外加直流电场熔渣脱氧过程中氧传递机理研究
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摘要
科学技术的进步和市场需求的发展，对钢铁产品质量的要求越来越高。大量事实证明，钢液中溶解氧会严重影响钢材的质量，传统的脱氧方法已经无法满足对钢材质量的需求，亟待寻求一种洁净方法脱除钢中的氧。基于此，周国治等提出渣金间外加直流电场熔渣脱氧法：在钢液与熔渣之间施加稳定的外电场，控制氧离子在熔渣体系中的传导方向，实现钢液的有序脱氧。理论分析和前期研究证明了该方法的可行性。
为了进一步对渣金间外加直流电场熔渣脱氧工艺进行系统研究，围绕此主题，通过对CaO-Al_2O_3基预熔渣物性研究，确立组分对熔渣物性的影响，从而获得良好脱氧能力的熔渣；通过对Mo-ZrO_2金属陶瓷的组分和烧结工艺的研究，以获得基本满足脱氧实验要求的电极材料；分别采用碳钢、IF钢和X70管线钢，进行熔渣平衡脱氧和外加电场脱氧对比实验，研究钢液初始氧含量、熔渣成分和外电势等因素对钢液脱氧过程的影响；通过对渣金间氧的传输过程进行分析，建立脱氧过程的动力学模型；探索渣金间外加电场方法应用于熔渣电化学脱氧脱硫的可行性。论文主要内容归纳如下：
1、熔渣密度和粘度随温度的升高而降低，电导率随温度的升高而增加；在CaO-Al_2O_3-MgO体系低熔点区中，随着MgO含量的增加，熔点、密度、表面张力和粘度总体趋势为先降低后升高，电导率变化则是先升高后降低；熔渣物性随CaO/Al_2O_3质量比的变化，与熔渣物性随MgO含量的变化基本一致。在CaO-7%MgO-Al_2O_3-SiO_2体系低硅区范围内，熔渣熔点随着熔渣聚合度NBO/T值的升高而降低，电导率随NBO/T值的增大而增加；随着NBO/T值的增加，表面张力先显著下降随后缓慢升高，粘度先略升高然后降低。
_2、采用的粉末冶金工艺成功制备出了Mo-ZrO_2金属陶瓷电极。金属陶瓷的电导率随金属含量的增加而增大，随温度升高电导率呈现线性降低；Mo-ZrO_2金属陶瓷电导率与ZrO_2陶瓷相体积分数的关系，可用GEM方程进行描述，其临界体积分数为0.84，临界指数t为2.51。提高烧结温度或延长保温时间，可提高金属陶瓷的电导率。侵蚀结果表明：随着Mo金属相含量的减少，试样耐钢液侵蚀性能增强，耐CaO-Al_2O_3-MgO预熔碱性渣侵蚀性能减弱。钢液主要侵蚀金属陶瓷中的Mo金属相，熔渣主要侵蚀金属陶瓷中的ZrO_2陶瓷相。50%molMo-ZrO_2试样具有较好的综合性能，能够基本满足外加电场脱氧试验的要求。
3、CaO-Al_2O_3基预熔渣脱氧实验结果表明：MgO含量在0.0-5.0%；CaO/Al_2O_3为0.9-1.0的熔渣具有良好的脱氧能力；对比碳钢、X70管线钢和IF钢的熔渣平衡脱氧和外加电场熔渣脱氧实验结果表明：外加电场脱氧速率明显高于平衡脱氧速率，且未对渣样及钢样组分造成明显变化；提高外加电势，可提高脱氧速率，并降低了钢液的氧含量；还原性气氛下外加电场能够将X70管线钢的氧含量降低到29ppm的水平，将IF钢的氧含量降低到_25ppm的水平。
4、金属熔渣界面反应过程研究结果表明：循环伏安曲线中，随着扫描次数和扫描速率的增加，渣金反应电流增加；交流阻抗谱中，随着过电位的增加，脱氧反应的电荷传递电阻Rct明显降低，扩散阻抗随着过电位的增加而降低，钢液中氧的扩散增强；计时电流曲线中，脱氧过程中电极上发生的反应为[O]+2e=(O2-)；电流大小I对t-1/2呈线性衰减，不同电势下通过Cottrell方程计算的氧在熔渣中的扩散系数，随着外加电势的增加而急剧增加。
5、通过对渣金间氧的传输过程进行分析，利用等效电路描述带电粒子迁移过程，建立了外加电场熔渣脱氧过程的动力学模型，并通过实验数据与模型计算的对比，验证了所建立模型的正确性。
6、外加电场熔渣电化学脱硫实验结果表明：所选渣系具有很好的脱硫能力，外加电场的加入明显提高了钢液的脱硫速率和脱硫能力，降低了终渣FeO含量；证明了该方法脱硫的可行性。
With the progress of science and technology and the development of market, highquality steel product is on demand. It is known that the oxygen level dissolved in steelhas tremendous influence on the quality and performance. Since the traditionaldeoxidization methods could not satisfy some special requirements on the oxygenlevel in steel, it is necessary to look for alternative methods to reduce the oxygencontent in steel. In such a background，Chou put forward the deoxidization technologyof applied external voltage between molten steel and slag. This deoxidization methodcan control conduction direction of oxygen ions in the melt slag system so thatdeoxidization from liquid steel orderly can be carried out. It is observed from thetheoretical analysis and previous results that it is reliable to accelerate the reaction bythis method.
The aim of the present work is to further investigate the technology ofdeoxidization. The physicochemical properties of the selected CaO-Al_2O_3based slagsystem were investigated to explore a reasonable slag system for the requirement ofthis method, and the effects of component content on the physicochemical propertieswas investigated. In order to explore a reasonable electrode material for therequirement, The Mo-ZrO_2system cermet was chosen as the electrode material,mainly research