在固态合成过程中相变化的监测

用实时测量介电损耗的方法研究了氧化物SrFeCo0.5Oy和LiMn2O4的固相合成过程，结果表明，在固相合成过程中，材料的介电损耗突变点对应材料中相的变化，材料介电损耗的变化对应固相保成过程中材料相含量的相对变化，实时测量材料在合成过程中的介电损耗是得到性能优异材料的重要手段之一。     

协同制备氧化物SrFeCo0.5Oy的研究

采用柠檬酸溶胶凝胶合成法协同微波加热烧结制备了混合导体氧化物SrFeCo0.5Oy。利用差热分析（DTA）、X-射线衍射(XRD)、电子透射电镜(TEM)与电子扫描电镜(SEM)对合成与烧结样品进行了分析与表征，当羧酸根，硝酸根的比值(α)为0．64时，在550℃下焙烧干凝胶即可得到单相钙钛矿结构的Sr-Fe-Co0.5Oy混合氧化物，而且合成的氧化物SrFeCo0.5Oy颗粒细小、分布均匀。微波协同烧结制备的SrFeCoO.5Oy，氧化物的样品相对密度达到96％。与常规烧结样品相比较，协同烧结制备温度低，时间短；所得样品的绝对主相为钙钛矿型SrFe1-xCoxO3-δ相。     

混合导体氧化物SrFeCo0.5Oy粉末的微波合成与表征

采用微波加热方法与常规高温固相法合成了Sr-Fe-Co-O系混合导体陶瓷氧化物粉末.利用XRD,TEM/EDX及SEM等测试方法分析与表征粉体.用微波加热合成的粉体颗粒尺寸分布均匀,一次颗粒尺寸较小,结晶度也好于用常规加热合成的粉体.微波加热合成粉体的结晶相结构是钙钛矿结构Sr(Fe,Co)1.5Oy相,并有少量的正交结构相和尖晶石(Co,Fe)3O4相;高温固相法合成粉末由Sr4(Fe,Co)6O13±δ相及少量的Sr(Fe1-xCox)O3-δ相和CoO相组成.     

微波固相法合成四方相钛酸钡纳米粉体

以BaCO_3、TiO_2为原料,SiC微球为微波良导体材料,原料经球磨,砂磨细化后与SiC微球均匀混合,采用微波微区加热技术合成BaTiO_3粉体。利用XRD、Raman和FT-IR确定合成温度以及定性分析、SEM进行形貌表征,PSD进行粒度分析,BET测试比表面积。结果表明,采用微波固相法,引入微波良导体SiC形成微波微区域加热制备出粒径400 nm,粒度分布均匀的四方相钛酸钡粉体,相比于传统固相法粒径更小,分散性良好。为钛酸钡粉体的微波固相法合成提供了新思路。     

锂离子电池正极材料锰酸锂的优化合成

运用动态多重扫描速率法，根据四条不同升温速率下的DSC曲线，计算出在空气气氛下动态合成LiMn2O4过程中的动力学参数，据此提出一个优化的LiMn2O4固相合成工艺，采用固相分段焙烧法制备LiMn2O4正极材料，第一段和第二段的温度分别设在600和830℃。用XRD对合成的粉体材料进行了相结构分析；用恒电流充放电仪对LiMn2O4的电化学性能进行测试，结果表明，合成样品具有良好的尖晶石相结构，在充放电循环时初始放电容量达122mAh／g，同时具备良好的容量保持能力。     

微波法合成锂离子电池正极材料LiCoO2

从节约能源、降低成本及保护环境出发,利用微波加热特点,采用微波技术对微波法制备LiCoO2正极材料进行了研究.在一定的微波功率、辐射时间制度下制备出LiCoO2样品并进行了电化学性能测试.通过X射线衍射(XRD)、扫描电镜(SEM)研究了样品的物相结构和形貌.结果表明:在一定的微波功率、辐射时间制度下,可以快速得到单一相的层状LiCoO2正极材料,与传统高温固相法相比,采用微波合成的LiCoO2材料不仅具有同样优越的电化学性能及形貌结构,而且合成时间短,生产成本低.     

