低碳微合金高强度钢中铁素体的形核、三维形态与长大动力学
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摘要
在新一代钢铁材料的发展中，固态相变过程中进行最终组织控制已经成为提高钢铁材料性能最有效的方法之一。奥氏体→铁素体相变通常是钢铁材料冷却过程中最先发生的固态相变，铁素体晶粒尺寸和形态对钢的力学性能有重要的影响。基于其重要的理论意义和工业应用价值，近60年来，奥氏体→铁素体相变一直是钢铁材料研究领域中的热点。因此，深入理解不同铁素体组织的形核、三维形态以及长大动力学将有助于精确地预测钢铁材料微观结构的演变，设计最合适的化学成分和热处理工艺路线。
本文采用连续截面和计算机辅助三维重建技术、高温共聚焦激光显微镜技术、热压连接、电子背散射衍射技术等实验方法以及热力学和第一原理计算等手段对低碳微合金高强度钢中奥氏体母相不同位置铁素体的形核、三维形态以及长大动力学等进行了系统的研究。主要研究结果如下：
(1)晶界铁素体是高温奥氏体相冷却过程中最先出现的相。奥氏体晶界面上形成的铁素体在二维截面上形态多样，但其三维形态往往在一个维度上尺寸较大，在其他维度上尺寸较小表现为长条状；奥氏体晶界棱上形成的铁素体在二维截面表现为三角形，其三维形态表现为金字塔形；奥氏体晶界角上形成的铁素体具有不规则的形状，填充晶界角。奥氏体晶界面上形成的铁素体在长大过程中会相互碰撞、融合，形成大块状铁素体，覆盖奥氏体晶界。
(2)在低过冷度下，在奥氏体晶内夹杂物上形核生成的等轴形铁素体，随着等温保持时间的延长，等轴形铁素体的数量增加而其仍保持等轴形态；在高过冷度下，等轴形铁素体和针状铁素体均能在夹杂物上形成，但样品在等温保持过程中等轴形铁素体由于其亚板条的生长速度差异而逐渐失去初期的形态特征；形成晶内铁素体的夹杂物为以Al2O3为核心外层包裹MnS的复合夹杂物，本研究中晶内铁素体的形核方式可能为夹杂物周围形成锰贫乏区而促进铁素体形核。同时通过氧化物双重热压连接实验以及第一性原理计算等对锰贫乏区促进铁素体的形核机制进行了进一步的实验和理论验证。等轴形铁素体具有亚结构，且各个亚结构之间取向差较小；等轴形铁素体的三维形态表现为多面体。
(3)在较大的过冷度下，在奥氏体晶内夹杂物上可形核生成晶内针状铁素体。针状铁素体的三维形态为板条状而不是二维截面上观察到的针状。针状铁素体板条具有特殊的长大方向，这是针状铁素体与奥氏体具有特殊取向关系的结果。针状铁素体晶粒细化的机制为：先形成的针状铁素体板条对奥氏体晶粒进行分割而限制后形成铁素体等组织的尺寸而细化晶粒。晶内针状铁素体的原位观察测量的板条伸长速率与魏氏铁素体板条的伸长速率相近。
(4)相对于奥氏体晶界面上形成的铁素体，在奥氏体晶界棱上形成的铁素体具有较大的长大速率常数；随着过冷度的减小，晶内等轴形铁素体与奥氏体晶界面上形成铁素体的长大速率常数的变化趋势具有很好的连续性；实验中观察到在替代型合金元素分配与不分配转变温度以下，随着过冷度的减小铁素体的长大模式从准平衡模型向局域平衡模型过渡，此现象可以通过溶质拖曳效应理论解释。
(5)魏氏铁素体的形成温度低于晶内等轴形铁素体的形成温度，但高于晶内针状铁素体的形成温度。魏氏铁素体板条的三维形态表现为板状；魏氏铁素体锯齿条具有三棱柱的形态；魏氏铁素体板条可以在奥氏体晶界面上直接形成，也可在已经形成的晶界铁素体上激发形核形成，或者在已经存在的魏氏铁素体板条的宽面形成。高温共聚焦激光显微镜技术原位观察结果表明，魏氏铁素体板条的生长并不是匀速的而是伴随着减速和加速，长大过程中存在微调其长大方向而取得更大速率的现象。在样品内部测得的魏氏铁素体板条的生长速率接近于局域平衡模型理论预测值，而在样品表面原位观察测量得到生长速率的最大值接近于准平衡模型下的预测值。这种差异表明，合金元素在样品内部和样品表面铁素体长大过程中的参与方式或者程度等方面存在差异。
In the new generation steel, the microstructure control in the solid-state phasetransformation process has become the most effective way to improve the performances of thesteels. Austenite to ferrite transformation is usually the first solid-state phase transformation insteels during cooling. The grain size and morphology of the ferrite significantly influence thehardenability and mechanical properties of the steels. Based on its industrial application valueand important theoretical significance, the diffusion phase transformation from austenite toferrite has been intensely studied in the last nearly60years. Hence, the deeper understanding inthe3-dimentional morphology and growth kinetics of ferrite in the low carbon high strengthmicro-alloyed steels will significantly contribute to the accurate prediction in the microstructureevolution, and to the designs of the most suitable chemical composition and heat treatmentprocessto obtain the steels with the desired microstructures.
