低介电常数多孔氮化硅陶瓷的制备

采用凝胶注模成型工艺,以SiO2含量大于等于95%的空芯玻璃微珠作造孔剂,通过控制造孔剂的加入量和调节造孔剂的孔径成功制备出低介电常数、高强度的多孔Si3N4陶瓷。结果表明,随着造孔剂含量的增加,试样气孔率增大,弯曲强度降低,ε和tanδ都相应降低,ε最低为1.77;在造孔剂加入量为10%时,随着造孔剂的孔径尺寸变大,试样的孔径变大,弯曲强度降低,试样的ε和tanδ也相应降低。当造孔剂含量为10%、孔径尺寸为80μm时制备的多孔氮化硅陶瓷ε为2.13,弯曲强度达到38MPa,适合作为宽频带天线罩的夹层材料。     

天线罩用多孔氮化硅陶瓷的制备

采用反应烧结工艺,通过添加成孔剂的方法,制备出具有球形宏观孔的低密度多孔氮化硅陶瓷,研究了球形宏观孔和烧结工艺对多孔氮化硅陶瓷性能的影响.实验结果表明,与未添加成孔剂的样品相比,成孔剂的添加有效降低了材料的气孔率,使材料的介电常数ε'和介电损耗tanδ下降.孔的加入能促进针状氮化硅的生成,降低单位体积中产生的热量,防止...     

Properties of porous Si3N4 ceramic electromagnetic wave transparent materials prepared by technique combining freeze drying and oxidation sintering

A simple and low-cost technique combining freeze drying and oxidation sintering is explored to prepare Si₃N₄ ceramics with high porosity and complex shape. The effects of sintering temperature and time on the phase composition, microstructure, porosity, pore size and dielectric constant of the porous Si₃N₄ ceramics are studied. Due to the variations of phase composition and microstructure, the porous Si₃N₄ ceramics sintered at different temperature possess characteristic in flexural strength. The porous Si₃N₄ ceramics sintered at 1,300 °C for 2–3 h have the highest flexural strength of 71–74 MPa. The changes of porosity and composition have much effect on the dielectric constant of porous Si₃N₄ ceramics. Because of the high porosity and SiO₂ volume fraction, the porous Si₃N₄ ceramics sintered at 1,300 °C for 2–3 h possess low dielectric constant of 3.4–3.6 and small pore size of 0.9 μm. The porous Si₃N₄ ceramics are good structural/functional and promising electromagnetic wave transparent material.     

Preparation and properties of pressureless-sintered porous Si3N4

Wave-transparent materials used at high temperature environment generated by high supersonic and hypersonic speeds must possess excellent mechanical property. In this paper, porous Si₃N₄ ceramics with high strength were fabricated by low molding pressure (10 MPa) and pressureless sintering process, without any other pore forming agents. The sintering behavior and the effect of porosity on the mechanical strength and dielectric properties were investigated. The flexural strength of porous Si₃N₄ ceramics was up to 57–176 MPa with porosity of 45–60%, dielectric constant of 2.35–3.39, and dielectric loss of 1.6–3.5 × 10⁻³ in the frequency range of 8–18 GHz, at room temperature. With the increase of porosity, the flexural strength, dielectric constant, and dielectric loss all decreased.     

The effects of oxygen content on bonding configurations and properties of low-k organosilicate glass dielectric films

The low dielectric constant SiOC:H films of plasma enhanced chemical vapor deposition method have been developed with various precursor ratio. The reduction of the dielectric constant has been achieved by increasing the porosity in the films through the change of precursor ratio. In order to clarify the relation between dielectric constant and film porosity, the small angle X-ray scattering technique has been applied for characterizing pore size in the porous low-k dielectric films. The effects of the oxygen on the bonding configuration and electrical properties were investigated by adjusting TMS/O2 gas ratios. The porous SiOC:H film displays the small pore sizes and lower dielectric constant. It is found that the pore size of SiOC:H film is significant smaller than 1 nm and the pore size attributed to Si-O-Si cage structure change.     

氮化硅晶须对反应烧结氮化硅多孔陶瓷介电性能的影响

以硅粉和氮化硅晶须为原料,通过添加30%(质量分数)成孔剂球形颗粒,以聚乙烯醇作粘结剂,采用干压成型工艺,反应烧结制备了多孔氮化硅陶瓷,分析对比了氮化硅晶须对反应烧结氮化硅多孔陶瓷介电性能的影响.实验结果表明,随着氮化硅晶须加入量的升高,氮化硅多孔陶瓷的介电常数和介电损耗都升高,介电性能恶化.     

