聚二甲基硅氧烷/二氧化硅复合网络及环氧树脂/聚二甲基硅氧烷互穿网络的研究
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摘要
互穿聚合物网络(Interpenetrating Polymer Network，IPN)是由两种或两种以上聚合物通过网络的互相贯穿缠结而形成的一类独特的聚合物共混物或聚合物合金。网络之间的互穿为材料带来许多独特性能，如“强迫互容”和协同效应等，使得IPN在增韧树脂、增强橡胶、阻尼材料等多方面得到广泛应用。
环氧树脂作为一种工业广泛使用的材料，它具有许多优异的性能，但质脆、耐冲击性较差和容易开裂的弱点限制了环氧树脂的应用。用聚二甲基硅氧烷(PDMS)改性环氧树脂既能降低环氧树脂的内应力，又能保持环氧树脂体系原有特性并提高其热稳定性和阻燃能力，因此PDMS用于改性环氧树脂是较好的选择。但由于PDMS与环氧树脂热力学不相容，故PDMS增韧环氧树脂仅限于官能团端基反应、嵌段及接枝改性等方法，这些方法在增韧环氧树脂的同时常会带来环氧树脂某些性能如模量的大幅下降。故合成环氧树脂／PDMS IPN成为一个研究热点。
本文采用改性二氧化硅作为增容剂，设计了一种半分步、半同步的方法合成(双酚A型环氧树脂／环氧改性二氧化硅)／PDMS互穿网络[(DGEBA／e-silica)／PDMS IPN]。在制备过程中首先在二氧化硅表面接枝环氧基团，然后将经过适当预聚的PDMS与DGEBA、e-silica混合于三氯甲烷中。在此过程中，e-silica充当增容剂：一方面，e-silica表面的环氧基团能参与DGEBA固化反应；另一方面，二氧化硅表面的羟基与PDMS之间又发生氢键作用。依靠e-silica的增容，相分离被有效抑制。因氢键生成与作用时间有关，故在PDMS适当预聚后再与DGEBA及e-silica体系混合进行同步反应，这是该方法采用半分步、半同步的原因。在接下来的反应中，PDMS与DGEBA的反应同步但独立进行。合成的(DGEBA／m-silica)／PDMS IPN用示差扫描量热法(DSC)、透射电镜(TEM)及扫描电镜(SEM)等进行表征。DSC表征发现IPN存在三个玻璃化转变，其中两个玻璃化转变向中间靠拢并变宽，第三个玻璃化温度表明分子水平的互穿。TEM研究发现二氧化硅在IPN呈纳米水平分散，试样断面的SEM照片表明DGEBA由脆性断裂转变为IPN的韧性断裂。互穿网络拉伸强度随PDMS及二氧化硅含量的增加出现一个极大值，该值大于纯DGEBA的拉伸强度。冲击强度及断裂伸长率则随PDMS含量的增加而增加。IPN耐热性能随PDMS含量的增加而提高，热稳定性优于纯DGEBA。
本文设计了共同溶剂法同步合成了最小相畴尺寸为5纳米的DGEBA／PDMS互穿网络。共同溶剂的使用保证了DGEBA与PDMS处于单体阶段的相容性。保证DGEBA与PDMS在凝胶前固化速率一致，就能够获得接近分子水平的互穿。与一般共混法制备的DGEBA／PDMS共混物相比，IPN中相畴显著变小，动态储能模量下降较少。DSC研究发现IPN呈现两个明显相互靠拢的玻璃化温度区。IPN扫描断面均较光滑，看不到明显的两相结构及界面。扫描电镜结合X射线能谱仪(SEM-EDX)结果发现IPN断面20μm区域中与其中任意局部约1μm区域中的元素分布相同。原子力显微镜(AFM)研究发现DGEBA／PDMS IPN的相畴尺寸为5～10 nm。
本文提出了复合网络法用乙烯基二氧化硅(vi-silica)对PDMS进行增强的新方法。先通过干法用乙烯基三乙氧基硅烷对二氧化硅进行表面处理，得到的vi-silica能够参与硅氢化反应，从而在二氧化硅与PDMS之间形成化学键，形成无机-有机复合网络。在不同气氛及不同乙烯基与氢基摩尔比情况下测得的凝胶含量均证实vi-silica参与了硅氢化作用。正是由于无机有机复合网络的生成使二氧化硅填充PDMS体系具有良好的机械性能。
针对二氧化硅填充PDMS体系的凝胶时间及性能，本文研究了二氧化硅预处理温度对改性的影响。当二氧化硅用六甲基二硅胺烷及六甲基环三硅氧烷(D3)处理时，发现二氧化硅预处理温度越高，二氧化硅填充PDMS体系凝胶时间越长，但机械性能并随之下降；预处理温度越低，二氧化硅填充体系凝胶时间越短，机械性能增强。
本论文通过对DGEBA、PDMS、二氧化硅各种组合体系的系统研究，发现了DGEBA／PDMS互穿网络、增强PDMS的制备新方法，提出了上述体系增强、增韧的新机理，对实际生产具有一定的指导意义。
An interpenetrating polymer network (IPN) is a composition of two or more chemically distinct polymer networks held together exclusively by their permanent mutual entanglements. Three-dimensional cross-linked structures that contain entangled polymeric segments generate Synergistic effects induced by forced compatibility of the components and thus can be used for toughening, reinforcing, and damping, etc.
