新型高Cr铁素体耐热钢的相变行为研究
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摘要
高Cr铁素体耐热钢具备优异的高温持久性能和蠕变性能、良好的热导率、低热膨胀系数和较高的性能价格比,因此已广泛用于先进火力发电站机组中的高温部件(如主蒸汽管道、过热器和再热器管道等)。此外,由于高Cr铁素体耐热钢具有出色的抗辐照性能,其还是核电站结构部件的候选材料。随着能源短缺和环境污染等问题的日益突出,提高高Cr铁素体耐热钢的耐热温度以及提高电厂热效率的研究势在必行。
作为高Cr铁素体耐热钢的代表钢种,T91钢已广泛用于火力发电站的耐热材料之中,并且已经成为开发满足更高温度要求的新型高Cr铁素体耐热钢的研究标准。基于本课题组前期对T91钢相变及强化工艺的研究,以及组织强化机理和合金化原理,开发了四种新型高Cr铁素体耐热钢。并针对新型高Cr铁素体耐热钢进行了显微组织分析和力学性能测试,以确定其是否具备优越的热强性和热稳定性,是否可成为650 oC用耐热钢的候选。为更深入的研究其相变过程和机理,组织形成与演化规律,以及探索控轧控冷的新工艺,采用高精度差分膨胀测量以及显微硬度测试等试验手段,对新型高Cr铁素体耐热钢的加热、冷却、保温及回火阶段的相变行为进行了系统研究。并在此基础上针对各阶段的相变动力学建立了相应的动力学模型。得出结论如下:
(1)对自行研发的新型高Cr铁素体耐热钢进行了组织分析和力学性能测试。新型高Cr铁素体耐热钢的正火组织主要由高密度位错的马氏体板条和少量的δ-铁素体组成。回火后组织中析出大量晶内和晶界沉淀,此外位错密度有所降低,板条呈现变宽的趋势。新型高Cr铁素体耐热钢最佳热处理工艺为:1100 oC正火+750 oC回火;与传统高Cr铁素体耐热钢(如T91钢和T92钢等)相比,新型高Cr铁素体耐热钢热处理后其拉伸及屈服强度显著提高,具有更高的回火抗力,在高温回火条件下其回复及再结晶趋势更为缓慢。
(2)对新型高Cr铁素体耐热钢的连续加热过程中奥氏体相变行为及动力学进行了研究。不同的加热速率会显著影响新型高Cr铁素体耐热钢的奥氏体相变开始温度A_(c1)和结束温度A_(c3),加热速率越快,A_(c1)和A_(c3)越高,奥氏体相变被推迟到更高的温度。提高加热速度导致合金元素扩散速率的增加,从而加快了扩散控制生长的奥氏体相变的速率,缩短了相变所需时间。对连续加热过程中的奥氏体相变过程进行了基于JMAK模型的动力学建模,该模型采用位置饱和形核、扩散控制生长的相变方式,能较为精确的描述新型高Cr铁素体耐热钢的奥氏体相变行为,模型的数值拟合精度和各动力学参数的物理意义都能较好的符合实际的相变过程。随着加热速率的升高,由于奥氏体相变时间的缩短,合金元素的溶解不充分,导致奥氏体相变过程的扩散激活能Qd_由130.1kJ/mol逐渐降低为79.0 kJ/mol,相变完成之后,合金元素继续进行溶解,导致了热膨胀曲线的偏离。
(3)对T91钢和新型高Cr铁素体耐热钢奥氏体之后的冷却阶段的相变进行了系统研究,在此基础上建立了马氏体相变动力学模型,并推广到应变诱发马氏体相变的动力学研究。T91钢在奥氏体化之后的空冷过程中会析出针状M_3C沉淀相,而水冷则会抑制M_3C相的析出,而且M_3C相的析出发生于马氏体相变之前的亚稳奥氏体中,并导致了马氏体相变的分裂行为。高冷速同样抑制了新型高Cr铁素体耐热钢组织中M_3C相的析出,随着冷速的提高,组织内淬火空位和位错密度也增加,导致M_s点稍微上升,正是由于缺陷的增加提高了母相的强度,从而减缓了由切变主导的马氏体相变的长大速率。在Koistinen-Marburger模型的基础上提出了适用于新型高Cr铁素体耐热钢的马氏体相变动力学模型,对其非热激活马氏体相变特征进行了描述,模型分析表明,冷速的增加略微提高了马氏体相变的形核率,明显阻碍了马氏体相界面的移动速率,从而导致相变速率的降低。对预应力加载下的新型高Cr铁素体耐热钢的应变诱发马氏体相变进行了显微组织和相变行为研究,并建立了相变动力学模型,研究表明,预应力的存在导致了晶粒的破碎和马氏体板条的细化,通过增加晶内缺陷的方式提高了形核率,导致M_s点的提高,同时还通过对母相的强化降低了马氏体长大的界面移动速率,造成了相变速率的降低,进而导致相变时间的延长。
