高硅氧/酚醛复合材料的烧蚀机理及热—力学性能研究
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摘要
随着长时间飞行器需求的不断增长，对长时间中低热流环境下的热防护材料需求也越来越迫切。作为树脂基防热材料的一种，高硅氧/酚醛复合材料具有较低的密度和热导率、优良的吸热能力、耐烧蚀性能和热稳定性等特点，且成本低廉、工艺周期短、高温性能优异。该类型材料既能适用于长时间飞行、中等焓值、中低热流的防热要求，又能耐长时间烧蚀和高气流剪切，且具有较好的隔热性能，因而被广泛应用于长时间飞行器的烧蚀热防护。在高温环境下，高硅氧/酚醛复合材料会发生复杂的物理-化学变化和烧蚀-相变过程，包括酚醛树脂的热解反应、热解气体的扩散流动、孔隙压力、热阻塞效应、热膨胀现象、边界移动等过程。另外，气动加热会使防热材料及其结构产生热变形，且在气动力和气动热载荷作用下防热材料的强度和承载能力也会有明显的衰减。因此，有必要研究高硅氧/酚醛复合材料在长时间中低热流环境下的烧蚀防热机理，预报材料的烧蚀性能及高温热力学性能，对该类型复合材料防热层的结构设计、完整性及可靠性评价有重要的意义。
本文系统研究了高硅氧/酚醛复合材料在烧蚀环境下的质量损失机理及吸热机理，基于表面烧蚀理论和气体边界层理论，建立了防热材料的表面烧蚀性能预报方法，根据质量守恒和能量守恒原理，建立了聚合物基复合材料热-力学行为的多场耦合模型，给出了防热材料的高温刚度和强度性能预报方法，并设计相关实验验证了预报模型的正确性。
首先对高硅氧/酚醛复合材料进行静态/动态烧蚀实验，通过热失重率和吸放热曲线研究材料在不同温度与加温速率下的热解反应，利用一阶Arrhenius方程，建立了防热材料的热解动力学模型。通过对烧蚀过程中材料表面的烧蚀现象及热暴露后试样切片的微观结构进行观测，揭示了高硅氧/酚醛复合材料在高温环境下的烧蚀/防隔热机理。考虑硅基复合材料烧蚀表面的熔融液态层，预报了给定气动热环境下高硅氧/酚醛复合材料的表面烧蚀后退速率、壁面温度等烧蚀性能，预报结果与氧乙炔焰烧蚀实验结果比较吻合较好。结合表面烧蚀理论和边界层气体动力学关系，推导了材料的热容吸热、树脂热解吸热、表面材料的热辐射、热阻塞效应、熔融SiO2的蒸发吸热对材料总吸热能力的贡献权重，讨论了树脂含量、热传导系数、比热容等对防热材料烧蚀性能的影响。
其次考虑热解过程中热解气体聚集和流动造成的孔隙压力变化及材料内部的热-质传递过程，利用有限差分方法建立了高硅氧/酚醛复合材料在单侧辐射热流作用下的一维热响应模型。在模型中充分考虑了热膨胀引起的边界移动和热阻塞效应，预报了防热材料在体积烧蚀过程中的温度分布、孔隙压力分布、组分相体积含量变化、热解反应进行程度和气体质量流率。以外界自然光为光源，设计了太阳光辐射加热实验，测量了单侧热流载荷下高硅氧/酚醛复合材料试样不同厚度位置处的温度变化曲线，实验结果与计算结果吻合较好，验证了热响应模型的正确性。
聚合物基复合材料的热化学分解过程是一个热-力-化学多场耦合问题。根据质量守恒和能量守恒原理，充分考虑温度/扩散/变形的耦合作用，建立了多孔弹性体高温环境下热-力学行为的多物理场耦合分析模型。应用Bubnov-Galerkin有限元方法将高硅氧/酚醛复合材料热-力学响应的控制微分方程改写为单元代数方程组。利用高斯消去法求解最终整合的整体代数方程组，预报了材料在热流载荷下的高温变形、热应变和热应力。基于数字图像相关技术，设计了非接触式高温变形测量实验，获得了试样测量表面的全场变形和应变。应变测量结果和计算结果吻合较好，验证了多场耦合分析模型的准确性。
最后考虑聚合物基复合材料因热软化效应及基体热解反应引起的力学性能衰减，根据Mori-Tanaka方法和Eshelby等效夹杂理论，建立了高硅氧/酚醛复合材料高温刚度性能的细观力学预报方法。由高温压缩实验获得了防热材料的压缩强度随温度的变化关系曲线。基于热响应分析，给出了高硅氧/酚醛复合材料的高温压缩强度计算公式，预报了防热材料在单侧辐射热流和静态压缩载荷作用下强度性能随温度及加热时间的衰减规律。
With increasing of demand of long time space vehicles, thermal protectionmaterials which used in long time low-medium heat flux environment have been paidmore and more attention. As a kind of resin-matrix thermal protective material,silica/phenolic composites have many advantages, such as low density and thermalconductivity, good endothermic ability, ablation resistant performance and thermalstability, as well as short processing cycle, cheap cost and excellent high-temperatureproperties. This kind of material can not only meet the thermal protectiverequirements of long time flying, medium level enthalpy and low-medium heat flux,but also resist long time ablation and shearing action of high-velocity gas flow.Additionally, there are good heat-insulating properties of silica/phenolic composites.For this reason, they are widely used in the ablation and thermal protection of longtime flight vehicles. The complex physico-chemical changes, ablation and phasetransition processes of silica/phenolic composite can take place when exposed to hightemperature. That is generally associated with pyrolysis reaction of phenolic resin,diffusion and flow of decomposition gases, pore pressure, thermal blockade effect,thermal expansion phenomenon and moving boundary. Furthermore, aerodynamicheating can cause thermal deformation of the thermal protective material and itsstructure. Strength and loading capacity of the material significantly degrade whensubjected to aerodynamic mechanical and thermal loading. Therefore, it is necessaryto study the ablation and thermal protective mechanism of silica/phenolic compositeunder long time low-medium heat flux environment and predict ablation propertiesand high-temperature thermomechanical behavior, and which is significant forstructure design, evaluation of integrity and reliability of heat shield for this kind ofcomposite.
The mass loss mechanism and endothermic mechanism in ablation environmentwere studied in detail in this dissertation. Based on the surface ablation theory andboundary layer aerodynamics theory, a prediction method of surface ablationproperties was established. According to mass and energy conservation principles, amulti-physics field coupling model was proposed to predict the thermomechanicalbehavior of polymer composites. Prediction methods of high temperature stiffness and strength for thermal protective materials were presented. The above-mentionedprediction models were validated by relevant experiments.