As one of the most important engineering polymeric materials epoxy resin possesses excellent properties. However, the low crack growth resistance restricts application. Polydimethylsiloxane (PDMS) was generally selected as a modifier to improve the thermal stability, hydrophobicity, and flexibility at low temperatures of epoxy resin. Unfortunately, PDMS is immiscible with epoxy resins. In order to improve the miscibility of epoxy and PDMS, some approaches have been tried including functional group capping, block inserting, as well as grafting. However, the above approaches have some disadvantage, especially reducing the modulus of epoxy resin. It is interesting to notice that the IPN technique constituted an effective method to inhibit the decreasing of modulus.
A novel semi-simultaneous, semi-sequential methodology wasdesigned to prepare a (diglycidylether of bisphenol A / epoxy modifiedsilica)/ PDMS IPN [(DGEBA/e-silica)/PDMS IPN] in this paper. Firstcrude silica was modified using silsisquioxane to introduce epoxy groupsonto the surface of silica. The vinyl-terminated PDMS (vinyl-DPMS) andhydrogen-containing PDMS(H-PDMS) were pre-cured throughhydrosilylation to some degree of crosslinking, into which DGEBA ande-silica were subsequently introduced as a solution in trichloromethane.The e-silica played a role as a compatibilizer: it co-cured with DGEBA andgenerated H-bonding with the oxygen atoms on the PDMS, and thus thecuring-induced phase separation was inhibited. Due to the formation ofH-bonding depending on time, the mixing of PDMS system with DGEBAsystem was carried out after an adequate pre-curing, consequently themethod was denoted as "semi-simultaneous, semi-sequential". In thesubsequent reactions, the curing reactions of DGEBA and the PDMSoccurred independently and simultaneously, an IPN structure was generated.The IPN sample was characterized using differential scanning calorimetry(DSC), (Transmission electron microscopy) TEM, and scanning electron microscopy (SEM). DSC indicated three glass transitions on the spectrum, with two for the parent polymers displaced toward the center of the spectrum, the third one indicating the intermolecular interactions between the components. TEM indicated that silica was dispersed in matrix in nanometer level. SEM showed that the interpenetrating of PDMS with DGEBA in form of networks caused a brittle-ductile transition of the latter resulting in better ductility and toughness. The tensile strength of the IPN exhibited a maximum as the fraction of PDMS network and e-silica increased. The elongations at break and impact strength kept increasing with increasing content of PDMS. Thermal stability increased with increasing content of PDMS, and a better thermal stability was obtained than the neat DGEBA.