Al2O3添加剂对合成MgTiO3陶瓷相组成及介电性能的影响

研究了添加剂Al2O3对MgO和TiO2合成MgTiO3陶瓷烧结性，物相组成和微波介电性能的影响。XRD分析结果表明，没有添加Al2O3是，合成的MgTiO3陶瓷中只含有MgTiO3和MgTi5相,加入Al2O3，MgTiO3陶瓷中除了MgTiO3和MgTi2O5相外，还出现了MgAl2O4相，这是上由于Al2O3和MgO发生固相反应，MgAl2O4的出现虽然阻碍材料的致密化并导致密度下降，但是可能降低反应烧结合成MgTiO3陶瓷的相对介电常数和介电损耗。     

多铁性材料BiFe_(1-x)Co_xO_3的微波吸收特性研究

用溶胶-凝胶法制备BiFe1-x Cox O3样品,用X射线衍射仪、扫描电镜、能谱分析对样品的结构、微观形貌、元素组成进行了表征,用微波矢量网络分析仪测试了样品在2～18GHz微波频率范围的复介电常数、复磁导率,并计算了损耗角正切及微波反射率。结果表明,当掺杂量x=0、x=0.1、x=0.2,煅烧温度800℃时,产物的主相为钙钛矿型BiFeO3,同时还有杂相Bi25FeO40,颗粒形貌为尺寸约1.5μm的立方形;Co的掺入有利于提高体系的微波吸收性能。当样品厚度为1.8mm,x=0.2时,吸收峰值为-26.5dB,带宽为2.08GHz,在高频段有良好的微波吸收,材料兼具介电损耗和磁损耗但介电损耗相对较强。     

燃烧合成法制备IP板荧光粉工艺参数的研究

涂在IP板(Imaging Plate,简称IP)上的荧光粉BaFBrEu2+可存储X线影像,并通过光激励发光读出存储的光信息.BaFBrEu2+传统的制备方法是高温固相法,而燃烧合成法一直应用在合成金属氧化物和难熔金属之间的合成上,用这种方法制备不含氧的化合物还未见报道.本文报道了如何利用燃烧合成法制备IP板荧光粉一种不含氧的化合物,着重讨论了燃烧合成法的工艺对材料的结构和性能的影响.     

纳米羟基磷灰石合成的两种新方法

介绍了用溶剂热和微波辅助固相手段合成羟基磷灰石 (HAP)的两种新方法 ,得到了HAP纳米粒子和纳米棒。与传统水热合成法相比 ,溶剂热方法首次实现了在非水体系中纳米HAP的合成。微波固相合成法则得到了具有较好形貌和结构的HAP纳米粒子和纳米棒。该方法反应条件温和、反应时间极短、反应步骤简单且易于操作 ,因此有望实现HAP材料的大规模产业化。用X 射线衍射仪、扫描电子显微镜和红外光谱仪对产物的结构和形貌进行了表征。同时 ,也对微波固相反应的机理进行了初步探讨。     

SrTiO3-BiCrO3 solid solutions: Synthesis, x-ray diffraction study, and dielectric properties in the microwave range

SrTiO₃-BiCrO₃ ceramics were prepared by solid-state reactions. The materials were single-phase by x-ray diffraction and had a cubic perovskite structure up to 70 mol % BiCrO₃. Low-frequency conductivity measurements revealed semiconducting behavior of the solid solutions. Dielectric measurements in the microwave range revealed flat maxima of a relaxation nature in the temperature dependences of the dielectric permittivity and tan δ for the samples containing 30 and 40 mol % BiCrO₃. The solid solutions were found to exhibit relatively high dielectric losses in the microwave range.     

