薄层纤维素醚改性水泥浆体水化历程和微观结构研究
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摘要
我国目前正处于城镇化高速发展的关键时期,外墙外保温系统作为建筑节能的主要技术途径,其中,粘结砂浆和抗裂砂浆等薄层砂浆对于保证外墙外保温系统的节能效果和耐久性的实现起着重要的作用,在此背景下,研究薄层砂浆的水化关键问题具有特别重要的意义。本研究工作来源于“十二五”国家科技支撑计划项目(2011BAJ04802)和国家自然科学基金(50902107)。通过研究纤维素醚(cellulose ether,CE)改性水泥浆体的流变性能和热-电特性,探明多因素环境下水泥浆体的水化动力学过程。根据薄层CE改性水泥浆体的使用环境的不同,研究了快速失水条件下水泥浆体的水化规律。基于薄层水泥浆体流变特性、水化动力学过程和快速失水条件下的水化规律建立了薄层CE改性水泥浆体水化过程和界面过渡区微观结构模型,阐述了薄层CE改性水泥浆体的水化特征。
本文主要的工作及所取得的重要成果如下：
1.根据CE在水溶液(拌和阶段环境)和水泥浆体(水化阶段环境)2种液相环境中的流变特性,系统研究了CE成膜过程及溶液环境(温度、pH值、离子的种类和价态)对水溶液和水泥浆体流变特性的影响,揭示了CE在不同液相环境中成膜过程及温度、pH值、离子对其在水溶液和水泥浆体中的作用机理。
以表观粘度、剪切应力、屈服应力和塑性粘度为评价指标,研究了CE种类和掺量对水溶液和水泥浆体流变特性的影响。探讨了不同温度和pH值时CE在水溶液和水泥浆体中的流变特性,确立了CE的低临界溶解温度和等电点。分别研究了阳离子、阴离子及其价态对CE溶液表观粘度的影响,基于“感胶离子序”的规律阐述了离子种类和价态对CE溶液表观粘度的作用机理,揭示了CE在复杂液相环境中的成膜特征,为研究塑性阶段CE改性水泥浆体的流变特性提供了理论依据。
2.提出了CE-聚水与缓释组分(CWRC)改性水泥浆体水化动力学过程的设计与制备方法,基于对水化热和电阻率微分曲线分析,掌握了水泥水化初期的宏观热学效应及电化学特征变化规律,研究了水化热和电阻率与水泥水化进程的关系,建立了CE-CWRC-水泥三元体系水化热-电模型。
分别研究了CE和CWRC对水泥水化热和电阻率的影响,指出CWRC对水泥水化各阶段的延迟作用小于CE。研究了电阻率和水化放热量与Ca(OH)2和化学结合水含量的关系,发现具有线性相关性,为研究水泥水化早期结构形成及水化进程提供了一种新的结构参数。通过对水化热和电阻率微分曲线分析,建立了CE-CWRC-水泥三元体系水化热-电模型,将水泥水化过程分为：溶解-析出平衡期、结构形成期、结构发展期和结构稳定期4个阶段,且模型中水化热和电阻率微分在表征水泥早期水化动力学过程具有较好的一致性,可以准确描述水泥水化历程及结构形成的瞬时状态。
3.首次提出了CE改性薄层水泥浆体在快速失水条件下的试验设计与评价方法,通过改变水泥浆体厚度、养护温度和基体材料的种类,系统研究了CE改性薄层水泥浆体的早期失水特征、界面性能和微观分析,探明了薄层水泥浆体的水化规律和微观结构发展机制。
以失水速度和失水率为评价指标,研究了薄层水泥浆体在快速失水条件下的早期失水特征,并阐述了其失水机制。分析了水泥浆体厚度、养护温度和基体材料的种类对薄层水泥浆体界面性能的影响,指出了不同龄期时的界面破坏形式。通过XRD、FTIR和TG-DSC分析,研究了薄层水泥浆体在快速失水条件下的水化规律。通过对快速失水条件下水泥浆体表层、中间层和界面层3个区域的微观分析,探明了水化产物沿水泥浆体厚度方向上的分布规律,揭示了薄层水泥浆体的界面破坏原理,为研究外墙外保温系统中保温层脱落和保护层的空鼓、开裂等问题奠定了理论基础。
4.根据薄层水泥-CE浆体中水分和离子的迁移、CE成膜、水泥浆体的硬化过程,分析了水化产物沿薄层水泥浆体厚度方向上的分布规律,建立了实际服役环境下的薄层水泥-CE浆体水化过程和界面过渡区微观结构模型。
根据CE成膜与溶解过程、薄层水泥浆体的失水机制与离子迁移过程、水化历程与微观结构发展机制、水化产物的分布规律,建立了实际服役环境下薄层水泥-CE浆体的水化过程模型。根据基体材料的孔结构与吸水特性,分析了薄层水泥浆体的失水特征、界面微结构的变化、水化产物的种类和数量分布,建立了薄层水泥浆体与基体材料间的界面过渡区微观结构模型,对于研究薄层水泥-CE浆体水化规律具有重要的理论与实际意义。
At present, urbanization in our country is in a rapid growth. External thermal insulation system is main technical approaches of building energy efficiency. Adhesive mortar and anti-crack mortar play an important role in protecting energy-saving effect and durability. Against this background, it has especially important significance of research of hydration key problems of thin layer mortar. The research was funded by National science and technology support project (No.2011BAJ04B02)" and Youth Fund of National Natural Science Foundation of China (No.50902107)". In multiple factors environment, kinetics of hydration process of cement paste modified with cellulose ether (CE) was