先驱体转化多孔硅氧碳陶瓷及其复合材料的制备与性能研究
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摘要
多孔陶瓷是材料科学领域中一类倍受关注的新型材料。由于多孔陶瓷具有良好的耐高温、抗热震、高强度、高化学稳定性和高比表面积等优异性能,在过滤器、热交换器、催化剂载体、光电器件及传感器等领域具有重要的应用价值。与传统制备方法相比,先驱体转化制备多孔陶瓷具有烧结温度低、良好的加工性、分子可设计性和分级多孔结构等优点。其中,采用模板法能制备出可设计的孔隙度和孔径分布的多孔陶瓷,且制备工艺简单。
本研究以多孔陶瓷的设计、制备及性能研究为主旨,通过改变陶瓷前驱体及多孔模板类型,或加入惰性填料,成功制备了多孔SiOC陶瓷及多孔SiOC/BN复合材料,所得多孔陶瓷具有可控的开口气孔率和孔径分布。本论文研究了不同的工艺条件对所得多孔SiOC陶瓷及其复合材料的微观形貌、结构及性能的影响,并分析了多孔结构中纳米线的生长机理。主要研究结果如下：
以聚氨酯海绵为人工模板、有机硅树脂(R9801)为陶瓷前驱体,浸渍后再烧结制备了多孔SiOC陶瓷。SiOC陶瓷具有蜂窝状的多孔形貌,开口气孔率最高达85%。随着烧结温度的升高,样品中SiOC玻璃相产生相分离向SiO2、SiC纳米晶和SiC纳米线转变。当烧结温度较高或保温时间较长时,多孔SiOC陶瓷具有较好的氮吸附性能,半导体特性和热稳定性。
以滤纸为生物模板,有机硅树脂为陶瓷前驱体,热压成型后烧结制备了层状多孔SiOC陶瓷,样品保留了滤纸原有的纤维形貌,开口气孔率最高达55%。随着烧结温度的升高,样品的SiOC玻璃相逐渐向SiC转变。层状多孔SiOC陶瓷具有宏孔一介孔分级多孔结构,烧结温度的升高使多孔陶瓷的比表面积和孔容都增大,孔径分布由单峰模式(3—11nm)转为双峰模式(3-4nm和4-23nm)。同时,随着烧结温度的升高,导电性能和热稳定性能都逐渐提高。
采用木粉为天然生物模板,有机硅树脂为陶瓷前驱体,经浸渍、热压成型、烧结后制备了多孔SiOC陶瓷,开孔气孔率最高达54%。随着烧结温度的升高,样品的比表面积先增大后减小,而孔容逐渐增大,孔径分布由单峰模式(3-4.3nm)转为双峰模式(3-4.5nm和4.5-60nm)。当烧给温度为1300℃时,随着木粉含量的增大,多孔SiOC陶瓷的比表面积逐渐降低,孔体积也减小。随着烧结温度的升高或木粉含量的提高,多孔SiOC陶瓷的导电性能和热稳定性能都提高。
以含氢硅油为前驱体,二乙烯基苯为交联剂,氯铂酸为催化剂,合成了固体聚硅氧烷,再将木粉与固体聚硅氧烷复合后烧结制备了多孔SiOC陶瓷。多孔SiOC陶瓷的开口气孔率最高为59%。随着烧结温度的升高,多孔陶瓷中形成了β-SiC及较多含量的SiO2。样品的比表面积由6.1m2／g升高至180.5m2／g,孔容也逐渐增大,孔径分布由单峰模式(3—5nm)转为多峰模式(3-4nm、7-9.5nm和10-12nm)。多孔陶瓷的摩擦学性能与材料本身的气孔率和微观结构密切相关。在摩擦过程中,低温下制备的多孔陶瓷的表面较易形成润滑膜,摩擦学性能较好。
以BN为惰性填料,与木粉和聚硅氧烷混合后热压成型,再高温烧结制备了多孔SiOC/BN复合陶瓷,开口气孔率最高达52%。随着烧结温度的升高,SiC含量逐渐增多；样品的比表面积和孔容都逐渐增大,比表面积最高达81.2m2／g,孔径分布由单峰模式(3-4.5nm)转为双峰模式(2.6-4nm和10.5-25nm)。BN作为良好的润滑剂,加速了表面润滑膜的形成,使多孔陶瓷表现出更好的摩擦学性能。多孔SiOC陶瓷和SiOC/BN陶瓷的摩擦磨损机制主要表现为磨粒磨损。
在适当的工艺条件下,以不同种类的模板和陶瓷前驱体制备的多孔陶瓷中都能生成纳米线。以海绵为模板,多孔SiOC陶瓷的孔洞中生成了竹节状和链状SiC纳米线。以滤纸为模板,层状多孔SiOC陶瓷的界面通道和孔洞中生长了SiC/SiO2纳米线和SiC纳米线。以木粉和有机硅树脂为原料,多孔SiOC陶瓷中生长了直线状和念珠状SiC纳米线。同时,以木粉和固体聚硅氧烷为原料制备的SiOC陶瓷或多孔SiOC/BN陶瓷的孔结构中都生成了直线状和弯曲状纳米线。所得的纳米线的生长机理主要为气_、液一固(VLS)和气一固(VS)机制。这些纳米线的生成赋予了多孔陶瓷具有分级多孔结构和更良好的性能(如高比表面积)。
本论文以人工模板和天然生物模板制备了具有不同孔结构的多孔陶瓷,在微观结构和性能上都存在明显差异。以海绵为模板制备的多孔陶瓷可获得较大尺寸的宏孔(200-300μm),且能获得较高的开口气孔率。以滤纸为模板制备的多孔陶瓷具有层状多孔结构,宏孔尺寸也能达100μm。以木粉为模板,有机硅树脂为陶瓷前驱体制备的多孔陶瓷具有最高的比表面积达245m2/g。以木粉与固体聚硅氧烷复合后制备的多孔陶瓷具有良好的摩擦学性能,当以BN为填料时,制备的多孔SiOC/BN陶瓷的摩擦学性能(相同条件下)优于多孔SiOC陶瓷。本研究为多孔陶瓷的研制和相关领域的应用提供了理论依据和应用基础。
