氧化铝和氧化硅多孔陶瓷冷凝成型与组织性能研究
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摘要
多孔陶瓷作为一种重要的材料,由于其具有密度小、耐高温、耐腐蚀、比表面积高等优点,在工程上被广泛应用于各个领域。在过去几十年,大量的技术被发展用于多孔陶瓷的制备,但由于其自身的特点,所得材料孔的性质被限制在一定范围内。冷凝成型工艺,利用成型剂晶体生长与升华的制备技术,以其材料组织性能可控、环境友好等特性,为多孔陶瓷的制备提供新的途径。
针对这种新型的成型技术,结合颗粒对凝固系统温度与浓度场的影响,从理论上确定固-液界面的稳定性条件,并根据移动界面与颗粒之间的相互作用,获得界面捕获与排出颗粒的临界速率。利用固-液界面的不稳定及颗粒从界面排除的判定条件,采用浆料底部匀速降温的定向凝固方式设计和制备了具有单向宏孔排列结构的材料,并从浆料组成成分与冷凝成型技术的角度对所制备材料的组织性能进行研究。
实验结果表明,在氧化铝浆料引入甘油作为抗冻剂,冷凝成型制备的多孔陶瓷的力学性能可能被提高。通过研究不同固相含量浆料中,甘油浓度对凝固过程、陶瓷显微结构和抗压强度的影响,认为甘油的添加增加了浆料的粘度和烧结样品的致密度,促进陶瓷中宏孔结构的转变和陶瓷层间的连接。这种良好的连接使多孔陶瓷获得高的力学性能。对于30 vol.%固相含量的水-甘油基浆料而言,制备陶瓷的轴向和侧向抗压强度分别达到255.1 MPa和105.8 MPa。
除了浆料组分的改变可以对多孔陶瓷的组织性能调节外,冷凝成型技术的改进也能达到相同的目的。例如通过采用浸渍与定向凝固结合的技术制备了具有复杂三维连通孔结构的氧化铝陶瓷。在这个过程中,聚氨酯海绵被浸渍于含有20 vol.%氧化铝浆料的模具内,随后使浆料底部以6℃/min的降温速率定向凝固。经过预制件的干燥与烧结后,具有明显层状结构的多孔陶瓷被获得,其层厚与层间距分别为~9μm和~15μm。来源于海绵骨架烧蚀形成的大孔均匀分布在陶瓷样品中,这些大孔的存在导致了层状结构的局部中断,但所制备的多孔陶瓷仍保持高的力学性能。
在定向凝固过程中,电场的引入也被用于致密/多孔双层氧化铝陶瓷的制备。其中致密层的厚度能够通过调节电压强度的大小进行控制,当加载的电压从15 V增加至90 V时,致密层厚度由51μm相应地增加到155μm。而在多孔层部分,所有制备的陶瓷都表现出相同的、具有良好连接的层状结构,其层厚与层间距分别为~14μm和~24μm。
由于催化和吸附等领域的实际应用,具有等级孔系统的单向宏孔排列氧化硅陶瓷通过可溶性淀粉模板的矿化被原位合成。该过程由两步所构成,第一步采用可溶性淀粉水溶胶或水凝胶的定向冷凝制备具有单向宏孔通道的块体材料;第二步,使用制备的淀粉材料作为模板浸渍于含有表面活性剂的溶胶-凝胶溶液中,进行模板结构的矿化。实验结果表明,所制备可溶性淀粉材料的宏孔尺寸、壁厚及宏孔形貌可以通过调节其浆料的含量控制。当淀粉初始含量由10 wt.%改变为15 wt.%时,模板材料的宏孔尺寸减小,而壁厚增加。经过对第二步处理得到材料的干燥和煅烧后,多孔氧化硅陶瓷被获得。这些陶瓷完整地复制了模板的精细结构,展示了狭窄的宏孔分布。就其孔径而言,当浸渍时间从36 h增加到84 h时,平均尺寸由4.1μm减小到3.6μm。此外,在纳米尺度内,所有氧化硅陶瓷都展现出均匀的蠕虫状纳米孔与层状相的共存结构和高的BET、微孔比表面积。
Porous ceramics as a technological important material have been widely applied in various regions, because they are lightweight, can withstand high temperature and corrosion, and exhibit high specific surface aera. In the past few decades, a large number of techniques are developed for the fabrication of such materials. However, all processing routes suffer from themselves inherent limitation: pore characteristics of ceramics which prepared by these techniques are limited to a narrow range. Freeze-casting technique, a manufacture method which uses growth and sublimation of vehicle crystal, possesses controllable microstructure and properties and environmental friendliness, and supplys a new route to prepare porous ceramics.
