高Nb微合金钢中Nb的溶解/析出及其对组织演变影响的研究
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摘要
高Nb X80管线钢已经在油气管线工程中得到应用，然而，如何充分发挥Nb在钢中的作用，实现Nb的有效利用，还需要对Nb的溶解和析出以及Nb的这种变化对组织和性能的影响进行定量的研究。本文以六种高Nb钢为研究对象，定量研究了Nb在加热过程中的溶解规律，Nb的固溶和析出对热变形行为、静态软化行为及相变的影响，目的是定量阐明Nb在钢中的作用机制。
本文首先提出了一种测定钢中固溶Nb和未溶Nb含量的方法。该方法包括化学溶解、过滤分离和电感耦合等离子体原子发射光谱(Inductively Coupled PlasmaAtomic Emission Spectroscopic, ICP-AES)分析，通过测定溶液及溶解残渣中的Nb含量，即可确定钢中的固溶Nb和未溶Nb含量。在此基础上，定量研究了六种高Nb钢在加热过程中Nb的溶解规律，结果表明：对于微Ti处理的高Nb钢，随着加热温度的升高，Nb的固溶量增加，但在1300℃保温3h后，Nb仍不会完全溶解。钢中的C、Nb含量对Nb的固溶量有显著影响，随着C含量的降低和(或)Nb含量的增加，固溶Nb含量增加，在此基础上，建立了固溶Nb量与加热温度以及钢中的C、Nb含量之间的关系。
采用Gleeble-3500热模拟试验机和固溶Nb的定量分析方法，研究了固溶Nb、未溶Nb及变形过程中Nb的动态析出对热变形行为的影响，结果表明：加热过程中的未溶析出物对变形激活能和峰值应变没有显著影响，但可以增加热变形过程中的流变应力；由于析出量较少，在变形过程中Nb的动态析出对峰值应力和峰值应变均没有明显影响；固溶Nb对动态再结晶有强烈的抑制作用，每增加1%的固溶Nb便可以使变形激活能提高1599.9±137.7kJ/mol。
采用应力松弛法和双道次变形背插法研究了变形后等温过程中的应变诱导析出和静态软化行为，并定量研究了未溶Nb、固溶Nb对应变诱导析出的影响，以及Nb的固溶和析出对静态软化规律的影响。在变形后的等温过程中，未溶析出物能够作为应变诱导析出物的非均匀形核点，但这种析出对应力松弛曲线影响很小，相反由于其降低了固溶Nb含量，从而推迟了应力松弛曲线上所显示出的应变诱导析出开始时间。应变诱导析出所需的孕育期与钢中过饱和固溶Nb的量呈线性关系，随着过饱和Nb含量的增加，PTT曲线向短时间和高温区移动。
固溶Nb和应变诱导析出均能抑制变形道次间回复和静态再结晶的发生，从而降低软化率，但应变诱导析出对回复和静态再结晶的抑制作用更大。应变诱导析出未发生时，变形道次间的软化率与钢中的固溶Nb含量呈线性关系。当应变诱导析出发生之后，软化率与析出Nb的量保持线性关系。但随着保温时间的延长，析出物尺寸增大，其对软化的抑制作用逐渐减弱。
利用Gleeble-3500热模拟试验机并结合相变组织观察，绘制了实验钢的连续冷却转变(CCT)曲线，研究了不同实验条件下高Nb钢的相变行为。低的固溶Nb含量以及变形和变形后的等温处理都可以提高相变温度，促进多边形铁素体转变，使CCT曲线向左上方移动。增加钢中的固溶Nb有利于低温组织的形成，扩大CCT曲线中的针状铁素体转变区。变形在促进多边形铁素体转变的同时还可以细化铁素体晶粒。变形次数越多，其作用越明显。在变形后的等温过程中，回复和再结晶的发生降低了相变形核率，从而导致了相变组织的粗化。
相变组织硬度随冷速的增加而增大。变形及变形后的等温处理都可以促进NbC的析出。NbC的析出降低了钢中固溶的Nb、C含量，从而减弱了其固溶强化作用，导致多边形铁素体硬度下降。
High-Nb X80pipeline steels have being applied in many pipeline projects. In orderto increase the effectiveness of Nb in Nb-bearing microalloyed steel, it is necessary toquantitatively research the dissolution and precipitation regular of Nb and their effects onmicrostrctures and properties. In this paper, six high-Nb microalloyed steels are taken asresearch objects, the dissolution regular of Nb during heating process and the effects ofdissolution and precipitation of Nb on the hot deformation, static softening and phasetransformation behaviors were investigated quantitatively to elucidate the mechanism ofNb in high-Nb microalloyed steels.
