PP/POE共混体系的微结构与性能
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摘要
多相聚合物微结构与材料的性能有着密切联系,而微结构的形成强烈地依赖于加工条件。研究材料的凝聚态结构、形成条件及其与材料性能之间的关系,对于高分子材料的设计和性能优化具有十分重要的意义。本文采用熔融共混法制备了等规聚丙烯(PP)/乙烯-辛烯共聚物(POE)共混物,研究了PP/POE共混物的熔融结晶行为、压力-体积-温度(PVT)属性、力学性质和粘弹性,探讨了PP/POE共混物在注射成型过程中分散相结构演化和多层结构,得出主要结论如下:
1、当POE含量较低时,PP的表观诱导期(⊿t_1)随着POE含量的增加而下降,POE的加入加速了PP的结晶过程(表观总结晶期⊿t_c减少);当POE含量较高时,PP的⊿t_i和⊿t_c随着POE含量的增加而延长。随着POE含量增加,共混体系中PP相的T_m,T_(mp)和T_(m,onset)均向低温偏移,表明PP与POE分子间存在一定的作用力,具有一定程度的相容性。随着POE的加入,不仅使PP晶区变小,而且破坏了PP的球晶结构。对PP/POE共混体系的结晶动力学模型分析,发现Ozawa模型不适合描述该体系的结晶过程,莫志深法和Urbanovici-Segal模型可以很好地描述该体系的非等温结晶动力学。
2、采用毛细管流变仪和Haake转矩流变仪对PP/POE共混体系测试的结果基本一致,共混物熔体表现为假塑性流变行为。随着POE含量的增加,PP/POE共混物熔体的表观黏度和非牛顿指数表现为负偏差行为,粘流活化能则表现出正负偏差行为。
3、PP/POE共混物在注塑成型过程中形成多层结构,即表层、过渡层、剪切层和芯层。其中剪切层中POE的形变度(D)最大,POE被拉长、断裂,并呈现为扁椭球形,而芯层和过渡层形变度较小。另一方面,表层中无POE相存在,而芯层POE含量最大,剪切层POE含量次之,据此提出了PP/POE共混物在注塑成型过程中分散相形态演化的多层结构模型。此外,剪切对PP/POE共混物中PP的β晶形成影响很大,在表层和特别是剪切层中含有较多的β晶,而在芯层则没有发现β晶的存在。
4、在PP/POE共混物注塑制品中,表层的PP熔点接近于纯PP,而其它层中的PP的熔点均比表层低。芯层的T_(peak)和T_(end)比过渡层和剪切层略高,但比表层低。由于表层降温快,导致该层PP的熔程宽,结晶度低,而芯层PP的结晶度最大。PP/POE共混物的结晶温度与压力的关系符合线性关系T_c=T_(c,0)+kp。随着POE含量增加,高压下结晶的PP/POE共混物中PP熔融行为与常压下结晶的正好相反。
5、注塑制品各层的DMA研究表明:在相同的加工温度下,芯层的储能模量较剪切层大。提高加工温度,无论是芯层还是过渡层,其储能模量均提高。此外芯层和剪切层的储能模量对不同频率的响应也不同。当加工温度较低时,增大实验频率,芯层的E′比剪切层的E′响应更明显,而加工温度较高时,芯层的E′和剪切层的E′的响应趋于一致。
6、Tait状态方程可用来预测部分相容的、半结晶PP/POE共混物的PVT性质、结晶行为。PP结晶前后的比容变化比POE的大得多,随着POE含量的增加,PP/POE共混物结晶前和结晶后比容的变化均逐渐减小。PP在熔融状态下的热膨胀系数(α)比固体状态的大,而POE正好相反。PP/POE共混物的α随温度、压力的变化与其组成密切相关。此外,采用Simha-Somcynsky模型(S-S)模型计算得到的V_(sp)结果值与PP/POE熔融态实验值吻合得非常好,说明S-S理论模型可以很好地描述PP/POE共混体系熔融态的PVT行为。
7、随着POE含量增加,PP/POE共混物的储能模量逐渐减小,而损耗模量、力学损耗增大。PP/POE共混物中PP和POE的T_g均随着POE含量的增大而升高,其中POE相T_g升高的幅度大于PP相T_g升高的幅度。PP/POE共混体系中PP和POE玻璃化温度的变化反映了PP和POE之间有较强的相互作用力,说明了PP与POE有一定的相容性。Kerner分散相模型和连续相模型可以很好地预测PP/POE共混物的粘弹性和相形态结构。
8、随着POE含量增加,共混体系的常温冲击强度和低温冲击强度都表现为增加的趋势,但拉伸强度和模量逐渐减小。当POE的含量达到30%左右时,常温缺口冲击强度增长幅度迅速增大,出现脆韧转变(BDT)。POE的增韧机理主要为银纹支化机理和逾渗机理。
Properties of multiphase polymeric materials are related to their microstructure greatly,and the formation of their microstructure depends on processing condition.It is very important for the structural design and modification of polymeric materials.In this dissertation, isotactic polypropylene(PP)/ethylene-octene copolymer(POE) blends were prepared in melting state,their melting and crystallization behaviors,P-V-T properties,mechanical properties and viscoelasticity were systematically investigated,the morphological evolution of the dispersed phases and multi-layered microstructures of PP/POE blends during injection molding were discussed.The main conclusions are as following:
1) At the low content of POE,the addition of POE decreases the apparent incubation period (⊿t_i) and the apparent total crystallization period(⊿t_c) of PP in blends due to the heterogeneous nucleation of POE.However,at high content of POE,the addition of POE decreases the mobility of PP segments due to their strong interrnolecular interaction and chain entanglements,resulting in retarding the crystallization of PP,decreasing in the amount ofβ-form PP crystals,and increasing in⊿t_i and⊿t_c of PP in blends.T_m,T_(mp) and T_(m,onset) of PP in PP/POE blends all shift towards lower temperature with addition of POE. The depressions in melting temperature of PP phase in the blends indicate that there might be a strong intermolecular interaction between PP and POE.PP spherulites in blends are defective and their crystallization behavior is influenced intensely by the incorporation of POE.Additionally,the non-isothermal crystallization of blends were analysed by Jeziorny, Ozawa,Urbanovici-segal,Mo and Ziabicki models,respectively.Urbanovici-segal and Mo models are more suitable to describe the non-isothermal crystallization of the blends.
