聚乳酸复合体系在体积拉伸流场中相态演化与机理研究
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摘要
聚合物材料的微结构与性能显著地受到聚合物成型加工流场的影响。传统的螺杆为核心的成型加工方法都是基于剪切流场为主导，叶片塑化输送设备开创了无螺杆的体积拉伸形变主导作用的成型加工新技术，实现了聚合物成型加工原理由剪切流场支配到拉伸流场支配的革新。与传统的螺杆成型加工设备相比，叶片塑化输送设备体积小，加工能耗低并具有更广的物料适应性等独特的优点。因此，结合叶片塑化输送设备的结构及聚合物材料的本征特性，深入地研究体积拉伸流场对聚合物材料相态结构的影响、聚合物复合体系的分散混炼效果等，为系统地分析体积拉伸流场支配下的聚合物成型加工原理及推进聚合物材料先进成型加工技术及设备的发展具有重要的意义。
利用体积拉伸形变主导的叶片挤出机或剪切形变主导的双螺杆挤出机分别进行聚乳酸单组份的塑化输运加工，采用骤冷拆机取样方法进行观察挤出机各区段的聚乳酸结晶形态及取向行为。通过广角X-射线衍射仪、差示扫描量热仪及偏光显微镜分别测试了各区段聚乳酸的结晶性态、结晶性能及晶体形貌，通过小角X-射线散射仪观察了不同组叶片塑化单元内的聚乳酸的取向行为。结果发现：与剪切流场主导的双螺杆挤出机制备的相比，基于体积拉伸流场主导的叶片挤出机制备的聚乳酸产生了明显的β晶且结晶度有所提高。同时，针对叶片挤出机成型加工下的聚乳酸晶体形貌，富熔体段呈现为尺寸较大且数目较少的球形晶体，熔融段呈现为尺寸较小且数目众多的球晶。另外，小角X-射线散射图样呈现了叶片挤出机熔融段的取向度明显高于富熔融段的。这些结果表明：与剪切形变主导作用相比，体积拉伸形变主导作用具有显著的诱导结晶作用；经历更持久拉伸形变作用将获得更加强烈的取向行为，这种拉伸取向行为促使聚合物材料的有序化排列及原位成纤。
利用体积拉伸形变主导的叶片挤出机或剪切形变主导的双螺杆挤出机分别进行固定组份比的聚乳酸/热塑性聚氨酯合金制备，采用骤冷拆机取样方法进行观察挤出机各区段的聚乳酸/热塑性聚氨酯合金的分散相形态及演化行为；针对叶片挤出机或双螺杆挤出机制备的不同组份比的聚乳酸/热塑性聚氨酯合金进行相应分散相形态、结晶性能及力学性能研究。通过高分辨率扫描电子显微镜观察了聚乳酸/热塑性聚氨酯合金的分散相形态，广角X-射线衍射仪、差示扫描量热仪及偏光显微镜分别测试了其合金的结晶性态、结晶性能及晶体形貌，动态热机械分析仪分析了其合金相容性变化。结果发现：与剪切流场主导的双螺杆挤出机制备的相比，体积拉伸流场主导的叶片挤出机制备的聚乳酸/热塑性聚氨酯合金更易产生纤维状分散粒子，且分散粒子尺寸更加细小。同时，较双螺杆挤出机制备的相比，基于叶片挤出机制备的聚乳酸/热塑性聚氨酯合金有着更高的结晶度及更好的相容性。清晰地表明：全局的连续的体积拉伸形变作用可以促使聚合物共混物中的分散相原位成纤，强烈的传质传热作用改善了共混物的分散互融从而提高了相容性，为改善不相容聚合物共混物的力学性能提供了切实可行的加工方法。
利用体积拉伸形变主导的叶片挤出机或剪切形变主导的双螺杆挤出机分别进行聚乳酸/云母复合材料制备。通过对分散相形态、结晶性能及力学性能分析发现：与双螺杆挤出机制备的相比，基于体积拉伸形变主导的叶片挤出机制备的复合材料中云母粒子的分散更加均匀，球晶尺寸更加均匀且结晶度有所提高，最终在宏观上表现出更优越的力学性能。这些结果表明：体积拉伸形变加工方法具有分散混合效果好、机械热历程短、取向作用明显以及对物料的低剪切、低损伤等独特的加工特性。
通过硅烷偶联剂或钛酸酯偶联剂对云母表面进行改性，再利用体积拉伸形变主导的叶片挤出机分别制备了未改性云母、改性云母的聚乳酸/热塑性聚氨酯/云母多相体系。采用傅里叶变换红外光谱仪进行了云母表面接枝测试，透射电子显微镜细致观察了多相体系中分散相形态及云母粒子的分布，动态热机械分析仪表征了多相体系的相容性，广角X-射线衍射仪、差示扫描量热仪及偏光显微镜分别测试了多相体系的结晶形态、结晶性能及晶体形貌；另外，建立了多相体系的应力应变与其微观形貌的关系。结果发现：云母粒子更易趋向分布在热塑性聚氨酯相，成功表面改性的多相体系相容性进一步得到改善，相应的结晶度也产生了一定的提高，最终表现出更好的力学性能；同时发现多相体系中大量的长纤维结构显著地提高了拉伸应力及应变。这些说明：通过化学改性可以将体积拉伸形变作用的多相体系中相界面产生更牢固的吸附，为最终的高性能聚合物多相材料的稳定应用提高保障。
结合体积拉伸形变主导的叶片塑化单元结构及相应的实验结果，建立了体积拉伸形变作用下聚合物材料的取向及诱导结晶、分散相形态的演化的物理模型。表明叶片挤出机周期的收敛形变促使分子链有效的线性排列，有序取向；同时强的传质传热能力提高聚合物熔体的分散效果。这些实验结果及模型解析为体积拉伸形变加工技术的发展及推广提供了有力的支撑。
Polymer processing flow field plays a significant role for microstructure and propertiesof polymer materials. Screw is regarded as the core part for traditional polymer processingdevices, and processing methods are based on the shear flow field. Unlike screw processingdevices, vane plasticizing conveying equipment invented by Prof. Qu, which generateselongational deformation, inaugurates a new type of polymer processing device. It has owncharacteristics in