A method of determining the content of soluble and undissolved Nb in steel has beenpresented. By dissolving, filtering and Inductively Coupled Plasma Atomic EmissionSpectroscopic (ICP-AES) analysis, the content of Nb in filtrate (soluble Nb) and residue(undissolved Nb) was determined. The dissolution regular of Nb in tested steels duringheating process was investigated with this method. The result shows that the soluble Nbcontent in the traceTi treated high-Nb steels increases with the heating temperature. Yet,the Nb in tested steels still can not completely dissolve after the holding of3h at1300°C.The soluble Nb content increases with the decrease of C content and/or the increase of Nbcontent in steel. On this basis, a model was built to describe the relation among the solubleNb content, heating temperature and the content of C and Nb in steel.
The effects of soluble Nb, undissolved precipitates and dynamic precipitation of Nbduring deformation on hot deformation behavior were researched by Gleeble-3500thermo-mechanical simulator and the method of determining soluble Nb content. Theresults show that the undissolved precipitates have no obvious effect on the deformationactivation energy and peak strain, but increase the flow stress during deformation. Thedynamic precipitation of Nb during deformation can not significantly affect the peakstress and strain because the precipitates are less. Soluble Nb can strongly delay thedynamic recrystallization. For every1wt%increase in soluble Nb, the deformationactivation energy increases1599.9±1.37.7kJ/mol.
By the stress relaxation way and back extrapolation method, the strain induced precipitation and static softening behaviors during the holding process after deformationwere investigated; the effects of undissolved Nb and soluble Nb on the strain inducedprecipitation of Nb were researched quantitatively and the influences of soluble Nb andprecipitation on static softening were also analyzed. During the holding process afterdeformation, the undissolved precipitates can also act as heterogenous nucleation sitesfor the precipitates induced by strain. However, this precipitation has no obvious effecton the stress relaxation curves. In contrast, the supersaturation of Nb in austenite isreduced due to the heterogeneous nucleation, which delays the precipitation start timeshown in the stress relaxation curves. Moreover, the incubation time of strain-inducedprecipitation is linearly related to the content of supersaturated Nb. Increasing the contentof supersaturated Nb can shift the nose of the precipitation C-curve to shorter time andhigher temperature.
Both soluble Nb and strain induced precipitates can restrain the recover and staticrecrystallization and then decrease the softening ratio. Yet, the precipitates induced bystrain have more strong retarding effect on the recover and static recrystallization than thesolid solution Nb atoms. The softening ratio is linear with the dissolved Nb content beforethe strain-induced precipitation and with the precipitable Nb content after thestrain-induced precipitation. However, the retarding effect decreases with the prolongingof holding time and the coarsening of precipitate.
The continuous cooling transformation (CCT) curves were constructed and the phasetransformation behanviors of tested steels were researched by Gleeble-3500thermo-mechanical simulator and metallographic observation. The lower soluble Nbcontent, hot deformation and holding treatment after deformation can increase phasetransformation temperature, promote the transformation of polygonal ferrite and move theCCT curves upper left. The increase of soluble Nb content promotes the low temperaturemicrostructure transformation and enlarges the acicular ferrite area in CCT curves.Deformation not only increases the phase transformation temperature, but also refinesferrite grains. This effect is more obvious with the increase of deformation pass. Therecovery and recrystallization occur during holding process, which decreases thenucleation rate and cause the coarsening of microstructure.