Porous material is a new type material that has received much attention in the field of materials science. Porous materials have excellent properties such as good heat-resistance, thermal shock resistance, high strength, high chemical stability and high specific surface area. Therefore, these materials have important applications in filters, heat exchangers, catalyst supports, photoelectric devices and sensors etc. Using the conversion of precursor polymer to prepare porous ceramics has advantages over the traditional methods of ceramic preparation such as the low temperature processing, versatile shaping, designable molecular structure and hierarchical porous structure. The porosity and pore size distribution of the porous ceramics can be designed using the template method, and the preparation technology is very simple.
In this work, the design, preparation and properties of the porous ceramics were as the research targets, porous SiOC ceramics and porous SiOC/BN composites were successfully prepared by changing the preceramic precursors and templates, or adding the inert filler. These porous ceramics displayed the controlled open porosity and pore size distribution. The effects of the technological parameters on the morphologies, microstructures and properties of the SiOC ceramics and their composites were observed. Furthermore, the growth mechanism of the nanowires in the pores was investigated. The main results were as follows:
Porous SiOC ceramics were prepared by sintering after impregnation, using the polyurethane sponge as the template and silicone resin as the preceramic precursor. These SiOC ceramics displayed the honeycombed porous structure, and the open porosity of the samples was up to85%. With the increase of the sintering temperature, the SiOC glassses of the samples showed the phase separation, and were converted into SiO2, SiC nanocrystalline and SiC nanowires. When the sintering temperature was higher or the holding time was longer, the porous SiOC ceramics showed good N2absorption property, semiconductor property and thermal stability.