polymer processing technology. Compared with the traditional screwprocessing equipment, the unique advantages of vane plasticizing conveying equipment aresmall in size, and low energy consumption and the wide adaptability for materials processing.Therefore, combined with the structure of vane plasticizing conveying equipment and theintrinsic characteristics of polymer materials, to deep study effects of the volume elongationalflow field on the crystallization and orientation of polymer materials, and dispersion mixingof polymer composite system, to systematically analyze polymer processing principle ofvolume elongational flow field for promoted the development of polymer materials, advancedprocessing technology and equipment have the vital significance.
Vane extruder (VE) dominated by volume elongational flow field and/or twin-screwextruder (TSE) dominated by shear flow field plasticized and conveyed polylactic acid (PLA)material, respectively. The shock cooling, disassembling and sampling method was used forobservation of the crystalline form and orientation of PLA of extruder each section. Wideangle X-ray diffraction (WAXD) and polarizing microscope (POM), differential scanningcalorimeter (DSC) were adopted to test crystalline form, crystallization properties and crystalmorphology of PLA, small angle X-ray scattering (SAXS) was used to observe orientationbehaviors of PLA of the different set of vane plasticizing and conveying unit (VPCU). Theresults showed that: compared to those of TSE dominated by shear flow field, the PLAproduced by VE based on volume elongational flow field generated obvious β crystal andincreased crystallinity. Moreover, in view of crystal morphology based on VE, spherocrystalof PLA of rich solid state appeared as large size, and the spherical crystal of high integrity,that of rich melting state presented a number of smaller size, and that of the melting statepresented amount of small and uniform spherical crystal. In addition, SAXS patternspresented that orientation degree of PLA sampled from melting state of the VE was obviouslyhigher than those of rich solid state and rich melt state. These results indicate that VEdominated by the volume elongational deformation has strong induced crystallization capacity,compared with TSE dominated by shear deformation; more longer time elongational deformation, more strong orientation behavior. The elongational orientation behavior couldurge ordering arrangement of molecular chains materials and make insitu fibrillation.
