新型溶胶凝胶法制备SiCN（O）陶瓷前驱体及相应陶瓷材料的高温热行为研究
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摘要
用新型无氧溶胶凝胶法制备的硅碳氮基前驱体陶瓷材料具有优异的力学和高温抗氧化、抗腐蚀性以及其他的功能特性，在高温材料和功能材料方面有着重要的应用前景。为了更深一步认识此类硅基前驱体陶瓷的结构与性能之间的关系，通过分子设计制备了含有不同功能基团的硅基前驱体陶瓷，研究了材料的高温热行为以及相应的结构转变。
通过六氯硅氧烷与双（三甲基硅基）碳化二亚酰胺(BTSC)反应合成了硅碳氧氮陶瓷前驱体，将氧定量可控地引入到硅碳氮三维网络结构中。研究了催化剂吡啶对前驱体交联度的影响，得到Cl_3Si-O-SiCl_3(pyridine)_2晶体。量子化学计算证实Cl_3Si-O-SiCl_3(pyridine)_2是存在于反应过程中的中间体，可以加速前驱体的交联进程。还研究了前驱体交联度受交联温度和时间的影响。此前驱体在1000°C热解后的陶瓷产率为50%，SiCON陶瓷化的基体呈现无定形态，分析认为主要是Si_2N_2O的无定形相。进一步在1400～1500°C热处理后，无定形态的Si2N2O相的量逐渐减少而Si_3N_4相的量逐渐增加，在1500°C时两相均以晶体形态从陶瓷基体中析出。分析认为1000°C热解后陶瓷基体中的C在高温热处理过程中与Si_2N_2O相反应而消耗掉，因此1500°C热处理后的陶瓷体中主要是Si_3N_4晶相以及少量的Si_2N_2O相，而没有发现碳化硅相。
为了提高陶瓷产率，将具有高交联活性的乙烯基引入。通过乙烯基三氯硅烷与BTSC反应合成了聚乙烯基硅基碳氮亚酰胺聚合物。在1000°C热解此前驱体聚合物获得了产率高达70%的陶瓷，由Si-C-N相组成，陶瓷体呈现无定形纳米多孔结构，孔的大小为十几到几十纳米。进一步研究此硅碳氮前驱体陶瓷在1000～1500°C的高温热行为发现，随着温度的升高陶瓷体中的气孔尺寸减小，并有结晶Si_3N_4相从无定形SiCN基体中析出。
为了制备无模板添加的多孔陶瓷材料，通过乙烯基三氯硅烷、甲基二氯硅烷共同与BTSC反应合成了一种聚双功能基硅基碳氮亚酰胺聚合物，这种聚合物同时具有三维和二维的结构单元。此硅碳氮前驱体聚合物在1000°C热解后，获得无定形微米多孔结构的陶瓷体，气孔率为85%，孔尺寸平均约为10μm。尽管随着温度的升高孔径会有所减小，但这种多孔结构会一直保持到1500°C。在1500°C热处理后，结晶化的Si_3N_4相从无定形SiCN基体中析出。
为了研究前驱体陶瓷中不同碳含量对陶瓷的结构和性能的影响，通过三种含有不同功能基团的氯硅烷与BTSC恒温回流反应合成了聚硅基碳氮亚酰胺陶瓷前驱体。在1000°C氮气气氛下热解后得到产率不同的陶瓷材料。三种前驱体陶瓷材料均呈现出无定形微米多孔结构。在1400°C热处理后，前驱体陶瓷出现析晶趋势。但具体的析晶温度依赖于陶瓷基体内的碳含量。碳含量高的材料在较高的温度从无定形SiCN基体中析出Si_3N_4晶相，表明其具有较高的热力学稳定性。
The silicon carbonitride based ceramics, which are fabricated via the novel sol-gelprocess, possess excellent mechanical properties, oxidation and corrosion resistance athigh temperature and other functional properties, and they are promising materials forthe application as high-temperature structural and functional materials. In order toknow further the relationship between their structure and properties of this kind ofsilicon based precursor derived ceramics, different functional groups-containingpolysilylcarbodiimides precursor ceramics were fabricated by the design at amolecular level. The thermolysis behavior and relevant structure transformation ofthis precursor derived ceramics were investigated.
