水泥基材料低温结晶过程孔隙力学研究
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摘要
冻融破坏是水泥基材料主要耐久性问题之一。量化分析降温过程中孔隙溶液结晶过程以及该过程产生的孔隙压力是尚未解决的理论问题。本文在孔隙介质力学框架下，开展了降温过程中水泥基材料孔隙溶液结晶过程理论与实验研究。
本文首先研究了孔隙溶液结晶的基本物理化学过程，利用Gibbs-Tomson方程描述了冰晶体随着孔隙尺寸的扩展过程，考虑了溶液中离子对孔隙溶液结冰过程的影响。利用材料的性质以及成核理论，预测孔隙溶液的成核过冷度。论文扩展了非饱和孔隙介质力学理论，考虑了孔隙溶液压力和盐浓度对毛细压力的影响，考虑了压力和浓度梯度形成的水和溶质迁移。最终建立了多孔材料低温结晶过程的温度、压力、水分和离子的孔隙介质力学模型，并通过对经典问题的计算，验证了模型的有效性。论文选定了水泥基材料并特别设计了冻融变形测量装置，系统地研究了复合水泥基材料的孔隙结构，分析了压汞和氮气吸附法的测量特征以及应用范围，表征了水泥基材料的孔隙率、特征孔径、孔隙分布和比表面积，分析了孔隙表面的分形维和孔隙连通度，探讨了不同干燥方法对水泥基材料微结构的影响，测量了不同气泡含量干燥净浆和砂浆试件的温度变形，以及饱盐溶液水泥浆体试件的冻融变形。最后，本文利用建立的孔隙介质力学模型分析了非排水条件下不同浓度孔隙溶液结晶过程产生的变形，以及产生变形的原因，分析了排水和非排水边界条件下引气试件的低温变形。
研究显示，x冰与孔隙壁的接触角随着盐浓度的增加而降低； y在降温过程中，孔隙水的负压导致引气水泥基材料的持续收缩，而孔隙结晶压力导致非引气水泥基材料的持续膨胀； z过冷水结冰产生的巨大静水压力和瞬时温度升高导致了材料在结冰成核点附近的瞬时膨胀；{水泥基材料的孔隙结构表现出与尺寸相关的性质；|冰冻干燥只能干燥毛细孔水和部分低密度凝胶孔隙水；}材料的热膨胀系数与孔隙率成指数函数关系：α=α0(1)C；~非引气试件的低温膨胀变形与孔隙结构有关，引气试件的膨胀变形与气泡饱和度有关；非排水条件的非引气试件低温膨胀主要取决于结冰形成的静水压，而引气试件的低温变形取决于气泡形成的孔隙水压力边界条件。
Freeze-thaw (F-T) deterioration is one of the most important durability problem-s. Quantitative analysis of the pore pressure when pore solution solidifies, is still anopen question. Within the poromechanical frameworks, the present work studies thecrystallization processes of pore solution confined in cement based materials (CBM)theoretically and experimentally.
In the present work, the ice formation processes were first studied according tothermodynamic equilibrium, and the penetration of ice into thinner pores with temper-ature was described by Gibbs-Tomson equation. The impact of solutes was retained tomodify the solidification processes of pore solution. By means of material propertiesand heterogeneous nucleation (HN) theory, the relation between supercooled tempera-ture and the salt concentration of pore solution was established. From the poro-elastictheory, a poromechanical model was established to bridge over the crystallization ofpore solution and the macro behaviors of CBM under freezing. The Darciean and Fick-ian transport in porous medium were considered together in the present poromechan-ical model. The conservation equations for ions, water and energy were establishedon the basic variables: liquid pressure, salt concentration and temperature. The classicproblems of air-entrained CBM and the effect of supercooling were analyzed by theestablished model to verify its robustness.
The CBM samples were prepared and the set-up of deformation measurement ofCBM under F-T loadings was designed specially. The pore structure of samples werecharacterized comprehensively by mercury intrusion porosimetry (MIP) and Nitrogenadsorption/desorption (NAD). The porosity, characteristic pore size (CPS), pore sizedistribution (PSD) and specific surface area (SSA) were evaluated and discussed com-bined with the hydration processes. The fractal dimensions and drying effect of freeze-drying (F-drying) were discussed as well. The F-T deformation of dried pastes andmortars, entrained with different dosages of air-voids, were measured to obtain the ther-mal expansion coefficient (TEC). The F-T deformation of samples saturated with salinesolution were measured comprehensively. Poromechanical analysis was performed onthe sealed pastes saturated with saline solution under F-T loading, where the sources for deformation during freezing were specified in detail. The drained and undrainedconditions, corresponding to the empty and saturated air voids respectively, were usedto analyze the freezing deformation of air entrained CBM.
The study indicates that: x The contact angle between ice and pore wall decreaseswith salt concentrations; y Continual shrinkage of air-entrained paste (AEP) is dueto the negative liquid pressure and cryo-suction of ice formed on the interface of airvoids, while continual expansion of ordinary paste (OP) is due to the hydraulic pressureinduced by ice formation; z the instantaneous ice formation and the corresponding heatreleasing account for the ice nucleation significant deformation;{The blended cementpastes show the scale related properties;|F-drying only removes capillary water andpartial gel water confined in low density C-S-H;} The TEC of CBM is related to theporosity in form of power law: α=α0(1)C;~The F-T deformation of OP is relatedintimately to the pore structure, while the F-T deformation of AEP highly depends onthe saturation degree of air voids;The deformation of OP under undrained freezingis associated with the amount of ice formation, while the deformation of AEP dependson the boundary conditions charged by the saturation degree of air voids.