VE based on volume elongational flow field and/or TSE based on shear flow field wereused to prepare polylactic acid/thermoplastic polyurethane (PLA/TPU) blend for fixedcomponent ratio, respectively. The shock cooling, disassembling and sampling method wasused for in situ observation of dispersed phase morphologies and theirs evolution ofPLA/TPU blend derived from different segment of VE and/or TSE. Meanwhile, PLA/TPUblends for different component ratio were prepared by VE and/or TSE, and theirs dispersedphase morphology, crystalline properties and mechanical properties were observed andmeasured, respectively. High resolution scanning electron microscope (SEM) was adopted toobserve the dispersed phase morphology of PLA/TPU blends, WAXD, POM and DSC wereused to test crystalline form, crystallization properties and crystal morphology, respectively.Dynamic thermal mechanical analysis (DMA) was used to measure compatibility ofPLA/TPU blends. The results showed that: compared to that of TSE dominated by shear flowfield, dispersed phase morphologies of PLA/TPU blends prepared by VE had more apparentfibrous structure, and more uniform particles size. And PLA/TPU blends prepared by VE hada higher degree of crystallinity and better compatibility than that of TSE. These resultssuggest that insitu fibrillation capacity of polymer compound via elongational flow field hassuperior to that of TSE via shear flow field, its strong the mass and heat transfer ability canpromote the compatibility and improve the mechanical properties of the immiscible polymermaterials, which provide a novel and feasible polymer processing method.
VE dominated by volume elongational flow field and/or TSE dominated by shear flowfield were used to prepare polylactic acid/mica (PLA/Mica) composites, respectively.Analysis of dispersed phase morphology, crystalline properties and mechanical propertiesfound that: mica particles in the composites prepared by VE had more uniform dispersionthan that of TSE. Compared with that of TSE, the degree of crystallinity showed a slightincrease. Eventually, mechanical properties of PLA/Mica composites prepared by VE weresuperior those of TSE. These results infer that VE via the volume elongational flow field hasthe better dispersive mixing effect, shorter mechanical thermal process, more strong theorientation effect and lower structure damage than TSE via shear flow field. The uniqueprocessing features will advance the processing device and technology of polymer material.
Using silane coupling agent and titanate coupling agent modified Mica surface, thepreparation of the unmodified and/or modification Mica of PLA/TPU/Mica multiphasesystem were prepared by VE based on volume elongational flow field, respectively. Fourier transform infrared spectrometer (FTIR) was used to measure the Mica surface graftingcharacteristic, transmission electron microscopy (TEM) was adopted to carefully observedispersed phase morphology of the PLA/TPU/Mica multiphase system and distribution ofMica particles, DMA was used to characterize compatibility of the multiphase system, WAXD,POM and DSC were used to test crystal form, crystallization properties and crystalmorphology of the multiphase system, respectively. In addition, the relationship of betweenphase morphologies of the multiphase system and stress-strain curves was established. Theresults showed that: Mica particles were more likely to tend to distribution in thethermoplastic polyurethane phase, compatibility of the multiphase system for Mica modifiedby coupling agent were successfully improved. Moreover, crystallinity of the multiphasesystem were also a certain amount of increase, and the mechanical properties were slightincrease. In addition, a large number of long fiber structure of the multiphase system couldsignificantly increase the tensile stress and strain. These results indicate that: PLA/TPU/Micamultiphase materials based on volume elongational deformation with chemical modificationhave more strong adsorption than that of the multiphase system without surface modification.Finally, stability and security of the multiphase materials application are further promoted.