The hardness of phase transformation microstructure increases with the cooling rate.Moreover, both deformation and the holding process after deformation promote straininduced precipitation of NbC and decrease the content of Nb and C in solid solution,which weakens the solid solution strengthening of Nb and C and decreases the hardness ofpolygonal ferrite.
本文首先提出了一种测定钢中固溶Nb和未溶Nb含量的方法。该方法包括化学溶解、过滤分离和电感耦合等离子体原子发射光谱(Inductively Coupled PlasmaAtomic Emission Spectroscopic, ICP-AES)分析，通过测定溶液及溶解残渣中的Nb含量，即可确定钢中的固溶Nb和未溶Nb含量。在此基础上，定量研究了六种高Nb钢在加热过程中Nb的溶解规律，结果表明：对于微Ti处理的高Nb钢，随着加热温度的升高，Nb的固溶量增加，但在1300℃保温3h后，Nb仍不会完全溶解。钢中的C、Nb含量对Nb的固溶量有显著影响，随着C含量的降低和(或)Nb含量的增加，固溶Nb含量增加，在此基础上，建立了固溶Nb量与加热温度以及钢中的C、Nb含量之间的关系。
采用Gleeble-3500热模拟试验机和固溶Nb的定量分析方法，研究了固溶Nb、未溶Nb及变形过程中Nb的动态析出对热变形行为的影响，结果表明：加热过程中的未溶析出物对变形激活能和峰值应变没有显著影响，但可以增加热变形过程中的流变应力；由于析出量较少，在变形过程中Nb的动态析出对峰值应力和峰值应变均没有明显影响；固溶Nb对动态再结晶有强烈的抑制作用，每增加1%的固溶Nb便可以使变形激活能提高1599.9±137.7kJ/mol。
采用应力松弛法和双道次变形背插法研究了变形后等温过程中的应变诱导析出和静态软化行为，并定量研究了未溶Nb、固溶Nb对应变诱导析出的影响，以及Nb的固溶和析出对静态软化规律的影响。在变形后的等温过程中，未溶析出物能够作为应变诱导析出物的非均匀形核点，但这种析出对应力松弛曲线影响很小，相反由于其降低了固溶Nb含量，从而推迟了应力松弛曲线上所显示出的应变诱导析出开始时间。应变诱导析出所需的孕育期与钢中过饱和固溶Nb的量呈线性关系，随着过饱和Nb含量的增加，PTT曲线向短时间和高温区移动。
固溶Nb和应变诱导析出均能抑制变形道次间回复和静态再结晶的发生，从而降低软化率，但应变诱导析出对回复和静态再结晶的抑制作用更大。应变诱导析出未发生时，变形道次间的软化率与钢中的固溶Nb含量呈线性关系。当应变诱导析出发生之后，软化率与析出Nb的量保持线性关系。但随着保温时间的延长，析出物尺寸增大，其对软化的抑制作用逐渐减弱。
利用Gleeble-3500热模拟试验机并结合相变组织观察，绘制了实验钢的连续冷却转变(CCT)曲线，研究了不同实验条件下高Nb钢的相变行为。低的固溶Nb含量以及变形和变形后的等温处理都可以提高相变温度，促进多边形铁素体转变，使CCT曲线向左上方移动。增加钢中的固溶Nb有利于低温组织的形成，扩大CCT曲线中的针状铁素体转变区。变形在促进多边形铁素体转变的同时还可以细化铁素体晶粒。变形次数越多，其作用越明显。在变形后的等温过程中，回复和再结晶的发生降低了相变形核率，从而导致了相变组织的粗化。
相变组织硬度随冷速的增加而增大。变形及变形后的等温处理都可以促进NbC的析出。NbC的析出降低了钢中固溶的Nb、C含量，从而减弱了其固溶强化作用，导致多边形铁素体硬度下降。
High-Nb X80pipeline steels have being applied in many pipeline projects. In orderto increase the effectiveness of Nb in Nb-bearing microalloyed steel, it is necessary toquantitatively research the dissolution and precipitation regular of Nb and their effects onmicrostrctures and properties. In this paper, six high-Nb microalloyed steels are taken asresearch objects, the dissolution regular of Nb during heating process and the effects ofdissolution and precipitation of Nb on the hot deformation, static softening and phasetransformation behaviors were investigated quantitatively to elucidate the mechanism ofNb in high-Nb microalloyed steels.