In this paper, the serial-sectioning and computer-aided three-dimensional reconstructiontechnique, high temperature confocal laser microscopy, electron back-scattering diffractiontechnology et.al have been utilized to systematically investigate nucleation and growthmechanisms, three dimensional morphology, and growth kinetics of the ferrite formed in a lowcarbon micro-alloyed steel. Main results for this study are as follows：
(1) Grain boundary ferrite is the first decomposition product of the high temperatureaustenite during cooling. The morphology of ferrite allotriomorphs nucleated in the grainboundary face varied considerably from one grain to another, even on the same grain boundaryface. Most of face-nucleated ferrite allotriomorphs appeared to be large in one dimension andsmaller in other dimensions. They are better to be described as prolate ellipsoids rather thanexhibiting an equiaxed pancake shape along the grain boundary faces as usually assumed. Ferriteallotriomorphs nucleated at austenite grain boundary edges show the triangular-line shape on thetwo dimensional sections and take the form of triangular pyramids as the three dimensionalmorphology. Ferrite allotriomorphs nucleated at austenite grain boundary corners exhibitirregular shapes. During growth grain boundary ferrite starts to impinge against each other,coarsen and finally cover the austenite grain boundary.
(2) Intragranular ferrite idiomorph can be formed at both low and high undercoolings. Atlow undercooling the number and size of intragranular ferrite idiomorphs increased withincreasing holding time. At high undercooling, intragranular ferrite idiomorph formed prior toacicular ferrite. However, they gradually lost its morphological characteristics with increasingholding time and the acicular ferrite began to dominate the microstructure. Intragranular ferriteidiomorph was nucleated on inclusions. The non-specific orientation relationship of intragranularferrite idiomorph to austenite was probably the underlying reason for the formation of theequiaxed shape.
(3) Acicular ferrite can be formed on the inclusions under a larger under cooling; thethree-dimensional morphology of acicular ferrite is of a lath rather than a needle as traditionallyassumed; Acicular ferrite lath has special growth directions and its broad face is also parallel tosome special lattice planes of the austenite, which is resulted by its the special orientation relationship to the austenite. The grain refinement mechanism of acicular ferrite is that thepre-formed ferrite lath can partition austenite grains into compartments. The growth ofintragranular ferrite grains formed at later stages during isothermal holding or at lowertransformation temperatures during continuous cooling are thus confined to the smaller zonesand thus have smaller sizes. Intragranular acicular ferrite shows similar growth kinetics withWidmanst tten sideplates in in-situ observation.
(4)The growth rate constant of ferrite in nucleated grain boundary edge is larger than thosenucleated in grain boundary face and intragranular ferrite idiomorph. Growth kinetics ofintragranular ferrite idiomorph was similar to that of grain boundary ferrite allotriomorph andfell between paraequilibrium and local equilibrium prediction limits. A transition in proeutectoidferrite growth kinetics from para-equlibrium to negligible partion local equilibrium was observedfrom650°C to750°C below the partion local equilibrium/negligible partition local equilibriumtransition temperature in the investigated steel. This transition is explained in terms of the drageffect of the substitutional alloying elements.
