Preparation and Properties of Si2N2O Ceramics for Microwave Sintering Furnaces

Si2N2O ceramics were prepared using amorphous Si3N4 as the raw material and Li2CO3 as the sintering additive through vacuum multi-stage sintering.The influence of the Li2CO3 addition(0%,1%,2%,3%,and 5%,by mass)on the phase composition,the microstructure,the porosity,the mechanical properties,the dielectric constant and the tangent of the dielectric loss angle of the porous Si2N2O ceramics was investigated.The results reveal that a suitable addition of Li2CO3 can promote the generation of Si2N2O but excessive or inadequate Li2CO3 causes decomposition of Si2N2O ceramics.The prepared porous Si2N2O ceramics have good mechanical properties,good thermal shock resistance,and low dielectric properties,which have excellent potential for application in microwave sintering furnaces.

RESEARCH ON MICROWAVE SINTERING ALUMINA CERAMICS

This paper introduces the characteristic of microwave sintering,introduces and analyses the process of microwave sintering of thealumina ceramics, moreover, compared with the experiments ofconventional sintering method. Based on the research, some resultsare obtained, and experimental basis for microwave sintering ofceramics is put forward.

Low-Temperature Sintering and Microwave DielectricProperties of Ba_2Ti_3Nb_4O_(18) Ceramics

The effects of CuO and H3BO3 additions on the low-temperature sintering,microstructure,and microwave dielectric properties of Ba2Ti3Nb4O18 ceramics were investigated.The addition of less amount of CuO （ 〈1 wt%） considerably facilitated the densification of Ba2Ti3Nb4O18 ceramics.Appropriate addition of H3BO3 （ 〈3.5 wt%） remarkably improved the microwave dielectric properties of ceramics.The addition of H3BO3 and CuO successfully reduced the sintering temperature of Ba2Ti3Nb4O18 ceramics from 1300 to 1050 ℃.Ba2Ti3Nb4O18 ceramics sintered at 1 050 ℃ for 4 h with the addition of 1.0 wt% CuO and 3.5 wt% H3BO3 exhibited good microwave dielectric properties：er=33.74,Q？f=13 812 GHz,and tf=-5.35 ppm/°C at about 5.0 GHz.

Development of calcium stabilized nitrogen rich α-sialon ceramics along the Si_(3)N_(4):1/2Ca_(3)N_(2):3AlN line using spark plasma sintering

Calcium stabilized nitrogen rich sialon ceramics having a general formula of Ca_(x)Si_(12-2x)Al_(2x)N_(16) with x value(x is the solubility of cation Ca in α-sialon structure)in the range of 0.2-2.2 for compositions lying along the Si_(3)N_(4):1/2Ca_(3)N_(2):3AlN line were synthesized using nano/submicron size starting powder precursors and spark plasma sintering(SPS)technique.The development of calcium stabilized nitrogen rich sialon ceramics at a significantly low sintering temperature of 1500℃(typically reported a temperature of 1700℃ or greater)remains to be the highlight of the present study.The SPS processed sialons were characterized for their microstructure,phase and compositional analysis,and physical and mechanical properties.Furthermore,a correlation was developed between the lattice parameters and the content(x)of the alkaline metal cation in the α-sialon phase.Well-densified single-phase nitrogen rich α-sialon ceramics were achieved in the range of 0.53(3)≤x≤1.27(3).A nitrogen richα-sialon sample possessing a maximum hardness of 22.4 GPa and fracture toughness of 6.1 MPa·m^(1/2) was developed.

Preparation of ZrN(ZrON)-SiAION Composite Ceramics via a Pressureless Sintering Process

