高氮无镍奥氏体不锈钢的微观结构和力学性能研究
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摘要
奥氏体不锈钢是一种在工业上得到广泛应用的结构材料。与传统奥氏体不锈钢相比较，高氮奥氏体不锈钢具有许多优异的性能，比如高强度、高韧性、高应变硬化能力、强耐蚀性和低磁化性能等。高氮奥氏体不锈钢的上述优异性能使其逐渐地发展成为一种重要的新型结构材料，同时开发高性能高氮奥氏体不锈钢是目前国内外学界的研究热点之一。目前已开展了关于高氮奥氏体不锈钢微观结构和力学性能的研究，但对于固溶、冷轧、温轧和热轧这些处理方式对高氮奥氏体不锈钢微观结构和力学性能的影响却仍然有待深入系统的研究。因此，研究这些处理方式对高氮奥氏体不锈钢微观结构和力学性能的影响，可对高氮奥氏体不锈钢塑性变形规律及相关机制有一个全面而深入的认识，为其合理应用提供理论基础和数据积累。
本文通过对热成型高氮无镍奥氏体不锈钢原始钢板进行固溶处理，获得固溶态高氮钢；采用冷轧制固溶态高氮钢的方法，得到不同变形量的冷轧态高氮钢；通过时效处理的方法，获得不同微观结构的时效态高氮钢；分别采用400C和600C轧制固溶态高氮钢的方法，得到不同变形量的温轧态高氮钢；通过1140C轧制固溶态高氮钢的方法，获得不同变形量的热轧态高氮钢。使用拉伸实验测试系统和纳米压痕仪进行一系列的力学性能测试。采用X-射线衍射仪、扫描电子显微镜、透射电子显微镜等实验手段，对变形前和变形后的试样进行系统表征，并揭示相关的变形机制。
本文的主要研究结果如下：
1)1150C下固溶处理8h随后水淬可得平均晶粒尺寸为40m、存在大量孪晶的单相固溶态高氮无镍奥氏体不锈钢。拉伸实验显示，随应变速率的增加，屈服强度和抗拉强度增加(0.2=528-712MPa， UTS=957-1004MPa)，均匀应变和断裂应变明显下降(u=44.6-72.2%， f=60.4-87.6%)。流变应力表现出较高的应变速率敏感性，应变速率敏感性和激活体积分别为0.03和17b3，表明变形主要由位错-孪晶相互作用控制。变形表面和断口表面观察揭示，固溶态高氮无镍奥氏体不锈钢较高的强度和非常高的塑性，以及强度和塑性与应变速率的关系与其大量的晶内孪晶结构以及较低层错能导致的位错-孪晶相互作用有关。
2)采用冷轧变形方法获得了变形量为0%-70%的冷轧态高氮无镍奥氏体不锈钢，其显微组织主要为孪晶结构。随轧制变形量的增加，孪晶结构细化，数量增加。拉伸实验发现，随着轧制变形量的增加，屈服强度和抗拉强度增加(0.2=589-1885MPa， UTS=1001-2236MPa)，均匀应变和断裂应变降低(u=5.9-64.1%， f=12.3-86.6%)。70%冷轧态高氮无镍奥氏体不锈钢的综合力学性能(UTS=2236MPa， f=12.3%)是迄今报导的奥氏体不锈钢的最高综合力学性能之一。极高的强度和较高塑性源于其非常细小的孪晶结构。50%冷轧态高氮无镍奥氏体不锈钢的应变速率敏感性和激活体积分别为0.04和6b3，表明其变形主要由位错-孪晶相互作用控制。
3)50%冷轧态高氮无镍奥氏体不锈钢经200至600C时效处理3h后孪晶结构逐渐消失，微观结构粗化；800C时效处理3h后，发生明显的再结晶，形成等轴晶粒结构，析出铁素体和Cr2N相。拉伸实验显示，随时效温度从200C增至600C，时效态高氮无镍奥氏体不锈钢屈服强度和抗拉强度增加(0.2=1494-1545MPa， UTS=1834-1974MPa)，均匀应变先降低后增加(u=6.31-7.85%)，断裂应变趋于降低(f=9.04-9.60%)。800C以下时效态高氮钢强度的增加与析出微细Cr2N相及氮原子的偏聚对位错的钉扎作用有关，塑性明显降低则是由于微观结构的粗化和细小孪晶结构的消失。800C时效时强度和塑性的降低则是由于Cr2N相的晶界析出以及氮原子在晶界上的偏聚产生的晶界脆化作用。
4)采用1140C热轧变形方法获得了变形量分别为30%、50%和70%的热轧态高氮无镍奥氏体不锈钢，采用400C和600C温轧变形方法得到了变形量分别为50%和70%的温轧态高氮无镍奥氏体不锈钢。拉伸实验发现，对于热轧态高氮无镍奥氏体不锈钢，随应变速率的增加，强度增加，塑性呈下降趋势；随轧制变形量的增加，强度增加，塑性下降。对于温轧态高氮无镍奥氏体不锈钢，随轧制变形量的增加，强度增加，但塑性降低；随轧制温度的提高，其强度降低，塑性降低。高轧制变形量的热轧态高氮无镍奥氏体不锈钢较高的强度源于孪晶结构的细化和大量的小角度晶界的增加，塑性的降低源于大角度晶界数量的明显降低。高轧制变形量的温轧态高氮无镍奥氏体不锈钢较高的强度源于结构的细化，塑性的降低源于带状铁素体相的析出。
5)不同加载应变速率下的纳米压痕实验表明，与固溶态高氮无镍奥氏体不锈钢相比，70%冷轧态高氮无镍奥氏体不锈钢保载过程显示明显的蠕变变形。蠕变应变与微观结构和加载应变速率有关。显微组织越细小，加载应变速率越高，保载阶段产生的蠕变应变越大，蠕变速率越高。明显的蠕变变形主要是由于加载阶段存储的高密度位错结构在保载阶段会快速释放，产生明显的蠕变塑性变形。固溶态高氮无镍奥氏体不锈钢加载过程会形成稳定的位错结构，所以不产生明显的蠕变塑性变形。
Austenitic stainless steel has been used widely as one of the most important structuralmaterials nowadays. Compared with the conventional austenitic stainless steels, high nitro-gen austenitic stainless steels possess lots of attractive mechanical properties such as highstrength and ductility, high work hardening ability, excellent corrosion resistance and lowmagnetic susceptibility. The excellent performance above