模拟热态钢渣直接熔制微晶玻璃晶化规律研究
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摘要
热态钢渣是炼钢过程中产生的含有大量热能的液态或半液态副产物。传统的热态钢渣处理工艺存在能量浪费大、物质消耗多、环境污染重、后续利用难、产品附加值低等诸多问题。利用热态钢渣直接制备微晶玻璃的技术不仅可以实现热态钢渣物质和能量的双重利用，减少能源和环境问题，而且制备的微晶玻璃产品附加值高，经济效益好，是钢铁行业实现节能减排的重要研究课题之一。
通过建立并求解多元方程组的方法计算制备给定组分基础玻璃所需的钢渣及各辅料组分的用量；采用液-液混熔的方法进行热态钢渣与适当辅料的混合与均化从而制备玻璃熔体；利用差热分析，粉晶X-射线衍射以及扫描电镜等分析方法探讨了不同辅料含量、不同热处理制度对钢渣微晶玻璃晶化、显微结构和性能的影响；运用非等温动力学理论分析了不同铁含量微晶玻璃晶体生长特性及机理。
（1）研究了不同混合辅料制备透辉石体系钢渣微晶玻璃。在700℃核化2h，900℃晶化2h的相同热处理条件下，不同辅料含量的微晶玻璃中晶相的类型和形貌存在差别。辅料用量较多的微晶玻璃样品，其耐酸性、显微硬度、吸水率、密度等值较低，抗折强度随辅料含量的减少而增大。相同组分的基础玻璃样品，随着晶化温度的增加，微晶玻璃样品的显微硬度逐渐增加，密度呈现先增加后减小的趋势。
（2）研究了以废玻璃为辅料的钢渣微晶玻璃。在惰性气氛下，采用液-液混熔方法制备的钢渣掺量为50%的基础玻璃，经700℃核化2h、900℃晶化2h热处理后微晶玻璃的主晶相为透辉石。当晶化温度高于900℃时，在微晶玻璃热处理过程中Fe~(2+)和Fe~(3+)发生易位和有序度变化，形成磁铁矿（Fe3O4）晶相，使微晶玻璃具有磁性。由基础玻璃在不同加热速率下DTA曲线分析来研究析晶动力学。基础玻璃样品的结晶活化能为450KJ/mol，晶体生长指数n的平均值为1.7。晶体生长的机制是表面控制下的三维析晶。随着晶化温度的升高，微晶玻璃样品中晶体的微观形貌由针状转变为片状，最后变成球状。晶形转变主要控制因素由界面能转变为应变能。
（3）研究了不同铁含量的钢渣微晶玻璃。随着铁含量的增加（5%-15%），基础玻璃的结晶活化能呈增大趋势，由494KJ/mol（铁含量为5.79%的基础玻璃样品Fe-1）升高到517KJ/mol（铁含量为15.38%的基础玻璃样品Fe-3）。晶体生长指数为1.69，晶体生长是整体成核、扩散控制下的三维析晶过程。在相同热处理条件下，不同铁含量的微晶玻璃样品析出的晶体种类不同。其中透辉石[Diopside(72-1379)]为共有的主晶相。微晶玻璃所析出的晶体的稳定性随着铁含量的增加而增强，耐酸性能随着铁含量的增加而减弱。
本文开展的配方优化设计、热态混熔工艺研究、热处理过程中相转变规律及晶体生长机理对热态钢渣资源化的应用具有参考价值。
Molten steel slag with the state of liquid or semi-liquid, which is generated in thesteel-making process, contains much thermal energy. There are many problems in thetraditional hot slag treatment process, such as large energy consumption, much materialwaste, serious environmental pollution, difficulty of reutilization, and low value-addedproducts. The novel process and technique of glass-ceramics preparation directly from hotsteel slag can not only use both hot slag material and energy, thus reducing energy andenvironmental issues, but also prepare high value-added products, thus promoting goodeconomic benefits. It is one of the important research topics for iron and steel industry toachieve energy-saving and emission-reduction.
The amount of steel slag and additives used for the preparation ofspecific-component glass-ceramics was calculated by establishing and solving themulti-equations. Mixing and homogenization of molten steel slag and additives wereproposed for preparation of glass melts by using liquid-liquid mixing method. Theinfluence of the additive content, different heat treatment conditions on the crystallization,microstructure and properties of glass-ceramics was investigated by using differentialthermal analysis, X-ray powder diffraction and scanning electron microscopy. Crystalgrowth characteristics and mechanism of glass-ceramics with different iron content werestudied using non-isothermal kinetic theory.