verified by the research of rheological properties and heat-electrical characteristics. According to different service environment of cement paste, hydration mechanism of cement paste was studied under the condition of rapid water loss. To elaborate hydration characteristics of thin layer cement paste modified with CE, the model of hydration process and interface transition zone microstructure of thin layer cement paste modified with CE was established based on rheological properties, kinetics of hydration process and hydration mechanism under the condition of rapid water loss of cement paste modified with CE.
The main research and obtained important achievement of this article as follows:
1. Based on rheological behavior of CE in aqueous solution (mixing stage environment) and (hydration stage environment),film-forming process of CE and influence of solution environment (temperature, pH, ion species and valence) on rheological behavior of aqueous solution and cement pastes were studied. Film-forming process of CE in different liquid phase environment and mechanism of temperature, pH, ion species and valence were obtained.
Apparent viscosity, shear stress, yield stress and plastic viscosity were used as index system. The influence of kind and dosage of CE on rheological behavior was studied. Rheological properties of aqueous solution and cement paste which modified with CE were discussed under different temperature and pH. At the same time, the lower critical solution temperature and isoelectric point of CE were obtained. The sensitivity of HPMC, HEMC and HEC to pH is different. The influence of cations, anions and its valence on apparent viscosity of CE solution was respectively studied. Mechanism of ions species and valence was expounded based on lyotropic series and revealed the film-forming characteristics of CE in complex liquid phase environment. Theoretical basis was provided for studying the rheological properties of cement paste modified with CE in plastic stage.
2. Design and preparation methods of kinetics of hydration process of cement pastes modified with CE and cohesion water and slow release components (CWRC) were put forward. Based on hydration exothermic rate curve and derivate of resistivity curve of cement hydration, macro thermal effect and electrochemical characteristics change rule of early stage of cement hydration were mastered and the relationship among hydration exothermic, resistivity and cement hydration process was studied. Heat-electric model of system composed of CE, CWRC and cement was established.
