高温合金K465和DZ40M纯净化工艺及机理研究
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摘要
本文研究了镍基高温合金K465新料与钴基高温合金DZ40M返回料的纯净化工艺及机理,分析了纯净化处理后DZ40M返回料的组织结构与性能。利用氧、氮分析仪测定O、N含量,定硫仪测定S含量;在光学显微镜(OM)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)下分析合金的组织结构及断口形貌,对比分析新料和纯净化处理后返回料的拉伸、持久及蠕变性能,结果表明:
(1) K465镍基高温合金在1580℃高温精炼时,向熔体中加入0.02%C和0.5%Al后,O含量可降至5ppm;分两次向熔体中加Al,每次加入0.5%,可将N含量控制在5ppm;采用CaO坩埚熔炼合金时,向熔体中加少量Al后,脱S效果明显,可将S含量降至9ppm,最后采用加Ca终脱S,S含量最终控制在8ppm;
(2)采用高温熔体处理,电磁感应搅拌可以使熔体成分均匀,加速熔体表面反应,促进了N的脱除;精炼温度高及精炼时间长,有利于C脱O反应和脱N反应进行,也利于微量有害杂质的挥发;利用熔体阶段冷却法可以使合金中氧化物、氮化物、硫化物以及缩松缩孔减少;DZ40M返回料显微组织是在钴基奥氏体上,分布着由Ti、Zr、Ta、W等强碳化物形成元素组成的碳化物MC和富Cr的M7C3碳化物,与新料一致。
(3)在750℃～980℃/83～345MPa持久条件及700～900℃/125～360MPa蠕变条件下,DZ40M纯净化处理后合金的性能整体上高于DZ40M新料的性能,在拉伸变形期间,有细小二次M_(23)C_(6)沉淀析出,增加了合金的形变抗力;对拉伸条件为室温20℃、中温700℃、高温900℃和1000℃下的性能分析表明,纯净化处理后DZ40M返回料的强度和塑性基本达到新料的水平;纯净化处理工艺使返回料性能达到了预期的效果。
This thesis introduces the process and mechanism of cleaning treatment for the Ni-base alloy K465 and the recycled Co-base alloy DZ40M, analyses microstructures and the mechanical properties of the recycled Co-base alloy DZ40M after cleaning treatment.
Contents of oxygen and nitrogen are examined by Oxygen-nitrogen analyzer and the content of sulfur are measured by Sulfur Determination Device; Microstructures of virgin alloy and cleaning treatment recycled alloy, the fracture morphology of alloys after broken were investigated and analyzed by Optical Microscope(OM), Scanning Electron Microscope(SEM) and Transmission Electron Microscope (TEM); Stress rupture and creep, room temperature tensile properties, high-temperature tensile properties of cleaning treatment recycled alloy DZ40M have been compared with the virgin alloy, the results are as follows:
(1)Adding 0.02%C and 0.5%Al into Ni-base alloy K465 melting when it was refined at high temperature 1580℃, the content of O was decreased to 5ppm; When adding Al twice total 1%, each adding 0.5%, the content of N was reduced to 5ppm; When the CaO crucible were used to melt alloy, the effect of desulfurization was evident after adding a little Al into melting and it was decreased to 9ppm, adding Ca before tapping, as a result, the final content of S was 8ppm;
(2)Melt superheating treatment and electromagnetic stirring made the melt composition uniformity, speed up the melt surface reaction, promoted denitrogenation; high temperature and longtime refining was beneficial to the reaction of carbon deoxidization reaction and denitrogenation reaction, meanwhile facilitating volatilization of toxic harmful trace elements; Shrinkage cavity and porosity, oxides, nitrides and sulfides have been reduced by use of stage cooling of melt , as a result, the microstructure of recycled alloy DZ40M is Cobalt-based Austenite distributed by Carbides M7C3 and other Carbides MC. M7C3 is rich in Cr, MC is made up of strong carbide forming elements, such as Ti, Zr, Ta, W and so on.
(3)The mechanical properties of recycled alloy DZ40M have been analyzed in the following conditions: the stress rupture condition were 750～980℃/83～345MPa; the creep condition were 700～900℃/125MPa～360MPa,the overall properties of the cleaning treatment recycled alloy were higher than the properties of the virgin alloy, meanwhile, during the tensile deformation, some fine secondary precipitation phase M23C6 carbides released which strengthen the matrix; Tensile conditions were room temperature 20℃, intermediate temperature 700℃, high temperature 900℃and 1000℃; the result shows that the strength and the plasticity of cleaning treatment recycled alloy DZ40M have reached the level of virgin DZ40M's. It is concluded that properties of recycled alloy achieved the desired effect after cleaning treatment.