本文首先研究了孔隙溶液结晶的基本物理化学过程，利用Gibbs-Tomson方程描述了冰晶体随着孔隙尺寸的扩展过程，考虑了溶液中离子对孔隙溶液结冰过程的影响。利用材料的性质以及成核理论，预测孔隙溶液的成核过冷度。论文扩展了非饱和孔隙介质力学理论，考虑了孔隙溶液压力和盐浓度对毛细压力的影响，考虑了压力和浓度梯度形成的水和溶质迁移。最终建立了多孔材料低温结晶过程的温度、压力、水分和离子的孔隙介质力学模型，并通过对经典问题的计算，验证了模型的有效性。论文选定了水泥基材料并特别设计了冻融变形测量装置，系统地研究了复合水泥基材料的孔隙结构，分析了压汞和氮气吸附法的测量特征以及应用范围，表征了水泥基材料的孔隙率、特征孔径、孔隙分布和比表面积，分析了孔隙表面的分形维和孔隙连通度，探讨了不同干燥方法对水泥基材料微结构的影响，测量了不同气泡含量干燥净浆和砂浆试件的温度变形，以及饱盐溶液水泥浆体试件的冻融变形。最后，本文利用建立的孔隙介质力学模型分析了非排水条件下不同浓度孔隙溶液结晶过程产生的变形，以及产生变形的原因，分析了排水和非排水边界条件下引气试件的低温变形。
研究显示，x冰与孔隙壁的接触角随着盐浓度的增加而降低； y在降温过程中，孔隙水的负压导致引气水泥基材料的持续收缩，而孔隙结晶压力导致非引气水泥基材料的持续膨胀； z过冷水结冰产生的巨大静水压力和瞬时温度升高导致了材料在结冰成核点附近的瞬时膨胀；{水泥基材料的孔隙结构表现出与尺寸相关的性质；|冰冻干燥只能干燥毛细孔水和部分低密度凝胶孔隙水；}材料的热膨胀系数与孔隙率成指数函数关系：α=α0(1)C；~非引气试件的低温膨胀变形与孔隙结构有关，引气试件的膨胀变形与气泡饱和度有关；非排水条件的非引气试件低温膨胀主要取决于结冰形成的静水压，而引气试件的低温变形取决于气泡形成的孔隙水压力边界条件。
Freeze-thaw (F-T) deterioration is one of the most important durability problem-s. Quantitative analysis of the pore pressure when pore solution solidifies, is still anopen question. Within the poromechanical frameworks, the present work studies thecrystallization processes of pore solution confined in cement based materials (CBM)theoretically and experimentally.
In the present work, the ice formation processes were first studied according tothermodynamic equilibrium, and the penetration of ice into thinner pores with temper-ature was described by Gibbs-Tomson equation. The impact of solutes was retained tomodify the solidification processes of pore solution. By means of material propertiesand heterogeneous nucleation (HN) theory, the relation between supercooled tempera-ture and the salt concentration of pore solution was established. From the poro-elastictheory, a poromechanical model was established to bridge over the crystallization ofpore solution and the macro behaviors of CBM under freezing. The Darciean and Fick-ian transport in porous medium were considered together in the present poromechan-ical model. The conservation equations for ions, water and energy were establishedon the basic variables: liquid pressure, salt concentration and temperature. The classicproblems of air-entrained CBM and the effect of supercooling were analyzed by theestablished model to verify its robustness.
The CBM samples were prepared and the set-up of deformation measurement ofCBM under F-T loadings was designed specially. The pore structure of samples werecharacterized comprehensively by mercury intrusion porosimetry (MIP) and Nitrogenadsorption/desorption (NAD). The porosity, characteristic pore size (CPS), pore sizedistribution (PSD) and specific surface area (SSA) were evaluated and discussed com-bined with the hydration processes. The fractal dimensions and drying effect of freeze-drying (F-drying) were discussed as well. The F-T deformation of dried pastes andmortars, entrained with different dosages of air-voids, were measured to obtain the ther-mal expansion coefficient (TEC). The F-T deformation of samples saturated with salinesolution were measured comprehensively. Poromechanical analysis was performed onthe sealed pastes saturated with saline solution under F-T loading, where the sources for deformation during freezing were specified in detail. The drained and undrainedconditions, corresponding to the empty and saturated air voids respectively, were usedto analyze the freezing deformation of air entrained CBM.
The study indicates that: x The contact angle between ice and pore wall decreaseswith salt concentrations; y Continual shrinkage of air-entrained paste (AEP) is dueto the negative liquid pressure and cryo-suction of ice formed on the interface of airvoids, while continual expansion of ordinary paste (OP) is due to the hydraulic pressureinduced by ice formation; z the instantaneous ice formation and the corresponding heatreleasing account for the ice nucleation significant deformation;{The blended cementpastes show the scale related properties;|F-drying only removes capillary water andpartial gel water confined in low density C-S-H;} The TEC of CBM is related to theporosity in form of power law: α=α0(1)C;~The F-T deformation of OP is relatedintimately to the pore structure, while the F-T deformation of AEP highly depends onthe saturation degree of air voids;The deformation of OP under undrained freezingis associated with the amount of ice formation, while the deformation of AEP dependson the boundary conditions charged by the saturation degree of air voids.
引文
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