ZrN-SiAlON composite materials were synthesized at 1 550 ℃ for 6 h via a carbothermal reduction nitridation route using fly ash （≤74 μm）,zircon （≤ 44 μm） and active carbon as starting materials.The processed ZrN-SiAlON composite micropowders were mixed with polyvinyl alcohol as binder to prepare ZrN （ZrON）-SiAlON composite ceramics by carbon-embedded pressureless firing at 1 450,1 500 and 1 550 ℃ for 1 h,respectively.Influences of firing temperature on the phase compositions,microstructure and sintering properties of the ceramics were investigated.The results show that：（1） β-SiAlON based composite ceramics with different compositions can be prepared by controlling firing temperature,and the main crystalline phases of the specimen fired at 1 550 ℃ for 1 h involve ZrN,ZrON and β-SiAlON （z =2,Si4Al2O2N6）; （2） ZrN （ZrON）,β-SiAlON and a Fe-Si based compound can be observed in the microstructures of the specimens fired at different temperatures.ZrN （ZrON） particles distribute homogeneously in the β-SiAlON matrix; （3） raising firing temperature can increase the shrinkage ratio of the ceramics,and the volume shrinkage ratio increases from 19.4％ to 40.3％ when the firing temperature rises from 1 450 to 1 550 ℃.

Microwave dielectric properties and compatibility with silver of low-fired Li_2MgTi_3O_8 ceramics with Li_2O-MgO-B_2O_3 frit

The effects of Li2O-MgO-B2O3 （LMB） glass additive on the sintering characteristics, phase purity, microstructure, and microwave dielectric properties of Li2MgTi3O8 ceramics were investigated. The experimental results demonstrate that the addition of LMB glass effectively lowers the sintering temperature of Li2MgTi3O8 ceramic from 1025 ℃ to 875 ℃ and induces no obvious degradation of the microwave dielectric properties. Typically, the 1.5%LMB glass-added Li2MgTi3O8 ceramic sintered at 875 ℃ for 4 h shows excellent microwave dielectric properties of Q×f=45403 GHz, εr=25.9 and τf≈0 ℃-1. The dielectric ceramic exhibits stability against the reaction with the Ag electrode, which indicates that the ceramics could be applied in multilayer microwave devices requiring low firing temperatures.

微波烧结SiAlON陶瓷立铣刀力学性能和切削性能研究

采用微波烧结方法制备了用于磨削SiAlON陶瓷立铣刀的棒料,研究了压制方式及压力对微波烧结SiAlON陶瓷棒料微观结构和力学性能的影响规律,制备了SiAlON陶瓷立铣刀,并对其切削性能进行了研究。结果表明:对于大长径比SiAlON陶瓷,径向压制可以获得密度分布更加均匀的生坯,压制压力为100MPa时,SiAlON陶瓷试样无微观缺陷,具有良好的机械性能。微波烧结的SiAlON陶瓷立铣刀可用于镍基高温合金高速切削,刀具寿命是进口涂层刀具的2倍。

Facile synthesis of Ca-SiAlON:Eu^(2+) phosphor by the microwave sintering method and its photoluminescence properties

Pure Ca-SiAlON:Eu2+ was synthesized by microwave sintering method at a relatively low temperature of 1550℃.Photoluminescence intensity of the resultant phosphor was higher than those of the samples synthesized by conventional gas-pressure sintering technique at 1750℃.When it was excited at 450 nm,the as-prepared yellow Ca-SiAlON:Eu2+ sample had an external quantum efficiency of 42%,comparable to the sample synthesized at 1750℃ under 0.5 MPaN2 gas pressure by the GPS method reported in reference.The experimental results demonstrated that the microwave sintering method was also an interesting approach for synthesizing nitride phosphors,which promises lower firing temperature than those by carbothermal reduction and nitridation (CRN) methods,higher heating rate and shorter duration time compared with those by gas-pressure sintering.

Preparation of large size ZTA ceramics with eccentric circle shape by microwave sintering

Ultra-large zirconia toughened alumina (ZTA,mass ratio of Al2O3 and ZrO2 is 78∶22) ceramics with eccentric circle shape were successfully sintered by microwave sintering with a multi-mode cavity at 2.45 GHz.The dimension of ZTA ceramics (green body) is 165 mm (outer diameter) × 25 mm (thickness).The optimized sintering temperature of microwave sintering is about 1500 ℃ for 30 min,and the total sintering time is about 4 h which is much shorter than that of conventional sintering.An auxiliary-heating insulation device was designed based on the principle of local caloric compensation to guarantee the intact sintered samples.With the increasing of sintering temperature,more and more microwave energy is absorbed within the entire sample,volumetric densification performs,and phases shift from m-ZrO2 phase to t-ZrO2 phase and cause Al2O3 grain growth.