Gd和Sn掺杂BaTiO3陶瓷的介电性能

通过固相反应法制备了掺杂0.5%(摩尔比)Gd和10%(摩尔比)Sn的BaTiO3陶瓷材料,并对样品的介电性能在不同频率、温度下进行了研究.结果表明掺杂之后材料的居里点向低温方向移动,材料的介电常数显著增加.其中同时对BaTiO3的A位掺杂0.5%的Gd,对B位掺杂10%的Sn时,其居里点降至60℃,介电常数在0.005、1、100kHz下的峰值分别达到54000、51000、45000,而对应的tgδ分别为0.053、0.066、0.092.     

Dielectric properties in GHz range of porous Si3N4–BN–SiO2 ceramics with considerable flexural strength prepared by low temperature sintering in air

Abstract

Porous Si₃N₄–BN–SiO₂ ceramics with ultimate apparent porosities between 0·140 and 0·799 were fabricated in air at 1100°C by partial sintering using core starch as both consolidator and pore former in the green bodies. The pores were derived from burning off the starch, the partial oxidation of silicon nitride and the stack of particles of the start materials. Effect of retaining time on the microstructure of sintering bodies was analysed by SEM analysis. Reference intensity ratio (RIR) technique based on the X-ray diffractometry results demonstrated the phase components content of sintered bodies. Influence of porosity on the flexural strength of porous Si₃N₄–BN–SiO₂ ceramics was investigated. The ceramic with a porosity of 0·140 attained a maximal flexural strength of 60±4·11 MPa. In addition, the dielectric constants and loss tangents were presented for porous Si₃N₄–BN–SiO₂ triphase ceramics in the frequency range of 18–40 GHz, and the real part of dielectric constant of the materials reached as low as 2·67 at the porosity of 0·732 at a frequency of 20 GHz.     

Quantitative dependence of the properties of Pb0.99(Zr0.95Ti0.05)0.98Nb0.02O3 ferroelectric ceramics on porosity

Porous Pb_0.99(Zr_0.95Ti_0.05)_0.98Nb_0.02O₃ ferroelectric ceramics with a pore size of the order of the crystalline grain size were prepared and the microstructure and the properties were investigated. Based on this microstructure, the net porosity of the ceramics can be attributed to the intentionally introduced extrinsic porosity and thus the quantitative dependence of ferroelectric and dielectric properties of the ceramics on the porosity can be established respectively. A good agreement with experimental measurements was obtained. Our work represents the first attempt to tailor the properties of ferroelectric ceramics via varying the porosity from the viewpoint of application.     

A dielectric anomaly in electrolyte-saturated porous alumina ceramics

In order to understand the relation between the conductivity and the dielectric properties of porous materials and their pore fluid content, we report and discuss dielectric constant measurements of brine-saturated porous alumina ceramics which exhibit a gigantic increase of the low frequency dielectric constantwhile the sample remains conducting. Generalizing a model derived to study the properties of porous sedimentary rocks, where such an effect has been known for more than two decades, we discuss the effect of the pore geometry on the frequency, salinity and porosity variation of the ceramic dielectric constant and conductivity. This can provide a partial explanation of the reported measurements. Such a study provides a new and interesting method to investigate the microgeometry of composite materials and in particular the pore geometry of ceramics.     

Quantitative microstructural analysis of reaction-bonded silicon nitride

Quantitative analysis of the essential microstructural parameters of injection-moulded reaction-bonded silicon nitride was performed. The effect of silicon grain size on the porosity, the pore size distribution, the degree of reaction and the proportions of the alpha and beta modifications and the grain size of these phases was studied under constant processing conditions. With increasing silicon grain size the degree of reaction and the total porosity and density remain unaffected. The percentage of beta phase, the grain size of alpha and beta modifications as well as the mean pore diameter increase with increasing grain size of the starting powders. The effect of the structural parameters on the room-temperature strength is discussed.     