Laminated porous SiOC ceramics were prepared by sintering after hot-pressing, using the filter paper as the bio-template and silicone resin as the preceramic precursor. These SiOC ceramics retained the fiber morphology of the filter paper, and the open porosity of the samples was up to55%. With the increase of the sintering temperature, the SiOC glassses of the samples were converted into SiC. Laminated porous ceramics showed the hierarchical porous structure with macro-and mesoporous. The increase of the temperature resulted in the increase of the specific surface area and pore volume, and the pore size distribution was converted from unimodal (3-11nm) into bimodal pattern (3-4nm and4-23nm). Furthermore, with increasing the temperature, the electrical conductivity and thermal stability were improved.
Porous SiOC ceramics were obtained through impregnating, hot-pressing and sintering, using the wood powders as the natural bio-template and silicone resin as the preceramic precursor. The open porosity of the samples was up to54%. With increasing the temperature, the specific surface area of the samples increased first and then decreased, and the pore volume increased. The pore size distribution was converted from unimodal (3-4.3nm) into bimodal pattern (3-4.5nm and4.5-60nm). When the temperature was1300℃, with the increase of the amount of the wood powders, the specific surface area and pore volume of the samples decreased. With the increase of the temperature or amount of the wood powders, the electrical conductivity and thermal stability were improved.
Solid polysiloxanes were synthetized from poly (methylhydrosiloxane) as the precursor, divinylbenzene as the crosslinking agent and chloroplatinic acid (H2PtCl6) as the catalyst. Then the porous SiOC ceramics were prepared by sintering the composites of the wood powders and solid polysiloxanes The open porosity of the porous SiOC ceramics was up to59%. With the increase of the sintering temperature, the β-SiC and a large amount of SiO2in the porous ceramics were observed. The specific surface area of the samples was from6.1m2/g up to180.5m2/g, and the pore volume increased gradually. And the pore size distribution was converted from unimodal (3-5nm) into multimodal distribution (3-4nm,7-9.5nm and10-12nm). The tribological performances of the porous composite ceramics were closely related to the porosity and microstructures of the material itself. The tribological performances of the porous ceramics obtained at a lower temperature were better due to the formation of the lubricating film during the friction process.
Porous SiOC/BN composite ceramics were prepared by sintering the mixtures of the wood powders, solid polysiloxanes and BN as the inter filler, through hot pressing process. The open porosity of these ceramics was up to52%. With the increase of the temperature, the amount of SiC of the samples increased. The specific surface area and pore volume of the samples both increased, and the specific surface area was up to81.2m2/g. And the pore size distribution was converted from unimodal (3-4.5nm) into bimodal pattern (2.6-4nm and10.5-25nm). BN as a good lubricant could accelerate the formation of the lubrication film on the surface of the samples, which made the porous ceramics show better tribological properties. The wear mechanism of these porous SiOC and SiOC/BN ceramics was abrasive wear mechanism.
The nanowires can be formed in the porous SiOC ceramics using different types of templates or polyceramic precursors under proper technological conditions. The bamboo-like and chain-like nanowires were formed in the porous structure of the ceramics using the sponge as the template. SiC/SiO2nanowires and SiC nanowires were formed in the interfacial channels and pores of the porous ceramics using the filter paper as the template. The straight and bead-like SiC nanowires were formed in the porous ceramics prepared from wood powders and silicone resin. Meanwhile, the straight and curve nanowires could be formed in the porous structure of the SiOC ceramics and SiOC/BN ceramics from wood powders and solid polysiloxanes. The growth mechanism of these nanowires was vapor-liquid-solid (VLS) and vapor-solid (VS) growth model. The generation of these nanowires gave the porous ceramics hierarchical porous structure and more excellent performances (such as high specific surface area).
Porous ceramics prepared by different types of templates or ceramic precursors showed obvious differences in microstructures and properties. The porous SiOC ceramics prepared from sponge can obtain larger macropores (200-300μm) and open porosity. And the porous SiOC ceramics prepared from filter paper have laminated porous structure and the size of the macropores is up to100μm. The highest specific surface area of the porous SiOC ceramic obtained from wood powders as the template and silicone resin as the preceramic precursor is up to245m2/g. Furthermore, the porous SiOC ceramics show the good tribological performances. The porous SiOC/BN ceramics have the better tribological performances than that of SiOC ceramics (in the same process). This work provides the theoretical basis and application foundation for the development of the porous ceramics and the application of the related fields.