Microstructure and microwave dielectric properties of ZnO-B_2O_3 added (Ca_(0.254)Li_(0.19)Sm_(0.14))TiO_3 ceramics

The effects of ZnO-B2O3 （ZB2） on the sintering behavior and microwave dielectric properties of （Ca0.254Li0.19Sm0.14）TiO3 ceramics were investigated. The densities of the specimens reached the maximum value by adding 3 wt.% ZB2 and then decreased. The sintering temperature of the specimens was lowered from 1300 to 1100℃ without degradation of the microwave dielectric properties. The （Ca0.254Li0.19Sm0.14）TiO3＋ 3 wt.% ZB2 sintered at 1100℃ for 3 h showed good microwave dielectric properties, εr= 108.2, Qf= 6545 GHz, and rf= 6.5 ppm/℃, respectively, indicating that ZB2 was an effective sintering aid to improve the densification and microwave dielectric properties of （Ca0.254Li0.19Sm0.14）TiO3 ceramics.

Sialon粉体的无压烧结

为获得致密的Sialon陶瓷材料,采用自制Sialon粉末,分别添加8.5%Al2O3-1.5%Y2O3和8.5%Si3N4-1.5%Y2O3(均为质量分数)系两种烧结助剂后进行充分混合,混合物粉末在钢模中冷压成两种压坯试样,然后在N2气氛中分别在1600℃保温4h和1550℃保温4h进行无压烧结。利用XRD、SEM等技术表征反应过程和产物特征。试样的体积密度分别达到最高值3.1g/cm3和3.02g/cm3;显微硬度分别为1639HV/GPa0.5和1651HV/GPa0.5。

FINITE ELEMENT COMPUTER MODEL OF MICROWAVE HEATED CERAMICS

At present,the concerned papers appeared in special magazines about discussing or introducing finite element method for calculating temperature distribution in ceramic body during microwave sintering, are not a good many, but it seems that finite element method is more convenient than finite difference method in dealing with special or complex geometry of ceramic body. In this paper, we describe a 3D finite element model simulating the heating pattern of ceramic microwave sintering in TE(10N) single-mode rectangular cavity in which the microwave energy deposition pattern in the samples can be expressed as an analysis function of space, and present a series of transient temperature distributions and heating rates of ceramic cylinders and cuboids tender variable thermal conductivities, dieletric loss factors,power consumer-levels, etc. These digital solutions may provide a better understanding of eliminating thermal runaway and improving temperature homogeneity.

Sialon陶瓷的常压烧结

在Si3N4 ,Al2 O3,AlN和Y2 O3 混合料常压烧结过程中 ,由于过程反应生成SiO ,CO ,N2 等气相物质和由于Si3N4原料在高温常压下分解压高 ,从而常压烧结致密化过程始终伴随着一个失重的塑致密化过程 .为了解决这一问题 ,作者研究了填料成分、烧结温度、烧结时间等工艺条件对Sialon陶瓷常压烧结密度的影响 ,分析了烧结过程的物理化学机制和致密化机制 .4种填料分别为Si3N4 ,Si3N4 +SiO2 ,Si3N4 +Al2 O3+AlN和Si3N4 +Al2 O3+AlN +BN .被烧料典型配方为 :Si3N4 6 5 %～ 70 % ,Al2 O32 0 %～ 2 5 % ,AlN 10 % ,另加 6 %Y2 O3.当填料成分为 70 %Si3N4 + 2 4%Al2 O3+ 3 %AlN + 3%BN时 ,制得了相对密度达 99% ,抗弯强度达 6 12 .2MPa的常压烧结Sialon陶瓷 .研究结果表明 :对于通式为Si6-ZAlZOZN8-Z的Sialon陶瓷 ,当Z =2时 ,其最佳烧结温度为 175 0℃ ,烧结时间为 40min ;Sialon的烧结过程是 1个多因素控制的瞬时液相烧结过程 .

