含铝碳化硅纤维的连续化制备与研究
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摘要
研制和开发耐1500℃或更高温度的连续SiC纤维,即耐超高温SiC纤维是先驱体转化法制备SiC纤维的主要发展方向。制备耐超高温SiC纤维理想的方法是在SiC纤维的先驱体中引入少量铝元素,其起到烧结助剂和抑晶的作用,从而在高温烧结下脱去氧和富余碳,可以生成含少量铝的近化学计量比的SiC纤维。
本研究首次在国内突破了先驱体法制备耐超高温SiC纤维的连续化工艺。制备含铝碳化硅纤维的连续化工艺包括先驱体聚铝碳硅烷(PACS)的放大合成、连续熔融纺丝、原纤维的不熔化处理和不熔化纤维的连续烧成和烧结。1350℃烧成制得连续含有少量铝和较多氧的Si-Al-C-O纤维,即KD-A纤维。KD-A纤维再经1800℃烧结转化为含少量铝和少量氧的Si-Al-C纤维,即KD-SA纤维。本论文对上述工艺进行了详细地研究,对过程中的中间产物和两种含铝碳化硅纤维的多级结构和多项性能进行了系统的分析和表征。
聚硅碳硅烷(PSCS)和乙酰丙酮铝(Al(AcAc)_3)是合成先驱体PACS的理想反应物。具有良好可纺性且可生成高质量的含铝碳化硅纤维的先驱体PACS的熔点为185～200℃,相应合成条件为:Al(AcAc)_3含量3～5wt%,反应温度360～420℃,裂解温度450～500℃,保温时间7～10h。利用此工艺成功地实现了先驱体PACS的规模化合成。PACS中含有0.9～2wt%的铝和2～4wt%的氧,C/Si原子比约为2。PACS以Si—C键为主链,侧基为CH_3和H,分子支化较多。铝在PACS中主要以Si—O—Al键形式存在,形成4、5、6三种配位结构,铝在其中起到了交联点的作用,使小部分分子链形成高度交联。
通过以上对PACS的结构控制,实现了PACS的多孔熔融纺丝。连续PACS原纤维采用热空气流方法进行不熔化处理。PACS的不熔化处理机理与PCS类似,都是Si—H键氧化,氧增重的过程。PACS由于铝的作用,只需8～9%的增重率,引入较少的氧即可达到不熔化的效果。采用一步连续烧成工艺制备了连续KD-A纤维,KD-A纤维再经1800℃烧结制备了KD-SA纤维。
To develop continuous SiC fibers with high temperature resistance above 1500℃ is the main goal for preparing polymer-derived ceramic fibers. Up to date, the most successful strategy to establish super-high-temperature resistant SiC fibers is manufacturing near-stoichiometric SiC fibers through introducing small amount of heteroelement, such as aluminum into the precursor polymer. The Al atoms in the SiC fibers play important roles as both sintering aids and grain growth inhibitor, so that the extra oxygen and free carbon can be eliminated in sintering at high temperature.In this work, a break through was made in the continuous procedure of preparing super-high-temperature resistant SiC fibers by polymer precursor route, which includes the synsthesis of precursor polyaluminocarbosilane (PACS) on larger scale, continuous melten-spinning, curing of the green fibers in air, continuous pyrolysis of the cured fibers and sintering to obtain Al-containing SiC fibers. When the pyrolysis is at 1350℃, Si-Al-C-0 fiber, named KD-A fiber, is resulted, which contains small amount of aluminum and some oxygen. The KD-A fiber can be converted, by an extra sintering at 1800℃, into Si-Al-C fiber, or KD-SA fiber, which contains aluminum and much lower amount of oxygen. In this paper, the above manufactural processes were studied in details and the structures and properties of all products and the two kinds of Al-containing SiC fibers were analysed and characterized systematically.The precursor PACS was synthesized by the reaction of aluminum acetylacetonate (Al(AcAc)3) with polysilacarbosilane (PSCS). The properties of PACS suitatable for preparing Al-containing SiC fibers with high quality include: the contents of 0.9 ~ 2 wt% of Al and 2 ~ 4 wt % of O, the atomic ratio C/Si of 2 or above, moderate molecular weight and soften point around 185 ~ 200 ℃ and a good spinnability. The corresponding PACS was synthesized by the reaction of PSCS with 3 ~ 5% of Al(AcAc)_3
at reaction temperature 360 ~ 420°C and pyrolysis temperature 450 ~ 500°C for 7 ~ lOhrs. The PACS thus synthesed is made of Si—C main chain with methyl and H as side groups. The Al in PACS exists in the manner of Si—O—Al bonds with coordination numbers of 4, 5 and 6, so that the Al atoms act as crosslinking point in some of the chains.The PACS resulted by the above procedure was shaped into green fibers by multi-orifice melten-spinning. In the curing of the PACS green fibers in air, a different mechanism was found that for the suitable infusiblity, a smaller amount of oxidation extend than that of PCS is necessary. The processes of continuous pyrolysis of the cured fibers in inert gas up to 1350°C to obtain KD-A fibers and sintering of KD-A fibers to convert into KD-SA fibers at 1800°C were also investigated.The formula of KD-A fiber is SiC1.31O025Alo.oi8 with C and O rich on the surface. The fiber is made up of some P-SiC cystalline