Effect of sintering parameters on the microstructure and properties of strontium modified PZT ceramics prepared using spray-dried powders

PZT powders of the composition Pb_0.94Sr_0.06 (Zr_0.53Ti_0.47)O₃, prepared by spray drying and calcining techniques, were processed to sintered ceramics by conventional cold pressing and sintering at various temperatures and periods between 1000 to 1250°C for 0.5 to 12h. Sintered ceramics were evaluated for their microstructure and electromechanical properties. Highly dense ceramics having bulk density of the order of 97% of the theoretical value could be obtained after sintering at a considerably lower temperature of 1000°C in comparison to the 1300°C generally required for powders prepared by conventional ceramic processing. However, the increase in sintering temperature of reactive spray-dried powders causes the entrapment of closed pores as a result of exaggerated grain growth and subsequent pore coarsening thereby leading to a decrease in the bulk density of the ceramics. It has been observed that minor variations in the sintering parameters influence the porosity, grain size and electromechanical properties. Values of the dielectric constant, piezoelectric strain coefficient and electromechanic coupling factor increase with the increase in grain size and decrease with the increase in porosity of the sintered ceramic whereas the dielectric dissipation factor decreases with the increase in sintering temperature.     

造孔剂含量对多孔BiScO3-PbTiO3高温压电陶瓷性能的影响

为研究造孔剂含量对多孔BiScO_3-PbTiO_3(记作BS-PT)高温压电陶瓷性能的影响,采用炭黑作为造孔剂,通过传统固相烧结法对不同初始固相体积分数的准同型相界附近的BS-PT/炭黑混合物制备出多孔高温压电陶瓷.利用X射线衍射仪对多孔陶瓷进行物相分析,通过扫描电子显微镜观察样品的新鲜断面和抛光热腐蚀后的表面显微结构,并对其压电、介电和水声性能进行研究.结果表明:制备的不同初始BS-PT体积分数多孔压电陶瓷均为立方钙钛矿相结构,孔隙通道密实化清晰可见,没有显著的缺陷,气孔的形状是长条形的,长度从几微米到几十甚至上百微米不一,气孔之间是孤立的;随着造孔剂炭黑的体积分数从20%增加至50%,气孔率线性地从8.3%增加至22.1%,εr、d33及d31逐渐下降,静水压优值(HFOM)逐渐增大.多孔压电陶瓷的性能强烈依赖于孔隙空间结构,如气孔率、孔径、孔隙形态及连接方式.     

石墨烯改性PDC-SiCNO陶瓷的制备及其介电性能

以聚乙烯基硅氮烷(PVSZ)为原料,氧化石墨烯(GO)为碳源,无水乙醇(ETOH)为分散剂,制备石墨烯球增强SiCNO陶瓷(SiCNO-GO)。利用拉曼光谱(Raman)、电子自旋共振(EPR)和扫描电子显微镜(SEM)等表征手段,研究SiCNO-GO陶瓷结构对其介电性能的影响。结果表明:SiCNO-GO陶瓷的微球密度和粒径的大小与GO的含量有关;随着SiCNO-GO陶瓷中GO含量的增加,SiCNO-GO陶瓷的介电常数和介电损耗也随之增大,在GO含量为0.1%(质量分数)时达到最大值,而当GO质量分数为0.3%时,SiCNO-GO陶瓷的介电常数和介电损耗降低。     

Pore size and pore volume effects on alumina and TCP ceramic scaffolds

Controlled porosity alumina and β-tricalcium phosphate ceramic scaffolds with pore sizes in the range of 300–500 μm and pore volumes in the range of 25–45% were processed using the indirect fused deposition process. Samples having different pore sizes with constant volume fraction porosity and different volume fractions porosity with a constant pore size were fabricated to understand the influence of porosity parameters on mechanical and biological properties. In vitro cell proliferation studies were carried out with OPC1 human osteoblast cell line for 28 days with different scaffolds. Variation in pore size did not show any conclusive differences, but samples with higher volume fraction porosity showed some evidence of increased cell growth. Volume fraction porosity also showed a stronger influence on the mechanical properties under uniaxial compression loading. Compression strength dropped significantly for samples with higher volume fraction porosity, but changed marginally when only the pore size was varied.     