本研究以多孔陶瓷的设计、制备及性能研究为主旨,通过改变陶瓷前驱体及多孔模板类型,或加入惰性填料,成功制备了多孔SiOC陶瓷及多孔SiOC/BN复合材料,所得多孔陶瓷具有可控的开口气孔率和孔径分布。本论文研究了不同的工艺条件对所得多孔SiOC陶瓷及其复合材料的微观形貌、结构及性能的影响,并分析了多孔结构中纳米线的生长机理。主要研究结果如下：
以聚氨酯海绵为人工模板、有机硅树脂(R9801)为陶瓷前驱体,浸渍后再烧结制备了多孔SiOC陶瓷。SiOC陶瓷具有蜂窝状的多孔形貌,开口气孔率最高达85%。随着烧结温度的升高,样品中SiOC玻璃相产生相分离向SiO2、SiC纳米晶和SiC纳米线转变。当烧结温度较高或保温时间较长时,多孔SiOC陶瓷具有较好的氮吸附性能,半导体特性和热稳定性。
以滤纸为生物模板,有机硅树脂为陶瓷前驱体,热压成型后烧结制备了层状多孔SiOC陶瓷,样品保留了滤纸原有的纤维形貌,开口气孔率最高达55%。随着烧结温度的升高,样品的SiOC玻璃相逐渐向SiC转变。层状多孔SiOC陶瓷具有宏孔一介孔分级多孔结构,烧结温度的升高使多孔陶瓷的比表面积和孔容都增大,孔径分布由单峰模式(3—11nm)转为双峰模式(3-4nm和4-23nm)。同时,随着烧结温度的升高,导电性能和热稳定性能都逐渐提高。
采用木粉为天然生物模板,有机硅树脂为陶瓷前驱体,经浸渍、热压成型、烧结后制备了多孔SiOC陶瓷,开孔气孔率最高达54%。随着烧结温度的升高,样品的比表面积先增大后减小,而孔容逐渐增大,孔径分布由单峰模式(3-4.3nm)转为双峰模式(3-4.5nm和4.5-60nm)。当烧给温度为1300℃时,随着木粉含量的增大,多孔SiOC陶瓷的比表面积逐渐降低,孔体积也减小。随着烧结温度的升高或木粉含量的提高,多孔SiOC陶瓷的导电性能和热稳定性能都提高。
以含氢硅油为前驱体,二乙烯基苯为交联剂,氯铂酸为催化剂,合成了固体聚硅氧烷,再将木粉与固体聚硅氧烷复合后烧结制备了多孔SiOC陶瓷。多孔SiOC陶瓷的开口气孔率最高为59%。随着烧结温度的升高,多孔陶瓷中形成了β-SiC及较多含量的SiO2。样品的比表面积由6.1m2／g升高至180.5m2／g,孔容也逐渐增大,孔径分布由单峰模式(3—5nm)转为多峰模式(3-4nm、7-9.5nm和10-12nm)。多孔陶瓷的摩擦学性能与材料本身的气孔率和微观结构密切相关。在摩擦过程中,低温下制备的多孔陶瓷的表面较易形成润滑膜,摩擦学性能较好。
以BN为惰性填料,与木粉和聚硅氧烷混合后热压成型,再高温烧结制备了多孔SiOC/BN复合陶瓷,开口气孔率最高达52%。随着烧结温度的升高,SiC含量逐渐增多；样品的比表面积和孔容都逐渐增大,比表面积最高达81.2m2／g,孔径分布由单峰模式(3-4.5nm)转为双峰模式(2.6-4nm和10.5-25nm)。BN作为良好的润滑剂,加速了表面润滑膜的形成,使多孔陶瓷表现出更好的摩擦学性能。多孔SiOC陶瓷和SiOC/BN陶瓷的摩擦磨损机制主要表现为磨粒磨损。
在适当的工艺条件下,以不同种类的模板和陶瓷前驱体制备的多孔陶瓷中都能生成纳米线。以海绵为模板,多孔SiOC陶瓷的孔洞中生成了竹节状和链状SiC纳米线。以滤纸为模板,层状多孔SiOC陶瓷的界面通道和孔洞中生长了SiC/SiO2纳米线和SiC纳米线。以木粉和有机硅树脂为原料,多孔SiOC陶瓷中生长了直线状和念珠状SiC纳米线。同时,以木粉和固体聚硅氧烷为原料制备的SiOC陶瓷或多孔SiOC/BN陶瓷的孔结构中都生成了直线状和弯曲状纳米线。所得的纳米线的生长机理主要为气_、液一固(VLS)和气一固(VS)机制。这些纳米线的生成赋予了多孔陶瓷具有分级多孔结构和更良好的性能(如高比表面积)。
本论文以人工模板和天然生物模板制备了具有不同孔结构的多孔陶瓷,在微观结构和性能上都存在明显差异。以海绵为模板制备的多孔陶瓷可获得较大尺寸的宏孔(200-300μm),且能获得较高的开口气孔率。以滤纸为模板制备的多孔陶瓷具有层状多孔结构,宏孔尺寸也能达100μm。以木粉为模板,有机硅树脂为陶瓷前驱体制备的多孔陶瓷具有最高的比表面积达245m2/g。以木粉与固体聚硅氧烷复合后制备的多孔陶瓷具有良好的摩擦学性能,当以BN为填料时,制备的多孔SiOC/BN陶瓷的摩擦学性能(相同条件下)优于多孔SiOC陶瓷。本研究为多孔陶瓷的研制和相关领域的应用提供了理论依据和应用基础。
Porous material is a new type material that has received much attention in the field of materials science. Porous materials have excellent properties such as good heat-resistance, thermal shock resistance, high strength, high chemical stability and high specific surface area. Therefore, these materials have important applications in filters, heat exchangers, catalyst supports, photoelectric devices and sensors etc. Using the conversion of precursor polymer to prepare porous ceramics has advantages over the traditional methods of ceramic preparation such as the low temperature processing, versatile shaping, designable molecular structure and hierarchical porous structure. The porosity and pore size distribution of the porous ceramics can be designed using the template method, and the preparation technology is very simple.