Combination of the structure of VPCU dominated by volume elongational deformationand the corresponding experimental results, the special physical models for effects of thevolume elongational deformation on induced crystallization and orientation behavior and theevolution of dispersed phase morphology were established. These models explained that thevolume elongational deformation had more easier to accelerate ordering of molecular chainand insitu fibrillation of dispersed phase; and strong capacity of heat transfer and masstransfer could remarkably improve the disperse efficiency of polymer materials. The resultsfor the volume elongational deformation processing technology could prove an experimentand mechanism basis for development and promotion of advanced polymer processing.
利用体积拉伸形变主导的叶片挤出机或剪切形变主导的双螺杆挤出机分别进行聚乳酸单组份的塑化输运加工，采用骤冷拆机取样方法进行观察挤出机各区段的聚乳酸结晶形态及取向行为。通过广角X-射线衍射仪、差示扫描量热仪及偏光显微镜分别测试了各区段聚乳酸的结晶性态、结晶性能及晶体形貌，通过小角X-射线散射仪观察了不同组叶片塑化单元内的聚乳酸的取向行为。结果发现：与剪切流场主导的双螺杆挤出机制备的相比，基于体积拉伸流场主导的叶片挤出机制备的聚乳酸产生了明显的β晶且结晶度有所提高。同时，针对叶片挤出机成型加工下的聚乳酸晶体形貌，富熔体段呈现为尺寸较大且数目较少的球形晶体，熔融段呈现为尺寸较小且数目众多的球晶。另外，小角X-射线散射图样呈现了叶片挤出机熔融段的取向度明显高于富熔融段的。这些结果表明：与剪切形变主导作用相比，体积拉伸形变主导作用具有显著的诱导结晶作用；经历更持久拉伸形变作用将获得更加强烈的取向行为，这种拉伸取向行为促使聚合物材料的有序化排列及原位成纤。
利用体积拉伸形变主导的叶片挤出机或剪切形变主导的双螺杆挤出机分别进行固定组份比的聚乳酸/热塑性聚氨酯合金制备，采用骤冷拆机取样方法进行观察挤出机各区段的聚乳酸/热塑性聚氨酯合金的分散相形态及演化行为；针对叶片挤出机或双螺杆挤出机制备的不同组份比的聚乳酸/热塑性聚氨酯合金进行相应分散相形态、结晶性能及力学性能研究。通过高分辨率扫描电子显微镜观察了聚乳酸/热塑性聚氨酯合金的分散相形态，广角X-射线衍射仪、差示扫描量热仪及偏光显微镜分别测试了其合金的结晶性态、结晶性能及晶体形貌，动态热机械分析仪分析了其合金相容性变化。结果发现：与剪切流场主导的双螺杆挤出机制备的相比，体积拉伸流场主导的叶片挤出机制备的聚乳酸/热塑性聚氨酯合金更易产生纤维状分散粒子，且分散粒子尺寸更加细小。同时，较双螺杆挤出机制备的相比，基于叶片挤出机制备的聚乳酸/热塑性聚氨酯合金有着更高的结晶度及更好的相容性。清晰地表明：全局的连续的体积拉伸形变作用可以促使聚合物共混物中的分散相原位成纤，强烈的传质传热作用改善了共混物的分散互融从而提高了相容性，为改善不相容聚合物共混物的力学性能提供了切实可行的加工方法。
利用体积拉伸形变主导的叶片挤出机或剪切形变主导的双螺杆挤出机分别进行聚乳酸/云母复合材料制备。通过对分散相形态、结晶性能及力学性能分析发现：与双螺杆挤出机制备的相比，基于体积拉伸形变主导的叶片挤出机制备的复合材料中云母粒子的分散更加均匀，球晶尺寸更加均匀且结晶度有所提高，最终在宏观上表现出更优越的力学性能。这些结果表明：体积拉伸形变加工方法具有分散混合效果好、机械热历程短、取向作用明显以及对物料的低剪切、低损伤等独特的加工特性。
通过硅烷偶联剂或钛酸酯偶联剂对云母表面进行改性，再利用体积拉伸形变主导的叶片挤出机分别制备了未改性云母、改性云母的聚乳酸/热塑性聚氨酯/云母多相体系。采用傅里叶变换红外光谱仪进行了云母表面接枝测试，透射电子显微镜细致观察了多相体系中分散相形态及云母粒子的分布，动态热机械分析仪表征了多相体系的相容性，广角X-射线衍射仪、差示扫描量热仪及偏光显微镜分别测试了多相体系的结晶形态、结晶性能及晶体形貌；另外，建立了多相体系的应力应变与其微观形貌的关系。结果发现：云母粒子更易趋向分布在热塑性聚氨酯相，成功表面改性的多相体系相容性进一步得到改善，相应的结晶度也产生了一定的提高，最终表现出更好的力学性能；同时发现多相体系中大量的长纤维结构显著地提高了拉伸应力及应变。这些说明：通过化学改性可以将体积拉伸形变作用的多相体系中相界面产生更牢固的吸附，为最终的高性能聚合物多相材料的稳定应用提高保障。
结合体积拉伸形变主导的叶片塑化单元结构及相应的实验结果，建立了体积拉伸形变作用下聚合物材料的取向及诱导结晶、分散相形态的演化的物理模型。表明叶片挤出机周期的收敛形变促使分子链有效的线性排列，有序取向；同时强的传质传热能力提高聚合物熔体的分散效果。这些实验结果及模型解析为体积拉伸形变加工技术的发展及推广提供了有力的支撑。