let high nitrogen austenitic stain-less steels become an increasingly important new class of structural materials and exploringgood quality of high nitrogen austenitic stainless steel has been intensive focus in the re-searchers domestically and overseas.So far, the mechanical properties and microstructure ofhigh nitrogen austenitic stainless steel have been intensively studied, however, few attentionhas been paid to the influence of solid solution, cold rolling, warm rolling and hot rolling onthe mechanical properties and microstructure systematically. To study these systematically isconducive to develop a deeper understanding of the plastic deformation and related mecha-nism, which can provide theoretical basis for the reasonable application of high nitrogenaustenitic stainless steel.
In this paper, solid solution-treated high nitrogen nickel-free austenitic stainless steel(HNS) samples were prepared by solution treatment. Cold-rolled HNS samples with differ-ent strains were produced by cold rolling at room temperature. By aging treatment, HNSsamples with different microstructures were produced. By rolling at400C and600C, thewarm-rolled HNS samples with different strains were prepared. By rolling at1140C, thehot-rolled HNS samples with different strains were prepared. The tensile testing system andnanoindentation were used to carry out a series of tests for mechanical properties. The X-raydiffraction, scanning electron microscopy and transmission electron microscopy were usedto characterize the specimens before and after deformation.
The main research results of current study are listed as follows:
1) Solid solution-treated HNS samples with single-phase and abundant intracrystalline twin were produced by solution treatment at1150C for8h and water quenching. The aver-age grain size is40m. Uniaxial tensile tests reveal that, with the increase of strain rate, theyield strength and ultimate tensile strength increase (0.2=528-712MPa, UTS=957-1004MPa) while the uniform plastic strain and tensile fracture strain decrease(u=44.6-72.2%, f=60.4-87.6%). It is noted that flow stress performs a relatively high strain rate sensitivity.The strain rate sensitivity and activation volume are0.03and17b3, respectively. This re-veals that the deformation mode is mainly the interaction between dislocation and twin. Sur-face and fracture of the deformed samples demonstrate that the relatively high strength, ul-tra-high elongation and the relation of strength and elongation with strain rate relate toabundant intracrystalline twin and the interaction between dislocation and twin caused bylow stacking fault energy.