(4)对新型高Cr铁素体耐热钢冷却阶段的等温停留过程进行了显微组织和相变行为研究,并建立了相应的贝氏体相变模型。在550℃或400℃的等温停留导致了贝氏体相变的发生,而且等温温度越低,生成的贝氏体数量也越多,由于贝氏体的生成,导致奥氏体热稳定化现象消失,随后马氏体相变的开始温度不降反升。650℃等温的试样中没有贝氏体相变的发生,但由于原奥氏体晶界处的碳化物沉淀相的析出,同样造成了奥氏体热稳定化现象的消失。对不同等温温度的贝氏体相变过程进行了动力学建模,证明其完全符合自催化形核的不完全贝氏体相变切变机制,其模型的数值拟合精度和所确定的动力学参数均能较好的符合实际相变过程。根据建立的动力学模型可知,等温贝氏体相变的临界温度为687.5℃,低于此温度才能发生贝氏体相变,而且等温温度越低,则相变驱动力越大,生成的贝氏体越多。等温温度越低,自催化形核的数量更多,且形核激活能越低,则相变速率越大。
(5)通过显微组织观察及相变行为分析,对T91钢和新型高Cr铁素体耐热钢回火阶段的组织演化和沉淀析出规律进行了系统研究。冷却过程中析出的M_3C沉淀相会对T91钢的早期回火行为造成影响,在回火之前如果组织中存在M_3C沉淀相,会导致M_(23)C_6沉淀相的颗粒尺寸更小,且数量密度更大,且M_(23)C_6沉淀相更倾向晶内析出,但是随着回火时间的延长,M_3C沉淀相的存在对M_(23)C_6相沉淀析出的影响逐渐变得不明显。T91钢的二次回火能够细化马氏体板条组织,并增加沉淀相颗粒的数量密度以及减少其尺寸,这是因为,在一次回火阶段,析出的少量沉淀相颗粒对板条和位错造成有效钉扎,在二次回火阶段,沉淀得以充分析出,而板条宽度和位错密度依然能维持在较为理想的水平。对新型高Cr铁素体耐热钢的回火动力学研究表明,非均匀形核的M_(23)C_6沉淀相的形核位置会随着沉淀相颗粒密度的增加而减少,导致其形核率随时间而衰减,回火前期M_(23)C_6沉淀相的长大符合Zenner扩散生长模型,其长大速率与溶质原子的扩散系数相关,而随着回火的继续进行,基体中溶质浓度不断下降,导致M_(23)C_6沉淀相的长大速率明显放缓,此外,回火阶段马氏体板条的迁移速率由晶界处原子的热激活扩散所控制,随着回火时间的延长,板条宽度不断增加;对新型高Cr铁素体耐热钢应变诱发马氏体的回火过程的研究表明,应力加载后的回火试样的板条宽度更小,应力加载还导致了在回火阶段亚晶粒的出现,这是因为残余应变能的存在导致系统自由能的增加,以及回复激活能的降低,从而引起板条回复的提前出现,此外,应力加载后的回火试样组织内的沉淀相颗粒的尺寸更细小,且数量密度更高,这是由于缺陷的增加导致形核场所的增多,从而提高了第二相颗粒的形核率。
High Cr ferritic heat-resistant steels are being considered as an attractive candidate material for high-temperature structural components such as main steam pipe, superheater tube and resuperheater tube in advanced power plants due to the good high-temperature endurance, creep resistance properties, excellent heat conductivity, low thermal expansion coefficient and high performance-cost ratio. Additionally, they are also the potential candidate for structural steel in nuclear reactors because of its outstanding irradiation resistance. Furthermore,under the pressure of energy shortage and environment pollution, the study on elevating the thermal efficiency of generating station and endure temperature of the boiler tube materials is also imperative.