on the influence of cermet compositions and sintering processes. Thedeoxidization experiments with Carbon steel, X70steel and IF steel were performedwith and without applied external voltage. And the factors such as the initial oxygencontent in steel, slag composition and the applied electric field potential wereinvestigated. To analyze the experimental results and understand the mechanism ofdeoxidization with applied external voltage, a kinetic model was proposed.Exploration on the possibility to enhance the rate of sulfur removal from metal to slagwith application of external voltage was studied. The major contents of this dissertation are epitomized as follows:
It is found experimentally that the density decreases approximately linearlywith an increasing temperature. The viscosity and conductivity decreases withincreasing temperature as expected. It is shown that the properties of selectedCaO-Al_2O_3-MgO slag system with low-melting-point zone, such as melting point,viscosity, surface tension and density the melting temperature, density, surfacetension and viscosity, decreased with increasing the MgO content, and following byan increase with further increasing of the MgO content. The conductivity increaseswith increasing the ratios of the MgO content, and following by a decrease withfurther increasing of the MgO content. The effect of the mass ratio of CaO/Al_2O_3ratio on the properties was similar to those changes with MgO content. Theproperties of the selected CaO-7mass%MgO-Al_2O_3-SiO_2with low silica weremeasured. The results indicated that while increasing the NBO/T ratio, not onlylower the melting temperature of slag, but also increase the conductivity of slag. Thesurface tension decrease first, then increase slowly again. The viscosity increaseswith increasing the ratios of the NBO/T ratio, and following by a decrease withfurther increasing of the NBO/T ratio.
The obtained results indicated that Mo-ZrO_2cermet can be successfullyprepared by the present powder metallurgy processes. The electrical conductivity ofcermets increased with decreasing the Mo content, and the high-temperatureelectrical conductivity increased linearly with increasing temperature. The GEMequation agrees well with the measured data. The model was proved to be promisingfor Mo-ZrO_2cermet dependence of ZrO_2volume ratio on conductivity of the cermet.The volume fraction of the ZrO_2phase is0.84, and the exponent for the percolationparameter is2.51. The results indicated that increasing sintering time and enhancingthe sintering temperature can lead to samples more compact in structure, and thusenhance the electrical conductivity of Mo-ZrO_2cermet. The corroded resultsindicated that the corrosion resistance of cermet to molten steel declines with the increase of Mo content. By contrast, the corrosion resistance of cermet toCaO-Al_2O_3-MgO slag declines with the reduction of Mo content. The property of50mol%Mo-ZrO_2is most superior, and can well be applied to the deoxidizationexperiment as electrode material.
