放电等离子烧结原位合成LaxCe1-xB6化合物及性能研究

以LaH₂, CeH₂纳米粉和无定形B粉为原料, 通过放电等离子烧结原位合成法制备了单相、高致密度的La_xCe_1-xB₆稀土六硼化物. 系统研究了该系列化合物的晶体结构、表面织构、力学性能、电输运特性及热发射性能. 结果表明, 该方法制备出的样品致密度均高于96%, 维氏硬度最高值达到2310 kg/mm², 说明具有良好的力学性能. 热发射结果表明, 当阴极温度为1873 K, 外加电压为1 kV时, La_0.6Ce_0.4B₆的最大发射电流密度达到40.7 A/cm², 该值高于单纯LaB₆和CeB₆电流密度值. 因此, La_xCe_1-xB₆多元稀土六硼化物作为热阴极材料将有良好的应用前景. 关键词： 稀土六硼化物 阴极材料 热电子发射