T91 steel is the representative of high Cr ferritic heat-resistant steels, which has been widely used as power plants materials, and regarded as research benchmark for the development of new ferritic heat-resistant steels with higher application temperature. Based on the previous research on phase transformations and strengthening processes of T91 steel by our group, and strengthening mechanism and alloying principle, four types of the modified high Cr ferritic heat-resistant steels have been developed. The microstructural analysis and mechanical properties testing has been also carried out to evaluate whether they have the superiorperformances for the 650℃grade power plant. Furthermore, to clarify the phase transformation process and mechanism, microstructural evolution and explore the controlled rolling and cooling process of the modified high Cr ferritic heat-resistant steels, the transformation behaviors during continuous heating and cooling, isothermal holding and tempering process were systematically investigated by means of microstructural observation, high-resolution differential dilatometric measurements, micro hardness testing and so on. On this basis, the models for phase transformation kinetics were developed to analyze the transformation behaviors. Results as following:
(1) Microstructural analysis and mechanical properties testing of the modified high Cr ferritic heat-resistant steels was carried out. The normalized microstructure of the modified high Cr ferritic heat-resistant steels is composed of martensitic laths with high density dislocation, and a small quantity ofδ-ferrite. During tempering, the precipitates form on the boundary and inside of grain, the density of dislocation decreases and the width of martensitic lath increases. The optimal parameter of heat treatment of the modified high Cr ferritic heat-resistant steels is normalizing at 1100℃+ tempering at 750℃. The results of mechanical properties testing suggest that, the tensile and yield strength of the modified high Cr ferritic heat-resistant steels is remarkably higher than that of the conventional high Cr ferritic heat-resistant steels as T91 and T92 steels. The experiment of resistance to tempering indicates that the modified high Cr ferritic heat-resistant steels, the rate of recovery and recrystallization of which is slow, possess the more excellent resistance to tempering than the conventional high Cr ferritic heat-resistant steels.
(2) The austenitic transformation behaviors and kinetics of the modified high Cr ferritic heat-resistant steel during continuous heating were studied. Variation of heating rates affects the austenitic transformation starting temperature, A_(c1), and finishing temperature, A_(c3). Both A_(c1) and A_(c3) increase as the heating rate applied is raised, which means that austenitic transformation is retarded to the higher temperature. The increase of heating rate results in the increase of diffusion rate, and thus promotes the diffusion-controlled austenitic transformation and shortens the transformation time. Based on the JMAK model, the isochronal austenitic transformation of the modified high Cr ferritic heat-resistant steel during continuous heating was described well by a phase-transformation model involving site saturation and diffusion-controlled growth. The precision and physical significance of the fitted kinetics parameters agree well with the actual austenitic phase transformation process. The increase of heating rate results in the contraction of austenitic transformation time and the incompletion of dissolution of alloying elements. Hence, the activation energy for diffusion during austenitic transformation decreases from 130.1 kJ/mol to 79.0 kJ/mol, while the heating rate increases from 10℃/min to 3000℃/min. After the accomplishment of austenitic transformation, the alloy elements continue to dissolve, which results in the deviation of thermal expansive curve.