The deoxidization experiments with CaO-Al_2O_3based slag showed that whenCaO/Al_2O_3ratio in the range from0.9to1.0and the MgO content was less than5%,the selected slag is a good oxygen ion carrier, and the slag could remove oxygenfrom molten steel effectively. The experimental results obtained from Carbon steel,X70steel and IF steel were indicated that application of external electrical voltage tothe slag steel system, not only was there an acceleration in the deoxidization rate, butalso that there was lower oxygen content in the steel melt and FeO content in thefinal slag than that dictated by chemical equilibrium of slag. And the finalcomposition of the slag did not change remarkablely with applied stable electricvoltage. The results show that under reducing atmosphere, the total oxygen contentof X70steel and IF steel with applied external voltage between molten steel and slag,were around_29ppm and_25ppm, respectively.
The interfacial deoxidization reaction kinetics between molten steel and moltenslag was studied. The CV results indicated that the current of interfacial reactionincrease with increasing scan rate and cycle times. The AC impedance resultsindicated that with rising applied potential, the charge transfer resistance of reaction(Rct) decreased obviously. And the diffusion resistance (Warburg impedance) whichdecreased with increasing applied potential indicated that the diffusivities of oxygenin molten steel increased with applied potential. The Chronoamperometry resultsindicated The interfacial reaction on deoxidization process is [O]+2e=(O~(2-)). Thecurrent of interfacial reaction decreases approximately linearly with t-1/_2, and thediffusivities of oxygen in molten slag calculated by Cottrell equation increaseddramatically with applied potential.
Using the equivalent circuit model, the experimental results are analyzed to understand the reaction process and mechanism of deoxidization, and a kineticmodel was proposed for the method. A reasonable agreement has been reachedbetween experimental data and model calculation.
It is observed from the present work that the slag could remove sulfur frommolten steel effectively. On application of electric voltage to the slag steel system,not only was there an acceleration in the desulphurization rate, but also that therewas lower sulfur content in the steel melt and FeO content in the final slag than thatdictated by chemical equilibrium of slag.
