高氮奥氏体不锈钢的组织稳定性研究
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摘要
近年来不断增长的不锈钢需求与有限的镍资源之间的矛盾日趋严重。另外,人体器官对作为生物工程材料的含镍奥氏体不锈钢存在过敏性。这些原因使得人们把目光聚焦到既具有低的成本又具有优异的力学性能及耐腐蚀、耐氧化、耐磨损等性能的资源节约型不锈钢——高氮不锈钢上。但是,对于这种新型的先进钢铁材料,在热加工、焊接和使用时,在奥氏体中可能会有碳氮化物和金属间化合物的析出发生,降低奥氏体的稳定性。这些第二相的析出将会严重破坏材料的各种加工和使用性能。因此,研究它的析出行为和对性能的影响具有重要的理论意义和实用价值。
本研究熔炼了一系列以Mn、N完全代Ni的高氮奥氏体不锈钢,通过金相显微镜、扫描电镜、透射电镜、X射线衍射、热模拟和显微硬度等测试技术和热力学计算,系统地研究了这种资源节约型不锈钢等温时效过程中第二相析出的热力学和动力学规律,合金成分、处理制度和第二相析出之间的关系,奥氏体组织稳定性对热塑性的影响,冷变形和合金元素Mn、Mo等对析出行为的影响。获得的主要结论如下：
1、Fe-18Cr-Mn-C-N系和Fe-18Cr-Mn-Mo-C-N系的热力学平衡相图计算所提供的信息与实验结果基本一致,表明此种热力学计算可为Fe-18Cr-Mn-C-N和Fe-18Cr-Mn-Mo-C-N合金系的合金设计、奥氏体化及等温时效处理工艺提供热力学依据。
2、在Cr-Mn-N系低碳高氮奥氏体不锈钢中,固溶处理后时效的析出相主要为M2N相。随着时效时间的增加,M2N相由晶界的粒状析出过渡到向晶内长大的胞状析出。当钢中残留少量的碳时,会有极少量的粒状M23C6相在晶界析出,随着时效时间的增加,M23C6的析出量没有增加。
3、在Fe-18Cr-12Mn-0.48N钢中,析出的温度区间为625-925℃。根据实验数据测定的M2N的析出动力学曲线,M2N析出的鼻尖温度为800℃,相应的孕育期为30min,析出激活能为296kJ/mol。
4、高氮奥氏体不锈钢Fe-18Cr-12Mn-0.55N的热塑性分为三个特征区：(1)高于1150℃的高温脆性区；(2)温度区间为850-150℃的高温塑性区；(3)低于850℃的中温半脆性区。高温脆性和中温半脆性分别由δ铁素体和M2N析出相在奥氏体晶界上的形成所致。在高温塑性区的优良的热塑性是由于在此温度区间拉伸试样为稳定的单相奥氏体组织。
5、冷变形促进M2N相的析出,除了在晶界上率先析出外,冷变形材料在孪晶界上也有析出；冷变形还促进金属间化合物σ相的析出。
6、实验用钢经30%冷变形以后,大约在750℃开始发生再结晶。在750℃时效过程中,析出的发生优先于再结晶,大量的第二相粒子在位错、晶界和亚晶界等缺陷位置优先形核,这些粒子的析出阻碍了再结晶晶核的形成。在900℃时效过程中,再结晶和析出同时发生,第二相粒子在亚晶和再结晶的晶界和晶内均有发生,M23C6、M2N析出发生在晶界上,σ相析出发生在晶内。
7、在低碳的Fe-18Cr-(18/12)Mn-0.4N高氮奥氏体不锈钢中,合金元素Mn的增加对析出类型没有影响,M2N仍然是主要的析出相。Mn的增加对M2N的析出有促进作用,会使M2N析出的上限温度提高。
8、高氮奥氏体不锈钢Fe-18Cr-18Mn-0.6N中添加Mo,使钢中出现另一种金属间化合物χ相,χ相不仅在晶界析出,也在晶内析出。加Mo的高氮奥氏体不锈钢的氮化物析出也呈现了不连续的胞状方式。
The contradiction between continuously increasing requirement of stainless steels and limited Ni resources has become more and more serious in recent years. In addition, human organs exhibit irritability to austenitic stainless steel with Ni as bioengineering materials. As a result, great attention is now focused on resource-saving stainless steels, that is high-nitrogen stainless steel having not only low cost but also excellent mechanical properties, corrosion resistance, oxidization resistance and wear resistance etc.. However, the precipitation of carbides, nitrides and intermetallics may occur in austenite of this advanced steel material during thermal processes, welding and service at the elevated temperatures, which reduce austenitic stability. The precipitation of second phases will heavily damage various working and service properties of materials. Therefore, investigation on precipitation behavior and its effects on properties are of academic significance and practical importance.