In this work, the design, preparation and properties of the porous ceramics were as the research targets, porous SiOC ceramics and porous SiOC/BN composites were successfully prepared by changing the preceramic precursors and templates, or adding the inert filler. These porous ceramics displayed the controlled open porosity and pore size distribution. The effects of the technological parameters on the morphologies, microstructures and properties of the SiOC ceramics and their composites were observed. Furthermore, the growth mechanism of the nanowires in the pores was investigated. The main results were as follows:
Porous SiOC ceramics were prepared by sintering after impregnation, using the polyurethane sponge as the template and silicone resin as the preceramic precursor. These SiOC ceramics displayed the honeycombed porous structure, and the open porosity of the samples was up to85%. With the increase of the sintering temperature, the SiOC glassses of the samples showed the phase separation, and were converted into SiO2, SiC nanocrystalline and SiC nanowires. When the sintering temperature was higher or the holding time was longer, the porous SiOC ceramics showed good N2absorption property, semiconductor property and thermal stability.
Laminated porous SiOC ceramics were prepared by sintering after hot-pressing, using the filter paper as the bio-template and silicone resin as the preceramic precursor. These SiOC ceramics retained the fiber morphology of the filter paper, and the open porosity of the samples was up to55%. With the increase of the sintering temperature, the SiOC glassses of the samples were converted into SiC. Laminated porous ceramics showed the hierarchical porous structure with macro-and mesoporous. The increase of the temperature resulted in the increase of the specific surface area and pore volume, and the pore size distribution was converted from unimodal (3-11nm) into bimodal pattern (3-4nm and4-23nm). Furthermore, with increasing the temperature, the electrical conductivity and thermal stability were improved.