(1) Preparation of steel-slag based pyroxene system Glass-ceramics from variousadditive mixtures was investigated. In the same heat treatment conditions (nucleationtemperature700oC,2h; crystallization temperature900oC,2h), glass-ceramics whichcontain different amount of additives have different types of crystalline phase and crystalmorphology. The more contents of additives contain in glass-ceramics samples, the loweracid resistance, hardness, and water absorption. Flexural strength decreases with theincreasing contents of additives. With the increase in crystallization temperature, thehardness of basic glass-ceramic samples with the same components increases gradually,density increases at first and then decreases.
(2) Waste glass used as an adiitive to prepare steel-slag-based glass-ceramics wasstudied. After the parent glass sample, which contains50%steel slag, is heat-treated at thenucleation temperature of700oC and crystallization temperature of900oC for2hours respectively in an inert atmosphere, the main phase of the glass-ceramics is diopside. Fe~(2+)and Fe~(3+)in the parent glass sample, which is prepared using liquid-liquid mixing methodin the appropriate atmosphere, occurs translocation and degree of order change when thecrystallization temperature is higher than900oC during heat treatment. Theglass-ceramics sample crystallizes magnetite (Fe3O4) phase with the characteristics ofstrong magnetic. Crystallization activation energy of the glass-ceramics sample is450KJ/mol. Crystallization kinetics of parent glass was studied by analysis the DTA curveswhich obtained at different heating rates.The average crystal growth exponent of n is1.7.Crystal growth is three-dimensional crystallization under the control of surfacecrystallization.Crystal morphology is changed from flaky crystals and needle-like crystalinto spherical crystal with the increase of temperature. The main controlling factor forcrystal growth is changed from interfacial energy into strain energy with the increase oftemperature.
(3) Glass-ceramics with different iron content is investigated. The crystallizationactivation energy of glass-ceramics is increased from494KJ/mol (5.79%iron content inglass-ceramics samples, Fe-1) to517KJ/mol (15.38%iron content in glass-ceramicssamples, Fe-3) with the increasing contents of iron. The average crystal growth exponentof n is1.69. Crystal growth is an overall nucleation and three-dimensionaldiffusion-controlled crystallization process. In the same heat treatment conditions, theglass-ceramics samples with different iron content exhibit different types of crystallinephases. The main phase is Diopside (72-1379). The stability of the crystal increases withthe increase of iron content. Acid resistance increases with the decrease of iron content.
Studies on formulation optimization and mixing process in thermal state and theexperimental results of phase transition and crystal growth mechanism in this thesis have apositive effect on promoting hot steel slag recycling progress.
通过建立并求解多元方程组的方法计算制备给定组分基础玻璃所需的钢渣及各辅料组分的用量；采用液-液混熔的方法进行热态钢渣与适当辅料的混合与均化从而制备玻璃熔体；利用差热分析，粉晶X-射线衍射以及扫描电镜等分析方法探讨了不同辅料含量、不同热处理制度对钢渣微晶玻璃晶化、显微结构和性能的影响；运用非等温动力学理论分析了不同铁含量微晶玻璃晶体生长特性及机理。
（1）研究了不同混合辅料制备透辉石体系钢渣微晶玻璃。在700℃核化2h，900℃晶化2h的相同热处理条件下，不同辅料含量的微晶玻璃中晶相的类型和形貌存在差别。辅料用量较多的微晶玻璃样品，其耐酸性、显微硬度、吸水率、密度等值较低，抗折强度随辅料含量的减少而增大。相同组分的基础玻璃样品，随着晶化温度的增加，微晶玻璃样品的显微硬度逐渐增加，密度呈现先增加后减小的趋势。
（2）研究了以废玻璃为辅料的钢渣微晶玻璃。在惰性气氛下，采用液-液混熔方法制备的钢渣掺量为50%的基础玻璃，经700℃核化2h、900℃晶化2h热处理后微晶玻璃的主晶相为透辉石。当晶化温度高于900℃时，在微晶玻璃热处理过程中Fe~(2+)和Fe~(3+)发生易位和有序度变化，形成磁铁矿（Fe3O4）晶相，使微晶玻璃具有磁性。由基础玻璃在不同加热速率下DTA曲线分析来研究析晶动力学。基础玻璃样品的结晶活化能为450KJ/mol，晶体生长指数n的平均值为1.7。晶体生长的机制是表面控制下的三维析晶。随着晶化温度的升高，微晶玻璃样品中晶体的微观形貌由针状转变为片状，最后变成球状。晶形转变主要控制因素由界面能转变为应变能。
（3）研究了不同铁含量的钢渣微晶玻璃。随着铁含量的增加（5%-15%），基础玻璃的结晶活化能呈增大趋势，由494KJ/mol（铁含量为5.79%的基础玻璃样品Fe-1）升高到517KJ/mol（铁含量为15.38%的基础玻璃样品Fe-3）。晶体生长指数为1.69，晶体生长是整体成核、扩散控制下的三维析晶过程。在相同热处理条件下，不同铁含量的微晶玻璃样品析出的晶体种类不同。其中透辉石[Diopside(72-1379)]为共有的主晶相。微晶玻璃所析出的晶体的稳定性随着铁含量的增加而增强，耐酸性能随着铁含量的增加而减弱。
本文开展的配方优化设计、热态混熔工艺研究、热处理过程中相转变规律及晶体生长机理对热态钢渣资源化的应用具有参考价值。
