凝胶注模工艺制备高强度多孔氮化硅陶瓷

采用凝胶注模成型工艺,成功地制备了具有高强度、结构比较均匀并有较高气孔率的氮化硅多孔陶瓷。本文研究了制得的多孔氮化硅的力学性能和微观结构,并讨论了获得高性能的原因。结果表明,采用适当的成型条件可制备出结构均匀、强度高、加工性能优良的坯体,烧成的多孔氮化硅陶瓷强度均>150MPa,气孔率>50％。SEM照片显示气孔是由长柱状β-Si3N4晶搭接而成的。均匀的气孔分布和柱晶结构是获得高性能的主要原因。     

多孔氧化铝陶瓷的凝胶注模成型

选用石墨粉作为造孔剂,加入已分散良好的氧化铝浆料中,球磨均匀后注模成型。成型后的坯体在1520℃保温烧结2h,获得了分布均匀,孔径为15－30μm的多孔氧化铝陶瓷。     

多孔氧化铝陶瓷的凝胶注模成型

选用石墨粉作为造孔剂,加入到已分散良好的氧化铝浆料中,球磨均匀后注模成型。成型后的坯体在１５２０℃保温２ｈ,获得了分布均匀、孔径为１５～３０μｍ的多孔氧化铝陶瓷。本文对浆料的配制进行了详细地讨论。     

包覆和凝胶注模成型对氮化硅陶瓷性能的影响

利用含 Al (NO3) 3,Y (NO3) 3和尿素的水溶液中无机盐的沉淀再经煅烧在 Si3N4粉料的表面包覆 Y2 O3- Al2 O3层 ,作为氮化硅烧结的助烧剂。包覆层改变了 Si3N4粉料的电动性和胶态特性 ,从而提高了 Si3N4的分散性。研究表明 ,经包覆和凝胶注模成型的方法所制备的氮化硅烧结体较冷等静压方法所获得的烧结体的抗弯强度和 Weibull模数都大大提高     

凝胶注模法制备多孔碳化硅支撑体

以大颗粒碳化硅(SiC)为陶瓷骨料,采用凝胶注模法制备支撑体生坯,原位反应烧结制备大孔径、高渗透性的多孔SiC陶瓷支撑体,主要考察了有机单体含量和烧结制度对高温气固分离用陶瓷膜支撑体性能的影响.研究结果表明:适宜的有机单体含量有助于SiC颗粒稳定分散在悬浮液中,提高烧结温度和延长保温时间均可增加SiC颗粒的氧化程度,在1 550℃时,XRD图谱显示莫来石相生成,支撑体的抗弯强度有一定程度的提高.采用凝胶注模法制备的生坯在1 550℃,保温4h烧结后具有良好的性能:抗弯强度为20.4 MPa,孔隙率为37%,平均孔径为23μm,气体渗透率为2.01×10-12 m2.     

凝胶注模常温发泡制备氧化铝多孔陶瓷

以高纯氧化铝为原料,通过起泡结合凝胶注模成型的方法制备了孔隙率为77%～85%、孔径为40～200μm的氧化铝多孔陶瓷.多孔陶瓷组成为α-Al2O3.多孔陶瓷的微结构可通过固含量与发泡剂加入量的改变进行调控.多孔陶瓷的耐压强度为9.40～32.50MPa,且对其断裂方式进行了研究.多孔陶瓷在1000℃下的热导率为0.80 W.(m.K)-1.     

凝胶注模成型法制备多孔羟基磷灰石陶瓷

采用凝胶注模成型工艺制备了多孔羟基磷灰石陶瓷,并通过X射线分析了多孔陶瓷的相成分,采用扫描电镜观测了孔隙结构和形貌.结果表明,所制备的多孔羟基磷灰石陶瓷的孔隙率均大于80%;孔隙尺寸主要分布在350～600μm,孔壁上存在孔径为60～190μm的贯通孔;X射线衍射证明烧结过程未引入异质成分.所制备的多孔羟基磷灰石陶瓷具有适宜的孔隙直径和孔隙率,且孔隙间具有良好的贯通性.     

MMA-粉煤灰漂珠体系凝胶注模成型制备多孔陶瓷

以甲基丙烯酸甲酯(MMA)为单体,粉煤灰漂珠为骨料,采用非水基凝胶注模成型工艺制备多孔陶瓷。考察了MMA含量对浆料性能的影响、MMA预聚合方式对浆料成型的影响以及生坯的排胶与烧结方法,并对多孔陶瓷性能进行了表征。研究表明:微波预聚合可缩短诱导期、加速MMA本体聚合;过高的微波功率和引发剂用量使反应加速,不利于聚合稳定;提高预聚合程度有助于缩短浆料固化时间、降低生坯体积收缩;为保证浆料的流动性及生坯的完整性,应将MMA预聚液含量控制在45wt%~60wt%;生坯(MMA 50wt%)在380℃排胶1h、1050℃烧结2h,得到的多孔陶瓷抗弯强度为40.35MPa,显气孔率为42.03%,平均孔径为1.12μm。     