In the present study, a series of high-nitrogen austenitic stainless steels completely replacing Ni by Mn and N were smelted. Through optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), thermomechanical simulation, micro-hardness test and thermodynamic calculation, we systemically investigated the thermodynamic and kinetic behaviors of precipitation during isothermal aging, the relationship among alloy compositions, treatment conditions and second phase precipitation, the effect of austenitic stability on hot ductility and the effects of cold deformation and alloying elements of Mn and Mo on precipitation behavior. The major conclusions are as follows:
1. The information provided by calculation of thermodynamic equilibrium diagram on Fe-18Cr-Mn-C-N system and Fe-18Cr-Mn-Mo-C-N system is consistent with the experimental results, indicating that this kind of thermodynamic calculation can provide thermodynamic instructions for alloy composition design, establishing of austenization and isothermal aging heat treatment conditions in Fe-18Cr-Mn-C-N system and Fe-18Cr-Mn-Mo-C-N system.
2. M2N phase is the main precipitate in low carbon high-nitrogen Cr-Mn-N austenitic stainless steel during aging after solution treatment. The precipitation of M2N phase transits from initial granular precipitation at grain boundary to cellular precipitation growing towards to grain inside with increasing aging time. When small amount of carbon remains in the steels, thimbleful of granular M23C6 phase precipitates at grain boundary. The volume fraction of M23C6 precipitates does not increase with increasing aging time.
3. The temperature region of precipitation is between 625℃and 925℃in Fe-18Cr-12Mn-0.48N steel. According to the isothermal precipitation kinetics curve of M2N mensurated from experimental data, the nose temperature of M2N precipitation is determined to be 800℃, the corresponding incubation period is 30min and the corresponding activation energy of precipitation is calculated as 296 kJ/mol.
4. The hot ductility curve of Fe-18Cr-12Mn-0.55N high-nitrogen austenitic stainless steel can be divided into three regions:(1)the high-temperature brittlement region higher than 1150℃; (2)the high-temperature ductility region from 850℃to 1150℃; (3)the middle-temperature half brittlement region lower than 850℃. The high-temperature brittlement and middle-temperature half brittlement are caused by the appearances ofδferrite and the precipitation of M2N phase at austenitic grain boundaries, respectively. The excellent hot ductility region between the two brittlement temperature regions results from the stable single phase austenitic microstructure.
5. Cold deformation accelerates the precipitation of M2N phase. Beside the precipitation firstly occurs at grain boundaries, the precipitation also occurs at twin grain boundaries in cold-deformated materials. Cold deformation also induces the precipitation ofσphase.
6. After 30% cold deformation, the test steel begins to recrystallize at about 750℃. During aging at 750℃the precipitation occurs prior to recrystallization. Large numbers of the second phases preferentially nucleate at defect sites such as dislocations, grain boundaries and subgrain boundaries. The precipitation of these second-phase particles hinders the formation of recrystallization nucleus. During aging at 900℃, the recrystallization and precipitation simultaneously occur, the precipitation of second phases occurs both at subgrain and recrystallized grain boundaries and inside grains. M2N and M23C6 precipitation occurs at grain boundaries andσphase precipitation occurs inside grains.
7. In Fe-18Cr-(18/12)Mn-0.4N low carbon high-nitrogen austenitic stainless steels, increasing of Mn content has no effect on the precipitation type and M2N phase is still major precipitate. Increasing of Mn content accelerates precipitation of M2N phase and increases upper limit temperature of M2N precipitation.
