先进高强度钢的选择性氧化及镀锌性能的研究
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摘要
本工作首先研究了先进高强度钢板及模型合金在连续热浸镀锌过程中发生的选择性氧化的机理，然后探讨了选择性氧化对钢板镀锌性能的影响，最后探索了连续热浸镀锌工艺对钢板组织和性能的影响。
通过在合金表面建立氧化的热力学平衡区，可以预测钢的化学成分及退火气氛对选择性氧化的影响。计算结果发现，合金元素Al、Cr、Mn、P及Si等元素在传统连续热浸镀锌的退火过程中发生的选择性氧化是热力学支持的，是不可避免的，且在氧化过程中，表面氧化物的种类取决于钢中合金元素的种类及含量。Si，Al，Cr元素能与Mn元素结合生成复合氧化物，且分别遵循Mn-Si、Al-Mn及Mn-Cr规律。由于其活泼性与Fe相近，Mo元素并不参与选择性氧化。另外，结合本工作的实验结果发现，除从热力学角度考虑氧化过程外，还必须考虑氧和合金元素在热力学平衡区域的扩散动力学。
本工作利用了XPS及FESEM-EDS对4种模型合金在-30℃和+10℃两个露点下的选择性氧化进行了研究。结果发现，合金的化学成分、初始状态及退火气氛的露点影响着合金的选择性氧化行为。合金元素Mn和Si元素发生选择性氧化遵循热力学上的Mn-Si规律。在本工作的退火时间内（120s），高达1.5wt.%Si元素显著增加了合金表面的氧化物，Cr元素并未与Mn结合生成稳定的Mn-Cr-O复合氧化物，而只是生成了Cr的二元氧化物，且Cr元素在-30℃及+10℃两个露点下都发生了表面偏聚。同时，随着露点的升高，合金表面的氧化物由薄膜状或网络状转变成颗粒状，表面氧化物覆盖率有降低的趋势。由于铸造合金的晶粒粗大，晶界较少，合金元素的表面偏聚量较轧制合金低，且不易受退火气氛的露点的影响。而轧制合金的晶粒较小，晶界较多，合金元素的表面偏聚量较高，且合金元素的偏聚量受露点的影响。另外，合金的初始状态不影响表面生成的氧化物类型。
通过研究工业用TRIP钢的选择性氧化发现，露点影响钢板合金元素的表面偏聚状态及氧化行为。对于Al和Cr元素，提高露点能促进其发生内氧化。对于P元素，在低露点下，该元素不发生表面选择性氧化，而提高露点则会促进其表面偏聚。同时，露点的提高促使钢板表面的氧化物变成岛状或颗粒状，减少了表面的氧化物覆盖率。工业用双相钢的表面选择性氧化行为与TRIP钢类似。双相钢中加入Cr，Mo等元素会改变Mn，Si元素的偏聚行为。值得注意的是，由于内氧化及脱碳消耗合金元素，提高露点至+10℃会导致TRIP钢近表面产生铁素体带，促使双相钢近表面组织容易被硝酸酒精溶液腐蚀出凹坑。另外，往双相钢中加入Cr和Mo会改变内氧化物的形貌。
模型合金氧化表面对锌液润湿性能的分析结果表明，氧化物形貌影响着锌液对合金表面的润湿性能。氧化物呈细小颗粒状的表面容易被锌液润湿，且润湿动力学很快；而氧化物呈薄膜状或大颗粒状的表面不容易被锌液润湿，且润湿动力学慢。合金中高达1.5wt.%的Si严重影响着锌液对表面的润湿性能。通过分析润湿反应界面，本工作发现，所有的漏镀点皆处于晶界或者晶内氧化物密集的地方，即使在一些区域生成了金属间化合物层，这些化合物都不致密，且含有较多的氧元素。XPS分析表明，模型合金润湿界面处存在的单质态的Fe和Mn，这是锌液中的Al还原了铁氧化物和锰氧化物的结果。
工业用钢板的镀锌性能同样与表面的氧化物形貌紧密相关。薄膜状氧化物显著恶化镀锌性能，颗粒细小状的氧化物对镀锌性能的恶化作用较小。调节露点可以改变钢板表面的氧化物形貌，能从一定程度上改善钢板的可镀性，但是改善的能力有限。锌液中的Al能还原表面的氧化物，但是由于Al元素被消耗，贫Al区的存在会导致润湿界面处的金属间化合物具有不同的尺寸和致密度。由于晶界或某些晶粒内部的氧化物分布密集且致密，Al还原过程很难在短时间内完成，因而导致了那些地方不能被润湿，产生漏镀点。
本工作还发现，连续热浸镀锌工艺对TRIP钢和双相钢的力学性能有显著的影响。为了获得具有良好力学性能的TRIP钢，必须选择合适的热处理参数。适当增加冷却速率和缩短镀锌时间能使双相钢获得最佳的力学性能。Cr元素和Mo元素的添加能提高双相钢与传统连续热浸镀锌线的兼容性。
Firstly in this work, the surface selective oxidation of several advanced highstrength steels and model alloys was fundamentally investigated in the context of thecontinuous hot-dip galvanizing. Then the impact of selective oxidation on the gal-vanisability of sheet steel was examined. Finally, this work explored the influence ofthe galvanizing thermal route on the mechanical properties of three dual phase steelsand one TRIP-aided steel.
By establishing a local thermodynamic equilibrium region, the influence of steelchemisty and annealing atmosphere on the selective oxidation was investigated bythermodynamics. It was found that the selective oxidation of element Al, Cr, Mn, Pand Si occurred in the galvanizing atmosphere is thermodynamical favorable andunavoidable. The type of oxides present on the steel surface depends on the alloy el-ements and their content