2) The rheological results measured by the capillary and torque rheometers are almost similar.PP,POE and PP/POE blend melts are pseudoplastic fluids.With increasing the POE content in blends,their non-Newtonian constant and apparent viscosity exhibit the behavior of the negative deviation blend(NDB),but their flow activation energy shows the behavior of the positive negative deviation blend(PNDB).
3) During injection molding,PP/POE blends form the multi-layered structure,i.e.skin, transition,shear and core layers.In shear layer,POE phase has the largest deformation degree(D),thereby POE phases are elongated,broken and behave as flat ellipse ball.On the other hand,there exists no POE phase in the skin layer,but the content of POE phase in the core layer is highest.Based on experimental phenomena,a multi-layered structure model is proposed.Moreover,the shearing has an important effect on the formation ofβcrystals of PP phases in blends.There are someβcrystals of PP in skin and shear layers,but noβcrystal of PP appears in core layer. 4) The melting point(T_m) of PP phase in injection molding product at skin layer is closed to that of pure PP,and higher than those at other layers.T_(peak) and T_(end) of PP phase at core layer are a little higher than those at transitional and shear layers,but are lower than those of PP phase at core.Due to the rapid cooling rate at skin,the melting peak of PP phase at skin layer is wide and its crystallinity is low.However,the crystallinity of PP phase at core is highest.The dependence of crystallization temperature(T_c) of PP on pressure obeys the linear equation,T_c=T_(c.0)+kp.Additionally,with increasing POE content,the melting behaviors of PP phase in PP/POE blends at high pressure crystallization is different with those at low pressure crystallization.
5) At the same processing temperature,the storage modulus(E') of PP/POE blends at core layer is higher than that at shear layer.With increasing the processing temperature,all E' values at core and shear layer increase at the same time.Moreover,the E' respondence to DMA frequency is different for PP/POE blends at core and shear layers.At the low processing temperature,the E' respondence of PP/POE blends at core is more obvious than that at shear layer.However,at the high processing temperature,the E' respondences of PP/POE blends at core and shear layers are almost the same.
6) Tait Equation could be used to predict the P-V-T properties of PP/POE blends with partial compatibility and semi-crystallinity.The variation of specific volume(V_(sp)) value of PP during crystallization is bigger than that of POE.With increasing the POE content,the variation of V_(sp) value of PP/POE blend decreased during its crystallization.The expansivity coefficient(α) of PP in molten state is bigger than that in solid state,whilstαof POE at solid state is bigger than that at molten state.The variation ofαof PP/POE blend under different temperature and pressure depends on the composition of the blend.Additionally, Simha-Somcynsky model could be used to predict the P-V-T properties of blends in melting state.
7) With increasing the POE content,the storage moduli of PP/POE blends derease,but their loss moduli and tanδvalues increase.The glass transition temperature(T_g) of PP phase in blends tends to shift towards high temperature slightly with increasing the POE content, and T_g of POE shifts towards the low temperature obviously with increasing the PP content. T_g shifts of POE and PP phase in the blends indicate that there might be a strong intermolecular interaction between PP and POE.The Kerner's dispersed phase model and co-continuous phase model can reasonably predict the visco-elasticity and morphological structure of PP/POE blends with different composition.
