基于溶液前驱体浸渗调控陶瓷组成和性能的研究
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摘要
液相前驱体浸渗（liquid precursor infiltration）是一种可以实现高均匀度掺杂、表面改性、制备复合材料及梯度材料的工艺。将具有开口气孔的坯体置入液相前驱体中，含有改性组元的液相会沿孔隙结构渗入坯体内部，使材料的组成和性能得以改变。本文通过将浸渗工艺应用于之前涉及不多的几个材料体系，制备出了组织、性能具有明显优势的陶瓷材料，并详细地对比了浸渗与传统工艺的优缺点。
本文首先使用含有致色离子的水溶液浸渗水萃取脱脂的注射成型氧化锆坯体，从而制备了彩色氧化锆陶瓷部件，提供了一种普适性的方法。制备的材料具有厚度可控的宏观芯-壳结构。此外，萃取脱脂后的干燥制度影响传质机理，并导致了浸渗速率的明显变化。通过使用水-酒精混合溶液，解决了浸渗工艺在憎水型坯体上使用的问题。
使用循环浸渗-原位沉淀工艺向氧化铝坯体中引入了含量可控、尺寸细小、分布均匀的ZrO_2晶粒，制备了ZTA材料。浸渗在很低的ZrO_2添加量下（2.3vol%）成功地抑制了晶粒的异常长大，而传统上认为至少需要5vol%才能实现该目标。通过调整浸渗后的干燥温度，可以调节含锆沉淀物的分解行为，从而调控引入的ZrO_2的量。
接下来探索了几个工艺参数对浸渗效果的影响。发现降低溶液浓度、减小坯体尺寸，施加促进气体排出的辅助机制等方法有助于提高浸渗填充率并实现良好的均匀性。使用浸渗工艺对小尺寸陶瓷坯体进行低浓度掺杂，可以达到良好的分布均匀性和较为精确的添加剂引入量。
最后以浸渗硝酸盐水溶液的形式向氧化铝坯体中引入了添加剂，通过高温氢气气氛烧结制备了半透明氧化铝陶瓷。与传统球磨工艺相比，浸渗制备的样品添加剂分布均匀性更优，显微组织也更为细小。添加500ppm MgO制备的样品其平均晶粒尺寸仅有7μm，三点抗弯强度达到300MPa，综合性能明显优于球磨对照样。浸渗三种添加剂共掺杂可以实现更优的透光率。
Liquid precursor infiltration technique is capable of introducing dopants with highhomogeneity, realizing surface modification, manufacturing of composite and gradientmaterials. By immersing green body with open porosities in the liquid containingmodifying components, the liquid would migrate along the interconnected porousstructure into the inerior part of the preform, achieving manipulation of thecomposition and properties of the material. This study is mainly focused onapplication of infiltration technique in several materials. Various ceramic materialswith obviously improved microstructure and properties have been fabricated. Theadvantages and disadvantages of both infiltration and the conventional ceramicprocessing technologies have also been contrastively studied.
Firstly, ceramic parts have been developed by infiltrating aqueous solutionscontaining coloring ions into the water-debound green bodies prepared by ceramicinjection molding. Our strategy provided a general approach to the preparation ofcolored ceramics. The fabricated colored zirconia ceramics exhibits a macroscopiccore-shell structure with tunable thickness. Besides, the drying process influences theinfiltration rate by controlling the mass transferring mechanism. By adding ethanol tothe aqueous solution, the problem of applying infiltration to the hydrophobic greenbodies has been solved.
ZTA composites have been prepared by cyclic infiltration and in-situ precipitationtechnique. The fabricated material contains fine-sized, well-distributed ZrO_2grainsthroughout the bulk matrix. Compared with the conventional ball-milling approach,infiltration prepared material successfully inhibits the abnormal grain growthphenomenon at a ZrO_2content (2.3vol%) lower than the previously reported criticalvalue (5vol%). By adjusting the drying temperature after precipitation, thedecomposition behavior of zirconium-containing precipitates could be controlled,thereby adjusting the ZrO_2content introduced via infiltration.
The next section investigates factors influencing the amount of exotic components,distribution profiles and so forth. It is found that reducing the solution concentration,diminishing the size of green body and imposing assisting mechanisms which favor the evacuation of entrapped gas within the green compact is beneficial for achieving ahigh infiltration efficiency and enhanced homogeneity. The results indicate thatinfiltration is especially suitable for doping small-sized ceramic green bodies withlow-content exotic elements, achieving good distribution homogeneity and precisecontrol of the introduced amount.