The influence of CE and CWRC on hydration exothermic and resistivity of cement pastes was studied and delay effect of CWRC was less than CE on each stage of cement hydration was pointed out. It had linear dependence among Ca (OH)2content, chemically combined water content, hydration heat quantity and resistivity. A new structure parameter was provided to describe structure formation and hydration process. Heat-electric model of system composed of CE, CWRC and cement was established by analysis of hydration exothermic rate curve and derivate of resistivity curve of cement hydration. The process of cement hydration was divided into solution-precipitation equilibrium stage, structure formation stage, structure development stage and structure stability stage. It had a good consistency that description of hydration exothermic rate and derivate of resistivity on hydration kinetics process of cement in early stage. Instantaneous state of structure formation and process of cement hydration could be accurately described.
3. Trial design and evaluation methods of thin layer cement pastes modified with CE under rapid water-loss were first proposed. Water loss characteristics, interface properties and microscopic analysis were studied of cement pastes modified with CE in early stage by change of thickness of cement pastes, curing temperature and kinds of matrix materials. Hydration mechanism and principle of microstructure formation of thin layer cement pastes were found out.
Water-loss speed and water-loss rate were used as assessment criteria to study water-loss characteristics and mechanism of thin layer cement pastes under rapid water-loss. The influence of thickness of cement pastes, curing temperature and kinds of matrix materials on interface properties of thin layer cement pastes and described interface damage form of different ages. Hydration law of thin layer cement pastes under rapid water-loss was studied by XRD, FTIR and TG-DSC. Distribution regularities of hydration products along the thickness direction of cement paste were proved by microanalysis of surface layer, interlayer and interface layer of cement pastes under rapid water-loss. Principle of interfacial damage of thin layer cement paste was revealed and laid a theoretical basis for analysis of insulation layer drop and covering layer empty drum and cracking of external thermal insulation system.
4. Based on water and ion migration, CE film formation and hardening process of cement paste of thin layer cement pastes modified with CE, distribution regularities of hydration products along the thickness direction of cement paste were analyzed. The model of hydration process and interface transition zone microstructure of thin layer cement paste modified with CE under actual service environment was established.
The model of hydration process of cement paste modified with CE under actual service environment was established according to CE film formation and dissolve process, water-loss mechanism and ion migration process, hydration process and microstructure, distribution regularities of hydration products. Characteristics water-loss, changes of interface microstructure, kinds and amount of hydration products were analyzed on the basis of pore structure and water absorption of substrate materials and model between interface transition zone microstructure and matrix material of thin layer cement paste was established. It had important theoretical and practical significance of research on hydration mechanism of thin layer cement pastes modified with CE.