in the matrix. Element Si, Al and Cr can react with Mn aswell as O to form mixed oxides, which follows the so-called Mn-Si, Al-Mn or Mn-Crrules. Element Mo doesn’t take part in the selective oxidation due to its similarchemical stability with Fe. However, combining the experiment results of this work,it is nessaccery to point out that we must also consider the diffusion kinetics of oxy-gen and alloy elements through the local equilibrium region.
The selective oxidation behavior of four model alloys at two dew points,-30℃and+10℃, were studied by XPS and FESEM-EDS. The results show that the chem-ical composition of the alloy matrix, the initial status of the model alloy and the an-nealing dew point influenced the oxidation behavior. The oxidation of Mn and Sifollows the Mn-Si rule. In the annealing interval of120s, Si up to1.5wt.%in the ma-trix contributed a lot to the surface oxidation, and Cr failed to combine Mn to formthe Mn-Cr-O mixed oxide. Moreover, Cr segregated to the surface after annealed atboth dew points. As the dew point increases, the morphology of the surface oxidechanged from film/network shape to granular/island shape, and the surface coverage of oxide tends to decrease. Since the cast alloy has large grain size and small amountof grain bourdaries, the amout of surface segregation is low, and is not influenced bythe dew point. While for hot rolled samples, the amount of surface segregation ishigher than cast alloy, and is influenced by the dew point. However, the initial statushas no influence on the type of oxides on the surface.
Dew point significantly influenced the surface segregation and oxidation behav-ior of alloy elements in TRIP steel. The increase of the dew point leads to the internaloxidation of Al and Cr. When at low dew point-30℃, P does not take part in the sur-face segregation and selective oxidation, while increasing the dew point to+10℃leads to the surface segregation of this element.
Meanwhile, increase the dew point change the oxide from film shape to island orgranular shape, decreased the surface coverage. The selective oxidation behavior onthe surface of DP steels is similar with that of TRIP steel. The addition of Cr and Moto DP steel changed the segregation and oxidation behavior of Mn and Si. It shouldbe noted that due to the consumption of alloy elements by internal oxidation and de-carburization, increasing the dew point to+10℃led to the formation of a ferriteband in the subsurface area in TRIP steel, also made the subsurface of DP steel easierto be etched by1vol.%nital solution. Furthermore, the addition of Cr and Mo to DPsteel changed the morphology of the internal oxide.