Silicon oxycarbonitride (SiCON) ceramic precursors were fabricated by thereaction of hexachlorodisiloxane and bis(trimethylsilyl)carbodiimide (BTSC). Theoxygen was controllably introduced into Si-[NCN] network. The influence of pyridineas a catalyst for the cross-linking reaction was studied. The crystal structure ofCl_3Si-O-SiCl_3(pyridine)_2is presented. The result of quantum chemical calculations isin support of this adduct being a potential intermediate in the pyridine catalyzedsol-gel process. The degree of cross-linking is accelerated by the addition of pyridineand also depends on the aging time and temperature. The ceramic yield after pyrolysisat1000°C reaches up to50%. The ceramic reveals a porous SiCON matrixcomprised of Si_2N_2O phases. Further heat-treatment up to1500°C caused thetransformation of Si_2N_2O phase to crystalline Si_3N_4phase. The carbon in theSiCON ceramic matrix was consumed by Si_2N_2O with the increasing temperature.Thus, the final materials contain majority of Si_3N_4and minor Si_2N_2O crystallinephases, and no SiC phase was observed.
In order to enhance the ceramic yield of the silicon carbonitride precursors, activevinyl-containing polysilylcarbodiimides were synthesized by the reaction ofvinylchlorosilane and BTSC. The high ceramic yield of70%was obtained after thepyrolysis of the SiCN precursor. The SiCN ceramic exhibits an amorphousnano-porous structure with pore size of tens of nanometer. The thermolysis behaviorof the SiCN ceramics between1000and1500°C indicates that the pore size decreasesas the temperature rises and the separation of crystalline Si_3N_4phase from the amorphous SiCN ceramic matrix is observed.
In order to fabricate porous silicon carbonitride ceramics without any templates, anovel double functional groups-containing polysilylcarbodiimides were synthesizedby the reaction of a mixture of vinyltrichlorosilane and methyldichlorosilane withBTSC. The poly(R1R2silylcarbodiimide) precursor possesses three-andtwo-dimension structure units. The polymeric precursor was converted into anamorphous porous SiCN ceramic with85%porosity and about10micrometer poresby pyrolysis at1000°C in nitrogen. The porous structure keeps up to1500°C andpore size decreases slightly as the temperature rises. The separation of crystallineSi_3N_4from the amorphous SiCN ceramic matrix is observed at1500°C.
In order to study the influence of the content of carbon on the structure andproperties of polymer derived ceramics, polysilylcarbodiimides were synthesized bydifferent chlorosilanes (ethyltri-, hexyl-and benzyl-trichlorosilane) in reaction withBTSC. The ceramic yields of the three samples after pyrolysis at1000°C differ fromeach other due to various functional groups in the polysilylcarbodiimides. The SiCNceramics exhibit an amorphous porous structure at this temperature. All three SiCNmaterials convert from amorphous station to crystalline structure above1400°C.However, the temperature of crystallization depends on the content of carbon in theceramic matrix. In the sample with higher content of carbon the separation of Si_3N_4from the amorphous SiCN matrix is observed at higher temperature, demonstratingthe higher thermal stability against crystallization.
通过六氯硅氧烷与双（三甲基硅基）碳化二亚酰胺(BTSC)反应合成了硅碳氧氮陶瓷前驱体，将氧定量可控地引入到硅碳氮三维网络结构中。研究了催化剂吡啶对前驱体交联度的影响，得到Cl_3Si-O-SiCl_3(pyridine)_2晶体。量子化学计算证实Cl_3Si-O-SiCl_3(pyridine)_2是存在于反应过程中的中间体，可以加速前驱体的交联进程。还研究了前驱体交联度受交联温度和时间的影响。此前驱体在1000°C热解后的陶瓷产率为50%，SiCON陶瓷化的基体呈现无定形态，分析认为主要是Si_2N_2O的无定形相。进一步在1400～1500°C热处理后，无定形态的Si2N2O相的量逐渐减少而Si_3N_4相的量逐渐增加，在1500°C时两相均以晶体形态从陶瓷基体中析出。分析认为1000°C热解后陶瓷基体中的C在高温热处理过程中与Si_2N_2O相反应而消耗掉，因此1500°C热处理后的陶瓷体中主要是Si_3N_4晶相以及少量的Si_2N_2O相，而没有发现碳化硅相。
为了提高陶瓷产率，将具有高交联活性的乙烯基引入。通过乙烯基三氯硅烷与BTSC反应合成了聚乙烯基硅基碳氮亚酰胺聚合物。在1000°C热解此前驱体聚合物获得了产率高达70%的陶瓷，由Si-C-N相组成，陶瓷体呈现无定形纳米多孔结构，孔的大小为十几到几十纳米。进一步研究此硅碳氮前驱体陶瓷在1000～1500°C的高温热行为发现，随着温度的升高陶瓷体中的气孔尺寸减小，并有结晶Si_3N_4相从无定形SiCN基体中析出。
为了制备无模板添加的多孔陶瓷材料，通过乙烯基三氯硅烷、甲基二氯硅烷共同与BTSC反应合成了一种聚双功能基硅基碳氮亚酰胺聚合物，这种聚合物同时具有三维和二维的结构单元。此硅碳氮前驱体聚合物在1000°C热解后，获得无定形微米多孔结构的陶瓷体，气孔率为85%，孔尺寸平均约为10μm。尽管随着温度的升高孔径会有所减小，但这种多孔结构会一直保持到1500°C。在1500°C热处理后，结晶化的Si_3N_4相从无定形SiCN基体中析出。