(3) Phase transformation during continuous cooling after austenization, of T91 steel and the modified high Cr ferritic heat-resistant steel, was investigated systematically. The model for isochronal martensitic transformation kinetics of the modified high Cr ferritic heat-resistant steel was developed, and extended to strain-induced martensitic transformation kinetics. In T91 steel, the needle-liked M_3C precipitates generate during air cooling after austenization, while water cooling suppresses the formation of the M_3C phase. Furthermore, it was found that, precipitation of the M_3C phase takes place in metastable austenite, before martensitic transformation, and thus leads to the splitting phenomena of the martensitic transformation. In the modified high Cr ferritic heat-resistant steel, high cooling rate also blocks the precipitation of M_3C particles. With the increase of cooling rate, the number of quenching vacancy and density of dislocation increases, resulting in the slighte levation of M_s. Yet, the increase of defection density improves strength of the parent phase, and thus slows down the growth rate of shear dominant martensitic transformation. The model for martensitic transformation in the modified high Cr ferritic heat-resistant steel was developed base on the classical Koistinen-Marburger model. The present model describes the feature of athermal martensitic transformation well. The analysis of the model suggests that, increase of cooling rate slightly causes the slight increase of nucleation rate for martensitic transformation and remarkable decrease of interfacial migration rate for martensitic growth, namely retarding the progress of martensitic transformation. The pre-stress loading leads to the broken grains and narrow martensitic laths, and raises M_s due to the increase of defection density. Besides, pre-stress loading also decreases the interfacial migration rate for martensitic growth by means of strengthen the parent phase, and thus results in decrease of transformation rate and elongation of transformation time.
(4) Isothermal holding during cooling after austenization in the modified high Cr ferritic heat-resistant steel was studied by microstructural analysis and transformation behavior research. Furthermore, the model for bainitic transformation kinetics was developed. Isothermal holding at 550℃or 400℃results in the occurrence of bainitic transformation. The decrease of holding temperature promotes the bainitic transformation. The production of bainite causes the disappearance of thermal stabilization of austenite, namely the increase of M_s. Bainite is not observed in the sample after isothermal holding at 650℃. Nevertheless, thermal stabilization of austenite also does not occur because of the precipitation of carbide at the prior austenitic grain boundary. The isothermal bainitic transformation of the modified high Cr ferritic heat-resistant steel during isothermal holding was described well by an incomplete displacive bainitic transformation model in view of autocatalytic nucleation. The precision and physical significance of the fitted kinetics parameters agree well with the actual bainitic phase transformation process. According to the present model, the critical temperature for isothermal bainitic transformation is 687.5℃. With the decrease of isothermal temperature, the driving force of bainitic transformation and the amount of bainite increases. Reduction of holding temperature promotes to bainite transformation by means of increase of number of embryos for autocatalytic nucleation and decrease of activation energy.
(5) Microstructural evolution and precipitation of the second phase during tempering in T91 steel and the modified high Cr ferritic heat-resistant steel were investigated by microstructural and kinetic analysis. The M_3C precipitates formed during air cooling affect the early-stage tempering in T91 steel. The existence of the M_3C phase results in that the M_(23)C_6 particles become finer and denser, and intend to be precipitated within the grains. However, with the elongation of tempering time, the influence of the M_3C phase on precipitation of the M_(23)C_6 phase becomes not remarkable. The two-step tempering treatment leads to more precipitates, higher dislocation density and smaller martensitic lath width than that obtained from the traditional tempering process. This is because that, the firstly tempering at a low temperature forms some precipitates, which would pin the dislocation and martensitic lath, and the subsequent secondly tempering at a high temperature complete the precipitation of particles while the recovery of lath and dislocation remain a low level as before. The investigation of tempering kinetics in the modified high Cr ferritic heat-resistant steel indicates that, the heterogeneous nucleation sites of the M_(23)C_6 particles decrease with the increase of number density of precipitates, which leads to the decrease of nucleation rate. At the early stage of tempering, the growth of the M_(23)C_6 particles accords with the diffusion-controlled model developed by Zenner. The growth rate of the M_(23)C_6 phase is related to diffusion coefficient of the solute atoms. With the process of tempering, solute concentration in matrix declines, leading to the decrease of growth rate of the M_(23)C_6 phaes. Furthermore, the migration rate of martensitic lath is controlled by thermally activated diffusion of the atoms at the grain boundary. With the elongation of tempering time, the width of martensitic lath increases. The research on the tempering of strain-induced martensite in the modified high Cr ferritic heat-resistant steel suggests that, in the sample after tempering, pre-stress loading results in the reduction of width of martensitic lath, and formation of sub-grain. This is because that, existence of residual strain energy increases the system free energy and lowers the activation energy for recovery, so the phenomenon of recovery appears in advance. Besides, pre-stress loading also decreases the size of precipitates, and increases the number density of that. This is ascribed to that increase of defection results in the increase of nucleation sites, and thus improves the nucleation rate of the precipitates.