Polymer processing flow field plays a significant role for microstructure and propertiesof polymer materials. Screw is regarded as the core part for traditional polymer processingdevices, and processing methods are based on the shear flow field. Unlike screw processingdevices, vane plasticizing conveying equipment invented by Prof. Qu, which generateselongational deformation, inaugurates a new type of polymer processing device. It has owncharacteristics in polymer processing technology. Compared with the traditional screwprocessing equipment, the unique advantages of vane plasticizing conveying equipment aresmall in size, and low energy consumption and the wide adaptability for materials processing.Therefore, combined with the structure of vane plasticizing conveying equipment and theintrinsic characteristics of polymer materials, to deep study effects of the volume elongationalflow field on the crystallization and orientation of polymer materials, and dispersion mixingof polymer composite system, to systematically analyze polymer processing principle ofvolume elongational flow field for promoted the development of polymer materials, advancedprocessing technology and equipment have the vital significance.
Vane extruder (VE) dominated by volume elongational flow field and/or twin-screwextruder (TSE) dominated by shear flow field plasticized and conveyed polylactic acid (PLA)material, respectively. The shock cooling, disassembling and sampling method was used forobservation of the crystalline form and orientation of PLA of extruder each section. Wideangle X-ray diffraction (WAXD) and polarizing microscope (POM), differential scanningcalorimeter (DSC) were adopted to test crystalline form, crystallization properties and crystalmorphology of PLA, small angle X-ray scattering (SAXS) was used to observe orientationbehaviors of PLA of the different set of vane plasticizing and conveying unit (VPCU). Theresults showed that: compared to those of TSE dominated by shear flow field, the PLAproduced by VE based on volume elongational flow field generated obvious β crystal andincreased crystallinity. Moreover, in view of crystal morphology based on VE, spherocrystalof PLA of rich solid state appeared as large size, and the spherical crystal of high integrity,that of rich melting state presented a number of smaller size, and that of the melting statepresented amount of small and uniform spherical crystal. In addition, SAXS patternspresented that orientation degree of PLA sampled from melting state of the VE was obviouslyhigher than those of rich solid state and rich melt state. These results indicate that VEdominated by the volume elongational deformation has strong induced crystallization capacity,compared with TSE dominated by shear deformation; more longer time elongational deformation, more strong orientation behavior. The elongational orientation behavior couldurge ordering arrangement of molecular chains materials and make insitu fibrillation.