Dielectric spectroscopy of MgTiO3-based ceramics in the 109–1014Hz region

Magnesium titanate (MgTiO₃) powder was prepared by a chemical route (Pechini method) and different dopants were added to prepare several compositions. These pure and doped compositions were sintered in air and dense ceramics were obtained. The pure MgTiO₃ samples were also subjected to different heat treatments during sintering. Complex permittivity spectra of ceramic samples were determined by various techniques in the 10⁹–10¹⁴ Hz range. These techniques included infrared spectroscopy in transmission and reflectivity modes and microwave dielectric measurements. Extrapolation to microwave frequencies from infrared data, according to the proportionality (v) v, agrees quite well with the microwave data measured at 8 GHz and it is a useful procedure to estimate intrinsic microwave losses. Fast cooling from high temperatures of MgTiO₃ samples increased dielectric loss, probably due to a structural disorder. Dopants have two types of effect depending on whether they form a distinct second phase or a solid solution with MgTiO₃. In this last case intrinsic losses are strongly affected.     

分体圆柱谐振腔法用于金刚石膜微波介电性能测试的研究

针对金刚石膜微波介电损耗低、厚度薄带来的微波介电性能测试难点, 研制了一台分体圆柱谐振腔式微波介电性能测试装置。利用不同直径的蓝宝石单晶样品, 用上述装置对低损耗薄膜类样品微波介电性能的测试能力及样品直径对测试结果的影响进行了实验研究。在此基础上, 使用分体圆柱谐振腔式微波介电性能测试装置对微波等离子体化学气相沉积法和直流电弧等离子体喷射法制备的高品质金刚石膜在Ka波段的微波介电性能进行了测试比较。测试结果表明, 由Raman光谱、紫外-可见光谱等分析证明品质较优的微波等离子体化学气相沉积法制备的金刚石膜具有更高的微波介电性能, 其相对介电常数和微波介电损耗值均低于直流电弧等离子体喷射法制备的金刚石膜。     

Complex permittivity and conductivity of poly(<Emphasis Type="Italic">p</Emphasis>-phenylenediazomethine) and its blends at microwave frequencies

Poly(p-phenylenediazomethine) was synthesized by the condensation reaction between glyoxal and p-phenylene diamine in different solvents like methanol, toluene, m-cresol and N,N-dimethylformamide. The dielectric properties and microwave conductivity of the pelletized samples were measured using cavity perturbation technique. The measurements were done at 2.17 GHz at room temperature (25°C). The effect of dopants on the dielectric properties and conductivity was studied using HCl and HClO₄. Dielectric properties like dielectric constant, dielectric loss factor and microwave conductivity increased on doping with HCl and HClO₄. Conducting polymer composites were prepared by in situ polymerization of glyoxal and p-phenylenediamine in different solvents containing different amounts of PVC, and silica. The microwave conductivity and complex permittivity of each sample was measured. The effect of dopants like HClO₄ and HCl on these dielectric properties was also studied. The d.c. conductivity of the pressed samples measured by the two-probe method was also studied.     

Enhanced tunable characteristics of the Na0.5Bi0.5TiO3-NaTaO3 relaxor-type system

We have investigated the voltage-tunable characteristics of the Na(0.5)Bi(0.5)TiO(3)-NaTaO(3) homogeneity region, for which samples were prepared using a conventional solid-state reaction. The highest value of the relative tunability (n(r)) was obtained for the sample with 5 mol% of NaTaO(3), i.e., 47% at 1 MHz and a 70 kV/cm dc bias field. This sample also showed the highest value of the dielectric losses (tan delta) and temperature coefficient of the dielectric constant (tau(epsilon)), i.e., 0.05 and 4478 ppm/K, respectively. As the concentration of NaTaO(3) increased up to 90 mol% n(r), tan delta, and tau(epsilon) gradually decreased toward 22%, 0.0002 and -899 ppm/K, respectively. The dielectric constant of the samples varied in a similar manner between 662 and 130. At microwave frequencies, the dielectric losses of the samples substantially increased due to their relaxor-type nature. The lowest value was obtained for the samples with 90 mol% of NaTaO(3), i.e., 0.002. The tunable characteristics of the samples are related to the ferroelectric and dielectric properties, and it appears that the dielectric tunability of the Na(0.5)Bi(0.5)TiO(3)-NaTaO(3) system originates from its relaxor-type behavior.     