作为高Cr铁素体耐热钢的代表钢种,T91钢已广泛用于火力发电站的耐热材料之中,并且已经成为开发满足更高温度要求的新型高Cr铁素体耐热钢的研究标准。基于本课题组前期对T91钢相变及强化工艺的研究,以及组织强化机理和合金化原理,开发了四种新型高Cr铁素体耐热钢。并针对新型高Cr铁素体耐热钢进行了显微组织分析和力学性能测试,以确定其是否具备优越的热强性和热稳定性,是否可成为650 oC用耐热钢的候选。为更深入的研究其相变过程和机理,组织形成与演化规律,以及探索控轧控冷的新工艺,采用高精度差分膨胀测量以及显微硬度测试等试验手段,对新型高Cr铁素体耐热钢的加热、冷却、保温及回火阶段的相变行为进行了系统研究。并在此基础上针对各阶段的相变动力学建立了相应的动力学模型。得出结论如下:
(1)对自行研发的新型高Cr铁素体耐热钢进行了组织分析和力学性能测试。新型高Cr铁素体耐热钢的正火组织主要由高密度位错的马氏体板条和少量的δ-铁素体组成。回火后组织中析出大量晶内和晶界沉淀,此外位错密度有所降低,板条呈现变宽的趋势。新型高Cr铁素体耐热钢最佳热处理工艺为:1100 oC正火+750 oC回火;与传统高Cr铁素体耐热钢(如T91钢和T92钢等)相比,新型高Cr铁素体耐热钢热处理后其拉伸及屈服强度显著提高,具有更高的回火抗力,在高温回火条件下其回复及再结晶趋势更为缓慢。
(2)对新型高Cr铁素体耐热钢的连续加热过程中奥氏体相变行为及动力学进行了研究。不同的加热速率会显著影响新型高Cr铁素体耐热钢的奥氏体相变开始温度A_(c1)和结束温度A_(c3),加热速率越快,A_(c1)和A_(c3)越高,奥氏体相变被推迟到更高的温度。提高加热速度导致合金元素扩散速率的增加,从而加快了扩散控制生长的奥氏体相变的速率,缩短了相变所需时间。对连续加热过程中的奥氏体相变过程进行了基于JMAK模型的动力学建模,该模型采用位置饱和形核、扩散控制生长的相变方式,能较为精确的描述新型高Cr铁素体耐热钢的奥氏体相变行为,模型的数值拟合精度和各动力学参数的物理意义都能较好的符合实际的相变过程。随着加热速率的升高,由于奥氏体相变时间的缩短,合金元素的溶解不充分,导致奥氏体相变过程的扩散激活能Qd_由130.1kJ/mol逐渐降低为79.0 kJ/mol,相变完成之后,合金元素继续进行溶解,导致了热膨胀曲线的偏离。
(3)对T91钢和新型高Cr铁素体耐热钢奥氏体之后的冷却阶段的相变进行了系统研究,在此基础上建立了马氏体相变动力学模型,并推广到应变诱发马氏体相变的动力学研究。T91钢在奥氏体化之后的空冷过程中会析出针状M_3C沉淀相,而水冷则会抑制M_3C相的析出,而且M_3C相的析出发生于马氏体相变之前的亚稳奥氏体中,并导致了马氏体相变的分裂行为。高冷速同样抑制了新型高Cr铁素体耐热钢组织中M_3C相的析出,随着冷速的提高,组织内淬火空位和位错密度也增加,导致M_s点稍微上升,正是由于缺陷的增加提高了母相的强度,从而减缓了由切变主导的马氏体相变的长大速率。在Koistinen-Marburger模型的基础上提出了适用于新型高Cr铁素体耐热钢的马氏体相变动力学模型,对其非热激活马氏体相变特征进行了描述,模型分析表明,冷速的增加略微提高了马氏体相变的形核率,明显阻碍了马氏体相界面的移动速率,从而导致相变速率的降低。对预应力加载下的新型高Cr铁素体耐热钢的应变诱发马氏体相变进行了显微组织和相变行为研究,并建立了相变动力学模型,研究表明,预应力的存在导致了晶粒的破碎和马氏体板条的细化,通过增加晶内缺陷的方式提高了形核率,导致M_s点的提高,同时还通过对母相的强化降低了马氏体长大的界面移动速率,造成了相变速率的降低,进而导致相变时间的延长。
