热塑改性热固性树脂体系固化中的形貌—流变学研究
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摘要
以反应诱导相分离方法实现热塑性树脂TP增韧热固性树脂TS是很有希望的途径,其关键是TP分散状态的控制。本论文在较宽的时间—温度空间研究了众多热力学特征不同的TP改性TS体系(包括具有上临界共溶温度UCST相行为体系、具有下临界共溶温度LCST相行为体系)和液晶环氧单体改性热固性树脂体系的反应诱导相分离过程,其中基体TS树脂的化学反应有逐步聚合、链式聚合和催化聚合。主要的方法是以流变学与显微光学形态实时检测、配以热化学方法追踪固化分相转变,并与相分离动力学模拟结合,从而达到弄清分相机理,控制分相形貌,明确加工时间-温度空间的目的。
本实验室建立的高温倒置高分辨光学显微系统,成功的表征了众多TP改性TS体系的反应诱导相分离的起始、演化过程。在较宽的时间—温度空间研究了众多热力学特征不同的TP/TS体系和液晶环氧单体改性热固性树脂体系的反应诱导相分离过程。
反应诱导相分离过程中流变性质的转变符合临界凝胶理论。不同的转变分别对应不同的凝胶转变机理。在化学凝胶点之前发生相分离,由于TP相的富集浓缩而首先形成物理缠结网;在TS的化学凝胶点,由化学交联引起化学临界凝胶转变。在后固化中,也观察到了与TP相玻璃化有关的临界凝胶转变。各临界凝胶点对应不同的临界凝胶指数或分形维数,反映了不同的网络结构状态。对凝胶指数作了温度与浓度依赖性的分析,不同的临界凝胶指数具有温度或浓度依赖性。
发现TP改性TS体系的反应诱导相分离时间/N度遵循Arrhenius方程,具有普适性。相分离活化能E_a(ps)在实验的TP浓度范围内和温度范围内受化学环境和化学反应热力学与反应机理影响显著,而与TP含量、TP的分子量、反应速度和相分离检测手段等关系不大。利用二元相互作用能理论解释了一些UCsT体系E_a(ps)与组分化学结构的依赖关系。利用建立的反应诱导相分离的时间-温度依赖关系式,绘制了TP改性TS复合体系的含有相结构信息的时间—温度转化相图(TTT diagram)。
从光学、流变学、化学热力学等角度初步研究了热固性液晶单体改性氰酸酯体系的形貌-流变学特征。发现液晶环氧单体对基体热固性树脂的固化反应具有加速作用,并且提高基体树脂的初始粘度与模量;对于液晶热固性树脂改性TS体系,介观相分离结构的形成不是基体TS韧性提高的必要条件。
利用改进的弹性固体模型模拟了TP改性TS体系在离位层状化增韧过程中的反应诱导相分离形貌演化特征,与实验结果相符合。
Improving the toughness of TS (thermosetting resins) through cure induced phase separation is a promising approach with the prerequisite of appropriate control of the phase separated structure. The present work has been focused on the cure induced phase separation process in various TP (thermoplastics) toughened thermosetting systems including systems with UCST (upper critical solution temperature) or LCST (lower critical solution temperature) phase behavior in wide time/temperature window. The phase separation process was detected in situ by means of dynamic rheology and optical microscope, together with the thermal analysis. The morphology evolvement process in constrained space was simulated based on modified TGDL (time dependent Ginzberg Landau) function.
An inversed optical microscope system with high resolution and high temperature duration was set up which successfully characterized the onset and evolvement of the phase separation process in various TP/TS systems, including UCST/LCST systems, the liquid crystal monomer modified thermosetting systems.
The chemorheology of different TP/TS systems were analyzed and criticalgel transitions were found which arise from different gelation mechanism.Gelation at phase separation is the result of entanglement of TP macromolecules;gelation at chemical gel point corresponds to the branching and cross linking of thermosetting oligomers. Critical gelation transitions were also observed in the post cure stage which is a result of physical gelation arising from the glass transition of TP rich phase. The relaxation exponents of the gels formed at different cure stage show temperature and/or TP content dependence.
It was found that the cure induced phase separation time/temperature dependence can be well described by the Arrhenius equation. The phase separation activation energy E_α(ps) keeps constant with the variations of TP content, TP molecular weight, curing rate and phase separation detecting means, while varies with the chemical environments and the time/temperature dependence of the cure reaction. The change of E_α(ps) of some UCST TP/TS systems was elucidated in view of interaction energy density theory. It was shown that E_α(ps) decreases with the deterioration of miscibility of the blends and increase with the increase of the TP/TS miscibility. TTT (time temperature transformation diagram) with morphology was set up which can provide intellectual understanding of the cure process of TP/TS systems.
The morphology evolvement of systems in interleaves of TP and TS wassimulated by the modified TGDL (time dependent Ginzberg-Landau) functionwith pre-set concentration ingredient, and the simulated morphology is consistentwith the experimental results qualatitively.