本文主要的工作及所取得的重要成果如下：
1.根据CE在水溶液(拌和阶段环境)和水泥浆体(水化阶段环境)2种液相环境中的流变特性,系统研究了CE成膜过程及溶液环境(温度、pH值、离子的种类和价态)对水溶液和水泥浆体流变特性的影响,揭示了CE在不同液相环境中成膜过程及温度、pH值、离子对其在水溶液和水泥浆体中的作用机理。
以表观粘度、剪切应力、屈服应力和塑性粘度为评价指标,研究了CE种类和掺量对水溶液和水泥浆体流变特性的影响。探讨了不同温度和pH值时CE在水溶液和水泥浆体中的流变特性,确立了CE的低临界溶解温度和等电点。分别研究了阳离子、阴离子及其价态对CE溶液表观粘度的影响,基于“感胶离子序”的规律阐述了离子种类和价态对CE溶液表观粘度的作用机理,揭示了CE在复杂液相环境中的成膜特征,为研究塑性阶段CE改性水泥浆体的流变特性提供了理论依据。
2.提出了CE-聚水与缓释组分(CWRC)改性水泥浆体水化动力学过程的设计与制备方法,基于对水化热和电阻率微分曲线分析,掌握了水泥水化初期的宏观热学效应及电化学特征变化规律,研究了水化热和电阻率与水泥水化进程的关系,建立了CE-CWRC-水泥三元体系水化热-电模型。
分别研究了CE和CWRC对水泥水化热和电阻率的影响,指出CWRC对水泥水化各阶段的延迟作用小于CE。研究了电阻率和水化放热量与Ca(OH)2和化学结合水含量的关系,发现具有线性相关性,为研究水泥水化早期结构形成及水化进程提供了一种新的结构参数。通过对水化热和电阻率微分曲线分析,建立了CE-CWRC-水泥三元体系水化热-电模型,将水泥水化过程分为：溶解-析出平衡期、结构形成期、结构发展期和结构稳定期4个阶段,且模型中水化热和电阻率微分在表征水泥早期水化动力学过程具有较好的一致性,可以准确描述水泥水化历程及结构形成的瞬时状态。
3.首次提出了CE改性薄层水泥浆体在快速失水条件下的试验设计与评价方法,通过改变水泥浆体厚度、养护温度和基体材料的种类,系统研究了CE改性薄层水泥浆体的早期失水特征、界面性能和微观分析,探明了薄层水泥浆体的水化规律和微观结构发展机制。
以失水速度和失水率为评价指标,研究了薄层水泥浆体在快速失水条件下的早期失水特征,并阐述了其失水机制。分析了水泥浆体厚度、养护温度和基体材料的种类对薄层水泥浆体界面性能的影响,指出了不同龄期时的界面破坏形式。通过XRD、FTIR和TG-DSC分析,研究了薄层水泥浆体在快速失水条件下的水化规律。通过对快速失水条件下水泥浆体表层、中间层和界面层3个区域的微观分析,探明了水化产物沿水泥浆体厚度方向上的分布规律,揭示了薄层水泥浆体的界面破坏原理,为研究外墙外保温系统中保温层脱落和保护层的空鼓、开裂等问题奠定了理论基础。
4.根据薄层水泥-CE浆体中水分和离子的迁移、CE成膜、水泥浆体的硬化过程,分析了水化产物沿薄层水泥浆体厚度方向上的分布规律,建立了实际服役环境下的薄层水泥-CE浆体水化过程和界面过渡区微观结构模型。
根据CE成膜与溶解过程、薄层水泥浆体的失水机制与离子迁移过程、水化历程与微观结构发展机制、水化产物的分布规律,建立了实际服役环境下薄层水泥-CE浆体的水化过程模型。根据基体材料的孔结构与吸水特性,分析了薄层水泥浆体的失水特征、界面微结构的变化、水化产物的种类和数量分布,建立了薄层水泥浆体与基体材料间的界面过渡区微观结构模型,对于研究薄层水泥-CE浆体水化规律具有重要的理论与实际意义。
At present, urbanization in our country is in a rapid growth. External thermal insulation system is main technical approaches of building energy efficiency. Adhesive mortar and anti-crack mortar play an important role in protecting energy-saving effect and durability. Against this background, it has especially important significance of research of hydration key problems of thin layer mortar. The research was funded by National science and technology support project (No.2011BAJ04B02)" and Youth Fund of National Natural Science Foundation of China (No.50902107)". In multiple factors environment, kinetics of hydration process of cement paste modified with cellulose ether (CE) was verified by the research of rheological properties and heat-electrical characteristics. According to different service environment of cement paste, hydration mechanism of cement paste was studied under the condition of rapid water loss. To elaborate hydration characteristics of thin layer cement paste modified with CE, the model of hydration process and interface transition zone microstructure of thin layer cement paste modified with CE was established based on rheological properties, kinetics of hydration process and hydration mechanism under the condition of rapid water loss of cement paste modified with CE.
The main research and obtained important achievement of this article as follows:
1. Based on rheological behavior of CE in aqueous solution (mixing stage environment) and (hydration stage environment),film-forming process of CE and influence of solution environment (temperature, pH, ion species and valence) on rheological behavior of aqueous solution and cement pastes were studied. Film-forming process of CE in different liquid phase environment and mechanism of temperature, pH, ion species and valence were obtained.