Firstly, the static and dynamic ablation experiments of silica/phenolic compositewere conducted. Based on thermo-gravimetric and endothermic (exothermic) curves,the pyrolysis reaction of the material with different temperature and heated rates werestudied. A thermal decomposition kinetics model was presented using one-orderArrhenius equation. According to the ablation feature on material surface andmorphology of post-heated specimen segment, the ablation and thermal protectivemechanism of silica/phenolic composite were analyzed. Considering the fused liquidlayer on ablation surface of silica-reinforced composites, surface ablation recessionrate and wall temperature were predicted under given aerodynamics thermalenvironment. The predicted results were in good agreement with the oxyacetyleneexperimental results. The proportions of the endothermic mechanisms including heatabsorption of heat capacity of ablator, thermal decomposition of the resin, heatradiation of surface material, thermal blockade effect and evaporation of fused silicafiber in the total heat absorption were derived by combining with surface ablationtheory and boundary layer aerodynamics relationships. Moreover, the effects of resincontent, thermal conductivity and specific heat on ablation properties of thermalprotective materials were discussed.
Secondly, considering variation of the pore pressure and heat-mass transferprocesses within the materials, a one-dimensional thermal response model wasdeveloped using finite difference method when silica/phenolic composite wasexposed to one-sided radiant heat flux. The moving boundary caused by thermalexpansion and the thermal blockade effect were also considered in the model. Thetemperature distribution, pore pressure distribution, variation of volume content ofphase components, degree of decomposition and mass flux of gases of the thermalprotective material during volume ablation process were predicted. The sunlight wasused as the light source and the solar radiation heating experiment was carried out.The time-dependent temperature progressions at different material depths ofsilica/phenolic composite specimen were measured when exposed to one-sided heatflux. The experimental temperature profiles were in good agreement with thecalculated results. Furthermore, the accuracy of the thermal response model wasassessed.
Thermochemical decomposition process of polymer composites can be regardedas a thermal-mechanical-chemical multi-physics field coupling problem. Based onmass and energy conservation principles, a multi-physics field coupling analysismodel was proposed to predict the thermomechanical behavior of porous elastomersunder high temperatures. The coupling actions of temperature, diffusion anddeformation were taken into account in the model. The governing differentialequations of thermomechanical response of silica/phenolic composite were modifiedusing the Bubnov-Galerkin finite element method to obtain the generalized effectiveelement stiffness equation. Finally, the global stiffness equations were assembled,and solved by the Gaussian elimination method. The high temperature deformation,thermal strain and thermal stress of the material were predicted when subjected toheat flux. Additionally, non-contact high temperature deformation measurementexperiment was conducted by applying digital image correlation technique and fullfield deformation and strain on measured surface of the specimen were obtained. Theexperimental strain results were in good agreement with the calculated values.Consequently, the accuracy of the multi-physics field coupling analysis model wasevaluated.
