低温下结构陶瓷的相变、断裂机理与性能研究
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摘要
低温技术的不断发展使其应用于越来越多的领域中，例如航空航天、超导、核聚变等。在一些低温工程应用中，结构陶瓷有着其他材料不可替代的应用前景。然而，十分遗憾的是，目前关于结构陶瓷低温性能还缺乏系统和深入的研究。本文从低温与结构陶瓷中典型增韧机制的关系入手，研究了几种典型结构陶瓷在低温下的相变、断裂模式以及残余应力与其性能变化的关系。
研究发现3Y-TZP陶瓷低温下R曲线行为显著增强，这是传统理论没有预测到的，同时伴随着稳态断裂韧性、抗弯强度和韦伯模数同时提高，这是由于3Y-TZP陶瓷在低温下的相变增韧效应更加显著。此外，在测定材料室温及低温下相变区参数的基础上，从理论上计算了相变增韧对裂纹的屏蔽效应，并通过与实验结果的对比以及断裂形貌学的分析揭示了材料低温下断裂韧性的影响因素。
测定了2Y-TZP陶瓷在室温及低温下的临界晶粒尺寸，并发现在临界晶粒尺寸附近，材料的断裂韧性最大。此外，基于相变的形核和热力学理论，解释了室温下一定晶粒尺寸范围内材料断裂韧性保持不变的原因，同时还建立了温度与临界晶粒尺寸之间的关系，为制备低温下高韧性的2Y-TZP陶瓷提供了一条有效途径。
77K下Si_3N_4和RBSiC陶瓷的断裂韧性较室温明显升高，这是由于低温下材料中的残余应力增大：一方面导致低温下Si_3N_4陶瓷中的晶界弱化、沿晶断裂比例上升，强化了裂纹偏转、分枝等增韧效应，提高了其低温断裂韧性；另一方面增大了RBSiC陶瓷中裂纹扩展通过第二相Si时的阻力，使RBSiC陶瓷的低温断裂韧性升高。研究还发现没有明显增韧机制的Al_2O_3陶瓷在低温下抗弯强度变化很小，而99%Al_2O_3陶瓷的断裂韧性随温度降低有升高趋势。
综上，可以看出，结构陶瓷材料在低温下力学性能仍可保持较高水平甚至有显著提高，加之其在低温下的低热导率和良好的热稳定性，是低温工程中绝热和支撑部件的理想候选材料。
Currently, the rapid development of cryogenic techniques makes them required fora wide range of applications such as aeronautics&astronautics, superconducting fields,nuclear fusion and so on. Structural ceramics are promising cryogenic structuralmaterials which are prior to some kinds of metals and polymer materials in somespecific applications. However, more systematical and intensive researches on theproperties of structural ceramics at cryogenic temperatures are quite required becauseonly a small quantity of researches have been reported on such issues.
By considering the relationship between cryogenic temperatures and typicaltoughening mechanisms of structural ceramics, the correlation between cryogenicproperties and several important issues including transformation, fracture mechanismsand residual stress have been investigated.
A more pronounced R-curve behavior of3Y-TZP unanticipated by theconventional interpretation was found at cryogenic temperatures, which wasaccompanied by the concomitant increment of the fracture strength, toughness andWeibull modulus at cryogenic temperatures. This is due to the enhanced transformationtoughening effects at cryogenic temperatures. In addition, the transformation zoneparameters, discerned from accurate measurements with Raman microprobespectroscopy, were used to evaluate the shielding stress intensity factors. Bycomparison with the obtained experimental parameters from R-curve measurement andanalysis from the viewpoint of fractography at room and cryogenic temperatures, thefactors which may affect the cryogenic fracture toughness of3Y-TZP have beendiscussed.
The critical grain sizes of2Y-TZP at ambient and cryogenic temperatures havebeen determined. The grain size dependence of fracture toughness revealed that themaximum toughness value corresponds to the critical grain size at each temperature. Onthe basis of nucleation and thermodynamic theories, an established linear relationshipbetween inverse critical grain size and temperature has been explained and a basicunderstanding of grain size dependence of toughness at room temperature has been alsogained. It is believed that this relationship can provide an effective way to optimize the fracture toughness of2Y-TZP ceramics at cryogenic temperatures.
Fracture toughness values of Si_3N_4and RBSiC ceramics were found to beenhanced at cryogenic temperatures, respectively. On application of higher residualstress at77K, a larger number of Si_3N_4grains become involved in the crack deflectionprocess, leading to a larger percentage of intergranular fracture and thus enhancedfracture toughness of Si_3N_4ceramics. Moreover, the enhanced fracture toughness ofRBSiC ceramics at77K could be explained by the stronger resistance to crackpropagation resulting from higher residual stress at77K. Flexural strengths of Al_2O_3ceramics with no obvious toughening mechanisms were also found to be similar at bothcryogenic and ambient temperatures. However, fracture toughness of99%Al_2O_3ceramics tended to increase with decreasing temperatures.
