常规烧结和微波烧结的钛酸钡陶瓷介电和铁电性比较研究

采用溶胶-凝胶法制备钛酸钡粉体作为原料,分别采用常规马弗炉和家用微波炉烧结成陶瓷,研究其晶体结构,比较了两种烧结方式制备的钛酸钡陶瓷的介电和铁电性。结果表明:溶胶-凝胶法制备的钛酸钡粉体为单一赝立方相;采用家用微波炉可烧结得到致密的、单一四方相的钛酸钡陶瓷;微波烧结制备的钛酸钡陶瓷在居里点处的介电峰值远低于常规烧结的钛酸钡陶瓷;微波烧结工艺可使钛酸钡陶瓷在低频下(<800 Hz)的介质损耗有一定程度的降低;微波烧结的钛酸钡陶瓷的剩余极化强度和矫顽场强较常规烧结小。     

致密羟基磷灰石球粒的制备及其生物学性能研究

使用羧甲基壳聚糖(CMCS)和明胶(Gel)作为粘结剂, 以沉淀法制得的纳米羟基磷灰石(HA)浆料为原料, 采用溶胶-凝胶法制备出了粒径分布均匀, 几何形态良好的致密HA球粒. 其孔隙率为4.7%±0.6%, 单粒抗压强度为(8.9±0.4) MPa(颗粒直径为0.5 mm), 高于孔隙率为16.4%±0.5%的多孔球的抗压强度(7.9±0.2) MPa。仿生矿化和细胞培养的结果显示致密HA球粒具有良好的生物学性能。     

溶胶-凝胶法制备Na0.5Bi0.5TiO3基无铅压电陶瓷的研究进展

钛酸铋钠(Na0.5Bi0.5TiO3,简写为NBT)基无铅压电陶瓷由于具有良好的压电性、高居里温度和烧结过程中无毒、易控制性等优点而备受关注.综述了溶胶-凝胶法制备Na0.5Bi0.5TiO3粉体及制备出的陶瓷的结构和性能特点.总结了用溶胶-凝胶法制备压电和介电性能显著提高的钛酸铋钠基无铅压电陶瓷的研究进展.研究表明,溶胶-凝胶法在制备压电陶瓷方面具有均匀性好、纯度高,烧结温度低等优点.展望了该工艺的发展方向.     

细晶MgO·1.44Al2O3透明陶瓷的制备及其性能研究

晶粒细化是提高镁铝尖晶石透明陶瓷机械性能的有效途径之一。本研究采用单相MgO·1.44Al₂O₃陶瓷粉体, 首先通过放电等离子烧结进行成型和预致密化, 然后无压烧结达到烧结末期, 最终在180 MPa下1500 ℃热等静压烧结5 h, 制备出细晶MgO·1.44Al₂O₃透明陶瓷。无压烧结的结果表明: 缩窄气孔尺寸分布、降低平均气孔尺寸有助于显著促进陶瓷的致密化, 得到平均晶粒尺寸为1.4 μm、致密度为96.7%的闭气孔烧结体。透明陶瓷的平均晶粒尺寸为1.9 μm, 维氏硬度为(13.94±0.20) GPa, 杨氏模量为289 GPa。同时, 样品具有良好的光学透过率, 厚度为2 mm的样品在可见光和红外波段的最大直线透过率分别为70%和80%。     

纳米陶瓷微米高温合金复合涂层组织与性能

采用溶胶-凝胶化学包覆法制备纳米陶瓷微米高温合金复合粉末,用HVOF喷涂技术制备了复合涂层,采用SEM观察和摩擦磨损实验分析了复合粉末和复合涂层的组织和性能.研究表明:复合粉末是以纳米陶瓷为外壳包覆微米级高温合金颗粒核心的核壳式结构;陶瓷壳在喷涂过程中形成液相与高温合金液相熔合,烧结成致密陶瓷相,部分陶瓷在冷却过程中析出结晶体;复合涂层与基体的结合强度为59.2 MPa,摩擦系数为0.766,磨损率比纯高温合金涂层降低了32%.     