The last part is focused on preparing translucent alumina ceramics via infiltrationand H2sintering. Different from the conventional strategies of introducing dopants inthe ball-milling stage, pure alumina preforms were infiltrated using aqueous nitratesolutions. Infiltration prepared composites exhibit much improved homogneity ofintroduced sintering additives and finer microstructure. The sample containing500ppm MgO has an average grain size of only approximately7μm, flexural strengthof about300MPa, exhibiting much enhanced optical properties over the ball-millingprepared counterpart. Triple doping proved to be more beneficial for achieving highertransmission properties.
本文首先使用含有致色离子的水溶液浸渗水萃取脱脂的注射成型氧化锆坯体，从而制备了彩色氧化锆陶瓷部件，提供了一种普适性的方法。制备的材料具有厚度可控的宏观芯-壳结构。此外，萃取脱脂后的干燥制度影响传质机理，并导致了浸渗速率的明显变化。通过使用水-酒精混合溶液，解决了浸渗工艺在憎水型坯体上使用的问题。
使用循环浸渗-原位沉淀工艺向氧化铝坯体中引入了含量可控、尺寸细小、分布均匀的ZrO_2晶粒，制备了ZTA材料。浸渗在很低的ZrO_2添加量下（2.3vol%）成功地抑制了晶粒的异常长大，而传统上认为至少需要5vol%才能实现该目标。通过调整浸渗后的干燥温度，可以调节含锆沉淀物的分解行为，从而调控引入的ZrO_2的量。
接下来探索了几个工艺参数对浸渗效果的影响。发现降低溶液浓度、减小坯体尺寸，施加促进气体排出的辅助机制等方法有助于提高浸渗填充率并实现良好的均匀性。使用浸渗工艺对小尺寸陶瓷坯体进行低浓度掺杂，可以达到良好的分布均匀性和较为精确的添加剂引入量。
最后以浸渗硝酸盐水溶液的形式向氧化铝坯体中引入了添加剂，通过高温氢气气氛烧结制备了半透明氧化铝陶瓷。与传统球磨工艺相比，浸渗制备的样品添加剂分布均匀性更优，显微组织也更为细小。添加500ppm MgO制备的样品其平均晶粒尺寸仅有7μm，三点抗弯强度达到300MPa，综合性能明显优于球磨对照样。浸渗三种添加剂共掺杂可以实现更优的透光率。
Liquid precursor infiltration technique is capable of introducing dopants with highhomogeneity, realizing surface modification, manufacturing of composite and gradientmaterials. By immersing green body with open porosities in the liquid containingmodifying components, the liquid would migrate along the interconnected porousstructure into the inerior part of the preform, achieving manipulation of thecomposition and properties of the material. This study is mainly focused onapplication of infiltration technique in several materials. Various ceramic materialswith obviously improved microstructure and properties have been fabricated. Theadvantages and disadvantages of both infiltration and the conventional ceramicprocessing technologies have also been contrastively studied.
Firstly, ceramic parts have been developed by infiltrating aqueous solutionscontaining coloring ions into the water-debound green bodies prepared by ceramicinjection molding. Our strategy provided a general approach to the preparation ofcolored ceramics. The fabricated colored zirconia ceramics exhibits a macroscopiccore-shell structure with tunable thickness. Besides, the drying process influences theinfiltration rate by controlling the mass transferring mechanism. By adding ethanol tothe aqueous solution, the problem of applying infiltration to the hydrophobic greenbodies has been solved.
ZTA composites have been prepared by cyclic infiltration and in-situ precipitationtechnique. The fabricated material contains fine-sized, well-distributed ZrO_2grainsthroughout the bulk matrix. Compared with the conventional ball-milling approach,infiltration prepared material successfully inhibits the abnormal grain growthphenomenon at a ZrO_2content (2.3vol%) lower than the previously reported criticalvalue (5vol%). By adjusting the drying temperature after precipitation, thedecomposition behavior of zirconium-containing precipitates could be controlled,thereby adjusting the ZrO_2content introduced via infiltration.
The next section investigates factors influencing the amount of exotic components,distribution profiles and so forth. It is found that reducing the solution concentration,diminishing the size of green body and imposing assisting mechanisms which favor the evacuation of entrapped gas within the green compact is beneficial for achieving ahigh infiltration efficiency and enhanced homogeneity. The results indicate thatinfiltration is especially suitable for doping small-sized ceramic green bodies withlow-content exotic elements, achieving good distribution homogeneity and precisecontrol of the introduced amount.
The last part is focused on preparing translucent alumina ceramics via infiltrationand H2sintering. Different from the conventional strategies of introducing dopants inthe ball-milling stage, pure alumina preforms were infiltrated using aqueous nitratesolutions. Infiltration prepared composites exhibit much improved homogneity ofintroduced sintering additives and finer microstructure. The sample containing500ppm MgO has an average grain size of only approximately7μm, flexural strengthof about300MPa, exhibiting much enhanced optical properties over the ball-millingprepared counterpart. Triple doping proved to be more beneficial for achieving highertransmission properties.
引文
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