为了进一步对渣金间外加直流电场熔渣脱氧工艺进行系统研究，围绕此主题，通过对CaO-Al_2O_3基预熔渣物性研究，确立组分对熔渣物性的影响，从而获得良好脱氧能力的熔渣；通过对Mo-ZrO_2金属陶瓷的组分和烧结工艺的研究，以获得基本满足脱氧实验要求的电极材料；分别采用碳钢、IF钢和X70管线钢，进行熔渣平衡脱氧和外加电场脱氧对比实验，研究钢液初始氧含量、熔渣成分和外电势等因素对钢液脱氧过程的影响；通过对渣金间氧的传输过程进行分析，建立脱氧过程的动力学模型；探索渣金间外加电场方法应用于熔渣电化学脱氧脱硫的可行性。论文主要内容归纳如下：
1、熔渣密度和粘度随温度的升高而降低，电导率随温度的升高而增加；在CaO-Al_2O_3-MgO体系低熔点区中，随着MgO含量的增加，熔点、密度、表面张力和粘度总体趋势为先降低后升高，电导率变化则是先升高后降低；熔渣物性随CaO/Al_2O_3质量比的变化，与熔渣物性随MgO含量的变化基本一致。在CaO-7%MgO-Al_2O_3-SiO_2体系低硅区范围内，熔渣熔点随着熔渣聚合度NBO/T值的升高而降低，电导率随NBO/T值的增大而增加；随着NBO/T值的增加，表面张力先显著下降随后缓慢升高，粘度先略升高然后降低。
_2、采用的粉末冶金工艺成功制备出了Mo-ZrO_2金属陶瓷电极。金属陶瓷的电导率随金属含量的增加而增大，随温度升高电导率呈现线性降低；Mo-ZrO_2金属陶瓷电导率与ZrO_2陶瓷相体积分数的关系，可用GEM方程进行描述，其临界体积分数为0.84，临界指数t为2.51。提高烧结温度或延长保温时间，可提高金属陶瓷的电导率。侵蚀结果表明：随着Mo金属相含量的减少，试样耐钢液侵蚀性能增强，耐CaO-Al_2O_3-MgO预熔碱性渣侵蚀性能减弱。钢液主要侵蚀金属陶瓷中的Mo金属相，熔渣主要侵蚀金属陶瓷中的ZrO_2陶瓷相。50%molMo-ZrO_2试样具有较好的综合性能，能够基本满足外加电场脱氧试验的要求。
3、CaO-Al_2O_3基预熔渣脱氧实验结果表明：MgO含量在0.0-5.0%；CaO/Al_2O_3为0.9-1.0的熔渣具有良好的脱氧能力；对比碳钢、X70管线钢和IF钢的熔渣平衡脱氧和外加电场熔渣脱氧实验结果表明：外加电场脱氧速率明显高于平衡脱氧速率，且未对渣样及钢样组分造成明显变化；提高外加电势，可提高脱氧速率，并降低了钢液的氧含量；还原性气氛下外加电场能够将X70管线钢的氧含量降低到29ppm的水平，将IF钢的氧含量降低到_25ppm的水平。
4、金属熔渣界面反应过程研究结果表明：循环伏安曲线中，随着扫描次数和扫描速率的增加，渣金反应电流增加；交流阻抗谱中，随着过电位的增加，脱氧反应的电荷传递电阻Rct明显降低，扩散阻抗随着过电位的增加而降低，钢液中氧的扩散增强；计时电流曲线中，脱氧过程中电极上发生的反应为[O]+2e=(O2-)；电流大小I对t-1/2呈线性衰减，不同电势下通过Cottrell方程计算的氧在熔渣中的扩散系数，随着外加电势的增加而急剧增加。
5、通过对渣金间氧的传输过程进行分析，利用等效电路描述带电粒子迁移过程，建立了外加电场熔渣脱氧过程的动力学模型，并通过实验数据与模型计算的对比，验证了所建立模型的正确性。
6、外加电场熔渣电化学脱硫实验结果表明：所选渣系具有很好的脱硫能力，外加电场的加入明显提高了钢液的脱硫速率和脱硫能力，降低了终渣FeO含量；证明了该方法脱硫的可行性。
With the progress of science and technology and the development of market, highquality steel product is on demand. It is known that the oxygen level dissolved in steelhas tremendous influence on the quality and performance. Since the traditionaldeoxidization methods could not satisfy some special requirements on the oxygenlevel in steel, it is necessary to look for alternative methods to reduce the oxygencontent in steel. In such a background，Chou put forward the deoxidization technologyof applied external voltage between molten steel and slag. This deoxidization methodcan control conduction direction of oxygen ions in the melt slag system so thatdeoxidization from liquid steel orderly can be carried out. It is observed from thetheoretical analysis and previous results that it is reliable to accelerate the reaction bythis method.