DGEBA/PDMS IPN with domains of about 5 nm diameter was prepared via a simultaneous approach in a common solvent of DGEBA and PDMS. The common solvent supplied the initial miscibility between DGEBA and PDMS. The comparable gelling rates of the two systems before gelation are critical to prepare IPN near molecular level. Compared with plain DGEBA/PDMS blends, the domains size of the IPN is obvious smaller and thus fewer reduction in storage modulus. DSC indicated that broadened and displaced glass transitions for the segments of DGEBA resin which revealed a three-dimensional interlock structure of the two components. SEM indicated that the surface of IPN was smooth and no obvious phase boundary. Scanning electron microscopy-Energy dispersive X-ray (SEM-EDX) showed that the dispersion of elements is not different between domains 20μm and 1μm. Atomic force microscopy (AFM) conformed that the domain size in the IPN ranged from 5-10 nm.
A novel methodology of reinforcement of PDMS through formation of inorganic-organic hybrid network was proposed. Silica was modified with vinyltriethoxysilane through a dry method. The vinyl-modified silica (vi-silica) containing vinyl groups was employed to reinforce PDMS by participating in the hydrosilation reaction. An inorganic-organic hybrid network was formed to reinforce PDMS due to chemical bonding between vi-silica and PDMS. The gel contents resulting from various vinyl/hydrogen mole ratios and different atmospheres confirmed that vi-silica participated in the hydrosilation. The inorganic-organic hybrid network provided better mechanical properties.
The influence of pre-treatment temperature on gel time and mechanical properties of modified silica (m-silica) filled PDMS system was studied. Silica was modified with hexamethyldisilazane and hexamethyltrisiloxane (D3) via dry method. When the pre-treatment temperature was increased, the gel time of m-silica filled PDMS system increased but mechanical properties decreased. However, when the pre-treatment temperature was too low, the gel time decreased and the mechanical properties increase. For this reason the pre-treatment should be carried out at an optimal temperature.
In summary, the reinforcement and toughening approaches and mechanisms for various networks of DGEBA/PDMS/silica were explored in this dissertation. The discoveries made in this work will be valuable for the further research and practical production.
环氧树脂作为一种工业广泛使用的材料，它具有许多优异的性能，但质脆、耐冲击性较差和容易开裂的弱点限制了环氧树脂的应用。用聚二甲基硅氧烷(PDMS)改性环氧树脂既能降低环氧树脂的内应力，又能保持环氧树脂体系原有特性并提高其热稳定性和阻燃能力，因此PDMS用于改性环氧树脂是较好的选择。但由于PDMS与环氧树脂热力学不相容，故PDMS增韧环氧树脂仅限于官能团端基反应、嵌段及接枝改性等方法，这些方法在增韧环氧树脂的同时常会带来环氧树脂某些性能如模量的大幅下降。故合成环氧树脂／PDMS IPN成为一个研究热点。