and Si-C-O amorphous continuous phase with Al embedded uniformly. The average tensile strength, Young's modulus and diameter of the KD-A fiber are 2.3 ~ 2.6GPa, 190 ~ 230GPa and 12 ~ 14pm, respectively.For KD-SA fiber, nearly stoichiometric composition was confirmed as chemical composition of SiC1.03Oo.013Alo.024- The fiber is composed of large number of P-SiC grains, small amount of a-SiC crystalline and SiC amorphous phase. The Al in KD-SA fibers is mainly arranged on the surface of P-SiC grains and exists in two manners: Al — C bonds connected with the surfaces of the grains and Al —O bonds, or AI2O3, to the amorphous phase. The average tensile strength, Young's modulus and diameter of the KD-SA fiber are 2.0 ~ 2.2GPa, 370 ~ 410GPa and 10 ~ 12um, respectively.The KD-A fiber shows better oxidation resistance than Nicalon fibers because of smaller amount of oxygen involved. After oxidation tests at 1300°C for 30 hrs, KD-A fibers remained 40% of the initial strength, while the strength of Nicalon fiber lost completely. At super-high-temperature in Ar, KD-A fiber lost its strength gradually, but slower than Nicalon fiber, until 1500°C, but the strength increased rapidly above. The special "saddle" shape is similar with that of Tyranno-AM fiber.In the case of the KD-SA fiber, excellent oxidation resistance was exhibited. After
oxidation tests at 1300 °C for 100 hrs, KD-SA fiber maintained 55% of the initial strength, while that of Hi-Nicalon fiber was 23%. When KD-SA fiber was exposed in Ar, the tensile strength did not decrease even at 1800°C. KD-SA fiber showed the best creep resistance among all kinds of SiC fibers. At 1800°C, for example, the creep parameter m retained to 0.33, compared with Tyranno SA fiber, in which m decreased to 0. The high-temperature resistance of KD-SA fiber is based on two factors: the near stoichiometry provides chemical stability of the fiber at high temperature and the inhibility of Al around p-SiC grains prevents the growth of grain at super-high temperature.
本研究首次在国内突破了先驱体法制备耐超高温SiC纤维的连续化工艺。制备含铝碳化硅纤维的连续化工艺包括先驱体聚铝碳硅烷(PACS)的放大合成、连续熔融纺丝、原纤维的不熔化处理和不熔化纤维的连续烧成和烧结。1350℃烧成制得连续含有少量铝和较多氧的Si-Al-C-O纤维,即KD-A纤维。KD-A纤维再经1800℃烧结转化为含少量铝和少量氧的Si-Al-C纤维,即KD-SA纤维。本论文对上述工艺进行了详细地研究,对过程中的中间产物和两种含铝碳化硅纤维的多级结构和多项性能进行了系统的分析和表征。
聚硅碳硅烷(PSCS)和乙酰丙酮铝(Al(AcAc)_3)是合成先驱体PACS的理想反应物。具有良好可纺性且可生成高质量的含铝碳化硅纤维的先驱体PACS的熔点为185～200℃,相应合成条件为:Al(AcAc)_3含量3～5wt%,反应温度360～420℃,裂解温度450～500℃,保温时间7～10h。利用此工艺成功地实现了先驱体PACS的规模化合成。PACS中含有0.9～2wt%的铝和2～4wt%的氧,C/Si原子比约为2。PACS以Si—C键为主链,侧基为CH_3和H,分子支化较多。铝在PACS中主要以Si—O—Al键形式存在,形成4、5、6三种配位结构,铝在其中起到了交联点的作用,使小部分分子链形成高度交联。
通过以上对PACS的结构控制,实现了PACS的多孔熔融纺丝。连续PACS原纤维采用热空气流方法进行不熔化处理。PACS的不熔化处理机理与PCS类似,都是Si—H键氧化,氧增重的过程。PACS由于铝的作用,只需8～9%的增重率,引入较少的氧即可达到不熔化的效果。采用一步连续烧成工艺制备了连续KD-A纤维,KD-A纤维再经1800℃烧结制备了KD-SA纤维。
To develop continuous SiC fibers with high temperature resistance above 1500℃ is the main goal for preparing polymer-derived ceramic fibers. Up to date, the most successful strategy to establish super-high-temperature resistant SiC fibers is manufacturing near-stoichiometric SiC fibers through introducing small amount of heteroelement, such as aluminum into the precursor polymer. The Al atoms in the SiC fibers play important roles as both sintering aids and grain growth inhibitor, so that the extra oxygen and free carbon can be eliminated in sintering at high temperature.In this work, a break through was made in the continuous procedure of preparing super-high-temperature resistant SiC fibers by polymer precursor route, which includes the synsthesis of precursor polyaluminocarbosilane (PACS) on larger scale, continuous melten-spinning, curing of the green fibers in air, continuous pyrolysis of the cured fibers and sintering to obtain Al-containing SiC fibers. When the pyrolysis is at 1350℃, Si-Al-C-0 fiber, named KD-A fiber, is resulted, which contains small amount of aluminum and some oxygen. The KD-A