含Mn和P元素ULC-BH钢的显微分析和性能研究
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摘要
随着汽车减轻重量和节能减排需求的增大,越来越多的研究集中在如何改善汽车用钢板综合性能上。烘烤硬化(BH)钢作为一种重要的汽车车身用钢长期以来一直是科研和工业领域的研究热点之一。本文结合课题“超低碳含钒烘烤硬化钢的研究”,对经过不同处理尤其是不同退火处理后的BH钢的力学性能和BH性能进行测试;通过热力学计算并结合显微检测,对BH钢热轧、退火和变形过程的显微组织和织构、第二相粒子析出和固溶元素分布进行了分析。讨论了BH钢力学性能、BH性能和成形性能的影响因素,为高性能BH钢的研制提供理论指导。论文的主要研究结果如下:
根据热力学计算结果及相关理论支持设计了三种不同成分的BH钢(BH-0、BH-Mn、BH-P);对一系列经不同退火温度处理的BH钢进行显微硬度测试,确定了BH钢的再结晶温度;通过热膨胀试验测得三种BH钢的A_c1和A_c3温度;在再结晶温度和A_c1温度的退火温度区间内设计了两种不同的退火工艺,工艺1为直接水淬处理,工艺2在工艺1的基础上于冷却过程中增加了过时效过程。
退火工艺对BH钢性能的影响规律为:除n值外,BH钢的其它力学性能受退火温度影响不大,BH-Mn钢的综合力学性能优于其它两种BH钢。过时效过程导致三种BH钢的屈服强度、延伸率明显提高,但使得BH钢的抗拉强度略微降低。过时效过程对三种BH钢的r值的影响规律不同,其中BH-0钢经过过时效处理后r值变化不大,BH-Mn钢的r值明显降低,而BH-P钢的r值明显提高。为解释r值的变化原因,对BH-Mn和BH-P钢不同退火温度下的织构进行了检测。得出BH钢的充分再结晶对于形成有利的γ织构非常重要。当再结晶完成后,退火温度的升高对于BH钢织构的影响作用较弱。通过对BH-0、BH-Mn和BH-P钢经过两种退火工艺处理后的织构研究得出,过时效过程对三种BH钢织构的影响规律不同,显微织构对深冲性能的影响是有利织构和不利织构共同作用的结果。
通过对热轧态BH钢中的析出物类型及固溶元素分布形态的检测分析,得出Mn的添加能够提高MnS的析出温度约300℃。BH-Mn钢中Mn的添加能够形成复杂的含C化合物,这将导致基体中C浓度的降低。另外,BH-Mn钢中大部分碳化钒颗粒的尺寸都是几十纳米,Mn的添加会导致C和V的小至几纳米的团簇形成。在BH-P钢中,大部分碳化钒附着在MnS和TiS颗粒上共同析出而非单独析出,也有很多纳米级的硫化锰颗粒析出,部分硫化锰颗粒与TiS或Ti_4C_2S_2共同析出。P在BH-P钢中未形成沉淀颗粒,而是全部固溶在BH-P钢的基体中,并以偏聚形态存在。在热轧态BH-Mn和BH-P钢中均没有固溶Ti、N或S原子存在。
结合退火后BH钢的3DAP分析和拉伸性能测试结果得出,在BH-P钢中P以明显的偏聚形式存在,并和C发生共同偏聚的现象,从而造成对位错的强烈钉扎,这是导致BH-P钢产生明显屈服平台,即钢板表面质量变差的主要原因。同时,P和C对位错的共同钉扎导致BH-P钢水淬退火后的织构比BH-Mn钢织构弱,r值也比后者低。在BH-Mn钢中由于固溶Mn几乎不产生偏聚,而且固溶C的偏聚也很少,因此BH-Mn钢的屈服强度低于BH-P,塑性则优于后者。
通过对两种不同退火工艺处理后BH-Mn和BH-P钢的显微分析得出,经过时效处理,两BH钢的固溶C浓度降低,而V浓度升高。首次利用3DAP分析得出在过时效过程中没有VC析出,这与本文中的热力学计算结果相吻合。固溶C浓度的降低是由于C扩散至晶界或位错处并钉扎了位错。位错的钉扎是导致过时效后两BH钢屈服强度明显提高的主要原因。在BH-P钢中,P和C的共同偏聚对位错的钉扎是导致其过时效过程织构减弱的主要原因。并且正是由于C的这一扩散过程导致了试验钢的拉伸应力-应变曲线中屈服平台的伸长,即钢板表面质量变差。试验结果还得出预变形量必须大于屈服平台,即完全拖拽开被位错钉扎的柯氏气团才能够获得BH钢的BH现象。一旦预变形量大于屈服平台,两BH钢中的BH值受预变形量的影响不大。
通过对不同预变形量的BH钢的3DAP显微分析及BH性能测试得出,在BH-Mn钢中,C的分布形态随着预变形量的增加变化很小。而在BH-P钢中,随着预变形量的增加,C发生扩散导致更多的C团簇形成以及基体中C浓度的降低。通过基体中固溶元素分布形态以及最大距离法的测量结果得出,C的团簇是由C本身的偏聚以及C与P的共同偏聚形成,而非碳化钒析出。由于BH-P钢中大量固溶C尤其是足量位错的存在,使得BH-P钢不经过预变形直接烘烤后出现高达20MPa的BH值,这与BH-P钢室温拉伸时出现较长的屈服平台结果相吻合。
With the increasing requirement of vehicle weight reduction and energy conservation from automobile industry, the investigation and development of high strength steel sheet has been stressed extensively. BH steel, as an important kind of automotive body steel sheet, has been paied close attention from scientific and industry researcher. In the present work, project“research on ultra low carbon bake hardening steel”is used as research basic, mechanical properties and BH phenomenon is detected in BH steels after different heat treatment and especially different annealing processes; according to thermodynamic calculation and microanalysis results, microstructure, second phase precipitates and solute distributions were analyzed in hot-rolled, annealed and pre-deformed BH steels. The effect factors of mechanical properties, BH phenomenon and formability in BH steel was discussed; this provides theoretical guidance for preparing high performace BH steel. The main research result from the present work is as follows:
Three kinds of BH steels (BH-0, BH-Mn, BH-P) were prepared according to thermodynamic calculation results and related theory; micro hardness in BH steels with different annealing temperatures were tested, the recrystalization temperature of BH steels were thereby determined; Ac1 and Ac3 temperatures were determined according to thermal expansion test result; thermal expansion test result also shows that no martensite phase transformation was happened during annealing process in the three BH steels, that is, the microstructure is exclusive ferrite phase in BH steels after annealing; two different annealing processes were designed in the temperature range between recrystalization and Ac1, annealing process 1 is water quenching, annealing process 2 is added an over time aging stage as compared with process 1.
The effect law of annealing process on mechanical properties of BH steels is as follows: mechanical properties of BH steels were hardly affected by the annealing temperature except for n value; the general property of BH-Mn steel is better than BH-0 and BH-P steels. Over time aging process will induce increase of yield strength and tensile elongation as well as the slight decrease of tensile strength in BH steels. The effect law of over time aging on r value in the three BH steels is completely different, the r value in BH-0 steel changes little after over aging process, while it shows obvious decrease in BH-Mn steel and increase in BH-P steel. In order to explain the r value variation, micro texture in the three BH steels were detected after different annealing temperature and annealing processes. It is obtained that the completeness of recrystalization in BH steels is especially important for goodγtexture. Once after recrystalization, the increase of annealing temperature has slight effect on BH steel texture. According to the results of the three BH steels texture after two annealing processes, the effect law of over time aging on the three BH steels texture is quite different, the effect of texture on deep drawing property is induced by both advantageous and disadvantageous textures.
The addition of Mn will increase MnS precipitation temperature by about 300℃. The addition of Mn in BH steel will induce the formation of complicated compound and decrease the solubility of C. Besides, dimensions of most vanadium carbides are tens of nanometers in BH-Mn steel, addition of Mn induces the clusters of V and C with size of several nanometers in the matrix. In BH-P steel, however, more vanadium carbides precipitate over manganese sulfide and titanium sulfide rather than exist alone. Much nanometer-sized particles of manganese sulfide precipitate in the steel, part of which precipitate together with TiS (or Ti4C2S2). In addition, all P is dissolved in BH-P steel and exists as segregation rather than precipitates as particles. No free Ti, N or S atoms are dissolved in BH-Mn and BH-P steels.