The wetting experiment results on the oxidized surface of model alloys show thatthe morphology of the surface oxide determined the wetting property. Surface withsmall oxide particles is well wetted by zinc with a fast wetting kinetics, while surfacewith film-shape oxide or large size oxide particle is not wetted by the zinc with aslow wetting kinetics. The high content of Si up to1.5wt.%significantly deterioratethe wetting property of the alloy surface with zinc. The result of the reactive interfaceanalysis shows that all the bare spot are located at areas with thick oxide, such asgrain boundary. Although there are some intermetallic compounds on the interface,these compounds are not compact and with considerabe conent of oxygen. XPS anal- ysis on the interface shows that the metallic iron and Mn were present due to the re-duction effect of Al from the zinc drop.
The galvanisability of the industrial steels is also related to the morphology ofthe surface oxide. Film shape oxide deteriorated the galvanisability significantly,while small oxide particle showed less influence on the galvanisability. Variation ofthe dew point can change the morphology of the oxide and improve the galvanisabil-ity; however, this improvement is very limited. The effective Al in from the zinc bathcan reduce some oxide on the steel surface; however, the local depletion of Al influ-enced the size and compactness of the intermetallic compounds. Due to the thick ox-ide present on the grain boundary or some spot within steel grains, the Al can not re-duce all the oxides in a short dipping time. Therefore, those spots can not be wettedby zinc and become the bare spot after galvanizing.
The present work also found that the thermal route of continuous hot-dip galva-nizing has an impact on the mechanical properties of the industrial steels. For TRIPsteel, it is very important to employ appropriate parameters of heat treatment to pro-duce hot-dip galvanized products with promising mechanical properties. For DP steel,an increase of the cooling rate after inter-critical annealing and a decrease of dippingtime is benefit for the mechanical properties. Further, the addition of Cr and Mo canincrease the compactibility of DP steel with the continuous hot-dip galvanizing.
通过在合金表面建立氧化的热力学平衡区，可以预测钢的化学成分及退火气氛对选择性氧化的影响。计算结果发现，合金元素Al、Cr、Mn、P及Si等元素在传统连续热浸镀锌的退火过程中发生的选择性氧化是热力学支持的，是不可避免的，且在氧化过程中，表面氧化物的种类取决于钢中合金元素的种类及含量。Si，Al，Cr元素能与Mn元素结合生成复合氧化物，且分别遵循Mn-Si、Al-Mn及Mn-Cr规律。由于其活泼性与Fe相近，Mo元素并不参与选择性氧化。另外，结合本工作的实验结果发现，除从热力学角度考虑氧化过程外，还必须考虑氧和合金元素在热力学平衡区域的扩散动力学。