(5) Widmanst tten sideplates directly emanated from austenite grain boundaries or from theexisting ferrite allotriomorph through the mechanism of edge-to-face sympathetic nucleation.Face-to-face sympathetic nucleation also occurred on the broad faces of the pre-formed ferritesideplates. The growth of plate on the free surface did not occur at a constant rate but ischaracterized by the acceleration and deceleration. The average lengthening rate ofWidmanst tten sideplates measured in-situ was one order of magnitude larger than the bulk value.The former is close to the prediction assuming paraequilibrium and the later is closer to theprediction assuming the negligible partition local equilibrium.
本文采用连续截面和计算机辅助三维重建技术、高温共聚焦激光显微镜技术、热压连接、电子背散射衍射技术等实验方法以及热力学和第一原理计算等手段对低碳微合金高强度钢中奥氏体母相不同位置铁素体的形核、三维形态以及长大动力学等进行了系统的研究。主要研究结果如下：
(1)晶界铁素体是高温奥氏体相冷却过程中最先出现的相。奥氏体晶界面上形成的铁素体在二维截面上形态多样，但其三维形态往往在一个维度上尺寸较大，在其他维度上尺寸较小表现为长条状；奥氏体晶界棱上形成的铁素体在二维截面表现为三角形，其三维形态表现为金字塔形；奥氏体晶界角上形成的铁素体具有不规则的形状，填充晶界角。奥氏体晶界面上形成的铁素体在长大过程中会相互碰撞、融合，形成大块状铁素体，覆盖奥氏体晶界。
(2)在低过冷度下，在奥氏体晶内夹杂物上形核生成的等轴形铁素体，随着等温保持时间的延长，等轴形铁素体的数量增加而其仍保持等轴形态；在高过冷度下，等轴形铁素体和针状铁素体均能在夹杂物上形成，但样品在等温保持过程中等轴形铁素体由于其亚板条的生长速度差异而逐渐失去初期的形态特征；形成晶内铁素体的夹杂物为以Al2O3为核心外层包裹MnS的复合夹杂物，本研究中晶内铁素体的形核方式可能为夹杂物周围形成锰贫乏区而促进铁素体形核。同时通过氧化物双重热压连接实验以及第一性原理计算等对锰贫乏区促进铁素体的形核机制进行了进一步的实验和理论验证。等轴形铁素体具有亚结构，且各个亚结构之间取向差较小；等轴形铁素体的三维形态表现为多面体。
(3)在较大的过冷度下，在奥氏体晶内夹杂物上可形核生成晶内针状铁素体。针状铁素体的三维形态为板条状而不是二维截面上观察到的针状。针状铁素体板条具有特殊的长大方向，这是针状铁素体与奥氏体具有特殊取向关系的结果。针状铁素体晶粒细化的机制为：先形成的针状铁素体板条对奥氏体晶粒进行分割而限制后形成铁素体等组织的尺寸而细化晶粒。晶内针状铁素体的原位观察测量的板条伸长速率与魏氏铁素体板条的伸长速率相近。
(4)相对于奥氏体晶界面上形成的铁素体，在奥氏体晶界棱上形成的铁素体具有较大的长大速率常数；随着过冷度的减小，晶内等轴形铁素体与奥氏体晶界面上形成铁素体的长大速率常数的变化趋势具有很好的连续性；实验中观察到在替代型合金元素分配与不分配转变温度以下，随着过冷度的减小铁素体的长大模式从准平衡模型向局域平衡模型过渡，此现象可以通过溶质拖曳效应理论解释。
(5)魏氏铁素体的形成温度低于晶内等轴形铁素体的形成温度，但高于晶内针状铁素体的形成温度。魏氏铁素体板条的三维形态表现为板状；魏氏铁素体锯齿条具有三棱柱的形态；魏氏铁素体板条可以在奥氏体晶界面上直接形成，也可在已经形成的晶界铁素体上激发形核形成，或者在已经存在的魏氏铁素体板条的宽面形成。高温共聚焦激光显微镜技术原位观察结果表明，魏氏铁素体板条的生长并不是匀速的而是伴随着减速和加速，长大过程中存在微调其长大方向而取得更大速率的现象。在样品内部测得的魏氏铁素体板条的生长速率接近于局域平衡模型理论预测值，而在样品表面原位观察测量得到生长速率的最大值接近于准平衡模型下的预测值。这种差异表明，合金元素在样品内部和样品表面铁素体长大过程中的参与方式或者程度等方面存在差异。
In the new generation steel, the microstructure control in the solid-state phasetransformation process has become the most effective way to improve the performances of thesteels. Austenite to ferrite transformation is usually the first solid-state phase transformation insteels during cooling. The grain size and morphology of the ferrite significantly influence thehardenability and mechanical properties of the steels. Based on its industrial application valueand important theoretical significance, the diffusion phase transformation from austenite toferrite has been intensely studied in the last nearly60years. Hence, the deeper understanding inthe3-dimentional morphology and growth kinetics of ferrite in the low carbon high strengthmicro-alloyed steels will significantly contribute to the accurate prediction in the microstructureevolution, and to the designs of the most suitable chemical composition and heat treatmentprocessto obtain the steels with the desired microstructures.