微波烧结Al2O3/SiC纳米复合陶瓷的研究

以分析纯Al(NO3)3.9H2O·NH3.H2O和50 nm的SiC粉体为原料,采用溶胶-凝胶法制备干凝胶,经热处理合成Al2O3/SiC纳米复合粉体。利用微波烧结制备Al2O3/SiC纳米复合陶瓷,并与常规烧结比较,分析了两种烧结方法对制备试样的力学性能影响。结果表明,与常规烧结相比,微波烧结可以提高Al2O3/SiC纳米复合陶瓷的强度和韧性,改善材料的显微结构,促进致密化和晶粒生长。     

间苯二酚–甲醛辅助溶胶–凝胶法制备纳米Li2MnSiO4/C正极材料

采用间苯二酚–甲醛辅助溶胶–凝胶法制备了纳米Li₂MnSiO₄/C正极材料, 采用X射线衍射(XRD)、扫描电镜(SEM)和恒流充放电测试等方法对材料的结构、形貌以及电化学性能进行了分析和表征。结果表明, 所制备的样品属于正交晶系Pmn21空间群, 物相纯度很高, 颗粒尺寸细小(50 nm左右)且分布均匀, 并具有良好的电化学性能, 首次放电比容量为105.7 mAh/g, 50次循环后容量保持率高达90.7%。XRD图谱显示, 经过充放电循环后, Li₂MnSiO₄能始终保持稳定的晶体结构, 表明间苯二酚-甲醛在烧结过程中形成的网络包覆碳层不仅提高了材料的电子电导率, 还维持了材料结构的稳定。     

钛酸锶钡纳米粉体的溶胶-凝胶自蔓延燃烧制备及其介电性能研究

采用溶胶-凝胶和自蔓延燃烧技术,制备了平均晶粒尺寸约20nm的Ba0.5Sr0.5TiO3(BST)纳米粉体.将纳米粉体压制成形后进行烧结,得到BST陶瓷.采用XRD、SEM、TEM和LCR数字电桥研究了BST的结构、形貌和介电性质.结果表明,干凝胶自蔓延燃烧后,可直接形成分散性好、颗粒尺寸均匀、具有钙钛矿结构的BST纳米粉体.BST陶瓷压片经1250℃烧结2h后获得了致密的结构和相对较大的介电常数.粉体的结晶温度和烧结体的烧结温度均低于传统工艺.很明显,溶胶-凝胶自蔓延燃烧法在纳米材料的制备方面具有明显的技术优势.     

用溶胶—凝胶法合成功能材料

溶胶-凝胶法及其优缺点近年来,欧、美和日本等工业发达国家都在积极开展以金属醇盐 M(OR)_n(R 为烷基)或金属盐为初始出发原料合成玻璃、玻璃陶瓷和陶瓷(烧结多晶体)的所谓溶胶-凝胶法的研究工作。从溶胶-凝胶法的发展     

LiF对镁铝尖晶石透明陶瓷红外透过率的影响

以溶胶-凝胶法制备镁铝尖晶石(以下简称“尖晶石”)粉末, 掺入0~2.5wt%的LiF, 经球磨后, 测试混合粉末的物相组成. 采用热压(HP; 32 MPa/1550℃)及热压结合热等静压(HP/HIP; 热等静压工艺条件为150 MPa/1700℃)工艺制备出尖晶石透明陶瓷. 分析测试了掺入不同LiF的尖晶石陶瓷的结构和红外透过率, 采用感应耦合等离子体(Inductively Coupled Plasma, 或ICP)方法测定了LiF掺杂后的粉料和透明陶瓷中的Li离子含量. 实验显示, LiF的加入促进了尖晶石晶粒长大和气孔的排除, 并促进了尖晶石陶瓷烧结的致密化进程. 添加1.0wt%~1.5wt% LiF的尖晶石透明陶瓷具有最高的红外透过率. LiF在尖晶石陶瓷中形成残余物质, 添加过量的LiF对尖晶石陶瓷的光学性能会产生不利影响.     