(4)对新型高Cr铁素体耐热钢冷却阶段的等温停留过程进行了显微组织和相变行为研究,并建立了相应的贝氏体相变模型。在550℃或400℃的等温停留导致了贝氏体相变的发生,而且等温温度越低,生成的贝氏体数量也越多,由于贝氏体的生成,导致奥氏体热稳定化现象消失,随后马氏体相变的开始温度不降反升。650℃等温的试样中没有贝氏体相变的发生,但由于原奥氏体晶界处的碳化物沉淀相的析出,同样造成了奥氏体热稳定化现象的消失。对不同等温温度的贝氏体相变过程进行了动力学建模,证明其完全符合自催化形核的不完全贝氏体相变切变机制,其模型的数值拟合精度和所确定的动力学参数均能较好的符合实际相变过程。根据建立的动力学模型可知,等温贝氏体相变的临界温度为687.5℃,低于此温度才能发生贝氏体相变,而且等温温度越低,则相变驱动力越大,生成的贝氏体越多。等温温度越低,自催化形核的数量更多,且形核激活能越低,则相变速率越大。
(5)通过显微组织观察及相变行为分析,对T91钢和新型高Cr铁素体耐热钢回火阶段的组织演化和沉淀析出规律进行了系统研究。冷却过程中析出的M_3C沉淀相会对T91钢的早期回火行为造成影响,在回火之前如果组织中存在M_3C沉淀相,会导致M_(23)C_6沉淀相的颗粒尺寸更小,且数量密度更大,且M_(23)C_6沉淀相更倾向晶内析出,但是随着回火时间的延长,M_3C沉淀相的存在对M_(23)C_6相沉淀析出的影响逐渐变得不明显。T91钢的二次回火能够细化马氏体板条组织,并增加沉淀相颗粒的数量密度以及减少其尺寸,这是因为,在一次回火阶段,析出的少量沉淀相颗粒对板条和位错造成有效钉扎,在二次回火阶段,沉淀得以充分析出,而板条宽度和位错密度依然能维持在较为理想的水平。对新型高Cr铁素体耐热钢的回火动力学研究表明,非均匀形核的M_(23)C_6沉淀相的形核位置会随着沉淀相颗粒密度的增加而减少,导致其形核率随时间而衰减,回火前期M_(23)C_6沉淀相的长大符合Zenner扩散生长模型,其长大速率与溶质原子的扩散系数相关,而随着回火的继续进行,基体中溶质浓度不断下降,导致M_(23)C_6沉淀相的长大速率明显放缓,此外,回火阶段马氏体板条的迁移速率由晶界处原子的热激活扩散所控制,随着回火时间的延长,板条宽度不断增加;对新型高Cr铁素体耐热钢应变诱发马氏体的回火过程的研究表明,应力加载后的回火试样的板条宽度更小,应力加载还导致了在回火阶段亚晶粒的出现,这是因为残余应变能的存在导致系统自由能的增加,以及回复激活能的降低,从而引起板条回复的提前出现,此外,应力加载后的回火试样组织内的沉淀相颗粒的尺寸更细小,且数量密度更高,这是由于缺陷的增加导致形核场所的增多,从而提高了第二相颗粒的形核率。
High Cr ferritic heat-resistant steels are being considered as an attractive candidate material for high-temperature structural components such as main steam pipe, superheater tube and resuperheater tube in advanced power plants due to the good high-temperature endurance, creep resistance properties, excellent heat conductivity, low thermal expansion coefficient and high performance-cost ratio. Additionally, they are also the potential candidate for structural steel in nuclear reactors because of its outstanding irradiation resistance. Furthermore,under the pressure of energy shortage and environment pollution, the study on elevating the thermal efficiency of generating station and endure temperature of the boiler tube materials is also imperative.