8. The addition of Mo to Fe-18Cr-18Mn-0.6N high-nitrogen austenitic stainless steel causes the precipitation of another precipitate, intermetallicsχphase. The precipitation ofχphase occurs not only at grain boundaries but also inside grains. The nitrides also precipitate by the discontinuous cellular way in high-nitrogen austenitic stainless steel with Mo.
本研究熔炼了一系列以Mn、N完全代Ni的高氮奥氏体不锈钢,通过金相显微镜、扫描电镜、透射电镜、X射线衍射、热模拟和显微硬度等测试技术和热力学计算,系统地研究了这种资源节约型不锈钢等温时效过程中第二相析出的热力学和动力学规律,合金成分、处理制度和第二相析出之间的关系,奥氏体组织稳定性对热塑性的影响,冷变形和合金元素Mn、Mo等对析出行为的影响。获得的主要结论如下：
1、Fe-18Cr-Mn-C-N系和Fe-18Cr-Mn-Mo-C-N系的热力学平衡相图计算所提供的信息与实验结果基本一致,表明此种热力学计算可为Fe-18Cr-Mn-C-N和Fe-18Cr-Mn-Mo-C-N合金系的合金设计、奥氏体化及等温时效处理工艺提供热力学依据。
2、在Cr-Mn-N系低碳高氮奥氏体不锈钢中,固溶处理后时效的析出相主要为M2N相。随着时效时间的增加,M2N相由晶界的粒状析出过渡到向晶内长大的胞状析出。当钢中残留少量的碳时,会有极少量的粒状M23C6相在晶界析出,随着时效时间的增加,M23C6的析出量没有增加。
3、在Fe-18Cr-12Mn-0.48N钢中,析出的温度区间为625-925℃。根据实验数据测定的M2N的析出动力学曲线,M2N析出的鼻尖温度为800℃,相应的孕育期为30min,析出激活能为296kJ/mol。
4、高氮奥氏体不锈钢Fe-18Cr-12Mn-0.55N的热塑性分为三个特征区：(1)高于1150℃的高温脆性区；(2)温度区间为850-150℃的高温塑性区；(3)低于850℃的中温半脆性区。高温脆性和中温半脆性分别由δ铁素体和M2N析出相在奥氏体晶界上的形成所致。在高温塑性区的优良的热塑性是由于在此温度区间拉伸试样为稳定的单相奥氏体组织。
5、冷变形促进M2N相的析出,除了在晶界上率先析出外,冷变形材料在孪晶界上也有析出；冷变形还促进金属间化合物σ相的析出。
6、实验用钢经30%冷变形以后,大约在750℃开始发生再结晶。在750℃时效过程中,析出的发生优先于再结晶,大量的第二相粒子在位错、晶界和亚晶界等缺陷位置优先形核,这些粒子的析出阻碍了再结晶晶核的形成。在900℃时效过程中,再结晶和析出同时发生,第二相粒子在亚晶和再结晶的晶界和晶内均有发生,M23C6、M2N析出发生在晶界上,σ相析出发生在晶内。
7、在低碳的Fe-18Cr-(18/12)Mn-0.4N高氮奥氏体不锈钢中,合金元素Mn的增加对析出类型没有影响,M2N仍然是主要的析出相。Mn的增加对M2N的析出有促进作用,会使M2N析出的上限温度提高。
8、高氮奥氏体不锈钢Fe-18Cr-18Mn-0.6N中添加Mo,使钢中出现另一种金属间化合物χ相,χ相不仅在晶界析出,也在晶内析出。加Mo的高氮奥氏体不锈钢的氮化物析出也呈现了不连续的胞状方式。
The contradiction between continuously increasing requirement of stainless steels and limited Ni resources has become more and more serious in recent years. In addition, human organs exhibit irritability to austenitic stainless steel with Ni as bioengineering materials. As a result, great attention is now focused on resource-saving stainless steels, that is high-nitrogen stainless steel having not only low cost but also excellent mechanical properties, corrosion resistance, oxidization resistance and wear resistance etc.. However, the precipitation of carbides, nitrides and intermetallics may occur in austenite of this advanced steel material during thermal processes, welding and service at the elevated temperatures, which reduce austenitic stability. The precipitation of second phases will heavily damage various working and service properties of materials. Therefore, investigation on precipitation behavior and its effects on properties are of academic significance and practical importance.