纳米铌酸钾钠陶瓷的制备及性能

以新型溶胶-凝胶法制备的平均晶粒尺寸为30 nm的铌酸钾钠粉体为原料, 采用放电等离子体烧结工艺, 在烧结温度为900℃, 压力30 MPa, 烧结时间1 min的条件下, 制备得到纯正交相, 相对密度高达99%以上, 平均晶粒尺寸为40 nm的纳米铌酸钾钠陶瓷, 并对该陶瓷的相结构、微观形貌、介电性能和铁电性能进行了研究。结果表明, 与普通微米晶陶瓷不同, 纳米铌酸钾钠陶瓷的室温介电常数仅为341, 并且随温度变化不明显, 表现出明显的介电弛豫现象, 弥散因子γ为1.60, 并具有明显的电滞回线, 矫顽场强度为13.5 kV/cm, 剩余极化为1.5 μC/cm²。尺寸降低所引起的纳米铌酸钾钠陶瓷中晶界相所占的比例增大是其性能变化的主要原因, 并且可以推断, 如果铌酸钾钠陶瓷具有“临界尺寸”, 那么其值应该在40 nm以下。     

Strength and fatigue properties of three-step sintered dense nanocrystal hydroxyapatite bioceramics

Dense hydroxyapatite (HA) ceramic is a promising material for hard tissue repair due to its unique physical properties and biologic properties. However, the brittleness and low compressive strength of traditional HA ceramics limited their applications, because previous sintering methods produced HA ceramics with crystal sizes greater than nanometer range. In this study, nano-sized HA powder was employed to fabricate dense nanocrystal HA ceramic by high pressure molding, and followed by a three-step sintering process. The phase composition, microstructure, crystal dimension and crystal shape of the sintered ceramic were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Mechanical properties of the HA ceramic were tested, and cytocompatibility was evaluated. The phase of the sintered ceramic was pure HA, and the crystal size was about 200 nm. The compressive strength and elastic modulus of the HA ceramic were comparable to human cortical bone, especially the good fatigue strength overcame brittleness of traditional sintered HA ceramics. Cell attachment experiment also demonstrated that the ceramics had a good cytocompatibility.     

树脂包覆球形SiO2颗粒制备3D打印用陶瓷/树脂复合粉体

采用球形致密的SiO₂微米颗粒制备用于3D打印的陶瓷/树脂复合粉体, 并对粉体的固化和烧结性能进行了研究。结果显示, 随着温度升高或固体含量的增加, 包覆介质的粘度逐渐增大, 最佳树脂浓度为27wt%。均匀包覆的陶瓷/树脂复合粉体具有良好的分散性、流动性(25 (s/50 g))和较大的堆积密度(45.0%)。球形颗粒堆积形成的贯通孔道和球形颗粒表面均匀的吸附能对均匀包覆过程起到了至关重要的作用。包覆层的厚度(1.1~3.7 μm)可以通过调节抽滤过程的负压进行精确控制。由于颗粒之间形成了树脂颈部, 使制备的粉体具有很好的固化强度, 固化的陶瓷生胚经1250 ℃烧结后获得了性能优异的陶瓷: 压缩强度为10.2 MPa, 弯曲强度为2.7 MPa, 烧结收缩仅5%。上述结果表明, 复合粉体在3D打印产业上具有良好的应用前景。     

蜡球造孔法制备多孔HA陶瓷支架及其性能优化

组织工程支架的贯通性对其体内生物学表现具有重要影响。采用甲壳素溶胶体系和蜡球造孔剂制备多孔羟基磷灰石(HA)陶瓷支架, 考查在相同模压条件下, 不同浆料/造孔剂比例对多孔HA陶瓷支架的孔隙率、收缩率、贯通性、多孔结构以及抗压强度的影响。结果表明: 该方法可以制备具有高孔隙的多孔HA陶瓷支架, 随着造孔剂比例的增大, 支架的贯通性更好, 当浆料/造孔剂比例为1:1.2时可以得到孔隙率、贯通性、力学性能最优的多孔HA陶瓷支架。     