As discussed above, the mechanical properties of structural ceramics can be similaror even higher compared to those at ambient temperatures. Therefore, such favorableperformances coupled with low thermal conductivity and good thermal stability makestructural ceramics candidate materials for thermal insulation and supportingapplications in cryogenic engineering.
研究发现3Y-TZP陶瓷低温下R曲线行为显著增强，这是传统理论没有预测到的，同时伴随着稳态断裂韧性、抗弯强度和韦伯模数同时提高，这是由于3Y-TZP陶瓷在低温下的相变增韧效应更加显著。此外，在测定材料室温及低温下相变区参数的基础上，从理论上计算了相变增韧对裂纹的屏蔽效应，并通过与实验结果的对比以及断裂形貌学的分析揭示了材料低温下断裂韧性的影响因素。
测定了2Y-TZP陶瓷在室温及低温下的临界晶粒尺寸，并发现在临界晶粒尺寸附近，材料的断裂韧性最大。此外，基于相变的形核和热力学理论，解释了室温下一定晶粒尺寸范围内材料断裂韧性保持不变的原因，同时还建立了温度与临界晶粒尺寸之间的关系，为制备低温下高韧性的2Y-TZP陶瓷提供了一条有效途径。
77K下Si_3N_4和RBSiC陶瓷的断裂韧性较室温明显升高，这是由于低温下材料中的残余应力增大：一方面导致低温下Si_3N_4陶瓷中的晶界弱化、沿晶断裂比例上升，强化了裂纹偏转、分枝等增韧效应，提高了其低温断裂韧性；另一方面增大了RBSiC陶瓷中裂纹扩展通过第二相Si时的阻力，使RBSiC陶瓷的低温断裂韧性升高。研究还发现没有明显增韧机制的Al_2O_3陶瓷在低温下抗弯强度变化很小，而99%Al_2O_3陶瓷的断裂韧性随温度降低有升高趋势。
综上，可以看出，结构陶瓷材料在低温下力学性能仍可保持较高水平甚至有显著提高，加之其在低温下的低热导率和良好的热稳定性，是低温工程中绝热和支撑部件的理想候选材料。
Currently, the rapid development of cryogenic techniques makes them required fora wide range of applications such as aeronautics&astronautics, superconducting fields,nuclear fusion and so on. Structural ceramics are promising cryogenic structuralmaterials which are prior to some kinds of metals and polymer materials in somespecific applications. However, more systematical and intensive researches on theproperties of structural ceramics at cryogenic temperatures are quite required becauseonly a small quantity of researches have been reported on such issues.
By considering the relationship between cryogenic temperatures and typicaltoughening mechanisms of structural ceramics, the correlation between cryogenicproperties and several important issues including transformation, fracture mechanismsand residual stress have been investigated.
A more pronounced R-curve behavior of3Y-TZP unanticipated by theconventional interpretation was found at cryogenic temperatures, which wasaccompanied by the concomitant increment of the fracture strength, toughness andWeibull modulus at cryogenic temperatures. This is due to the enhanced transformationtoughening effects at cryogenic temperatures. In addition, the transformation zoneparameters, discerned from accurate measurements with Raman microprobespectroscopy, were used to evaluate the shielding stress intensity factors. Bycomparison with the obtained experimental parameters from R-curve measurement andanalysis from the viewpoint of fractography at room and cryogenic temperatures, thefactors which may affect the cryogenic fracture toughness of3Y-TZP have beendiscussed.
The critical grain sizes of2Y-TZP at ambient and cryogenic temperatures havebeen determined. The grain size dependence of fracture toughness revealed that themaximum toughness value corresponds to the critical grain size at each temperature. Onthe basis of nucleation and thermodynamic theories, an established linear relationshipbetween inverse critical grain size and temperature has been explained and a basicunderstanding of grain size dependence of toughness at room temperature has been alsogained. It is believed that this relationship can provide an effective way to optimize the fracture toughness of2Y-TZP ceramics at cryogenic temperatures.
Fracture toughness values of Si_3N_4and RBSiC ceramics were found to beenhanced at cryogenic temperatures, respectively. On application of higher residualstress at77K, a larger number of Si_3N_4grains become involved in the crack deflectionprocess, leading to a larger percentage of intergranular fracture and thus enhancedfracture toughness of Si_3N_4ceramics. Moreover, the enhanced fracture toughness ofRBSiC ceramics at77K could be explained by the stronger resistance to crackpropagation resulting from higher residual stress at77K. Flexural strengths of Al_2O_3ceramics with no obvious toughening mechanisms were also found to be similar at bothcryogenic and ambient temperatures. However, fracture toughness of99%Al_2O_3ceramics tended to increase with decreasing temperatures.
As discussed above, the mechanical properties of structural ceramics can be similaror even higher compared to those at ambient temperatures. Therefore, such favorableperformances coupled with low thermal conductivity and good thermal stability makestructural ceramics candidate materials for thermal insulation and supportingapplications in cryogenic engineering.
引文
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