(1) K465镍基高温合金在1580℃高温精炼时,向熔体中加入0.02%C和0.5%Al后,O含量可降至5ppm;分两次向熔体中加Al,每次加入0.5%,可将N含量控制在5ppm;采用CaO坩埚熔炼合金时,向熔体中加少量Al后,脱S效果明显,可将S含量降至9ppm,最后采用加Ca终脱S,S含量最终控制在8ppm;
(2)采用高温熔体处理,电磁感应搅拌可以使熔体成分均匀,加速熔体表面反应,促进了N的脱除;精炼温度高及精炼时间长,有利于C脱O反应和脱N反应进行,也利于微量有害杂质的挥发;利用熔体阶段冷却法可以使合金中氧化物、氮化物、硫化物以及缩松缩孔减少;DZ40M返回料显微组织是在钴基奥氏体上,分布着由Ti、Zr、Ta、W等强碳化物形成元素组成的碳化物MC和富Cr的M7C3碳化物,与新料一致。
(3)在750℃～980℃/83～345MPa持久条件及700～900℃/125～360MPa蠕变条件下,DZ40M纯净化处理后合金的性能整体上高于DZ40M新料的性能,在拉伸变形期间,有细小二次M_(23)C_(6)沉淀析出,增加了合金的形变抗力;对拉伸条件为室温20℃、中温700℃、高温900℃和1000℃下的性能分析表明,纯净化处理后DZ40M返回料的强度和塑性基本达到新料的水平;纯净化处理工艺使返回料性能达到了预期的效果。
This thesis introduces the process and mechanism of cleaning treatment for the Ni-base alloy K465 and the recycled Co-base alloy DZ40M, analyses microstructures and the mechanical properties of the recycled Co-base alloy DZ40M after cleaning treatment.
Contents of oxygen and nitrogen are examined by Oxygen-nitrogen analyzer and the content of sulfur are measured by Sulfur Determination Device; Microstructures of virgin alloy and cleaning treatment recycled alloy, the fracture morphology of alloys after broken were investigated and analyzed by Optical Microscope(OM), Scanning Electron Microscope(SEM) and Transmission Electron Microscope (TEM); Stress rupture and creep, room temperature tensile properties, high-temperature tensile properties of cleaning treatment recycled alloy DZ40M have been compared with the virgin alloy, the results are as follows:
(1)Adding 0.02%C and 0.5%Al into Ni-base alloy K465 melting when it was refined at high temperature 1580℃, the content of O was decreased to 5ppm; When adding Al twice total 1%, each adding 0.5%, the content of N was reduced to 5ppm; When the CaO crucible were used to melt alloy, the effect of desulfurization was evident after adding a little Al into melting and it was decreased to 9ppm, adding Ca before tapping, as a result, the final content of S was 8ppm;
(2)Melt superheating treatment and electromagnetic stirring made the melt composition uniformity, speed up the melt surface reaction, promoted denitrogenation; high temperature and longtime refining was beneficial to the reaction of carbon deoxidization reaction and denitrogenation reaction, meanwhile facilitating volatilization of toxic harmful trace elements; Shrinkage cavity and porosity, oxides, nitrides and sulfides have been reduced by use of stage cooling of melt , as a result, the microstructure of recycled alloy DZ40M is Cobalt-based Austenite distributed by Carbides M7C3 and other Carbides MC. M7C3 is rich in Cr, MC is made up of strong carbide forming elements, such as Ti, Zr, Ta, W and so on.
(3)The mechanical properties of recycled alloy DZ40M have been analyzed in the following conditions: the stress rupture condition were 750～980℃/83～345MPa; the creep condition were 700～900℃/125MPa～360MPa,the overall properties of the cleaning treatment recycled alloy were higher than the properties of the virgin alloy, meanwhile, during the tensile deformation, some fine secondary precipitation phase M23C6 carbides released which strengthen the matrix; Tensile conditions were room temperature 20℃, intermediate temperature 700℃, high temperature 900℃and 1000℃; the result shows that the strength and the plasticity of cleaning treatment recycled alloy DZ40M have reached the level of virgin DZ40M's. It is concluded that properties of recycled alloy achieved the desired effect after cleaning treatment.
引文
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