球形纳米氧化铝颗粒制备微晶陶瓷及传质动力学研究

采用球形纳米氧化铝颗粒制备氧化铝微晶陶瓷,研究造粒、烧结等工艺过程对陶瓷微观结构和力学性能的影响,并结合动力学计算分析球形颗粒在烧结过程中的传质特性。结果表明:通过液相造粒掺入0.8%(质量分数)的PVA能够优化球形颗粒的压制成型并提高坯体密度。烧结温度从1400℃提高至1550℃,陶瓷相对致密度由74.1%增大至97.5%,而晶粒尺寸由0.6μm仅增至1.4μm,这与球形颗粒自身稳定的形态及其堆积形成的均匀孔隙有关。在1550℃下烧结时间由30 min延长至120 min时,气孔率由4.8%降低至0.4%,晶粒尺寸则由1.2μm增至2.7μm。另外,通过动力学计算得出球形颗粒的烧结活化能为788 kJ/mol,证实球形颗粒在烧结前期和中期具有生长惰性,利于获得微晶结构。经1550℃保温90 min的陶瓷,其密度达到98.9%,平均晶粒尺寸仅为1.6μm,硬度达到26.4 GPa,弯曲强度为574 MPa。     

Formation of translucent hydroxyapatite ceramics by sintering in carbon dioxide atmospheres

Hydroxyapatite is used in a variety of clinical applications as a result of the apparent adherence to and mild reaction of bone and soft tissue to it owing to its structural similarity with bone mineral. Transparent hydroxyapatite has previously been fabricated by either or both of two methods; namely the application of pressure during sintering and/or the use of fine particle sized apatite prepared by either a sol-gel process or aqueous precipitation. Recently it has been shown that translucent carbonate hydroxyapatite may be formed by sintering nanocrystalline gels of carbonate hydroxyapatite in a wet carbon dioxide atmosphere. In this study we report for the first time that this atmosphere can be used to sinter microcrystalline powder compacts of hydroxyapatite to form translucent ceramics at ambient pressure. The effect of water partial pressure and sintering time at 1300°C on the optical transmission and microstructure of the ceramic was investigated. It was found that translucent ceramics were formed in all carbon dioxide atmospheres and that optical transmission varied with sintering time. Maximum transmission (13%) of 2 mm thick ceramic was obtained in materials sintered for four hours at 1300°C in a mixture of carbon dioxide containing water at a partial pressure of 4.6 kPa.     

Effects of rheological properties on ice-templated porous hydroxyapatite ceramics

Freeze casting of aqueous suspension was investigated as a method for fabricating hydroxyapatite (HA) porous ceramics with lamellar structures. The rheological properties of HA suspensions employed in the ice-templated process were investigated systematically. Well aligned lamellar pores and dense ceramic walls were obtained successfully in HA porous ceramics with the porosity of 68–81% and compressive strength of 0.9–2.4 MPa. The results exhibited a strong correlation between the rheological properties of the employed suspensions and the morphology and mechanical properties of ice-templated porous HA ceramics, in terms of lamellar pore characteristics, porosities and compressive strengths. The ability to produce aligned pores and achieve the manipulation of porous HA microstructures by controlling the rheological parameters were demonstrated, revealing the potential of the ice-templated method for the fabrication of HA scaffolds in biomedical applications.     

ZnO压敏陶瓷的微波烧结

对用纳米粉体制备的ZnO压敏生坯进行了微波烧结,通过XRD、SEM分析和电性能测试,与普通烧结比较,微波烧结可使ZnO压敏材料快速成瓷,显著缩短烧结时间;在相同晶粒尺寸下,微波烧结温度更低,瓷体更致密;并能获得较好电性能．微波烧结为ZnO压敏陶瓷材料制备提供了一条新的、高效节能的途径．