本工作利用了XPS及FESEM-EDS对4种模型合金在-30℃和+10℃两个露点下的选择性氧化进行了研究。结果发现，合金的化学成分、初始状态及退火气氛的露点影响着合金的选择性氧化行为。合金元素Mn和Si元素发生选择性氧化遵循热力学上的Mn-Si规律。在本工作的退火时间内（120s），高达1.5wt.%Si元素显著增加了合金表面的氧化物，Cr元素并未与Mn结合生成稳定的Mn-Cr-O复合氧化物，而只是生成了Cr的二元氧化物，且Cr元素在-30℃及+10℃两个露点下都发生了表面偏聚。同时，随着露点的升高，合金表面的氧化物由薄膜状或网络状转变成颗粒状，表面氧化物覆盖率有降低的趋势。由于铸造合金的晶粒粗大，晶界较少，合金元素的表面偏聚量较轧制合金低，且不易受退火气氛的露点的影响。而轧制合金的晶粒较小，晶界较多，合金元素的表面偏聚量较高，且合金元素的偏聚量受露点的影响。另外，合金的初始状态不影响表面生成的氧化物类型。
通过研究工业用TRIP钢的选择性氧化发现，露点影响钢板合金元素的表面偏聚状态及氧化行为。对于Al和Cr元素，提高露点能促进其发生内氧化。对于P元素，在低露点下，该元素不发生表面选择性氧化，而提高露点则会促进其表面偏聚。同时，露点的提高促使钢板表面的氧化物变成岛状或颗粒状，减少了表面的氧化物覆盖率。工业用双相钢的表面选择性氧化行为与TRIP钢类似。双相钢中加入Cr，Mo等元素会改变Mn，Si元素的偏聚行为。值得注意的是，由于内氧化及脱碳消耗合金元素，提高露点至+10℃会导致TRIP钢近表面产生铁素体带，促使双相钢近表面组织容易被硝酸酒精溶液腐蚀出凹坑。另外，往双相钢中加入Cr和Mo会改变内氧化物的形貌。
模型合金氧化表面对锌液润湿性能的分析结果表明，氧化物形貌影响着锌液对合金表面的润湿性能。氧化物呈细小颗粒状的表面容易被锌液润湿，且润湿动力学很快；而氧化物呈薄膜状或大颗粒状的表面不容易被锌液润湿，且润湿动力学慢。合金中高达1.5wt.%的Si严重影响着锌液对表面的润湿性能。通过分析润湿反应界面，本工作发现，所有的漏镀点皆处于晶界或者晶内氧化物密集的地方，即使在一些区域生成了金属间化合物层，这些化合物都不致密，且含有较多的氧元素。XPS分析表明，模型合金润湿界面处存在的单质态的Fe和Mn，这是锌液中的Al还原了铁氧化物和锰氧化物的结果。
工业用钢板的镀锌性能同样与表面的氧化物形貌紧密相关。薄膜状氧化物显著恶化镀锌性能，颗粒细小状的氧化物对镀锌性能的恶化作用较小。调节露点可以改变钢板表面的氧化物形貌，能从一定程度上改善钢板的可镀性，但是改善的能力有限。锌液中的Al能还原表面的氧化物，但是由于Al元素被消耗，贫Al区的存在会导致润湿界面处的金属间化合物具有不同的尺寸和致密度。由于晶界或某些晶粒内部的氧化物分布密集且致密，Al还原过程很难在短时间内完成，因而导致了那些地方不能被润湿，产生漏镀点。
本工作还发现，连续热浸镀锌工艺对TRIP钢和双相钢的力学性能有显著的影响。为了获得具有良好力学性能的TRIP钢，必须选择合适的热处理参数。适当增加冷却速率和缩短镀锌时间能使双相钢获得最佳的力学性能。Cr元素和Mo元素的添加能提高双相钢与传统连续热浸镀锌线的兼容性。
Firstly in this work, the surface selective oxidation of several advanced highstrength steels and model alloys was fundamentally investigated in the context of thecontinuous hot-dip galvanizing. Then the impact of selective oxidation on the gal-vanisability of sheet steel was examined. Finally, this work explored the influence ofthe galvanizing thermal route on the mechanical properties of three dual phase steelsand one TRIP-aided steel.
By establishing a local thermodynamic equilibrium region, the influence of steelchemisty and annealing atmosphere on the selective oxidation was investigated bythermodynamics. It was found that the selective oxidation of element Al, Cr, Mn, Pand Si occurred in the galvanizing atmosphere is thermodynamical favorable andunavoidable. The type of oxides present on the steel surface depends on the alloy el-ements and their content in the matrix. Element Si, Al and Cr can react with Mn aswell as O to form mixed oxides, which follows the so-called Mn-Si, Al-Mn or Mn-Crrules. Element Mo doesn’t take part in the selective oxidation due to its similarchemical stability with Fe. However, combining the experiment results of this work,it is nessaccery to point out that we must also consider the diffusion kinetics of oxy-gen and alloy elements through the local equilibrium region.