According to 3DAP analysis and tensile test result, P segregates mainly in BH-P steel, and part of P segregates together with C, which strongly pin the dislocations and is the main reason that induces the yield point elongation and the worsening of steel sheet surface quality during tensile process. This also induces the weaker microstructure and lower r value in BH-P steel as compared with BH-Mn steel. In BH-Mn steel, Mn hardly segregates in the matrix and C segregates very little, so the yield strength of BH-Mn steel is lower than that of BH-P steel, whereas the plasticity of it is better than the latter.
According to microanalysis of BH-Mn and BH-P steels with different annealing processes, it is found that C concentration decreases, whereas V increases during over time aging in the two BH steels. It is originally obtained by 3DAP that no vanadium carbide forms during overaging in the BH steels, this is in agreement with the thermodynamic calculation result. The decrease of C concentration is reasonably due to the diffusion of C to grain boundaries and/or dislocations. The pinning of dislocations by C is the key factor that induces the increase of yield strength in the two BH steels during over time aging. The together segregation of C and P is the main factor that induces the worsening of microstructure in BH-P steel during over time aging. This diffusion of C further induces the increase of yield point elongation and the worsening of steel sheet surface quality. Pre-deformation must be higher than the yield point elongation and totally drag away the Cottrell atmosphere formed during the over time aging in order to obtain the BH phenomenon. Results also reveal that once the pre-deformation is more than yield point elongation, BH value in the same BH steel will be affected slightly by the variation of pre-deformation.
Solute distributions in BH steels with different pre-deformations were investigated by 3DAP. BH values of these steels were tested by tensile experiments. Results indicate that C distribution changes little with the increase of pre-deformation in BH-Mn steel. In BH-P steel however, C diffuses during pre-deformation and baking process, which forms more C clusters and induces the decrease of C concentration in the matrix. Distribution patterns and maximum separation distance method results prove that the C cluster is just C segregation or C together with P segregation rather than vanadium carbides precipitate. BH value in BH-P steel without pre-deformation is 20MPa, much higher than that in BH-Mn steel, which is induced by the much solute C and enough dislocations in the BH-P matrix. This is in agreement with the result that there is a long yield point elongation in BH-P steel during tensile test.
根据热力学计算结果及相关理论支持设计了三种不同成分的BH钢(BH-0、BH-Mn、BH-P);对一系列经不同退火温度处理的BH钢进行显微硬度测试,确定了BH钢的再结晶温度;通过热膨胀试验测得三种BH钢的A_c1和A_c3温度;在再结晶温度和A_c1温度的退火温度区间内设计了两种不同的退火工艺,工艺1为直接水淬处理,工艺2在工艺1的基础上于冷却过程中增加了过时效过程。
退火工艺对BH钢性能的影响规律为:除n值外,BH钢的其它力学性能受退火温度影响不大,BH-Mn钢的综合力学性能优于其它两种BH钢。过时效过程导致三种BH钢的屈服强度、延伸率明显提高,但使得BH钢的抗拉强度略微降低。过时效过程对三种BH钢的r值的影响规律不同,其中BH-0钢经过过时效处理后r值变化不大,BH-Mn钢的r值明显降低,而BH-P钢的r值明显提高。为解释r值的变化原因,对BH-Mn和BH-P钢不同退火温度下的织构进行了检测。得出BH钢的充分再结晶对于形成有利的γ织构非常重要。当再结晶完成后,退火温度的升高对于BH钢织构的影响作用较弱。通过对BH-0、BH-Mn和BH-P钢经过两种退火工艺处理后的织构研究得出,过时效过程对三种BH钢织构的影响规律不同,显微织构对深冲性能的影响是有利织构和不利织构共同作用的结果。