T91 steel is the representative of high Cr ferritic heat-resistant steels, which has been widely used as power plants materials, and regarded as research benchmark for the development of new ferritic heat-resistant steels with higher application temperature. Based on the previous research on phase transformations and strengthening processes of T91 steel by our group, and strengthening mechanism and alloying principle, four types of the modified high Cr ferritic heat-resistant steels have been developed. The microstructural analysis and mechanical properties testing has been also carried out to evaluate whether they have the superiorperformances for the 650℃grade power plant. Furthermore, to clarify the phase transformation process and mechanism, microstructural evolution and explore the controlled rolling and cooling process of the modified high Cr ferritic heat-resistant steels, the transformation behaviors during continuous heating and cooling, isothermal holding and tempering process were systematically investigated by means of microstructural observation, high-resolution differential dilatometric measurements, micro hardness testing and so on. On this basis, the models for phase transformation kinetics were developed to analyze the transformation behaviors. Results as following:
(1) Microstructural analysis and mechanical properties testing of the modified high Cr ferritic heat-resistant steels was carried out. The normalized microstructure of the modified high Cr ferritic heat-resistant steels is composed of martensitic laths with high density dislocation, and a small quantity ofδ-ferrite. During tempering, the precipitates form on the boundary and inside of grain, the density of dislocation decreases and the width of martensitic lath increases. The optimal parameter of heat treatment of the modified high Cr ferritic heat-resistant steels is normalizing at 1100℃+ tempering at 750℃. The results of mechanical properties testing suggest that, the tensile and yield strength of the modified high Cr ferritic heat-resistant steels is remarkably higher than that of the conventional high Cr ferritic heat-resistant steels as T91 and T92 steels. The experiment of resistance to tempering indicates that the modified high Cr ferritic heat-resistant steels, the rate of recovery and recrystallization of which is slow, possess the more excellent resistance to tempering than the conventional high Cr ferritic heat-resistant steels.
(2) The austenitic transformation behaviors and kinetics of the modified high Cr ferritic heat-resistant steel during continuous heating were studied. Variation of heating rates affects the austenitic transformation starting temperature, A_(c1), and finishing temperature, A_(c3). Both A_(c1) and A_(c3) increase as the heating rate applied is raised, which means that austenitic transformation is retarded to the higher temperature. The increase of heating rate results in the increase of diffusion rate, and thus promotes the diffusion-controlled austenitic transformation and shortens the transformation time. Based on the JMAK model, the isochronal austenitic transformation of the modified high Cr ferritic heat-resistant steel during continuous heating was described well by a phase-transformation model involving site saturation and diffusion-controlled growth. The precision and physical significance of the fitted kinetics parameters agree well with the actual austenitic phase transformation process. The increase of heating rate results in the contraction of austenitic transformation time and the incompletion of dissolution of alloying elements. Hence, the activation energy for diffusion during austenitic transformation decreases from 130.1 kJ/mol to 79.0 kJ/mol, while the heating rate increases from 10℃/min to 3000℃/min. After the accomplishment of austenitic transformation, the alloy elements continue to dissolve, which results in the deviation of thermal expansive curve.
(3) Phase transformation during continuous cooling after austenization, of T91 steel and the modified high Cr ferritic heat-resistant steel, was investigated systematically. The model for isochronal martensitic transformation kinetics of the modified high Cr ferritic heat-resistant steel was developed, and extended to strain-induced martensitic transformation kinetics. In T91 steel, the needle-liked M_3C precipitates generate during air cooling after austenization, while water cooling suppresses the formation of the M_3C phase. Furthermore, it was found that, precipitation of the M_3C phase takes place in metastable austenite, before martensitic transformation, and thus leads to the splitting phenomena of the martensitic transformation. In the modified high Cr ferritic heat-resistant steel, high cooling rate also blocks the precipitation of M_3C particles. With the increase of cooling rate, the number of quenching vacancy and density of dislocation increases, resulting in the slighte levation of M_s. Yet, the increase of defection density improves strength of the parent phase, and thus slows down the growth rate of shear dominant martensitic transformation. The model for martensitic transformation in the modified high Cr ferritic heat-resistant steel was developed base on the classical Koistinen-Marburger model. The present model describes the feature of athermal martensitic transformation well. The analysis of the model suggests that, increase of cooling rate slightly causes the slight increase of nucleation rate for martensitic transformation and remarkable decrease of interfacial migration rate for martensitic growth, namely retarding the progress of martensitic transformation. The pre-stress loading leads to the broken grains and narrow martensitic laths, and raises M_s due to the increase of defection density. Besides, pre-stress loading also decreases the interfacial migration rate for martensitic growth by means of strengthen the parent phase, and thus results in decrease of transformation rate and elongation of transformation time.