稀土氧化物在SiAlON陶瓷材料中的应用研究进展

简要论述了稀土氧化物在SiAlON陶瓷材料中的应用研究概况;介绍了Y_2O_3、Sm_2O-3、Dy_2O_3和Nd_2O_3等单一稀土氧化物以及复合掺杂稀土氧化物在SiAlON陶瓷材料中的应用进展,并比较了它们对SiAlON陶瓷材料性能的影响;最后对稀土氧化物在SiAlON陶瓷材料中的应用前景作了扼要的分析和展望。

常压烧结制备ZrN(ZrON)-SiAlON复合陶瓷

以粉煤灰(≤74μm)、锆英石(≤44μm)和活性炭为原料,采用碳热还原氮化法在1 550℃保温6 h合成了ZrN-SiAlON复合材料。以加工成的ZrN-SiAlON复合微粉为主原料,加入聚乙烯醇结合剂,分别在1 450、1 500和1 550℃下埋炭粉常压烧结1 h制备ZrN(ZrON)-SiAlON复合陶瓷,研究了烧成温度对复合陶瓷相组成、显微结构和烧结性能的影响。结果表明:1)控制烧成温度可以制备出不同组成的β-SiAlON基复合陶瓷;在1 550℃保温1 h制备的复合陶瓷的主晶相为ZrN、ZrON和β-SiAlON(z=2,Si4Al2O2N6);2)从不同温度烧后试样的微观结构中均能观察到ZrN(ZrON)、β-SiAlON和一种铁硅系化合物存在,且ZrN(ZrON)颗粒均匀地分布于β-SiAlON基质中;3)提高烧成温度会使复合陶瓷的收缩率增大,当烧成温度由1 450℃升至1 550℃时,试样的体积收缩率由19.4%增加至40.3%。

烧结助剂MgO和烧结温度对β-Sialon陶瓷的力学性能影响

以α-Si3N4粉、α-Al2O3粉和Al N粉及烧结助剂MgO为原料,采用热压烧结的工艺制备了β-Sialon陶瓷材料,研究了烧结助剂MgO和烧结温度对sialon陶瓷力学性能和组织形貌的影响.结果表明,加入烧结助剂MgO提高了β-sialon陶瓷的致密度且降低了烧结温度,随着烧结温度的升高,β-sialon陶瓷抗弯强度、断裂韧性呈先增加后降低的变化规律,当烧结温度为1600℃时制备的β-sialon陶瓷材料结合紧密,抗弯强度以及断裂韧性达到最大,值分别为423 MPa、2.73 MPa·m1/2,材料的断裂方式主要是沿晶断裂.

Microstructure and strength modification of relaxor ferroelectric ceramics through microwave sintering for multilayer capacitors

Relaxor ferroelectric ceramics with the composition ofxPb(Mg1/3Nb2/3)O3-yPb(Zn1/3Nb2/3)O3-zPbTiO3 was fast sintered in a 2.45 GHz microwave system. Microwave-sintered samples illustrate more rapid densification and much smaller grain size microstructure than conventional sintered samples. Also the microwave processing significantly increases the dielectric strength and flexural strength of the relaxor so that its strength becomes comparable with modified BaTiO3, and could obtain comparable dielectric properties in comparison with conventional sintering process. Microwave processing has many advantages for sintering of relaxor ferroelectric ceramics used as multilayer capacitors.

透明α-Sialon的研究进展

从透明陶瓷的透明机理出发，概述了透明α-Sialon的制备工艺以及对其透明机理的研究进展，指出了当前对透明α-Sialon研究的相对局限，展望了透明α-Sialon的发展前景。

微波合成β-Sialon

研究了微波加热条件下合成温度、保温时间等对产物性能的影响。应用微波加热技术,以Al粉、Si粉、Al2O3粉为原料,成功地进行了不同Z值配比Sialon的合成。结果表明:利用微波反应合成β-Sialon,相比传统工艺具有降低烧结温度、缩短保温时间、节能省时等优势。

基于粉煤灰原料的β-Sialon粉体制备及其微波烧结性能

以粉煤灰为主要原料,采用碳热还原氮化法合成β-Sialon粉体,再以该粉体为主要原料,添加适量Y2O3烧结助剂,利用微波无压烧结技术研究β-Sialon陶瓷的微波烧结行为。结果表明:活性炭与粉煤灰质量比值(m c/m f)为0.43,氮气流量为0.5 L/min,合成温度为1450℃,保温6 h条件下,获得显微形貌为粒状,z=2的β-Sialon粉体;在微波烧结温度为1500℃,保温时间为20 min条件下,获得试样的密度为2.86 g/cm3,相对密度为92.3%,HV0.5为1528。