为了研究前驱体陶瓷中不同碳含量对陶瓷的结构和性能的影响，通过三种含有不同功能基团的氯硅烷与BTSC恒温回流反应合成了聚硅基碳氮亚酰胺陶瓷前驱体。在1000°C氮气气氛下热解后得到产率不同的陶瓷材料。三种前驱体陶瓷材料均呈现出无定形微米多孔结构。在1400°C热处理后，前驱体陶瓷出现析晶趋势。但具体的析晶温度依赖于陶瓷基体内的碳含量。碳含量高的材料在较高的温度从无定形SiCN基体中析出Si_3N_4晶相，表明其具有较高的热力学稳定性。
The silicon carbonitride based ceramics, which are fabricated via the novel sol-gelprocess, possess excellent mechanical properties, oxidation and corrosion resistance athigh temperature and other functional properties, and they are promising materials forthe application as high-temperature structural and functional materials. In order toknow further the relationship between their structure and properties of this kind ofsilicon based precursor derived ceramics, different functional groups-containingpolysilylcarbodiimides precursor ceramics were fabricated by the design at amolecular level. The thermolysis behavior and relevant structure transformation ofthis precursor derived ceramics were investigated.
Silicon oxycarbonitride (SiCON) ceramic precursors were fabricated by thereaction of hexachlorodisiloxane and bis(trimethylsilyl)carbodiimide (BTSC). Theoxygen was controllably introduced into Si-[NCN] network. The influence of pyridineas a catalyst for the cross-linking reaction was studied. The crystal structure ofCl_3Si-O-SiCl_3(pyridine)_2is presented. The result of quantum chemical calculations isin support of this adduct being a potential intermediate in the pyridine catalyzedsol-gel process. The degree of cross-linking is accelerated by the addition of pyridineand also depends on the aging time and temperature. The ceramic yield after pyrolysisat1000°C reaches up to50%. The ceramic reveals a porous SiCON matrixcomprised of Si_2N_2O phases. Further heat-treatment up to1500°C caused thetransformation of Si_2N_2O phase to crystalline Si_3N_4phase. The carbon in theSiCON ceramic matrix was consumed by Si_2N_2O with the increasing temperature.Thus, the final materials contain majority of Si_3N_4and minor Si_2N_2O crystallinephases, and no SiC phase was observed.
In order to enhance the ceramic yield of the silicon carbonitride precursors, activevinyl-containing polysilylcarbodiimides were synthesized by the reaction ofvinylchlorosilane and BTSC. The high ceramic yield of70%was obtained after thepyrolysis of the SiCN precursor. The SiCN ceramic exhibits an amorphousnano-porous structure with pore size of tens of nanometer. The thermolysis behaviorof the SiCN ceramics between1000and1500°C indicates that the pore size decreasesas the temperature rises and the separation of crystalline Si_3N_4phase from the amorphous SiCN ceramic matrix is observed.
In order to fabricate porous silicon carbonitride ceramics without any templates, anovel double functional groups-containing polysilylcarbodiimides were synthesizedby the reaction of a mixture of vinyltrichlorosilane and methyldichlorosilane withBTSC. The poly(R1R2silylcarbodiimide) precursor possesses three-andtwo-dimension structure units. The polymeric precursor was converted into anamorphous porous SiCN ceramic with85%porosity and about10micrometer poresby pyrolysis at1000°C in nitrogen. The porous structure keeps up to1500°C andpore size decreases slightly as the temperature rises. The separation of crystallineSi_3N_4from the amorphous SiCN ceramic matrix is observed at1500°C.
In order to study the influence of the content of carbon on the structure andproperties of polymer derived ceramics, polysilylcarbodiimides were synthesized bydifferent chlorosilanes (ethyltri-, hexyl-and benzyl-trichlorosilane) in reaction withBTSC. The ceramic yields of the three samples after pyrolysis at1000°C differ fromeach other due to various functional groups in the polysilylcarbodiimides. The SiCNceramics exhibit an amorphous porous structure at this temperature. All three SiCNmaterials convert from amorphous station to crystalline structure above1400°C.However, the temperature of crystallization depends on the content of carbon in theceramic matrix. In the sample with higher content of carbon the separation of Si_3N_4from the amorphous SiCN matrix is observed at higher temperature, demonstratingthe higher thermal stability against crystallization.
引文
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