8) With increasing the POE content,the impact strength values of the PP/POE blends at ambient and -18℃increase,but their tensile strength and modulus derease.Their brittle-ductile transition(BDT) at ambient temperature appears when POE content is about 30%.The toughening mechanism of POE can be understood by crazing branch and percolation.
1、当POE含量较低时,PP的表观诱导期(⊿t_1)随着POE含量的增加而下降,POE的加入加速了PP的结晶过程(表观总结晶期⊿t_c减少);当POE含量较高时,PP的⊿t_i和⊿t_c随着POE含量的增加而延长。随着POE含量增加,共混体系中PP相的T_m,T_(mp)和T_(m,onset)均向低温偏移,表明PP与POE分子间存在一定的作用力,具有一定程度的相容性。随着POE的加入,不仅使PP晶区变小,而且破坏了PP的球晶结构。对PP/POE共混体系的结晶动力学模型分析,发现Ozawa模型不适合描述该体系的结晶过程,莫志深法和Urbanovici-Segal模型可以很好地描述该体系的非等温结晶动力学。
2、采用毛细管流变仪和Haake转矩流变仪对PP/POE共混体系测试的结果基本一致,共混物熔体表现为假塑性流变行为。随着POE含量的增加,PP/POE共混物熔体的表观黏度和非牛顿指数表现为负偏差行为,粘流活化能则表现出正负偏差行为。
3、PP/POE共混物在注塑成型过程中形成多层结构,即表层、过渡层、剪切层和芯层。其中剪切层中POE的形变度(D)最大,POE被拉长、断裂,并呈现为扁椭球形,而芯层和过渡层形变度较小。另一方面,表层中无POE相存在,而芯层POE含量最大,剪切层POE含量次之,据此提出了PP/POE共混物在注塑成型过程中分散相形态演化的多层结构模型。此外,剪切对PP/POE共混物中PP的β晶形成影响很大,在表层和特别是剪切层中含有较多的β晶,而在芯层则没有发现β晶的存在。
4、在PP/POE共混物注塑制品中,表层的PP熔点接近于纯PP,而其它层中的PP的熔点均比表层低。芯层的T_(peak)和T_(end)比过渡层和剪切层略高,但比表层低。由于表层降温快,导致该层PP的熔程宽,结晶度低,而芯层PP的结晶度最大。PP/POE共混物的结晶温度与压力的关系符合线性关系T_c=T_(c,0)+kp。随着POE含量增加,高压下结晶的PP/POE共混物中PP熔融行为与常压下结晶的正好相反。
5、注塑制品各层的DMA研究表明:在相同的加工温度下,芯层的储能模量较剪切层大。提高加工温度,无论是芯层还是过渡层,其储能模量均提高。此外芯层和剪切层的储能模量对不同频率的响应也不同。当加工温度较低时,增大实验频率,芯层的E′比剪切层的E′响应更明显,而加工温度较高时,芯层的E′和剪切层的E′的响应趋于一致。
6、Tait状态方程可用来预测部分相容的、半结晶PP/POE共混物的PVT性质、结晶行为。PP结晶前后的比容变化比POE的大得多,随着POE含量的增加,PP/POE共混物结晶前和结晶后比容的变化均逐渐减小。PP在熔融状态下的热膨胀系数(α)比固体状态的大,而POE正好相反。PP/POE共混物的α随温度、压力的变化与其组成密切相关。此外,采用Simha-Somcynsky模型(S-S)模型计算得到的V_(sp)结果值与PP/POE熔融态实验值吻合得非常好,说明S-S理论模型可以很好地描述PP/POE共混体系熔融态的PVT行为。
7、随着POE含量增加,PP/POE共混物的储能模量逐渐减小,而损耗模量、力学损耗增大。PP/POE共混物中PP和POE的T_g均随着POE含量的增大而升高,其中POE相T_g升高的幅度大于PP相T_g升高的幅度。PP/POE共混体系中PP和POE玻璃化温度的变化反映了PP和POE之间有较强的相互作用力,说明了PP与POE有一定的相容性。Kerner分散相模型和连续相模型可以很好地预测PP/POE共混物的粘弹性和相形态结构。
8、随着POE含量增加,共混体系的常温冲击强度和低温冲击强度都表现为增加的趋势,但拉伸强度和模量逐渐减小。当POE的含量达到30%左右时,常温缺口冲击强度增长幅度迅速增大,出现脆韧转变(BDT)。POE的增韧机理主要为银纹支化机理和逾渗机理。
Properties of multiphase polymeric materials are related to their microstructure greatly,and the formation of their microstructure depends on processing condition.It is very important for the structural design and modification of polymeric materials.In this dissertation, isotactic polypropylene(PP)/ethylene-octene copolymer(POE) blends were prepared in melting state,their melting and crystallization behaviors,P-V-T properties,mechanical properties and viscoelasticity were systematically investigated,the morphological evolution of the dispersed phases and multi-layered microstructures of PP/POE blends during injection molding were discussed.The main conclusions are as following:
1) At the low content of POE,the addition of POE decreases the apparent incubation period (⊿t_i) and the apparent total crystallization period(⊿t_c) of PP in blends due to the heterogeneous nucleation of POE.However,at high content of POE,the addition of POE decreases the mobility of PP segments due to their strong interrnolecular interaction and chain entanglements,resulting in retarding the crystallization of PP,decreasing in the amount ofβ-form PP crystals,and increasing in⊿t_i and⊿t_c of PP in blends.T_m,T_(mp) and T_(m,onset) of PP in PP/POE blends all shift towards lower temperature with addition of POE. The depressions in melting temperature of PP phase in the blends indicate that there might be a strong intermolecular interaction between PP and POE.PP spherulites in blends are defective and their crystallization behavior is influenced intensely by the incorporation of POE.Additionally,the non-isothermal crystallization of blends were analysed by Jeziorny, Ozawa,Urbanovici-segal,Mo and Ziabicki models,respectively.Urbanovici-segal and Mo models are more suitable to describe the non-isothermal crystallization of the blends.