2) Cold rolled HNS samples with0%-70%rolling strain were produced respectively.The main structure of cold rolled HNS is twin. With the increase of rolling strain, the twinrefined and amount increased. Tensile tests reveal that, with the increase of rolling strain, theyield strength and ultimate tensile strength increase (0.2=589-1885MPa, UTS=1001-2236MPa), while the uniform plastic strain and tensile fracture ductility decrease (u=5.9-64.1%,
f=12.3-86.6%). It is noted that the mechanical properties (UTS=2236MPa, f=12.3%)of70%cold rolled HNS have been the most outstanding results compared with the HNS re-ported before. The ultra-high strength and excellent elongation are ascribed to the refinedtwin. For50%cold rolled HNS, which exhibits a relatively high strain rate sensitivity (0.04)and low activation volume (6b3). This shows that the deformation of cold-rolled HNS ismainly controlled by the interaction between dislocation and twin.
3) For50%cold-rolled HNS samples after aging treatment from200C to600C for3h, twin gradually disappears and grains become coarse. Aging at800C for3h, the obviousrecrystallization with the formation of equiaxed grains happen, meanwhile, the ferrite andCr2N precipitate. Tensile tests reveal that the yield strength and ultimate tensile strength of50%cold rolled HNS after aging from200C to600C can be improved significantly (0.2=1494-1545MPa, UTS=1834-1974MPa), while the uniform plastic strain has a slightly decrease and then increase (u=6.31-7.85%). The fracture ductility shows a decreasing ten-dency (f=9.04-9.60%). Under800C, the incensement of the strength is due to dislocationpinning caused by small Cr2N and segregation of nitrogen. Apparently decrease of elonga-tion is caused by coared-grain and the elimination of refined twin. At800C, the reduce ofstrength and elongation is caused by the grain boundary precipitation of Cr2N and segrega-tion of nitrogen, which result in embrittlement.
4) Hot rolled HNS samples were prepared by30%,50%and70%rolling at1140C.Warm rolled HNS samples were prepared by50%and70%rolling at400C and600C, re-spectively. Tensile tests reveal that the strength of hot rolled HNS increase with the increaseof strain rate and rolling strain, while the elongation shows a decrease tendency. For warmrolled HNS, with the increase of strain rate, the strength still has an enhancement but theelongation decrese. Elevating the warm rolling temperature is harmful for strength and elon-gation. For hot rolled HNS, refining twin and abundant low-angle boundaries in large rollingstrain are contributed to the enhancement of the strength and the decrease of high-angleboundaries is responsible for the decrease of elongation. For warm rolled HNS, the refinedstructure in large rolling strain is beneficial for the increase of strength and the precipitationof banded ferrite is harmful for the elongation.
5) Nanoindentation tests under different strain rates show that, compared with the solidsolution-treated HNS,70%cold rolled HNS exhibits significant creep deformation. Thecreep strain is related to the microstructure and loading strain rate. The creep strain and ratebecome much higher when the structure is refined and loading strain rate become higher.Creep deformation of70%cold rolled HNS is mainly dominated from the rapidly relaxationof the dislocations structures which generated in the loading regime. The high stability of thedislocation structures generated during loading should be responsible for the creep defor-mation in the solid solution-treated HNS.