The selective oxidation behavior of four model alloys at two dew points,-30℃and+10℃, were studied by XPS and FESEM-EDS. The results show that the chem-ical composition of the alloy matrix, the initial status of the model alloy and the an-nealing dew point influenced the oxidation behavior. The oxidation of Mn and Sifollows the Mn-Si rule. In the annealing interval of120s, Si up to1.5wt.%in the ma-trix contributed a lot to the surface oxidation, and Cr failed to combine Mn to formthe Mn-Cr-O mixed oxide. Moreover, Cr segregated to the surface after annealed atboth dew points. As the dew point increases, the morphology of the surface oxidechanged from film/network shape to granular/island shape, and the surface coverage of oxide tends to decrease. Since the cast alloy has large grain size and small amountof grain bourdaries, the amout of surface segregation is low, and is not influenced bythe dew point. While for hot rolled samples, the amount of surface segregation ishigher than cast alloy, and is influenced by the dew point. However, the initial statushas no influence on the type of oxides on the surface.
Dew point significantly influenced the surface segregation and oxidation behav-ior of alloy elements in TRIP steel. The increase of the dew point leads to the internaloxidation of Al and Cr. When at low dew point-30℃, P does not take part in the sur-face segregation and selective oxidation, while increasing the dew point to+10℃leads to the surface segregation of this element.
Meanwhile, increase the dew point change the oxide from film shape to island orgranular shape, decreased the surface coverage. The selective oxidation behavior onthe surface of DP steels is similar with that of TRIP steel. The addition of Cr and Moto DP steel changed the segregation and oxidation behavior of Mn and Si. It shouldbe noted that due to the consumption of alloy elements by internal oxidation and de-carburization, increasing the dew point to+10℃led to the formation of a ferriteband in the subsurface area in TRIP steel, also made the subsurface of DP steel easierto be etched by1vol.%nital solution. Furthermore, the addition of Cr and Mo to DPsteel changed the morphology of the internal oxide.
The wetting experiment results on the oxidized surface of model alloys show thatthe morphology of the surface oxide determined the wetting property. Surface withsmall oxide particles is well wetted by zinc with a fast wetting kinetics, while surfacewith film-shape oxide or large size oxide particle is not wetted by the zinc with aslow wetting kinetics. The high content of Si up to1.5wt.%significantly deterioratethe wetting property of the alloy surface with zinc. The result of the reactive interfaceanalysis shows that all the bare spot are located at areas with thick oxide, such asgrain boundary. Although there are some intermetallic compounds on the interface,these compounds are not compact and with considerabe conent of oxygen. XPS anal- ysis on the interface shows that the metallic iron and Mn were present due to the re-duction effect of Al from the zinc drop.
The galvanisability of the industrial steels is also related to the morphology ofthe surface oxide. Film shape oxide deteriorated the galvanisability significantly,while small oxide particle showed less influence on the galvanisability. Variation ofthe dew point can change the morphology of the oxide and improve the galvanisabil-ity; however, this improvement is very limited. The effective Al in from the zinc bathcan reduce some oxide on the steel surface; however, the local depletion of Al influ-enced the size and compactness of the intermetallic compounds. Due to the thick ox-ide present on the grain boundary or some spot within steel grains, the Al can not re-duce all the oxides in a short dipping time. Therefore, those spots can not be wettedby zinc and become the bare spot after galvanizing.
The present work also found that the thermal route of continuous hot-dip galva-nizing has an impact on the mechanical properties of the industrial steels. For TRIPsteel, it is very important to employ appropriate parameters of heat treatment to pro-duce hot-dip galvanized products with promising mechanical properties. For DP steel,an increase of the cooling rate after inter-critical annealing and a decrease of dippingtime is benefit for the mechanical properties. Further, the addition of Cr and Mo canincrease the compactibility of DP steel with the continuous hot-dip galvanizing.
引文
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