The liquid crystal epoxy monomer modified cyanate ester systems wasstudied primarily by rheology, thermal analysis and morphological approaches.The incorporation of liquid crystal monomer will accelerate the cure rate of the matrix resin and also increase the initial viscosity. It was found that the meso-scale phase separated structure is not a necessary condition for the toughness enhancement in the liquid crystal epoxy monomer modified cyanate ester systems.
本实验室建立的高温倒置高分辨光学显微系统,成功的表征了众多TP改性TS体系的反应诱导相分离的起始、演化过程。在较宽的时间—温度空间研究了众多热力学特征不同的TP/TS体系和液晶环氧单体改性热固性树脂体系的反应诱导相分离过程。
反应诱导相分离过程中流变性质的转变符合临界凝胶理论。不同的转变分别对应不同的凝胶转变机理。在化学凝胶点之前发生相分离,由于TP相的富集浓缩而首先形成物理缠结网;在TS的化学凝胶点,由化学交联引起化学临界凝胶转变。在后固化中,也观察到了与TP相玻璃化有关的临界凝胶转变。各临界凝胶点对应不同的临界凝胶指数或分形维数,反映了不同的网络结构状态。对凝胶指数作了温度与浓度依赖性的分析,不同的临界凝胶指数具有温度或浓度依赖性。
发现TP改性TS体系的反应诱导相分离时间/N度遵循Arrhenius方程,具有普适性。相分离活化能E_a(ps)在实验的TP浓度范围内和温度范围内受化学环境和化学反应热力学与反应机理影响显著,而与TP含量、TP的分子量、反应速度和相分离检测手段等关系不大。利用二元相互作用能理论解释了一些UCsT体系E_a(ps)与组分化学结构的依赖关系。利用建立的反应诱导相分离的时间-温度依赖关系式,绘制了TP改性TS复合体系的含有相结构信息的时间—温度转化相图(TTT diagram)。
从光学、流变学、化学热力学等角度初步研究了热固性液晶单体改性氰酸酯体系的形貌-流变学特征。发现液晶环氧单体对基体热固性树脂的固化反应具有加速作用,并且提高基体树脂的初始粘度与模量;对于液晶热固性树脂改性TS体系,介观相分离结构的形成不是基体TS韧性提高的必要条件。
利用改进的弹性固体模型模拟了TP改性TS体系在离位层状化增韧过程中的反应诱导相分离形貌演化特征,与实验结果相符合。
Improving the toughness of TS (thermosetting resins) through cure induced phase separation is a promising approach with the prerequisite of appropriate control of the phase separated structure. The present work has been focused on the cure induced phase separation process in various TP (thermoplastics) toughened thermosetting systems including systems with UCST (upper critical solution temperature) or LCST (lower critical solution temperature) phase behavior in wide time/temperature window. The phase separation process was detected in situ by means of dynamic rheology and optical microscope, together with the thermal analysis. The morphology evolvement process in constrained space was simulated based on modified TGDL (time dependent Ginzberg Landau) function.
An inversed optical microscope system with high resolution and high temperature duration was set up which successfully characterized the onset and evolvement of the phase separation process in various TP/TS systems, including UCST/LCST systems, the liquid crystal monomer modified thermosetting systems.
The chemorheology of different TP/TS systems were analyzed and criticalgel transitions were found which arise from different gelation mechanism.Gelation at phase separation is the result of entanglement of TP macromolecules;gelation at chemical gel point corresponds to the branching and cross linking of thermosetting oligomers. Critical gelation transitions were also observed in the post cure stage which is a result of physical gelation arising from the glass transition of TP rich phase. The relaxation exponents of the gels formed at different cure stage show temperature and/or TP content dependence.
It was found that the cure induced phase separation time/temperature dependence can be well described by the Arrhenius equation. The phase separation activation energy E_α(ps) keeps constant with the variations of TP content, TP molecular weight, curing rate and phase separation detecting means, while varies with the chemical environments and the time/temperature dependence of the cure reaction. The change of E_α(ps) of some UCST TP/TS systems was elucidated in view of interaction energy density theory. It was shown that E_α(ps) decreases with the deterioration of miscibility of the blends and increase with the increase of the TP/TS miscibility. TTT (time temperature transformation diagram) with morphology was set up which can provide intellectual understanding of the cure process of TP/TS systems.
The morphology evolvement of systems in interleaves of TP and TS wassimulated by the modified TGDL (time dependent Ginzberg-Landau) functionwith pre-set concentration ingredient, and the simulated morphology is consistentwith the experimental results qualatitively.
The liquid crystal epoxy monomer modified cyanate ester systems wasstudied primarily by rheology, thermal analysis and morphological approaches.The incorporation of liquid crystal monomer will accelerate the cure rate of the matrix resin and also increase the initial viscosity. It was found that the meso-scale phase separated structure is not a necessary condition for the toughness enhancement in the liquid crystal epoxy monomer modified cyanate ester systems.
引文
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