The aim of the present work is to further investigate the technology ofdeoxidization. The physicochemical properties of the selected CaO-Al_2O_3based slagsystem were investigated to explore a reasonable slag system for the requirement ofthis method, and the effects of component content on the physicochemical propertieswas investigated. In order to explore a reasonable electrode material for therequirement, The Mo-ZrO_2system cermet was chosen as the electrode material,mainly research on the influence of cermet compositions and sintering processes. Thedeoxidization experiments with Carbon steel, X70steel and IF steel were performedwith and without applied external voltage. And the factors such as the initial oxygencontent in steel, slag composition and the applied electric field potential wereinvestigated. To analyze the experimental results and understand the mechanism ofdeoxidization with applied external voltage, a kinetic model was proposed.Exploration on the possibility to enhance the rate of sulfur removal from metal to slagwith application of external voltage was studied. The major contents of this dissertation are epitomized as follows:
It is found experimentally that the density decreases approximately linearlywith an increasing temperature. The viscosity and conductivity decreases withincreasing temperature as expected. It is shown that the properties of selectedCaO-Al_2O_3-MgO slag system with low-melting-point zone, such as melting point,viscosity, surface tension and density the melting temperature, density, surfacetension and viscosity, decreased with increasing the MgO content, and following byan increase with further increasing of the MgO content. The conductivity increaseswith increasing the ratios of the MgO content, and following by a decrease withfurther increasing of the MgO content. The effect of the mass ratio of CaO/Al_2O_3ratio on the properties was similar to those changes with MgO content. Theproperties of the selected CaO-7mass%MgO-Al_2O_3-SiO_2with low silica weremeasured. The results indicated that while increasing the NBO/T ratio, not onlylower the melting temperature of slag, but also increase the conductivity of slag. Thesurface tension decrease first, then increase slowly again. The viscosity increaseswith increasing the ratios of the NBO/T ratio, and following by a decrease withfurther increasing of the NBO/T ratio.
The obtained results indicated that Mo-ZrO_2cermet can be successfullyprepared by the present powder metallurgy processes. The electrical conductivity ofcermets increased with decreasing the Mo content, and the high-temperatureelectrical conductivity increased linearly with increasing temperature. The GEMequation agrees well with the measured data. The model was proved to be promisingfor Mo-ZrO_2cermet dependence of ZrO_2volume ratio on conductivity of the cermet.The volume fraction of the ZrO_2phase is0.84, and the exponent for the percolationparameter is2.51. The results indicated that increasing sintering time and enhancingthe sintering temperature can lead to samples more compact in structure, and thusenhance the electrical conductivity of Mo-ZrO_2cermet. The corroded resultsindicated that the corrosion resistance of cermet to molten steel declines with the increase of Mo content. By contrast, the corrosion resistance of cermet toCaO-Al_2O_3-MgO slag declines with the reduction of Mo content. The property of50mol%Mo-ZrO_2is most superior, and can well be applied to the deoxidizationexperiment as electrode material.
The deoxidization experiments with CaO-Al_2O_3based slag showed that whenCaO/Al_2O_3ratio in the range from0.9to1.0and the MgO content was less than5%,the selected slag is a good oxygen ion carrier, and the slag could remove oxygenfrom molten steel effectively. The experimental results obtained from Carbon steel,X70steel and IF steel were indicated that application of external electrical voltage tothe slag steel system, not only was there an acceleration in the deoxidization rate, butalso that there was lower oxygen content in the steel melt and FeO content in thefinal slag than that dictated by chemical equilibrium of slag. And the finalcomposition of the slag did not change remarkablely with applied stable electricvoltage. The results show that under reducing atmosphere, the total oxygen contentof X70steel and IF steel with applied external voltage between molten steel and slag,were around_29ppm and_25ppm, respectively.
The interfacial deoxidization reaction kinetics between molten steel and moltenslag was studied. The CV results indicated that the current of interfacial reactionincrease with increasing scan rate and cycle times. The AC impedance resultsindicated that with rising applied potential, the charge transfer resistance of reaction(Rct) decreased obviously. And the diffusion resistance (Warburg impedance) whichdecreased with increasing applied potential indicated that the diffusivities of oxygenin molten steel increased with applied potential. The Chronoamperometry resultsindicated The interfacial reaction on deoxidization process is [O]+2e=(O~(2-)). Thecurrent of interfacial reaction decreases approximately linearly with t-1/_2, and thediffusivities of oxygen in molten slag calculated by Cottrell equation increaseddramatically with applied potential.
Using the equivalent circuit model, the experimental results are analyzed to understand the reaction process and mechanism of deoxidization, and a kineticmodel was proposed for the method. A reasonable agreement has been reachedbetween experimental data and model calculation.
It is observed from the present work that the slag could remove sulfur frommolten steel effectively. On application of electric voltage to the slag steel system,not only was there an acceleration in the desulphurization rate, but also that therewas lower sulfur content in the steel melt and FeO content in the final slag than thatdictated by chemical equilibrium of slag.
引文
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