Finally, the degradation in mechanical properties caused by the thermalsoftening effect and thermal decomposition of matrix material were studied. UsingMori-Tanaka method and Eshelby equivalent inclusion theory, a mesomechanicalmethod was proposed to predict high-temperature stiffness properties ofsilica/phenolic composite. Relationships between compression strength andtemperature of thermal protective material were obtained using high-temperaturecompression experiment. Based on thermal response analysis, the calculationformulas of high temperature compression strength for silica/phenolic compositewere presented. Degradation in strength properties with temperature and heated timewere predicted when the material subjected to one-sided radiant heat flux and staticcompression loading.
本文系统研究了高硅氧/酚醛复合材料在烧蚀环境下的质量损失机理及吸热机理，基于表面烧蚀理论和气体边界层理论，建立了防热材料的表面烧蚀性能预报方法，根据质量守恒和能量守恒原理，建立了聚合物基复合材料热-力学行为的多场耦合模型，给出了防热材料的高温刚度和强度性能预报方法，并设计相关实验验证了预报模型的正确性。
首先对高硅氧/酚醛复合材料进行静态/动态烧蚀实验，通过热失重率和吸放热曲线研究材料在不同温度与加温速率下的热解反应，利用一阶Arrhenius方程，建立了防热材料的热解动力学模型。通过对烧蚀过程中材料表面的烧蚀现象及热暴露后试样切片的微观结构进行观测，揭示了高硅氧/酚醛复合材料在高温环境下的烧蚀/防隔热机理。考虑硅基复合材料烧蚀表面的熔融液态层，预报了给定气动热环境下高硅氧/酚醛复合材料的表面烧蚀后退速率、壁面温度等烧蚀性能，预报结果与氧乙炔焰烧蚀实验结果比较吻合较好。结合表面烧蚀理论和边界层气体动力学关系，推导了材料的热容吸热、树脂热解吸热、表面材料的热辐射、热阻塞效应、熔融SiO2的蒸发吸热对材料总吸热能力的贡献权重，讨论了树脂含量、热传导系数、比热容等对防热材料烧蚀性能的影响。
其次考虑热解过程中热解气体聚集和流动造成的孔隙压力变化及材料内部的热-质传递过程，利用有限差分方法建立了高硅氧/酚醛复合材料在单侧辐射热流作用下的一维热响应模型。在模型中充分考虑了热膨胀引起的边界移动和热阻塞效应，预报了防热材料在体积烧蚀过程中的温度分布、孔隙压力分布、组分相体积含量变化、热解反应进行程度和气体质量流率。以外界自然光为光源，设计了太阳光辐射加热实验，测量了单侧热流载荷下高硅氧/酚醛复合材料试样不同厚度位置处的温度变化曲线，实验结果与计算结果吻合较好，验证了热响应模型的正确性。
聚合物基复合材料的热化学分解过程是一个热-力-化学多场耦合问题。根据质量守恒和能量守恒原理，充分考虑温度/扩散/变形的耦合作用，建立了多孔弹性体高温环境下热-力学行为的多物理场耦合分析模型。应用Bubnov-Galerkin有限元方法将高硅氧/酚醛复合材料热-力学响应的控制微分方程改写为单元代数方程组。利用高斯消去法求解最终整合的整体代数方程组，预报了材料在热流载荷下的高温变形、热应变和热应力。基于数字图像相关技术，设计了非接触式高温变形测量实验，获得了试样测量表面的全场变形和应变。应变测量结果和计算结果吻合较好，验证了多场耦合分析模型的准确性。
最后考虑聚合物基复合材料因热软化效应及基体热解反应引起的力学性能衰减，根据Mori-Tanaka方法和Eshelby等效夹杂理论，建立了高硅氧/酚醛复合材料高温刚度性能的细观力学预报方法。由高温压缩实验获得了防热材料的压缩强度随温度的变化关系曲线。基于热响应分析，给出了高硅氧/酚醛复合材料的高温压缩强度计算公式，预报了防热材料在单侧辐射热流和静态压缩载荷作用下强度性能随温度及加热时间的衰减规律。
With increasing of demand of long time space vehicles, thermal protectionmaterials which used in long time low-medium heat flux environment have been paidmore and more attention. As a kind of resin-matrix thermal protective material,silica/phenolic composites have many advantages, such as low density and thermalconductivity, good endothermic ability, ablation resistant performance and thermalstability, as well as short processing cycle, cheap cost and excellent high-temperatureproperties. This kind of material can not only meet the thermal protectiverequirements of long time flying, medium level enthalpy and low-medium heat flux,but also resist long time ablation and shearing action of high-velocity gas flow.Additionally, there are good heat-insulating properties of silica/phenolic composites.For this reason, they are widely used in the ablation and thermal protection of longtime flight vehicles. The complex physico-chemical changes, ablation and phasetransition processes of silica/phenolic composite can take place when exposed to hightemperature. That is generally associated with pyrolysis reaction of phenolic resin,diffusion and flow of decomposition gases, pore pressure, thermal blockade effect,thermal expansion phenomenon and moving boundary. Furthermore, aerodynamicheating can cause thermal deformation of the thermal protective material and itsstructure. Strength and loading capacity of the material significantly degrade whensubjected to aerodynamic mechanical and thermal loading. Therefore, it is necessaryto study the ablation and thermal protective mechanism of silica/phenolic compositeunder long time low-medium heat flux environment and predict ablation propertiesand high-temperature thermomechanical behavior, and which is significant forstructure design, evaluation of integrity and reliability of heat shield for this kind ofcomposite.