通过对热轧态BH钢中的析出物类型及固溶元素分布形态的检测分析,得出Mn的添加能够提高MnS的析出温度约300℃。BH-Mn钢中Mn的添加能够形成复杂的含C化合物,这将导致基体中C浓度的降低。另外,BH-Mn钢中大部分碳化钒颗粒的尺寸都是几十纳米,Mn的添加会导致C和V的小至几纳米的团簇形成。在BH-P钢中,大部分碳化钒附着在MnS和TiS颗粒上共同析出而非单独析出,也有很多纳米级的硫化锰颗粒析出,部分硫化锰颗粒与TiS或Ti_4C_2S_2共同析出。P在BH-P钢中未形成沉淀颗粒,而是全部固溶在BH-P钢的基体中,并以偏聚形态存在。在热轧态BH-Mn和BH-P钢中均没有固溶Ti、N或S原子存在。
结合退火后BH钢的3DAP分析和拉伸性能测试结果得出,在BH-P钢中P以明显的偏聚形式存在,并和C发生共同偏聚的现象,从而造成对位错的强烈钉扎,这是导致BH-P钢产生明显屈服平台,即钢板表面质量变差的主要原因。同时,P和C对位错的共同钉扎导致BH-P钢水淬退火后的织构比BH-Mn钢织构弱,r值也比后者低。在BH-Mn钢中由于固溶Mn几乎不产生偏聚,而且固溶C的偏聚也很少,因此BH-Mn钢的屈服强度低于BH-P,塑性则优于后者。
通过对两种不同退火工艺处理后BH-Mn和BH-P钢的显微分析得出,经过时效处理,两BH钢的固溶C浓度降低,而V浓度升高。首次利用3DAP分析得出在过时效过程中没有VC析出,这与本文中的热力学计算结果相吻合。固溶C浓度的降低是由于C扩散至晶界或位错处并钉扎了位错。位错的钉扎是导致过时效后两BH钢屈服强度明显提高的主要原因。在BH-P钢中,P和C的共同偏聚对位错的钉扎是导致其过时效过程织构减弱的主要原因。并且正是由于C的这一扩散过程导致了试验钢的拉伸应力-应变曲线中屈服平台的伸长,即钢板表面质量变差。试验结果还得出预变形量必须大于屈服平台,即完全拖拽开被位错钉扎的柯氏气团才能够获得BH钢的BH现象。一旦预变形量大于屈服平台,两BH钢中的BH值受预变形量的影响不大。
通过对不同预变形量的BH钢的3DAP显微分析及BH性能测试得出,在BH-Mn钢中,C的分布形态随着预变形量的增加变化很小。而在BH-P钢中,随着预变形量的增加,C发生扩散导致更多的C团簇形成以及基体中C浓度的降低。通过基体中固溶元素分布形态以及最大距离法的测量结果得出,C的团簇是由C本身的偏聚以及C与P的共同偏聚形成,而非碳化钒析出。由于BH-P钢中大量固溶C尤其是足量位错的存在,使得BH-P钢不经过预变形直接烘烤后出现高达20MPa的BH值,这与BH-P钢室温拉伸时出现较长的屈服平台结果相吻合。
With the increasing requirement of vehicle weight reduction and energy conservation from automobile industry, the investigation and development of high strength steel sheet has been stressed extensively. BH steel, as an important kind of automotive body steel sheet, has been paied close attention from scientific and industry researcher. In the present work, project“research on ultra low carbon bake hardening steel”is used as research basic, mechanical properties and BH phenomenon is detected in BH steels after different heat treatment and especially different annealing processes; according to thermodynamic calculation and microanalysis results, microstructure, second phase precipitates and solute distributions were analyzed in hot-rolled, annealed and pre-deformed BH steels. The effect factors of mechanical properties, BH phenomenon and formability in BH steel was discussed; this provides theoretical guidance for preparing high performace BH steel. The main research result from the present work is as follows:
Three kinds of BH steels (BH-0, BH-Mn, BH-P) were prepared according to thermodynamic calculation results and related theory; micro hardness in BH steels with different annealing temperatures were tested, the recrystalization temperature of BH steels were thereby determined; Ac1 and Ac3 temperatures were determined according to thermal expansion test result; thermal expansion test result also shows that no martensite phase transformation was happened during annealing process in the three BH steels, that is, the microstructure is exclusive ferrite phase in BH steels after annealing; two different annealing processes were designed in the temperature range between recrystalization and Ac1, annealing process 1 is water quenching, annealing process 2 is added an over time aging stage as compared with process 1.