本文通过对热成型高氮无镍奥氏体不锈钢原始钢板进行固溶处理，获得固溶态高氮钢；采用冷轧制固溶态高氮钢的方法，得到不同变形量的冷轧态高氮钢；通过时效处理的方法，获得不同微观结构的时效态高氮钢；分别采用400C和600C轧制固溶态高氮钢的方法，得到不同变形量的温轧态高氮钢；通过1140C轧制固溶态高氮钢的方法，获得不同变形量的热轧态高氮钢。使用拉伸实验测试系统和纳米压痕仪进行一系列的力学性能测试。采用X-射线衍射仪、扫描电子显微镜、透射电子显微镜等实验手段，对变形前和变形后的试样进行系统表征，并揭示相关的变形机制。
本文的主要研究结果如下：
1)1150C下固溶处理8h随后水淬可得平均晶粒尺寸为40m、存在大量孪晶的单相固溶态高氮无镍奥氏体不锈钢。拉伸实验显示，随应变速率的增加，屈服强度和抗拉强度增加(0.2=528-712MPa， UTS=957-1004MPa)，均匀应变和断裂应变明显下降(u=44.6-72.2%， f=60.4-87.6%)。流变应力表现出较高的应变速率敏感性，应变速率敏感性和激活体积分别为0.03和17b3，表明变形主要由位错-孪晶相互作用控制。变形表面和断口表面观察揭示，固溶态高氮无镍奥氏体不锈钢较高的强度和非常高的塑性，以及强度和塑性与应变速率的关系与其大量的晶内孪晶结构以及较低层错能导致的位错-孪晶相互作用有关。
2)采用冷轧变形方法获得了变形量为0%-70%的冷轧态高氮无镍奥氏体不锈钢，其显微组织主要为孪晶结构。随轧制变形量的增加，孪晶结构细化，数量增加。拉伸实验发现，随着轧制变形量的增加，屈服强度和抗拉强度增加(0.2=589-1885MPa， UTS=1001-2236MPa)，均匀应变和断裂应变降低(u=5.9-64.1%， f=12.3-86.6%)。70%冷轧态高氮无镍奥氏体不锈钢的综合力学性能(UTS=2236MPa， f=12.3%)是迄今报导的奥氏体不锈钢的最高综合力学性能之一。极高的强度和较高塑性源于其非常细小的孪晶结构。50%冷轧态高氮无镍奥氏体不锈钢的应变速率敏感性和激活体积分别为0.04和6b3，表明其变形主要由位错-孪晶相互作用控制。
3)50%冷轧态高氮无镍奥氏体不锈钢经200至600C时效处理3h后孪晶结构逐渐消失，微观结构粗化；800C时效处理3h后，发生明显的再结晶，形成等轴晶粒结构，析出铁素体和Cr2N相。拉伸实验显示，随时效温度从200C增至600C，时效态高氮无镍奥氏体不锈钢屈服强度和抗拉强度增加(0.2=1494-1545MPa， UTS=1834-1974MPa)，均匀应变先降低后增加(u=6.31-7.85%)，断裂应变趋于降低(f=9.04-9.60%)。800C以下时效态高氮钢强度的增加与析出微细Cr2N相及氮原子的偏聚对位错的钉扎作用有关，塑性明显降低则是由于微观结构的粗化和细小孪晶结构的消失。800C时效时强度和塑性的降低则是由于Cr2N相的晶界析出以及氮原子在晶界上的偏聚产生的晶界脆化作用。
4)采用1140C热轧变形方法获得了变形量分别为30%、50%和70%的热轧态高氮无镍奥氏体不锈钢，采用400C和600C温轧变形方法得到了变形量分别为50%和70%的温轧态高氮无镍奥氏体不锈钢。拉伸实验发现，对于热轧态高氮无镍奥氏体不锈钢，随应变速率的增加，强度增加，塑性呈下降趋势；随轧制变形量的增加，强度增加，塑性下降。对于温轧态高氮无镍奥氏体不锈钢，随轧制变形量的增加，强度增加，但塑性降低；随轧制温度的提高，其强度降低，塑性降低。高轧制变形量的热轧态高氮无镍奥氏体不锈钢较高的强度源于孪晶结构的细化和大量的小角度晶界的增加，塑性的降低源于大角度晶界数量的明显降低。高轧制变形量的温轧态高氮无镍奥氏体不锈钢较高的强度源于结构的细化，塑性的降低源于带状铁素体相的析出。
5)不同加载应变速率下的纳米压痕实验表明，与固溶态高氮无镍奥氏体不锈钢相比，70%冷轧态高氮无镍奥氏体不锈钢保载过程显示明显的蠕变变形。蠕变应变与微观结构和加载应变速率有关。显微组织越细小，加载应变速率越高，保载阶段产生的蠕变应变越大，蠕变速率越高。明显的蠕变变形主要是由于加载阶段存储的高密度位错结构在保载阶段会快速释放，产生明显的蠕变塑性变形。固溶态高氮无镍奥氏体不锈钢加载过程会形成稳定的位错结构，所以不产生明显的蠕变塑性变形。
Austenitic stainless steel has been used widely as one of the most important structuralmaterials nowadays. Compared with the conventional austenitic stainless steels, high nitro-gen austenitic stainless steels possess lots of attractive mechanical properties such as highstrength and ductility, high work hardening ability, excellent corrosion resistance and lowmagnetic susceptibility. The excellent performance above let high nitrogen austenitic stain-less steels become an increasingly important new class of structural materials and exploringgood quality of high nitrogen austenitic stainless steel has been intensive focus in the re-searchers domestically and overseas.So far, the mechanical properties and microstructure ofhigh nitrogen austenitic stainless steel have been intensively studied, however, few attentionhas been paid to the influence of solid solution, cold rolling, warm rolling and hot rolling onthe mechanical properties and microstructure systematically. To study these systematically isconducive to develop a deeper understanding of the plastic deformation and related mecha-nism, which can provide theoretical basis for the reasonable application of high nitrogenaustenitic stainless steel.