Porous SiOC ceramics were obtained through impregnating, hot-pressing and sintering, using the wood powders as the natural bio-template and silicone resin as the preceramic precursor. The open porosity of the samples was up to54%. With increasing the temperature, the specific surface area of the samples increased first and then decreased, and the pore volume increased. The pore size distribution was converted from unimodal (3-4.3nm) into bimodal pattern (3-4.5nm and4.5-60nm). When the temperature was1300℃, with the increase of the amount of the wood powders, the specific surface area and pore volume of the samples decreased. With the increase of the temperature or amount of the wood powders, the electrical conductivity and thermal stability were improved.
Solid polysiloxanes were synthetized from poly (methylhydrosiloxane) as the precursor, divinylbenzene as the crosslinking agent and chloroplatinic acid (H2PtCl6) as the catalyst. Then the porous SiOC ceramics were prepared by sintering the composites of the wood powders and solid polysiloxanes The open porosity of the porous SiOC ceramics was up to59%. With the increase of the sintering temperature, the β-SiC and a large amount of SiO2in the porous ceramics were observed. The specific surface area of the samples was from6.1m2/g up to180.5m2/g, and the pore volume increased gradually. And the pore size distribution was converted from unimodal (3-5nm) into multimodal distribution (3-4nm,7-9.5nm and10-12nm). The tribological performances of the porous composite ceramics were closely related to the porosity and microstructures of the material itself. The tribological performances of the porous ceramics obtained at a lower temperature were better due to the formation of the lubricating film during the friction process.
Porous SiOC/BN composite ceramics were prepared by sintering the mixtures of the wood powders, solid polysiloxanes and BN as the inter filler, through hot pressing process. The open porosity of these ceramics was up to52%. With the increase of the temperature, the amount of SiC of the samples increased. The specific surface area and pore volume of the samples both increased, and the specific surface area was up to81.2m2/g. And the pore size distribution was converted from unimodal (3-4.5nm) into bimodal pattern (2.6-4nm and10.5-25nm). BN as a good lubricant could accelerate the formation of the lubrication film on the surface of the samples, which made the porous ceramics show better tribological properties. The wear mechanism of these porous SiOC and SiOC/BN ceramics was abrasive wear mechanism.
The nanowires can be formed in the porous SiOC ceramics using different types of templates or polyceramic precursors under proper technological conditions. The bamboo-like and chain-like nanowires were formed in the porous structure of the ceramics using the sponge as the template. SiC/SiO2nanowires and SiC nanowires were formed in the interfacial channels and pores of the porous ceramics using the filter paper as the template. The straight and bead-like SiC nanowires were formed in the porous ceramics prepared from wood powders and silicone resin. Meanwhile, the straight and curve nanowires could be formed in the porous structure of the SiOC ceramics and SiOC/BN ceramics from wood powders and solid polysiloxanes. The growth mechanism of these nanowires was vapor-liquid-solid (VLS) and vapor-solid (VS) growth model. The generation of these nanowires gave the porous ceramics hierarchical porous structure and more excellent performances (such as high specific surface area).
Porous ceramics prepared by different types of templates or ceramic precursors showed obvious differences in microstructures and properties. The porous SiOC ceramics prepared from sponge can obtain larger macropores (200-300μm) and open porosity. And the porous SiOC ceramics prepared from filter paper have laminated porous structure and the size of the macropores is up to100μm. The highest specific surface area of the porous SiOC ceramic obtained from wood powders as the template and silicone resin as the preceramic precursor is up to245m2/g. Furthermore, the porous SiOC ceramics show the good tribological performances. The porous SiOC/BN ceramics have the better tribological performances than that of SiOC ceramics (in the same process). This work provides the theoretical basis and application foundation for the development of the porous ceramics and the application of the related fields.
引文
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