The mass loss mechanism and endothermic mechanism in ablation environmentwere studied in detail in this dissertation. Based on the surface ablation theory andboundary layer aerodynamics theory, a prediction method of surface ablationproperties was established. According to mass and energy conservation principles, amulti-physics field coupling model was proposed to predict the thermomechanicalbehavior of polymer composites. Prediction methods of high temperature stiffness and strength for thermal protective materials were presented. The above-mentionedprediction models were validated by relevant experiments.
Firstly, the static and dynamic ablation experiments of silica/phenolic compositewere conducted. Based on thermo-gravimetric and endothermic (exothermic) curves,the pyrolysis reaction of the material with different temperature and heated rates werestudied. A thermal decomposition kinetics model was presented using one-orderArrhenius equation. According to the ablation feature on material surface andmorphology of post-heated specimen segment, the ablation and thermal protectivemechanism of silica/phenolic composite were analyzed. Considering the fused liquidlayer on ablation surface of silica-reinforced composites, surface ablation recessionrate and wall temperature were predicted under given aerodynamics thermalenvironment. The predicted results were in good agreement with the oxyacetyleneexperimental results. The proportions of the endothermic mechanisms including heatabsorption of heat capacity of ablator, thermal decomposition of the resin, heatradiation of surface material, thermal blockade effect and evaporation of fused silicafiber in the total heat absorption were derived by combining with surface ablationtheory and boundary layer aerodynamics relationships. Moreover, the effects of resincontent, thermal conductivity and specific heat on ablation properties of thermalprotective materials were discussed.
Secondly, considering variation of the pore pressure and heat-mass transferprocesses within the materials, a one-dimensional thermal response model wasdeveloped using finite difference method when silica/phenolic composite wasexposed to one-sided radiant heat flux. The moving boundary caused by thermalexpansion and the thermal blockade effect were also considered in the model. Thetemperature distribution, pore pressure distribution, variation of volume content ofphase components, degree of decomposition and mass flux of gases of the thermalprotective material during volume ablation process were predicted. The sunlight wasused as the light source and the solar radiation heating experiment was carried out.The time-dependent temperature progressions at different material depths ofsilica/phenolic composite specimen were measured when exposed to one-sided heatflux. The experimental temperature profiles were in good agreement with thecalculated results. Furthermore, the accuracy of the thermal response model wasassessed.
Thermochemical decomposition process of polymer composites can be regardedas a thermal-mechanical-chemical multi-physics field coupling problem. Based onmass and energy conservation principles, a multi-physics field coupling analysismodel was proposed to predict the thermomechanical behavior of porous elastomersunder high temperatures. The coupling actions of temperature, diffusion anddeformation were taken into account in the model. The governing differentialequations of thermomechanical response of silica/phenolic composite were modifiedusing the Bubnov-Galerkin finite element method to obtain the generalized effectiveelement stiffness equation. Finally, the global stiffness equations were assembled,and solved by the Gaussian elimination method. The high temperature deformation,thermal strain and thermal stress of the material were predicted when subjected toheat flux. Additionally, non-contact high temperature deformation measurementexperiment was conducted by applying digital image correlation technique and fullfield deformation and strain on measured surface of the specimen were obtained. Theexperimental strain results were in good agreement with the calculated values.Consequently, the accuracy of the multi-physics field coupling analysis model wasevaluated.
Finally, the degradation in mechanical properties caused by the thermalsoftening effect and thermal decomposition of matrix material were studied. UsingMori-Tanaka method and Eshelby equivalent inclusion theory, a mesomechanicalmethod was proposed to predict high-temperature stiffness properties ofsilica/phenolic composite. Relationships between compression strength andtemperature of thermal protective material were obtained using high-temperaturecompression experiment. Based on thermal response analysis, the calculationformulas of high temperature compression strength for silica/phenolic compositewere presented. Degradation in strength properties with temperature and heated timewere predicted when the material subjected to one-sided radiant heat flux and staticcompression loading.
引文
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