The effect law of annealing process on mechanical properties of BH steels is as follows: mechanical properties of BH steels were hardly affected by the annealing temperature except for n value; the general property of BH-Mn steel is better than BH-0 and BH-P steels. Over time aging process will induce increase of yield strength and tensile elongation as well as the slight decrease of tensile strength in BH steels. The effect law of over time aging on r value in the three BH steels is completely different, the r value in BH-0 steel changes little after over aging process, while it shows obvious decrease in BH-Mn steel and increase in BH-P steel. In order to explain the r value variation, micro texture in the three BH steels were detected after different annealing temperature and annealing processes. It is obtained that the completeness of recrystalization in BH steels is especially important for goodγtexture. Once after recrystalization, the increase of annealing temperature has slight effect on BH steel texture. According to the results of the three BH steels texture after two annealing processes, the effect law of over time aging on the three BH steels texture is quite different, the effect of texture on deep drawing property is induced by both advantageous and disadvantageous textures.
The addition of Mn will increase MnS precipitation temperature by about 300℃. The addition of Mn in BH steel will induce the formation of complicated compound and decrease the solubility of C. Besides, dimensions of most vanadium carbides are tens of nanometers in BH-Mn steel, addition of Mn induces the clusters of V and C with size of several nanometers in the matrix. In BH-P steel, however, more vanadium carbides precipitate over manganese sulfide and titanium sulfide rather than exist alone. Much nanometer-sized particles of manganese sulfide precipitate in the steel, part of which precipitate together with TiS (or Ti4C2S2). In addition, all P is dissolved in BH-P steel and exists as segregation rather than precipitates as particles. No free Ti, N or S atoms are dissolved in BH-Mn and BH-P steels.
According to 3DAP analysis and tensile test result, P segregates mainly in BH-P steel, and part of P segregates together with C, which strongly pin the dislocations and is the main reason that induces the yield point elongation and the worsening of steel sheet surface quality during tensile process. This also induces the weaker microstructure and lower r value in BH-P steel as compared with BH-Mn steel. In BH-Mn steel, Mn hardly segregates in the matrix and C segregates very little, so the yield strength of BH-Mn steel is lower than that of BH-P steel, whereas the plasticity of it is better than the latter.
According to microanalysis of BH-Mn and BH-P steels with different annealing processes, it is found that C concentration decreases, whereas V increases during over time aging in the two BH steels. It is originally obtained by 3DAP that no vanadium carbide forms during overaging in the BH steels, this is in agreement with the thermodynamic calculation result. The decrease of C concentration is reasonably due to the diffusion of C to grain boundaries and/or dislocations. The pinning of dislocations by C is the key factor that induces the increase of yield strength in the two BH steels during over time aging. The together segregation of C and P is the main factor that induces the worsening of microstructure in BH-P steel during over time aging. This diffusion of C further induces the increase of yield point elongation and the worsening of steel sheet surface quality. Pre-deformation must be higher than the yield point elongation and totally drag away the Cottrell atmosphere formed during the over time aging in order to obtain the BH phenomenon. Results also reveal that once the pre-deformation is more than yield point elongation, BH value in the same BH steel will be affected slightly by the variation of pre-deformation.
Solute distributions in BH steels with different pre-deformations were investigated by 3DAP. BH values of these steels were tested by tensile experiments. Results indicate that C distribution changes little with the increase of pre-deformation in BH-Mn steel. In BH-P steel however, C diffuses during pre-deformation and baking process, which forms more C clusters and induces the decrease of C concentration in the matrix. Distribution patterns and maximum separation distance method results prove that the C cluster is just C segregation or C together with P segregation rather than vanadium carbides precipitate. BH value in BH-P steel without pre-deformation is 20MPa, much higher than that in BH-Mn steel, which is induced by the much solute C and enough dislocations in the BH-P matrix. This is in agreement with the result that there is a long yield point elongation in BH-P steel during tensile test.
引文
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