VE based on volume elongational flow field and/or TSE based on shear flow field wereused to prepare polylactic acid/thermoplastic polyurethane (PLA/TPU) blend for fixedcomponent ratio, respectively. The shock cooling, disassembling and sampling method wasused for in situ observation of dispersed phase morphologies and theirs evolution ofPLA/TPU blend derived from different segment of VE and/or TSE. Meanwhile, PLA/TPUblends for different component ratio were prepared by VE and/or TSE, and theirs dispersedphase morphology, crystalline properties and mechanical properties were observed andmeasured, respectively. High resolution scanning electron microscope (SEM) was adopted toobserve the dispersed phase morphology of PLA/TPU blends, WAXD, POM and DSC wereused to test crystalline form, crystallization properties and crystal morphology, respectively.Dynamic thermal mechanical analysis (DMA) was used to measure compatibility ofPLA/TPU blends. The results showed that: compared to that of TSE dominated by shear flowfield, dispersed phase morphologies of PLA/TPU blends prepared by VE had more apparentfibrous structure, and more uniform particles size. And PLA/TPU blends prepared by VE hada higher degree of crystallinity and better compatibility than that of TSE. These resultssuggest that insitu fibrillation capacity of polymer compound via elongational flow field hassuperior to that of TSE via shear flow field, its strong the mass and heat transfer ability canpromote the compatibility and improve the mechanical properties of the immiscible polymermaterials, which provide a novel and feasible polymer processing method.
VE dominated by volume elongational flow field and/or TSE dominated by shear flowfield were used to prepare polylactic acid/mica (PLA/Mica) composites, respectively.Analysis of dispersed phase morphology, crystalline properties and mechanical propertiesfound that: mica particles in the composites prepared by VE had more uniform dispersionthan that of TSE. Compared with that of TSE, the degree of crystallinity showed a slightincrease. Eventually, mechanical properties of PLA/Mica composites prepared by VE weresuperior those of TSE. These results infer that VE via the volume elongational flow field hasthe better dispersive mixing effect, shorter mechanical thermal process, more strong theorientation effect and lower structure damage than TSE via shear flow field. The uniqueprocessing features will advance the processing device and technology of polymer material.
Using silane coupling agent and titanate coupling agent modified Mica surface, thepreparation of the unmodified and/or modification Mica of PLA/TPU/Mica multiphasesystem were prepared by VE based on volume elongational flow field, respectively. Fourier transform infrared spectrometer (FTIR) was used to measure the Mica surface graftingcharacteristic, transmission electron microscopy (TEM) was adopted to carefully observedispersed phase morphology of the PLA/TPU/Mica multiphase system and distribution ofMica particles, DMA was used to characterize compatibility of the multiphase system, WAXD,POM and DSC were used to test crystal form, crystallization properties and crystalmorphology of the multiphase system, respectively. In addition, the relationship of betweenphase morphologies of the multiphase system and stress-strain curves was established. Theresults showed that: Mica particles were more likely to tend to distribution in thethermoplastic polyurethane phase, compatibility of the multiphase system for Mica modifiedby coupling agent were successfully improved. Moreover, crystallinity of the multiphasesystem were also a certain amount of increase, and the mechanical properties were slightincrease. In addition, a large number of long fiber structure of the multiphase system couldsignificantly increase the tensile stress and strain. These results indicate that: PLA/TPU/Micamultiphase materials based on volume elongational deformation with chemical modificationhave more strong adsorption than that of the multiphase system without surface modification.Finally, stability and security of the multiphase materials application are further promoted.
Combination of the structure of VPCU dominated by volume elongational deformationand the corresponding experimental results, the special physical models for effects of thevolume elongational deformation on induced crystallization and orientation behavior and theevolution of dispersed phase morphology were established. These models explained that thevolume elongational deformation had more easier to accelerate ordering of molecular chainand insitu fibrillation of dispersed phase; and strong capacity of heat transfer and masstransfer could remarkably improve the disperse efficiency of polymer materials. The resultsfor the volume elongational deformation processing technology could prove an experimentand mechanism basis for development and promotion of advanced polymer processing.
引文
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