超临界流体制备中间相沥青基泡沫炭及导热性研究
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摘要
中间相沥青基泡沫炭是将中间相沥青发泡,经氧化炭化以及石墨化处理后形成的一种新型低密度炭材料。与其他前驱体泡沫炭相比,中间相沥青基泡沫炭除了具备密度低、耐腐蚀、热膨胀系数小等优点外,由于中间相沥青的显著各向异性和可石墨化性能,导热性能显著提高,在航空航天以及民用领域有着广泛的应用前景。
本论文以中间相沥青为前驱体,利用超临界溶剂对中间相沥青良好的渗透性和溶解性,在高压反应釜内通过压力释放制备中间相沥青基泡沫炭,得到可控性良好的具有规整泡孔结构的泡沫炭。
在分析了不同溶剂在超临界状态下对中间相沥青泡沫炭结构性能的影响规律基础上,研究了混合溶剂对泡沫炭孔结构以及韧带结构的调控。研究了不同条件下发泡压力、温度、溶剂比例等因素对泡沫炭孔结构和韧带结构的影响。考察了不同氧化和炭化以及石墨化条件下泡沫炭导热性能的变化规律。分析了泡沫炭导热性能与其孔结构以及韧带结构的关系。研究发现,混合溶剂的中间相沥青的溶解性和均相成核性能得很大改善,使泡孔直径更加容易控制。通过选择不同混合比例的超临界流体、选择合适的发泡条件,可获得结构可控、密度分布在0.01～0.8g/cm3之间、孔径分布均匀、平均孔径在150～1100μm、壁厚15～100μm、孔隙率91%以上、开孔率高的泡沫炭,在此基础上,对不同孔结构的泡沫炭的导热性能进行研究。
利用已有的多孔材料中常用的分形理论分析了所制备炭材料的导热特性,尝试推导出并应用泡沫炭的面积分形堆数,构建了当量元泡根据截面分形空隙分数,提出了一个计算泡沫炭导热率的模型,并以此计算出泡沫炭的导热系数并和实验中得到的数据进行对比。
Mesophase pitch-based carbon foam, prepared from mesophase pitch, besides the low density, corrosion resistance and small thermal expansion coefficient like the carbon foams derived from other precursors, has high thermal conductivity for the anistropic structure of its precursor.
In this paper, mesophase pitch was foamed in a high-pressure reactor with supercritical solvents which have good permeability and solubility with the pitch. The size and structure of the pores could be controlled through pressure releasing.
After analyzing the law that different supercritical fluids effect the structure of the carbon foam, we could find the regulation of the carbon foam structure and ligament structure by mixed solvents. The pore and ligament structure of carbon foam formed under different conditions was studied: pressure, temperature, solvent sort and other factors. The changes of the thermal properties after carbonization and graphite were researched. The dependence of thermal properties of carbon foam on its pore and ligament structure was analyzed. It is found that the mixed solvents could have a good solubility with mesophase and improve the homogeneity. At the same time , the bubble diameter can be controlled easily . By choosing different mixing ratio of the supercritical fluid, we can get carbon foam with density in the range of 0.01～0.8g/cm~3, uniform size distribution between 150～1100μm, wall thickness of 15～100μm, porosity of 91% or more.
The thermal properties of carbon foam have been investigated and the mechanism of the thermal conductivity was analyzed on the model of thermal conductivity related to different pore structure. The carbon foam thermal conductivity calculation model have been established to calculate the thermal conductivity which was compared with the experimental data.
本论文以中间相沥青为前驱体,利用超临界溶剂对中间相沥青良好的渗透性和溶解性,在高压反应釜内通过压力释放制备中间相沥青基泡沫炭,得到可控性良好的具有规整泡孔结构的泡沫炭。
在分析了不同溶剂在超临界状态下对中间相沥青泡沫炭结构性能的影响规律基础上,研究了混合溶剂对泡沫炭孔结构以及韧带结构的调控。研究了不同条件下发泡压力、温度、溶剂比例等因素对泡沫炭孔结构和韧带结构的影响。考察了不同氧化和炭化以及石墨化条件下泡沫炭导热性能的变化规律。分析了泡沫炭导热性能与其孔结构以及韧带结构的关系。研究发现,混合溶剂的中间相沥青的溶解性和均相成核性能得很大改善,使泡孔直径更加容易控制。通过选择不同混合比例的超临界流体、选择合适的发泡条件,可获得结构可控、密度分布在0.01～0.8g/cm3之间、孔径分布均匀、平均孔径在150～1100μm、壁厚15～100μm、孔隙率91%以上、开孔率高的泡沫炭,在此基础上,对不同孔结构的泡沫炭的导热性能进行研究。
利用已有的多孔材料中常用的分形理论分析了所制备炭材料的导热特性,尝试推导出并应用泡沫炭的面积分形堆数,构建了当量元泡根据截面分形空隙分数,提出了一个计算泡沫炭导热率的模型,并以此计算出泡沫炭的导热系数并和实验中得到的数据进行对比。
Mesophase pitch-based carbon foam, prepared from mesophase pitch, besides the low density, corrosion resistance and small thermal expansion coefficient like the carbon foams derived from other precursors, has high thermal conductivity for the anistropic structure of its precursor.
In this paper, mesophase pitch was foamed in a high-pressure reactor with supercritical solvents which have good permeability and solubility with the pitch. The size and structure of the pores could be controlled through pressure releasing.
After analyzing the law that different supercritical fluids effect the structure of the carbon foam, we could find the regulation of the carbon foam structure and ligament structure by mixed solvents. The pore and ligament structure of carbon foam formed under different conditions was studied: pressure, temperature, solvent sort and other factors. The changes of the thermal properties after carbonization and graphite were researched. The dependence of thermal properties of carbon foam on its pore and ligament structure was analyzed. It is found that the mixed solvents could have a good solubility with mesophase and improve the homogeneity. At the same time , the bubble diameter can be controlled easily . By choosing different mixing ratio of the supercritical fluid, we can get carbon foam with density in the range of 0.01～0.8g/cm~3, uniform size distribution between 150～1100μm, wall thickness of 15～100μm, porosity of 91% or more.
The thermal properties of carbon foam have been investigated and the mechanism of the thermal conductivity was analyzed on the model of thermal conductivity related to different pore structure. The carbon foam thermal conductivity calculation model have been established to calculate the thermal conductivity which was compared with the experimental data.
引文
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