In view of the new formation technique, a stability condition of solid-liquid interface was determined, combined with effect of particles on temperature fields and concentration fields of solidification system. Based on the interaction between the moving interface and a particle, critical velocity of trapped particle was evaluated. Using the criteria condition of interface instability and particle expelled from interface and unidirectional solidification way under a constant cooling rate, porous materials with aligned channel morphology were fabricated. From the perspectives of slurry components and freeze-casting technique investigated effects of formation technics on microstructure and properties of prepared materials.
Experiment results indicated that mechanical properties of alumina porous ceramics might be improved by introducing glycerol into raw slurries. The effects of glycerol on the freeze-casting process and thereby on the microstructure and compression strength of porous ceramics obtained were investigated. It was shown that the addition of glycerol increased both the slurry viscosity and sample sintered density, promoting transition of macroporous structure and connection between ceramic lamellae. This connection made as-prepared porous ceramics obtain high mechanical properties. For the 30 vol.% alumina slurry with glycerol, the axial and radial compression strengths reached to, respectively, 255.1 MPa and 105.8 MPa.
In addition to changing slurry components, the change of freeze-casting technique could also adjust the microstructure and properties of porous ceramics. For instance, the ceramic with complex 3D interconnected porous structures could be fabricated by a combination of impregnating and unidirectional freeze-casting technique. In the process, the polyurethane sponge was impregnated in the mold with 20 vol% of aqueous alumina slurry, and then the bottom of the cast body was kept at a constant cooling rate of 6°C/min to induce solidification. After drying and sintering of the green part, porous ceramic with obvious lamellar architectures was obtained. The lamellae thickness and interlayer distance were as large as ~9μm and ~15μm, respectively. The large pores, which resulted from the burn-up of sponge struts, were homogeneously distributed in the sample. The existence of these large pores introduced some local interruption of the lamellar structures. However, high compression strength for the porous ceramics could still be remained.
In the unidirectional freeze-casting process, introduction of an electric field could also be used to prepare dense/porous bilayered ceramics. The thickness of dense layer in the sample could be controlled by tuning the electric field intensity. When the voltage was increased from 15 to 90 V, the dense layer thickness was increased from 51μm to 155μm, correspondingly. On the other hand, all samples exhibited an identical and good connective lamellar structure in the porous region. These lamellae thickness and interlayer distance were as large as ~14μm and ~24μm, respectively.
Because of practical application of materials in catalysis field and adsorption field, hierarchically porous silica ceramics with unidirectionally aligned channel morphology were in-situ synthesized by mineralization of soluble starch monolith. The procedure followed two steps. First, soluble starch monoliths with well defined uniaxial macroporous structures were prepared by unidirectional freeze-casting process of starch hydrosol or starch hydrogel. Second, these prepared artificial monoliths which used as templates were soaked into a surfactant-templated sol-gel solution to mineralize aligned channel structures in their tissues. It was shown that the macropore size, wall thickness, and macropore morphology of obtained starch materials may be controlled by adjusting the concentration of starch slurry. When initial concentration changed from 10 wt.% to 15 wt.%, the macropore size of soluble starch materials decreased, while the wall thickness increased. Through the second step, porous silica ceramics were obtained after drying and calcining of organic-inorganic hybrid silicate compounds from the solution. These resulting products preserved templates microstructure in great detail and exhibited narrow macropore size distributions. It was observed when the soaking time increased from 36 h to 84 h, the average pore size of silica ceramics was decreased from 4.1μm to 3.6μm. In addition, in nanopore regime, all of these silica monoliths presented the conexistence of uniform worm-like nanopore and lamellar phase feature, and large BET and microporous surface area.