本文采用改性二氧化硅作为增容剂，设计了一种半分步、半同步的方法合成(双酚A型环氧树脂／环氧改性二氧化硅)／PDMS互穿网络[(DGEBA／e-silica)／PDMS IPN]。在制备过程中首先在二氧化硅表面接枝环氧基团，然后将经过适当预聚的PDMS与DGEBA、e-silica混合于三氯甲烷中。在此过程中，e-silica充当增容剂：一方面，e-silica表面的环氧基团能参与DGEBA固化反应；另一方面，二氧化硅表面的羟基与PDMS之间又发生氢键作用。依靠e-silica的增容，相分离被有效抑制。因氢键生成与作用时间有关，故在PDMS适当预聚后再与DGEBA及e-silica体系混合进行同步反应，这是该方法采用半分步、半同步的原因。在接下来的反应中，PDMS与DGEBA的反应同步但独立进行。合成的(DGEBA／m-silica)／PDMS IPN用示差扫描量热法(DSC)、透射电镜(TEM)及扫描电镜(SEM)等进行表征。DSC表征发现IPN存在三个玻璃化转变，其中两个玻璃化转变向中间靠拢并变宽，第三个玻璃化温度表明分子水平的互穿。TEM研究发现二氧化硅在IPN呈纳米水平分散，试样断面的SEM照片表明DGEBA由脆性断裂转变为IPN的韧性断裂。互穿网络拉伸强度随PDMS及二氧化硅含量的增加出现一个极大值，该值大于纯DGEBA的拉伸强度。冲击强度及断裂伸长率则随PDMS含量的增加而增加。IPN耐热性能随PDMS含量的增加而提高，热稳定性优于纯DGEBA。
本文设计了共同溶剂法同步合成了最小相畴尺寸为5纳米的DGEBA／PDMS互穿网络。共同溶剂的使用保证了DGEBA与PDMS处于单体阶段的相容性。保证DGEBA与PDMS在凝胶前固化速率一致，就能够获得接近分子水平的互穿。与一般共混法制备的DGEBA／PDMS共混物相比，IPN中相畴显著变小，动态储能模量下降较少。DSC研究发现IPN呈现两个明显相互靠拢的玻璃化温度区。IPN扫描断面均较光滑，看不到明显的两相结构及界面。扫描电镜结合X射线能谱仪(SEM-EDX)结果发现IPN断面20μm区域中与其中任意局部约1μm区域中的元素分布相同。原子力显微镜(AFM)研究发现DGEBA／PDMS IPN的相畴尺寸为5～10 nm。
本文提出了复合网络法用乙烯基二氧化硅(vi-silica)对PDMS进行增强的新方法。先通过干法用乙烯基三乙氧基硅烷对二氧化硅进行表面处理，得到的vi-silica能够参与硅氢化反应，从而在二氧化硅与PDMS之间形成化学键，形成无机-有机复合网络。在不同气氛及不同乙烯基与氢基摩尔比情况下测得的凝胶含量均证实vi-silica参与了硅氢化作用。正是由于无机有机复合网络的生成使二氧化硅填充PDMS体系具有良好的机械性能。
针对二氧化硅填充PDMS体系的凝胶时间及性能，本文研究了二氧化硅预处理温度对改性的影响。当二氧化硅用六甲基二硅胺烷及六甲基环三硅氧烷(D3)处理时，发现二氧化硅预处理温度越高，二氧化硅填充PDMS体系凝胶时间越长，但机械性能并随之下降；预处理温度越低，二氧化硅填充体系凝胶时间越短，机械性能增强。
本论文通过对DGEBA、PDMS、二氧化硅各种组合体系的系统研究，发现了DGEBA／PDMS互穿网络、增强PDMS的制备新方法，提出了上述体系增强、增韧的新机理，对实际生产具有一定的指导意义。
An interpenetrating polymer network (IPN) is a composition of two or more chemically distinct polymer networks held together exclusively by their permanent mutual entanglements. Three-dimensional cross-linked structures that contain entangled polymeric segments generate Synergistic effects induced by forced compatibility of the components and thus can be used for toughening, reinforcing, and damping, etc.
As one of the most important engineering polymeric materials epoxy resin possesses excellent properties. However, the low crack growth resistance restricts application. Polydimethylsiloxane (PDMS) was generally selected as a modifier to improve the thermal stability, hydrophobicity, and flexibility at low temperatures of epoxy resin. Unfortunately, PDMS is immiscible with epoxy resins. In order to improve the miscibility of epoxy and PDMS, some approaches have been tried including functional group capping, block inserting, as well as grafting. However, the above approaches have some disadvantage, especially reducing the modulus of epoxy resin. It is interesting to notice that the IPN technique constituted an effective method to inhibit the decreasing of modulus.