fiber can be converted, by an extra sintering at 1800℃, into Si-Al-C fiber, or KD-SA fiber, which contains aluminum and much lower amount of oxygen. In this paper, the above manufactural processes were studied in details and the structures and properties of all products and the two kinds of Al-containing SiC fibers were analysed and characterized systematically.The precursor PACS was synthesized by the reaction of aluminum acetylacetonate (Al(AcAc)3) with polysilacarbosilane (PSCS). The properties of PACS suitatable for preparing Al-containing SiC fibers with high quality include: the contents of 0.9 ~ 2 wt% of Al and 2 ~ 4 wt % of O, the atomic ratio C/Si of 2 or above, moderate molecular weight and soften point around 185 ~ 200 ℃ and a good spinnability. The corresponding PACS was synthesized by the reaction of PSCS with 3 ~ 5% of Al(AcAc)_3
at reaction temperature 360 ~ 420°C and pyrolysis temperature 450 ~ 500°C for 7 ~ lOhrs. The PACS thus synthesed is made of Si—C main chain with methyl and H as side groups. The Al in PACS exists in the manner of Si—O—Al bonds with coordination numbers of 4, 5 and 6, so that the Al atoms act as crosslinking point in some of the chains.The PACS resulted by the above procedure was shaped into green fibers by multi-orifice melten-spinning. In the curing of the PACS green fibers in air, a different mechanism was found that for the suitable infusiblity, a smaller amount of oxidation extend than that of PCS is necessary. The processes of continuous pyrolysis of the cured fibers in inert gas up to 1350°C to obtain KD-A fibers and sintering of KD-A fibers to convert into KD-SA fibers at 1800°C were also investigated.The formula of KD-A fiber is SiC1.31O025Alo.oi8 with C and O rich on the surface. The fiber is made up of some P-SiC cystalline and Si-C-O amorphous continuous phase with Al embedded uniformly. The average tensile strength, Young's modulus and diameter of the KD-A fiber are 2.3 ~ 2.6GPa, 190 ~ 230GPa and 12 ~ 14pm, respectively.For KD-SA fiber, nearly stoichiometric composition was confirmed as chemical composition of SiC1.03Oo.013Alo.024- The fiber is composed of large number of P-SiC grains, small amount of a-SiC crystalline and SiC amorphous phase. The Al in KD-SA fibers is mainly arranged on the surface of P-SiC grains and exists in two manners: Al — C bonds connected with the surfaces of the grains and Al —O bonds, or AI2O3, to the amorphous phase. The average tensile strength, Young's modulus and diameter of the KD-SA fiber are 2.0 ~ 2.2GPa, 370 ~ 410GPa and 10 ~ 12um, respectively.The KD-A fiber shows better oxidation resistance than Nicalon fibers because of smaller amount of oxygen involved. After oxidation tests at 1300°C for 30 hrs, KD-A fibers remained 40% of the initial strength, while the strength of Nicalon fiber lost completely. At super-high-temperature in Ar, KD-A fiber lost its strength gradually, but slower than Nicalon fiber, until 1500°C, but the strength increased rapidly above. The special "saddle" shape is similar with that of Tyranno-AM fiber.In the case of the KD-SA fiber, excellent oxidation resistance was exhibited. After
oxidation tests at 1300 °C for 100 hrs, KD-SA fiber maintained 55% of the initial strength, while that of Hi-Nicalon fiber was 23%. When KD-SA fiber was exposed in Ar, the tensile strength did not decrease even at 1800°C. KD-SA fiber showed the best creep resistance among all kinds of SiC fibers. At 1800°C, for example, the creep parameter m retained to 0.33, compared with Tyranno SA fiber, in which m decreased to 0. The high-temperature resistance of KD-SA fiber is based on two factors: the near stoichiometry provides chemical stability of the fiber at high temperature and the inhibility of Al around p-SiC grains prevents the growth of grain at super-high temperature.
引文
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