针对这种新型的成型技术,结合颗粒对凝固系统温度与浓度场的影响,从理论上确定固-液界面的稳定性条件,并根据移动界面与颗粒之间的相互作用,获得界面捕获与排出颗粒的临界速率。利用固-液界面的不稳定及颗粒从界面排除的判定条件,采用浆料底部匀速降温的定向凝固方式设计和制备了具有单向宏孔排列结构的材料,并从浆料组成成分与冷凝成型技术的角度对所制备材料的组织性能进行研究。
实验结果表明,在氧化铝浆料引入甘油作为抗冻剂,冷凝成型制备的多孔陶瓷的力学性能可能被提高。通过研究不同固相含量浆料中,甘油浓度对凝固过程、陶瓷显微结构和抗压强度的影响,认为甘油的添加增加了浆料的粘度和烧结样品的致密度,促进陶瓷中宏孔结构的转变和陶瓷层间的连接。这种良好的连接使多孔陶瓷获得高的力学性能。对于30 vol.%固相含量的水-甘油基浆料而言,制备陶瓷的轴向和侧向抗压强度分别达到255.1 MPa和105.8 MPa。
除了浆料组分的改变可以对多孔陶瓷的组织性能调节外,冷凝成型技术的改进也能达到相同的目的。例如通过采用浸渍与定向凝固结合的技术制备了具有复杂三维连通孔结构的氧化铝陶瓷。在这个过程中,聚氨酯海绵被浸渍于含有20 vol.%氧化铝浆料的模具内,随后使浆料底部以6℃/min的降温速率定向凝固。经过预制件的干燥与烧结后,具有明显层状结构的多孔陶瓷被获得,其层厚与层间距分别为~9μm和~15μm。来源于海绵骨架烧蚀形成的大孔均匀分布在陶瓷样品中,这些大孔的存在导致了层状结构的局部中断,但所制备的多孔陶瓷仍保持高的力学性能。
在定向凝固过程中,电场的引入也被用于致密/多孔双层氧化铝陶瓷的制备。其中致密层的厚度能够通过调节电压强度的大小进行控制,当加载的电压从15 V增加至90 V时,致密层厚度由51μm相应地增加到155μm。而在多孔层部分,所有制备的陶瓷都表现出相同的、具有良好连接的层状结构,其层厚与层间距分别为~14μm和~24μm。
由于催化和吸附等领域的实际应用,具有等级孔系统的单向宏孔排列氧化硅陶瓷通过可溶性淀粉模板的矿化被原位合成。该过程由两步所构成,第一步采用可溶性淀粉水溶胶或水凝胶的定向冷凝制备具有单向宏孔通道的块体材料;第二步,使用制备的淀粉材料作为模板浸渍于含有表面活性剂的溶胶-凝胶溶液中,进行模板结构的矿化。实验结果表明,所制备可溶性淀粉材料的宏孔尺寸、壁厚及宏孔形貌可以通过调节其浆料的含量控制。当淀粉初始含量由10 wt.%改变为15 wt.%时,模板材料的宏孔尺寸减小,而壁厚增加。经过对第二步处理得到材料的干燥和煅烧后,多孔氧化硅陶瓷被获得。这些陶瓷完整地复制了模板的精细结构,展示了狭窄的宏孔分布。就其孔径而言,当浸渍时间从36 h增加到84 h时,平均尺寸由4.1μm减小到3.6μm。此外,在纳米尺度内,所有氧化硅陶瓷都展现出均匀的蠕虫状纳米孔与层状相的共存结构和高的BET、微孔比表面积。
Porous ceramics as a technological important material have been widely applied in various regions, because they are lightweight, can withstand high temperature and corrosion, and exhibit high specific surface aera. In the past few decades, a large number of techniques are developed for the fabrication of such materials. However, all processing routes suffer from themselves inherent limitation: pore characteristics of ceramics which prepared by these techniques are limited to a narrow range. Freeze-casting technique, a manufacture method which uses growth and sublimation of vehicle crystal, possesses controllable microstructure and properties and environmental friendliness, and supplys a new route to prepare porous ceramics.