A method of determining the content of soluble and undissolved Nb in steel has beenpresented. By dissolving, filtering and Inductively Coupled Plasma Atomic EmissionSpectroscopic (ICP-AES) analysis, the content of Nb in filtrate (soluble Nb) and residue(undissolved Nb) was determined. The dissolution regular of Nb in tested steels duringheating process was investigated with this method. The result shows that the soluble Nbcontent in the traceTi treated high-Nb steels increases with the heating temperature. Yet,the Nb in tested steels still can not completely dissolve after the holding of3h at1300°C.The soluble Nb content increases with the decrease of C content and/or the increase of Nbcontent in steel. On this basis, a model was built to describe the relation among the solubleNb content, heating temperature and the content of C and Nb in steel.
The effects of soluble Nb, undissolved precipitates and dynamic precipitation of Nbduring deformation on hot deformation behavior were researched by Gleeble-3500thermo-mechanical simulator and the method of determining soluble Nb content. Theresults show that the undissolved precipitates have no obvious effect on the deformationactivation energy and peak strain, but increase the flow stress during deformation. Thedynamic precipitation of Nb during deformation can not significantly affect the peakstress and strain because the precipitates are less. Soluble Nb can strongly delay thedynamic recrystallization. For every1wt%increase in soluble Nb, the deformationactivation energy increases1599.9±1.37.7kJ/mol.
By the stress relaxation way and back extrapolation method, the strain induced precipitation and static softening behaviors during the holding process after deformationwere investigated; the effects of undissolved Nb and soluble Nb on the strain inducedprecipitation of Nb were researched quantitatively and the influences of soluble Nb andprecipitation on static softening were also analyzed. During the holding process afterdeformation, the undissolved precipitates can also act as heterogenous nucleation sitesfor the precipitates induced by strain. However, this precipitation has no obvious effecton the stress relaxation curves. In contrast, the supersaturation of Nb in austenite isreduced due to the heterogeneous nucleation, which delays the precipitation start timeshown in the stress relaxation curves. Moreover, the incubation time of strain-inducedprecipitation is linearly related to the content of supersaturated Nb. Increasing the contentof supersaturated Nb can shift the nose of the precipitation C-curve to shorter time andhigher temperature.
Both soluble Nb and strain induced precipitates can restrain the recover and staticrecrystallization and then decrease the softening ratio. Yet, the precipitates induced bystrain have more strong retarding effect on the recover and static recrystallization than thesolid solution Nb atoms. The softening ratio is linear with the dissolved Nb content beforethe strain-induced precipitation and with the precipitable Nb content after thestrain-induced precipitation. However, the retarding effect decreases with the prolongingof holding time and the coarsening of precipitate.
The continuous cooling transformation (CCT) curves were constructed and the phasetransformation behanviors of tested steels were researched by Gleeble-3500thermo-mechanical simulator and metallographic observation. The lower soluble Nbcontent, hot deformation and holding treatment after deformation can increase phasetransformation temperature, promote the transformation of polygonal ferrite and move theCCT curves upper left. The increase of soluble Nb content promotes the low temperaturemicrostructure transformation and enlarges the acicular ferrite area in CCT curves.Deformation not only increases the phase transformation temperature, but also refinesferrite grains. This effect is more obvious with the increase of deformation pass. Therecovery and recrystallization occur during holding process, which decreases thenucleation rate and cause the coarsening of microstructure.
The hardness of phase transformation microstructure increases with the cooling rate.Moreover, both deformation and the holding process after deformation promote straininduced precipitation of NbC and decrease the content of Nb and C in solid solution,which weakens the solid solution strengthening of Nb and C and decreases the hardness ofpolygonal ferrite.
引文
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