Molten steel slag with the state of liquid or semi-liquid, which is generated in thesteel-making process, contains much thermal energy. There are many problems in thetraditional hot slag treatment process, such as large energy consumption, much materialwaste, serious environmental pollution, difficulty of reutilization, and low value-addedproducts. The novel process and technique of glass-ceramics preparation directly from hotsteel slag can not only use both hot slag material and energy, thus reducing energy andenvironmental issues, but also prepare high value-added products, thus promoting goodeconomic benefits. It is one of the important research topics for iron and steel industry toachieve energy-saving and emission-reduction.
The amount of steel slag and additives used for the preparation ofspecific-component glass-ceramics was calculated by establishing and solving themulti-equations. Mixing and homogenization of molten steel slag and additives wereproposed for preparation of glass melts by using liquid-liquid mixing method. Theinfluence of the additive content, different heat treatment conditions on the crystallization,microstructure and properties of glass-ceramics was investigated by using differentialthermal analysis, X-ray powder diffraction and scanning electron microscopy. Crystalgrowth characteristics and mechanism of glass-ceramics with different iron content werestudied using non-isothermal kinetic theory.
(1) Preparation of steel-slag based pyroxene system Glass-ceramics from variousadditive mixtures was investigated. In the same heat treatment conditions (nucleationtemperature700oC,2h; crystallization temperature900oC,2h), glass-ceramics whichcontain different amount of additives have different types of crystalline phase and crystalmorphology. The more contents of additives contain in glass-ceramics samples, the loweracid resistance, hardness, and water absorption. Flexural strength decreases with theincreasing contents of additives. With the increase in crystallization temperature, thehardness of basic glass-ceramic samples with the same components increases gradually,density increases at first and then decreases.
(2) Waste glass used as an adiitive to prepare steel-slag-based glass-ceramics wasstudied. After the parent glass sample, which contains50%steel slag, is heat-treated at thenucleation temperature of700oC and crystallization temperature of900oC for2hours respectively in an inert atmosphere, the main phase of the glass-ceramics is diopside. Fe~(2+)and Fe~(3+)in the parent glass sample, which is prepared using liquid-liquid mixing methodin the appropriate atmosphere, occurs translocation and degree of order change when thecrystallization temperature is higher than900oC during heat treatment. Theglass-ceramics sample crystallizes magnetite (Fe3O4) phase with the characteristics ofstrong magnetic. Crystallization activation energy of the glass-ceramics sample is450KJ/mol. Crystallization kinetics of parent glass was studied by analysis the DTA curveswhich obtained at different heating rates.The average crystal growth exponent of n is1.7.Crystal growth is three-dimensional crystallization under the control of surfacecrystallization.Crystal morphology is changed from flaky crystals and needle-like crystalinto spherical crystal with the increase of temperature. The main controlling factor forcrystal growth is changed from interfacial energy into strain energy with the increase oftemperature.
(3) Glass-ceramics with different iron content is investigated. The crystallizationactivation energy of glass-ceramics is increased from494KJ/mol (5.79%iron content inglass-ceramics samples, Fe-1) to517KJ/mol (15.38%iron content in glass-ceramicssamples, Fe-3) with the increasing contents of iron. The average crystal growth exponentof n is1.69. Crystal growth is an overall nucleation and three-dimensionaldiffusion-controlled crystallization process. In the same heat treatment conditions, theglass-ceramics samples with different iron content exhibit different types of crystallinephases. The main phase is Diopside (72-1379). The stability of the crystal increases withthe increase of iron content. Acid resistance increases with the decrease of iron content.
Studies on formulation optimization and mixing process in thermal state and theexperimental results of phase transition and crystal growth mechanism in this thesis have apositive effect on promoting hot steel slag recycling progress.
引文
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