孔径可控的多孔羟基磷灰石的制备工艺研究

采用添加造孔剂法,选择合适的造孔剂聚甲基丙烯酸甲酯（PMMA）,通过严格筛分,可烧结制得孔径可控的多孔基磷灰石陶瓷,气孔率可从20％到50％变化。并对烧结多孔体中孔的结构、孔径分布与特征,影响气孔率和力学性能的因素进行了研究与讨论。     

离心成型技术制备孔梯度分布的氧化锆多孔陶瓷

以2种粒径分布不同的ZrO_2微粉为原料,利用离心成型技术制备孔梯度分布的ZrO_2多孔陶瓷.测量了ZrO_2颗粒在不同pH值下的Zeta电位,研究了离心加速度和浆料固相含量对ZrO_2颗粒分离现象的影响,观察了烧结产物的微观形貌、孔隙度以及孔径分布.研究结果表明,在pH=10时,ZrO_2颗粒的Zeta电位最高,浆料具有良好的分散性.在较低的固相含量和较高的离心加速度下,ZrO_2颗粒的分离现象明显,孔隙呈梯度分布.40%(体积分数)固含量ZrO_2浆料离心所得样品在1400℃烧结3h后,孔隙呈现良好的梯度分布,其底部孔隙度为24.6%,气孔尺寸在1～3μm之间;顶部孔隙度为15.2%,气孔尺寸大多在0.3μm以下.     

原位反应结合碳化硅多孔陶瓷的制备与性能

以碳化硅(SiC)和氧化铝(Al₂O₃)为起始原料、石墨为造孔剂, 通过原位反应结合工艺制备SiC多孔陶瓷. XRD分析表明多孔陶瓷的主相是SiC, 结合相是莫来石与方石英; SEM观察到多孔陶瓷具有相互连通的开孔结构. 坯体在烧结前后具有很小的尺寸变化, 线收缩率约在±1.5%内. 多孔陶瓷的开口孔隙率随烧结温度和成型压力的增大而减小, 随石墨加入量的增加而增大; 而体密度具有相反的变化趋势. 随着石墨粒径的增大, 多孔陶瓷的孔径分布呈现双峰分布. 抗弯强度随烧结温度和成型压力的增大而增大, 随石墨加入量的增大而减小. 于1450℃保温4h烧成的样品在0～800℃的平均热膨胀系数为6.4×10^-6/K. 多孔陶瓷还表现出良好的透气性、抗高温氧化和耐酸腐蚀性, 但耐碱腐蚀性相对较差.     

Effect of Sintering Temperature on the Microstructure,Electrical, and Magnetic Properties of Bi 0 . 8 5 Eu 0 . 1 5 FeO 3 Ceramics

Polycrystalline Bi _0.85Eu _0.15FeO ₃ ceramics were synthesized by solid-state reaction method with rapid liquid phase sintering process at various sintering temperatures. The dependence of structural, microstructural, electrical, and magnetic properties on sintering temperature was systematically investigated. X-ray diffraction measurements reveal that single perovskite phase is developed in Bi _0.85Eu _0.15FeO ₃ ceramics sintered at 850 and 870^° C, while secondary phases can be detected in the samples sintered at 890^° C due to the volatilization of Bi ³⁺ ions, and the crystallinity increases with increasing sintering temperature from 850 to 890 °C. The scanning electron microscopy investigation has suggested that the grain size increases with increasing sintering temperature from 855 t o 890^° C; while the pore size decreases with increasing sintering temperature from 850 to 870^° C and then increases with a further increase of sintering temperature. The electrical and magnetic measurements show that the leakage current, dielectric constant, dielectric loss, and magnetic properties are strongly dependent on the sintering temperature. The Bi _0.85Eu _0.15FeO ₃ ceramics sintered at 870^° C have the lower leakage current, higher dielectric constant, and lower dielectric loss. The room temperature magnetization increases with increasing sintering temperature from 850 to 890 °C. The possible reason for all the above observations was discussed.     

碳热还原-反应烧结法制备多孔氮化硅陶瓷

以廉价的二氧化硅、炭黑和硅粉为起始原料, 利用碳热还原-反应烧结法制备了高气孔率、孔结构均匀的多孔氮化硅陶瓷, 考察了原料中硅粉含量对多孔氮化硅陶瓷微观组织和力学性能的影响。XRD分析表明烧结后的试样成分除了少量的α-Si₃N₄相和晶间相Y₂Si₃O₃N₄外, 其余都是β-Si₃N₄相; SEM分析显示微观组织由棒状β-Si₃N₄晶粒和均匀的孔组成。通过改变硅粉的含量, 制备了不同气孔率, 力学性能优异的多孔氮化硅陶瓷。