In the present study, a series of high-nitrogen austenitic stainless steels completely replacing Ni by Mn and N were smelted. Through optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), thermomechanical simulation, micro-hardness test and thermodynamic calculation, we systemically investigated the thermodynamic and kinetic behaviors of precipitation during isothermal aging, the relationship among alloy compositions, treatment conditions and second phase precipitation, the effect of austenitic stability on hot ductility and the effects of cold deformation and alloying elements of Mn and Mo on precipitation behavior. The major conclusions are as follows:
1. The information provided by calculation of thermodynamic equilibrium diagram on Fe-18Cr-Mn-C-N system and Fe-18Cr-Mn-Mo-C-N system is consistent with the experimental results, indicating that this kind of thermodynamic calculation can provide thermodynamic instructions for alloy composition design, establishing of austenization and isothermal aging heat treatment conditions in Fe-18Cr-Mn-C-N system and Fe-18Cr-Mn-Mo-C-N system.
2. M2N phase is the main precipitate in low carbon high-nitrogen Cr-Mn-N austenitic stainless steel during aging after solution treatment. The precipitation of M2N phase transits from initial granular precipitation at grain boundary to cellular precipitation growing towards to grain inside with increasing aging time. When small amount of carbon remains in the steels, thimbleful of granular M23C6 phase precipitates at grain boundary. The volume fraction of M23C6 precipitates does not increase with increasing aging time.
3. The temperature region of precipitation is between 625℃and 925℃in Fe-18Cr-12Mn-0.48N steel. According to the isothermal precipitation kinetics curve of M2N mensurated from experimental data, the nose temperature of M2N precipitation is determined to be 800℃, the corresponding incubation period is 30min and the corresponding activation energy of precipitation is calculated as 296 kJ/mol.
4. The hot ductility curve of Fe-18Cr-12Mn-0.55N high-nitrogen austenitic stainless steel can be divided into three regions:(1)the high-temperature brittlement region higher than 1150℃; (2)the high-temperature ductility region from 850℃to 1150℃; (3)the middle-temperature half brittlement region lower than 850℃. The high-temperature brittlement and middle-temperature half brittlement are caused by the appearances ofδferrite and the precipitation of M2N phase at austenitic grain boundaries, respectively. The excellent hot ductility region between the two brittlement temperature regions results from the stable single phase austenitic microstructure.
5. Cold deformation accelerates the precipitation of M2N phase. Beside the precipitation firstly occurs at grain boundaries, the precipitation also occurs at twin grain boundaries in cold-deformated materials. Cold deformation also induces the precipitation ofσphase.
6. After 30% cold deformation, the test steel begins to recrystallize at about 750℃. During aging at 750℃the precipitation occurs prior to recrystallization. Large numbers of the second phases preferentially nucleate at defect sites such as dislocations, grain boundaries and subgrain boundaries. The precipitation of these second-phase particles hinders the formation of recrystallization nucleus. During aging at 900℃, the recrystallization and precipitation simultaneously occur, the precipitation of second phases occurs both at subgrain and recrystallized grain boundaries and inside grains. M2N and M23C6 precipitation occurs at grain boundaries andσphase precipitation occurs inside grains.
7. In Fe-18Cr-(18/12)Mn-0.4N low carbon high-nitrogen austenitic stainless steels, increasing of Mn content has no effect on the precipitation type and M2N phase is still major precipitate. Increasing of Mn content accelerates precipitation of M2N phase and increases upper limit temperature of M2N precipitation.
8. The addition of Mo to Fe-18Cr-18Mn-0.6N high-nitrogen austenitic stainless steel causes the precipitation of another precipitate, intermetallicsχphase. The precipitation ofχphase occurs not only at grain boundaries but also inside grains. The nitrides also precipitate by the discontinuous cellular way in high-nitrogen austenitic stainless steel with Mo.
引文
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