Anisotropic Dielectric Properties of Carbon Fiber Reinforced Polymer Composites during Microwave Curing

Microwave cuing technology is a promising alternative to conventional autoclave curing technology in high efficient and energy saving processing of polymer composites. Dielectric properties of composites are key parameters related to the energy conversion efficiency during the microwave curing process. However, existing methods of dielectric measurement cannot be applied to the microwave curing process. This paper presented an offline test method to solve this problem. Firstly, a kinetics model of the polymer composites under microwave curing was established based on differential scanning calorimetry to describe the whole curing process. Then several specially designed samples of different feature cure degrees were prepared and used to reflect the dielectric properties of the composite during microwave curing. It was demonstrated to be a feasible plan for both test accuracy and efficiency through extensive experimental research. Based on this method, the anisotropic complex permittivity of a carbon fiber/epoxy composite during microwave curing was accurately determined. Statistical results indicated that both the dielectric constant and dielectric loss of the composite increased at the initial curing stage, peaked at the maximum reaction rate point and decreased finally during the microwave curing process. Corresponding mechanism has also been systematically investigated in this work.     

Dielectric Properties of Porous Reaction-boned Si3N4 Ceramics with Controlled Porosity and Pore Size

This paper presents the microwave dielectric properties of reaction bonded porous silicon nitride ceramics with variant porosity and pore size, which were prepared by adding pore-forming agent grains into the silicon powders. The experimental results show that the dielectric constant and the dielectric loss of the samples reduce evidently with increasing porosity in the sample. When the porosity is constant, the dielectric constant and the dielectric loss of the ceramics decrease visibly as the pore size increases. Among all the obtained samples, the minimum dielectric constant is about 2.4.     

Ba0.65Sr0.35TiO3陶瓷材料的制备及介电特性研究

采用溶胶-凝胶工艺制备了Ba_0.65Sr_0.35TiO₃粉体,并利用微波烧结技术对粉体进行了合成和烧结,研究分析了样品的介电特性,并与传统制备工艺获得的样品进行了性能比较.实验结果表明,获得的Ba_0.65Sr_0.35TiO₃粉体颗粒较细,其合成温度和烧结成瓷温度都较传统工艺有大幅度降低,分别为900和1310℃;可以获得晶粒尺寸在1μm以内的陶瓷;随晶粒的减小,材料的相对介电常数变化不大,而介电损耗大大降低.     

Influence of lead oxide addition on LnTiTaO<Subscript>6</Subscript> (Ln = Ce,Pr and Nd) microwave ceramics

The effect of PbO addition on the structural, processing and microwave dielectric properties of LnTiTaO₆ (Ln = Ce, Pr and Nd) ceramics are reported. Conventional solid state ceramic route was used for the preparation of samples. Phase pure LnTiTaO₆ (Ln = Ce, Pr and Nd) ceramics are prepared at a calcination temperature of 1300°C. The samples are sintered at optimized temperatures. Addition of PbO reduces the sintering temperature. The crystal structure of the materials was analysed using X-ray diffraction techniques and the surface morphology of the sintered samples was analysed using scanning electron microscopy. The dielectric constant at microwave frequency range decreases for higher PbO addition for all the samples but the quality factor improves on small PbO addition. The thermal stability of resonant frequency was also improved with PbO addition on all the systems. A number of samples with improved microwave dielectric properties were obtained on all the systems suitable for practical applications.     

低温烧结陶瓷BiMg2VO6的微波介电性能

通过传统的固相反应方法制备了低温烧结微波介质陶瓷BiMg₂VO₆, 研究了该陶瓷与银的化学兼容性、物相、形貌及在720~840℃内的密度和微波介电性质, 并测试了陶瓷的红外反射光谱。结果表明: 陶瓷在780℃条件下与银共烧不发生反应, 相对密度大于93.8%。在780℃条件下烧结2 h得到的陶瓷具有最好的微波介电性能: 介电常数为13.4, Q×f值为15610 GHz (f = 8.775 GHz), 温度系数为-87.2×10^-6/℃。红外反射谱数据处理显示, BiMg₂VO₆的光频介电常数ε_∞ = 3.4, 微波频段的外推值为13.5。BiMg₂VO₆陶瓷好的微波介电性能和低的烧结温度, 使其有望用作新的低温共烧陶瓷。