In this paper, solid solution-treated high nitrogen nickel-free austenitic stainless steel(HNS) samples were prepared by solution treatment. Cold-rolled HNS samples with differ-ent strains were produced by cold rolling at room temperature. By aging treatment, HNSsamples with different microstructures were produced. By rolling at400C and600C, thewarm-rolled HNS samples with different strains were prepared. By rolling at1140C, thehot-rolled HNS samples with different strains were prepared. The tensile testing system andnanoindentation were used to carry out a series of tests for mechanical properties. The X-raydiffraction, scanning electron microscopy and transmission electron microscopy were usedto characterize the specimens before and after deformation.
The main research results of current study are listed as follows:
1) Solid solution-treated HNS samples with single-phase and abundant intracrystalline twin were produced by solution treatment at1150C for8h and water quenching. The aver-age grain size is40m. Uniaxial tensile tests reveal that, with the increase of strain rate, theyield strength and ultimate tensile strength increase (0.2=528-712MPa, UTS=957-1004MPa) while the uniform plastic strain and tensile fracture strain decrease(u=44.6-72.2%, f=60.4-87.6%). It is noted that flow stress performs a relatively high strain rate sensitivity.The strain rate sensitivity and activation volume are0.03and17b3, respectively. This re-veals that the deformation mode is mainly the interaction between dislocation and twin. Sur-face and fracture of the deformed samples demonstrate that the relatively high strength, ul-tra-high elongation and the relation of strength and elongation with strain rate relate toabundant intracrystalline twin and the interaction between dislocation and twin caused bylow stacking fault energy.
2) Cold rolled HNS samples with0%-70%rolling strain were produced respectively.The main structure of cold rolled HNS is twin. With the increase of rolling strain, the twinrefined and amount increased. Tensile tests reveal that, with the increase of rolling strain, theyield strength and ultimate tensile strength increase (0.2=589-1885MPa, UTS=1001-2236MPa), while the uniform plastic strain and tensile fracture ductility decrease (u=5.9-64.1%,
f=12.3-86.6%). It is noted that the mechanical properties (UTS=2236MPa, f=12.3%)of70%cold rolled HNS have been the most outstanding results compared with the HNS re-ported before. The ultra-high strength and excellent elongation are ascribed to the refinedtwin. For50%cold rolled HNS, which exhibits a relatively high strain rate sensitivity (0.04)and low activation volume (6b3). This shows that the deformation of cold-rolled HNS ismainly controlled by the interaction between dislocation and twin.
3) For50%cold-rolled HNS samples after aging treatment from200C to600C for3h, twin gradually disappears and grains become coarse. Aging at800C for3h, the obviousrecrystallization with the formation of equiaxed grains happen, meanwhile, the ferrite andCr2N precipitate. Tensile tests reveal that the yield strength and ultimate tensile strength of50%cold rolled HNS after aging from200C to600C can be improved significantly (0.2=1494-1545MPa, UTS=1834-1974MPa), while the uniform plastic strain has a slightly decrease and then increase (u=6.31-7.85%). The fracture ductility shows a decreasing ten-dency (f=9.04-9.60%). Under800C, the incensement of the strength is due to dislocationpinning caused by small Cr2N and segregation of nitrogen. Apparently decrease of elonga-tion is caused by coared-grain and the elimination of refined twin. At800C, the reduce ofstrength and elongation is caused by the grain boundary precipitation of Cr2N and segrega-tion of nitrogen, which result in embrittlement.
4) Hot rolled HNS samples were prepared by30%,50%and70%rolling at1140C.Warm rolled HNS samples were prepared by50%and70%rolling at400C and600C, re-spectively. Tensile tests reveal that the strength of hot rolled HNS increase with the increaseof strain rate and rolling strain, while the elongation shows a decrease tendency. For warmrolled HNS, with the increase of strain rate, the strength still has an enhancement but theelongation decrese. Elevating the warm rolling temperature is harmful for strength and elon-gation. For hot rolled HNS, refining twin and abundant low-angle boundaries in large rollingstrain are contributed to the enhancement of the strength and the decrease of high-angleboundaries is responsible for the decrease of elongation. For warm rolled HNS, the refinedstructure in large rolling strain is beneficial for the increase of strength and the precipitationof banded ferrite is harmful for the elongation.
5) Nanoindentation tests under different strain rates show that, compared with the solidsolution-treated HNS,70%cold rolled HNS exhibits significant creep deformation. Thecreep strain is related to the microstructure and loading strain rate. The creep strain and ratebecome much higher when the structure is refined and loading strain rate become higher.Creep deformation of70%cold rolled HNS is mainly dominated from the rapidly relaxationof the dislocations structures which generated in the loading regime. The high stability of thedislocation structures generated during loading should be responsible for the creep defor-mation in the solid solution-treated HNS.
引文
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