Apparent viscosity, shear stress, yield stress and plastic viscosity were used as index system. The influence of kind and dosage of CE on rheological behavior was studied. Rheological properties of aqueous solution and cement paste which modified with CE were discussed under different temperature and pH. At the same time, the lower critical solution temperature and isoelectric point of CE were obtained. The sensitivity of HPMC, HEMC and HEC to pH is different. The influence of cations, anions and its valence on apparent viscosity of CE solution was respectively studied. Mechanism of ions species and valence was expounded based on lyotropic series and revealed the film-forming characteristics of CE in complex liquid phase environment. Theoretical basis was provided for studying the rheological properties of cement paste modified with CE in plastic stage.
2. Design and preparation methods of kinetics of hydration process of cement pastes modified with CE and cohesion water and slow release components (CWRC) were put forward. Based on hydration exothermic rate curve and derivate of resistivity curve of cement hydration, macro thermal effect and electrochemical characteristics change rule of early stage of cement hydration were mastered and the relationship among hydration exothermic, resistivity and cement hydration process was studied. Heat-electric model of system composed of CE, CWRC and cement was established.
The influence of CE and CWRC on hydration exothermic and resistivity of cement pastes was studied and delay effect of CWRC was less than CE on each stage of cement hydration was pointed out. It had linear dependence among Ca (OH)2content, chemically combined water content, hydration heat quantity and resistivity. A new structure parameter was provided to describe structure formation and hydration process. Heat-electric model of system composed of CE, CWRC and cement was established by analysis of hydration exothermic rate curve and derivate of resistivity curve of cement hydration. The process of cement hydration was divided into solution-precipitation equilibrium stage, structure formation stage, structure development stage and structure stability stage. It had a good consistency that description of hydration exothermic rate and derivate of resistivity on hydration kinetics process of cement in early stage. Instantaneous state of structure formation and process of cement hydration could be accurately described.
3. Trial design and evaluation methods of thin layer cement pastes modified with CE under rapid water-loss were first proposed. Water loss characteristics, interface properties and microscopic analysis were studied of cement pastes modified with CE in early stage by change of thickness of cement pastes, curing temperature and kinds of matrix materials. Hydration mechanism and principle of microstructure formation of thin layer cement pastes were found out.
Water-loss speed and water-loss rate were used as assessment criteria to study water-loss characteristics and mechanism of thin layer cement pastes under rapid water-loss. The influence of thickness of cement pastes, curing temperature and kinds of matrix materials on interface properties of thin layer cement pastes and described interface damage form of different ages. Hydration law of thin layer cement pastes under rapid water-loss was studied by XRD, FTIR and TG-DSC. Distribution regularities of hydration products along the thickness direction of cement paste were proved by microanalysis of surface layer, interlayer and interface layer of cement pastes under rapid water-loss. Principle of interfacial damage of thin layer cement paste was revealed and laid a theoretical basis for analysis of insulation layer drop and covering layer empty drum and cracking of external thermal insulation system.
4. Based on water and ion migration, CE film formation and hardening process of cement paste of thin layer cement pastes modified with CE, distribution regularities of hydration products along the thickness direction of cement paste were analyzed. The model of hydration process and interface transition zone microstructure of thin layer cement paste modified with CE under actual service environment was established.
The model of hydration process of cement paste modified with CE under actual service environment was established according to CE film formation and dissolve process, water-loss mechanism and ion migration process, hydration process and microstructure, distribution regularities of hydration products. Characteristics water-loss, changes of interface microstructure, kinds and amount of hydration products were analyzed on the basis of pore structure and water absorption of substrate materials and model between interface transition zone microstructure and matrix material of thin layer cement paste was established. It had important theoretical and practical significance of research on hydration mechanism of thin layer cement pastes modified with CE.
引文
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