A novel semi-simultaneous, semi-sequential methodology wasdesigned to prepare a (diglycidylether of bisphenol A / epoxy modifiedsilica)/ PDMS IPN [(DGEBA/e-silica)/PDMS IPN] in this paper. Firstcrude silica was modified using silsisquioxane to introduce epoxy groupsonto the surface of silica. The vinyl-terminated PDMS (vinyl-DPMS) andhydrogen-containing PDMS(H-PDMS) were pre-cured throughhydrosilylation to some degree of crosslinking, into which DGEBA ande-silica were subsequently introduced as a solution in trichloromethane.The e-silica played a role as a compatibilizer: it co-cured with DGEBA andgenerated H-bonding with the oxygen atoms on the PDMS, and thus thecuring-induced phase separation was inhibited. Due to the formation ofH-bonding depending on time, the mixing of PDMS system with DGEBAsystem was carried out after an adequate pre-curing, consequently themethod was denoted as "semi-simultaneous, semi-sequential". In thesubsequent reactions, the curing reactions of DGEBA and the PDMSoccurred independently and simultaneously, an IPN structure was generated.The IPN sample was characterized using differential scanning calorimetry(DSC), (Transmission electron microscopy) TEM, and scanning electron microscopy (SEM). DSC indicated three glass transitions on the spectrum, with two for the parent polymers displaced toward the center of the spectrum, the third one indicating the intermolecular interactions between the components. TEM indicated that silica was dispersed in matrix in nanometer level. SEM showed that the interpenetrating of PDMS with DGEBA in form of networks caused a brittle-ductile transition of the latter resulting in better ductility and toughness. The tensile strength of the IPN exhibited a maximum as the fraction of PDMS network and e-silica increased. The elongations at break and impact strength kept increasing with increasing content of PDMS. Thermal stability increased with increasing content of PDMS, and a better thermal stability was obtained than the neat DGEBA.
DGEBA/PDMS IPN with domains of about 5 nm diameter was prepared via a simultaneous approach in a common solvent of DGEBA and PDMS. The common solvent supplied the initial miscibility between DGEBA and PDMS. The comparable gelling rates of the two systems before gelation are critical to prepare IPN near molecular level. Compared with plain DGEBA/PDMS blends, the domains size of the IPN is obvious smaller and thus fewer reduction in storage modulus. DSC indicated that broadened and displaced glass transitions for the segments of DGEBA resin which revealed a three-dimensional interlock structure of the two components. SEM indicated that the surface of IPN was smooth and no obvious phase boundary. Scanning electron microscopy-Energy dispersive X-ray (SEM-EDX) showed that the dispersion of elements is not different between domains 20μm and 1μm. Atomic force microscopy (AFM) conformed that the domain size in the IPN ranged from 5-10 nm.
A novel methodology of reinforcement of PDMS through formation of inorganic-organic hybrid network was proposed. Silica was modified with vinyltriethoxysilane through a dry method. The vinyl-modified silica (vi-silica) containing vinyl groups was employed to reinforce PDMS by participating in the hydrosilation reaction. An inorganic-organic hybrid network was formed to reinforce PDMS due to chemical bonding between vi-silica and PDMS. The gel contents resulting from various vinyl/hydrogen mole ratios and different atmospheres confirmed that vi-silica participated in the hydrosilation. The inorganic-organic hybrid network provided better mechanical properties.
The influence of pre-treatment temperature on gel time and mechanical properties of modified silica (m-silica) filled PDMS system was studied. Silica was modified with hexamethyldisilazane and hexamethyltrisiloxane (D3) via dry method. When the pre-treatment temperature was increased, the gel time of m-silica filled PDMS system increased but mechanical properties decreased. However, when the pre-treatment temperature was too low, the gel time decreased and the mechanical properties increase. For this reason the pre-treatment should be carried out at an optimal temperature.
In summary, the reinforcement and toughening approaches and mechanisms for various networks of DGEBA/PDMS/silica were explored in this dissertation. The discoveries made in this work will be valuable for the further research and practical production.
引文
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