叔丁醇基凝胶注模工艺制备轻质、高强莫来石多孔陶瓷

以叔丁醇为成型溶剂, 莫来石粉为起始原料, 采用凝胶注模成型方法制备出轻质、高强莫来石多孔陶瓷. 莫来石多孔陶瓷中的孔隙形成于干燥过程中叔丁醇的快速挥发, 孔隙分布均匀且相互连通. 随烧结温度升高, 气孔率、开气孔率和比表面积分别由77.8%、76.0%和10.39m²/g下降到67.6%、65.5%和4.26m²/g, 而抗压强度则由3.29MPa显著提高到32.36MPa, 材料孔径大小受烧结温度影响较小, 孔径尺寸呈单峰分布, 且几乎所有的气孔都为开口气孔, 透气度与孔径尺寸具有一致的变化关系. 莫来石多孔陶瓷在高气孔率条件下仍然保持高强度的主要原因是材料中均匀的孔隙结构、孔径尺寸小且相对集中、以及因烧结颈的形成在空间上所表现出的一种颗粒搭接骨架结构.     

碳化硼陶瓷凝胶注模成型工艺研究

研究了分散剂用量、固相体积含量对碳化硼浆料粘度的影响,采用扫描电子显微镜(SEM)对素坯微观结构进行了表征。结果表明,以正辛醇为分散介质,当分散剂CH-10S用量为3%(质量分数)时,可以制得固相体积含量为55%的碳化硼浆料。素坯的抗弯强度为38MPa,且素坯中碳化硼颗粒堆积紧密,而且颗粒分散均匀。     

氮化硅层状陶瓷界面性能对力学性能的影响

通过加入Si₃N₄调节隔离层的性质, 研究了Si₃N₄/ BN 层状复合材料在不同界面结合情况下的力学性能变化规律。结果表明, 随着隔离层中Si₃N₄含量的提高, 基体片层之间的结合力不断增强。在结合力很强时, 层状材料具有与块状材料相同的破坏方式, 强度出现极值, 达到1000M Pa以上; 在结合力较弱时, 隔离层能够反复偏折裂纹, 层状材料表现出高达20M Pa?m1/2 的表观断裂韧性和约600M Pa 的强度。      

Synthesis of Si3N4 whiskers in porous SiC bodies

Si₃N₄ whiskers were synthesized by the carbothermal reduction process in porous SiC bodies. The SiC bodies had a sponge microstructure with pore sizes of approximately 600 μm. The raw materials for the Si₃N₄ whiskers were powder mixtures of Si₃N₄, SiO₂ and Si for silicon and phenolic resin for carbon. Cobalt was used as a metal catalyst. The carbothermal reaction was performed at 1400 °C or 1500 °C for 1 or 2 h. The α-Si₃N₄ whiskers grew inside the SiC pores by the VLS process, and their diameters ranged from 0.1 to 1.0 μm. The length of the grown Si₃N₄ whiskers was over 100 μm and their growth direction was [100].     

Effect of the microstructure of Si3N4 on the adhesion strength of TiN film on Si3N4

The effect of the microstructure of silicon nitride, which was used as a substrate, on the adhesion strength of physical vapor deposited TiN film on Si₃N₄ was investigated. Silicon nitride substrates with different microstructures were synthesized by controlling the size (fine or coarse), the phase ( or β) of starting Si₃N₄ powder, and sintering temperature. The microstructure of Si₃N₄ was characterized in terms of grain size, aspect ratio of the elongated grain, and β-to- phase ratio. For a given chemical composition but different mechanical properties, such as toughness, elastic modulus, and hardness of Si₃N₄ were obtained from the diverse microstructures. Hertzian indentation was used to estimate the yield properties of Si₃N_4, such as critical loads for yield (P_y) and for ring cracking (P_c). The effect of the microstructure of Si₃N₄ on adhesion strength evaluated by scratch test is discussed. TiN films on Si₃N₄ showed high adhesion strengths in the range of 80–140 N. Hardness and the P_y of Si₃N₄ substrate were the primary parameters influencing the adhesion strength of TiN film. In TiN coating on Si₃N₄, substrates with finer grain sizes and higher phase ratios, which show high hardness and high P_y, were suitable for higher adhesion strength of TiN film.     