In this paper, the serial-sectioning and computer-aided three-dimensional reconstructiontechnique, high temperature confocal laser microscopy, electron back-scattering diffractiontechnology et.al have been utilized to systematically investigate nucleation and growthmechanisms, three dimensional morphology, and growth kinetics of the ferrite formed in a lowcarbon micro-alloyed steel. Main results for this study are as follows：
(1) Grain boundary ferrite is the first decomposition product of the high temperatureaustenite during cooling. The morphology of ferrite allotriomorphs nucleated in the grainboundary face varied considerably from one grain to another, even on the same grain boundaryface. Most of face-nucleated ferrite allotriomorphs appeared to be large in one dimension andsmaller in other dimensions. They are better to be described as prolate ellipsoids rather thanexhibiting an equiaxed pancake shape along the grain boundary faces as usually assumed. Ferriteallotriomorphs nucleated at austenite grain boundary edges show the triangular-line shape on thetwo dimensional sections and take the form of triangular pyramids as the three dimensionalmorphology. Ferrite allotriomorphs nucleated at austenite grain boundary corners exhibitirregular shapes. During growth grain boundary ferrite starts to impinge against each other,coarsen and finally cover the austenite grain boundary.
(2) Intragranular ferrite idiomorph can be formed at both low and high undercoolings. Atlow undercooling the number and size of intragranular ferrite idiomorphs increased withincreasing holding time. At high undercooling, intragranular ferrite idiomorph formed prior toacicular ferrite. However, they gradually lost its morphological characteristics with increasingholding time and the acicular ferrite began to dominate the microstructure. Intragranular ferriteidiomorph was nucleated on inclusions. The non-specific orientation relationship of intragranularferrite idiomorph to austenite was probably the underlying reason for the formation of theequiaxed shape.
(3) Acicular ferrite can be formed on the inclusions under a larger under cooling; thethree-dimensional morphology of acicular ferrite is of a lath rather than a needle as traditionallyassumed; Acicular ferrite lath has special growth directions and its broad face is also parallel tosome special lattice planes of the austenite, which is resulted by its the special orientation relationship to the austenite. The grain refinement mechanism of acicular ferrite is that thepre-formed ferrite lath can partition austenite grains into compartments. The growth ofintragranular ferrite grains formed at later stages during isothermal holding or at lowertransformation temperatures during continuous cooling are thus confined to the smaller zonesand thus have smaller sizes. Intragranular acicular ferrite shows similar growth kinetics withWidmanst tten sideplates in in-situ observation.
(4)The growth rate constant of ferrite in nucleated grain boundary edge is larger than thosenucleated in grain boundary face and intragranular ferrite idiomorph. Growth kinetics ofintragranular ferrite idiomorph was similar to that of grain boundary ferrite allotriomorph andfell between paraequilibrium and local equilibrium prediction limits. A transition in proeutectoidferrite growth kinetics from para-equlibrium to negligible partion local equilibrium was observedfrom650°C to750°C below the partion local equilibrium/negligible partition local equilibriumtransition temperature in the investigated steel. This transition is explained in terms of the drageffect of the substitutional alloying elements.
(5) Widmanst tten sideplates directly emanated from austenite grain boundaries or from theexisting ferrite allotriomorph through the mechanism of edge-to-face sympathetic nucleation.Face-to-face sympathetic nucleation also occurred on the broad faces of the pre-formed ferritesideplates. The growth of plate on the free surface did not occur at a constant rate but ischaracterized by the acceleration and deceleration. The average lengthening rate ofWidmanst tten sideplates measured in-situ was one order of magnitude larger than the bulk value.The former is close to the prediction assuming paraequilibrium and the later is closer to theprediction assuming the negligible partition local equilibrium.
引文
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