(4) Isothermal holding during cooling after austenization in the modified high Cr ferritic heat-resistant steel was studied by microstructural analysis and transformation behavior research. Furthermore, the model for bainitic transformation kinetics was developed. Isothermal holding at 550℃or 400℃results in the occurrence of bainitic transformation. The decrease of holding temperature promotes the bainitic transformation. The production of bainite causes the disappearance of thermal stabilization of austenite, namely the increase of M_s. Bainite is not observed in the sample after isothermal holding at 650℃. Nevertheless, thermal stabilization of austenite also does not occur because of the precipitation of carbide at the prior austenitic grain boundary. The isothermal bainitic transformation of the modified high Cr ferritic heat-resistant steel during isothermal holding was described well by an incomplete displacive bainitic transformation model in view of autocatalytic nucleation. The precision and physical significance of the fitted kinetics parameters agree well with the actual bainitic phase transformation process. According to the present model, the critical temperature for isothermal bainitic transformation is 687.5℃. With the decrease of isothermal temperature, the driving force of bainitic transformation and the amount of bainite increases. Reduction of holding temperature promotes to bainite transformation by means of increase of number of embryos for autocatalytic nucleation and decrease of activation energy.
(5) Microstructural evolution and precipitation of the second phase during tempering in T91 steel and the modified high Cr ferritic heat-resistant steel were investigated by microstructural and kinetic analysis. The M_3C precipitates formed during air cooling affect the early-stage tempering in T91 steel. The existence of the M_3C phase results in that the M_(23)C_6 particles become finer and denser, and intend to be precipitated within the grains. However, with the elongation of tempering time, the influence of the M_3C phase on precipitation of the M_(23)C_6 phase becomes not remarkable. The two-step tempering treatment leads to more precipitates, higher dislocation density and smaller martensitic lath width than that obtained from the traditional tempering process. This is because that, the firstly tempering at a low temperature forms some precipitates, which would pin the dislocation and martensitic lath, and the subsequent secondly tempering at a high temperature complete the precipitation of particles while the recovery of lath and dislocation remain a low level as before. The investigation of tempering kinetics in the modified high Cr ferritic heat-resistant steel indicates that, the heterogeneous nucleation sites of the M_(23)C_6 particles decrease with the increase of number density of precipitates, which leads to the decrease of nucleation rate. At the early stage of tempering, the growth of the M_(23)C_6 particles accords with the diffusion-controlled model developed by Zenner. The growth rate of the M_(23)C_6 phase is related to diffusion coefficient of the solute atoms. With the process of tempering, solute concentration in matrix declines, leading to the decrease of growth rate of the M_(23)C_6 phaes. Furthermore, the migration rate of martensitic lath is controlled by thermally activated diffusion of the atoms at the grain boundary. With the elongation of tempering time, the width of martensitic lath increases. The research on the tempering of strain-induced martensite in the modified high Cr ferritic heat-resistant steel suggests that, in the sample after tempering, pre-stress loading results in the reduction of width of martensitic lath, and formation of sub-grain. This is because that, existence of residual strain energy increases the system free energy and lowers the activation energy for recovery, so the phenomenon of recovery appears in advance. Besides, pre-stress loading also decreases the size of precipitates, and increases the number density of that. This is ascribed to that increase of defection results in the increase of nucleation sites, and thus improves the nucleation rate of the precipitates.
引文
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