凝胶注模成型制备高性能氮化硅陶瓷(Ⅰ) 助烧剂包覆氮化硅粉料对材料性能的影响

用无机盐共沉淀法在氮化硅颗粒表面包覆一层纳米级的钇铝氧化物后,粉料的分散性大大提高,可用来制备固相体积分数为50%的悬浮体,利用凝胶注模成型和气压烧结制备了氮化硅陶瓷,与机械混合加入助烧剂相比,采用包覆法加入助烧剂能明显提高氮化硅陶瓷的抗弯强度和韦泊尔模数。     

Dense and near-net-shape fabrication of Si3N4 ceramics

With silicon nitride significant progress has been made in order to search for fully dense, strong, reliable structural ceramics to find wide use in applications at high temperatures which are allowing new and innovative solutions to component design problems. Taking into account that more and more ceramic components based on Si₃N₄ are being used in the aerospace and automobile industries, it is a great challenge to fabricate such complex-shaped components with high reliability and with defect-free microstructures such as pores, inclusions or any other inhomogeneity at acceptable costs. On the other side, the high hardness of Si₃N₄ ceramics is almost always cost prohibitive to shape components by hard machining. It is therefore great effort exhibited in the development of near-net-shape fabrication processes that can produce complex-shaped components with a minimum of machining as well as to minimize the number and size of microstructural defects within design limits. In this review, the fabrication of near-net-shape Si₃N₄ ceramics is given in detail. All kinds of these techniques (injection molding, gelcasting, robocasting, mold shape deposition, rapid prototyping) and their advantages and disadvantages are explained.     

Study on particle-stabilized Si3N4 ceramic foams

The stability of bubbles and the microstructures of sintered Si₃N₄ ceramic foams produced by direct foaming method were investigated. The bubbles produced by short-chain amphiphiles (propyl gallate) have higher stability as compared with that produced by long-chain surfactants (TritonX-114). Si₃N₄ ceramic foams using short-chain amphiphile are particle-stabilized one, the pore cells are spherical and closed, and cell surfaces are smooth and dense. The pore cells of sintered Si₃N₄ ceramic foams using TritonX-114 foaming are coarse and large, and pore cells are polyhedral. High gas-pressure sintering is conducive to the development of the whisker-like microstructures in Si₃N₄ ceramic foams. The sintered Si₃N₄ ceramic foams with the whisker-like microstructure are quite promising for improving the mechanical strength of the ceramics by a simple and safe way.     

注凝成型制备ZTA复相陶瓷

讨论了pH值、分散剂添加量、 ZrO₂(3Y)含量和固相体积分数对氧化锆增韧氧化铝(Zirconia toughened alumina, ZTA) 陶瓷注凝成型浆料粘度的影响,研究了注凝成型的烧结样品的性能和显微结构。结果表明,当pH值为8.5、分散剂添加量为0.9%时,可以制备固相体积分数达55%的低粘度ZTA (20%ZrO₂) 悬浮体。高固相悬浮体制备的烧结试样具有结构致密、ZrO₂分布较均匀和t-ZrO₂含量高等特征,其强度和断裂韧性分别达631.5 MPa和7.64 MPa · m1/2。      

Effect of Si3N4-particles addition in Ag-Cu-Ti filler alloy on Si3N4/TiAl brazed joint

A novel composite filler alloy was developed by introducing Si₃N_4p (p = particles) into Ag-Cu-Ti filler alloy. The brazing of Si₃N₄ ceramics and TiAl intermetallics was carried out using this composite filler alloy. The typical interfacial microstructure of brazed joints was: TiAl/AlCu₂Ti reaction layer/Ag_(s,s) + Al₄Cu₉ + Ti₅Si_3p + TiN_p/TiN + Ti₅Si₃ reaction layer/Si₃N₄. Effects of Si₃N_4p content in composite filler alloy on the interfacial microstructure and joining properties were investigated. The distribution of Ti₅Si_3p and TiN_p compounds in Ag-based solid solution led to the decrease of the mismatch of the coefficient of thermal expansion (CTE) and the Young's modulus between Si₃N₄ and TiAl substrate. The maximum shear strength of 115 MPa was obtained when 3 wt.% Si₃N_4p was added in the composite filler alloy. The fracture analysis showed that the addition of Si₃N_4p could improve the mechanical properties of the joint.     

Thermal stability and crystallization kinetics of sputtered amorphous Si3N4 films

The crystallization of thin silicon nitride (Si₃N₄) films deposited on polycrystalline SiC substrates was investigated by X-ray diffractometry as a function of annealing time. The amorphous Si₃N₄ films were produced by means of reactive r.f. magnetron sputtering. Annealing at temperatures between 1300 and 1700 °C led to the formation of crystalline films composed of -Si₃N₄ and β-Si₃N₄. The fraction of β-Si₃N₄ in the films reaches approximately 40% at temperatures above 1550 °C. Both polymorphic modifications were formed simultaneously during the crystallization process. A transformation of -Si₃N₄ to β-Si₃N₄ could not be observed in the time and temperature range investigated. The crystallization process of amorphous Si₃N₄ can be described according to the Johnson–Mehl–Avrami–Kolmogorov (JMAK) formalism, assuming a three-dimensional, interface controlled grain growth from pre-existing nuclei. The rate constants show an Arrhenius behaviour with an activation enthalpy of approximately 5.5 eV.