In view of the new formation technique, a stability condition of solid-liquid interface was determined, combined with effect of particles on temperature fields and concentration fields of solidification system. Based on the interaction between the moving interface and a particle, critical velocity of trapped particle was evaluated. Using the criteria condition of interface instability and particle expelled from interface and unidirectional solidification way under a constant cooling rate, porous materials with aligned channel morphology were fabricated. From the perspectives of slurry components and freeze-casting technique investigated effects of formation technics on microstructure and properties of prepared materials.
Experiment results indicated that mechanical properties of alumina porous ceramics might be improved by introducing glycerol into raw slurries. The effects of glycerol on the freeze-casting process and thereby on the microstructure and compression strength of porous ceramics obtained were investigated. It was shown that the addition of glycerol increased both the slurry viscosity and sample sintered density, promoting transition of macroporous structure and connection between ceramic lamellae. This connection made as-prepared porous ceramics obtain high mechanical properties. For the 30 vol.% alumina slurry with glycerol, the axial and radial compression strengths reached to, respectively, 255.1 MPa and 105.8 MPa.
In addition to changing slurry components, the change of freeze-casting technique could also adjust the microstructure and properties of porous ceramics. For instance, the ceramic with complex 3D interconnected porous structures could be fabricated by a combination of impregnating and unidirectional freeze-casting technique. In the process, the polyurethane sponge was impregnated in the mold with 20 vol% of aqueous alumina slurry, and then the bottom of the cast body was kept at a constant cooling rate of 6°C/min to induce solidification. After drying and sintering of the green part, porous ceramic with obvious lamellar architectures was obtained. The lamellae thickness and interlayer distance were as large as ~9μm and ~15μm, respectively. The large pores, which resulted from the burn-up of sponge struts, were homogeneously distributed in the sample. The existence of these large pores introduced some local interruption of the lamellar structures. However, high compression strength for the porous ceramics could still be remained.
In the unidirectional freeze-casting process, introduction of an electric field could also be used to prepare dense/porous bilayered ceramics. The thickness of dense layer in the sample could be controlled by tuning the electric field intensity. When the voltage was increased from 15 to 90 V, the dense layer thickness was increased from 51μm to 155μm, correspondingly. On the other hand, all samples exhibited an identical and good connective lamellar structure in the porous region. These lamellae thickness and interlayer distance were as large as ~14μm and ~24μm, respectively.
Because of practical application of materials in catalysis field and adsorption field, hierarchically porous silica ceramics with unidirectionally aligned channel morphology were in-situ synthesized by mineralization of soluble starch monolith. The procedure followed two steps. First, soluble starch monoliths with well defined uniaxial macroporous structures were prepared by unidirectional freeze-casting process of starch hydrosol or starch hydrogel. Second, these prepared artificial monoliths which used as templates were soaked into a surfactant-templated sol-gel solution to mineralize aligned channel structures in their tissues. It was shown that the macropore size, wall thickness, and macropore morphology of obtained starch materials may be controlled by adjusting the concentration of starch slurry. When initial concentration changed from 10 wt.% to 15 wt.%, the macropore size of soluble starch materials decreased, while the wall thickness increased. Through the second step, porous silica ceramics were obtained after drying and calcining of organic-inorganic hybrid silicate compounds from the solution. These resulting products preserved templates microstructure in great detail and exhibited narrow macropore size distributions. It was observed when the soaking time increased from 36 h to 84 h, the average pore size of silica ceramics was decreased from 4.1μm to 3.6μm. In addition, in nanopore regime, all of these silica monoliths presented the conexistence of uniform worm-like nanopore and lamellar phase feature, and large BET and microporous surface area.
引文
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