2) The rheological results measured by the capillary and torque rheometers are almost similar.PP,POE and PP/POE blend melts are pseudoplastic fluids.With increasing the POE content in blends,their non-Newtonian constant and apparent viscosity exhibit the behavior of the negative deviation blend(NDB),but their flow activation energy shows the behavior of the positive negative deviation blend(PNDB).
3) During injection molding,PP/POE blends form the multi-layered structure,i.e.skin, transition,shear and core layers.In shear layer,POE phase has the largest deformation degree(D),thereby POE phases are elongated,broken and behave as flat ellipse ball.On the other hand,there exists no POE phase in the skin layer,but the content of POE phase in the core layer is highest.Based on experimental phenomena,a multi-layered structure model is proposed.Moreover,the shearing has an important effect on the formation ofβcrystals of PP phases in blends.There are someβcrystals of PP in skin and shear layers,but noβcrystal of PP appears in core layer. 4) The melting point(T_m) of PP phase in injection molding product at skin layer is closed to that of pure PP,and higher than those at other layers.T_(peak) and T_(end) of PP phase at core layer are a little higher than those at transitional and shear layers,but are lower than those of PP phase at core.Due to the rapid cooling rate at skin,the melting peak of PP phase at skin layer is wide and its crystallinity is low.However,the crystallinity of PP phase at core is highest.The dependence of crystallization temperature(T_c) of PP on pressure obeys the linear equation,T_c=T_(c.0)+kp.Additionally,with increasing POE content,the melting behaviors of PP phase in PP/POE blends at high pressure crystallization is different with those at low pressure crystallization.
5) At the same processing temperature,the storage modulus(E') of PP/POE blends at core layer is higher than that at shear layer.With increasing the processing temperature,all E' values at core and shear layer increase at the same time.Moreover,the E' respondence to DMA frequency is different for PP/POE blends at core and shear layers.At the low processing temperature,the E' respondence of PP/POE blends at core is more obvious than that at shear layer.However,at the high processing temperature,the E' respondences of PP/POE blends at core and shear layers are almost the same.
6) Tait Equation could be used to predict the P-V-T properties of PP/POE blends with partial compatibility and semi-crystallinity.The variation of specific volume(V_(sp)) value of PP during crystallization is bigger than that of POE.With increasing the POE content,the variation of V_(sp) value of PP/POE blend decreased during its crystallization.The expansivity coefficient(α) of PP in molten state is bigger than that in solid state,whilstαof POE at solid state is bigger than that at molten state.The variation ofαof PP/POE blend under different temperature and pressure depends on the composition of the blend.Additionally, Simha-Somcynsky model could be used to predict the P-V-T properties of blends in melting state.
7) With increasing the POE content,the storage moduli of PP/POE blends derease,but their loss moduli and tanδvalues increase.The glass transition temperature(T_g) of PP phase in blends tends to shift towards high temperature slightly with increasing the POE content, and T_g of POE shifts towards the low temperature obviously with increasing the PP content. T_g shifts of POE and PP phase in the blends indicate that there might be a strong intermolecular interaction between PP and POE.The Kerner's dispersed phase model and co-continuous phase model can reasonably predict the visco-elasticity and morphological structure of PP/POE blends with different composition.
8) With increasing the POE content,the impact strength values of the PP/POE blends at ambient and -18℃increase,but their tensile strength and modulus derease.Their brittle-ductile transition(BDT) at ambient temperature appears when POE content is about 30%.The toughening mechanism of POE can be understood by crazing branch and percolation.
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