水辅助注塑聚烯烃基多相体系的形态与性能调控
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摘要
水辅助注塑（WAIM）技术可高效地成型形状复杂的中空或部分中空聚合物制品。由于WAIM工艺的复杂性，在其发展近期主要集中研究设备和工艺参数的优化，而对WAIM制品形态和结构演变机理的研究则偏少。因此，本文循序渐进地从研究WAIM单相聚烯烃形态和结构的演变机理出发，揭示利用共混改性和纳米复合技术调控WAIM聚烯烃形态和结构的机理，为实现WAIM聚烯烃制品高性能化和轻质化提供理论指导。
本文首先研究WAIM高密度聚乙烯（HDPE）和聚丙烯（PP）制品的结晶形态。发现，两种WAIM聚烯烃制品都呈现独特的“外表层-芯层-内表层”的多层次结晶形态，这与熔体在WAIM中所经历的应力场和温度场密切相关。对WAIM HDPE制品，HDPE分子量对其结晶形态有明显的影响。WAIM高分子量HDPE制品外表层以取向片晶为主，芯层和内表层以球晶为主；而WAIM低分子量HDPE制品外表层、芯层和内表层都以环带球晶为主，差别在于内、外表层环带球晶的尺寸比芯层的小。对WAIM PP制品，其外表层和内表层都形成了取向的晶体结构，但取向区域的厚度仅约占制品残留厚度的2%，而除取向区域外的其它区域都以球晶为主，其中芯层球晶的尺寸最大，平均约为45m。通过改变熔体温度、注水压力和注水延迟时间等加工参数并不能有效调控WAIMPP制品的结晶形态，仅是降低熔体温度有利于制品中形成少量（低于10%）的晶型。
通过对比研究普通注塑（CIM）和WAIM线性低密度聚乙烯（LLDPE）及LLDPE/HDPE共混物制品结晶形态的演变机理发现，CIM和WAIM LLDPE制品都以环带球晶为主，但HDPE的混入会影响LLDPE的结晶形态。在冷却速率较低（如CIM）时，HDPE先于LLDPE结晶，其晶片可诱导LLDPE发生异相成核而阻碍环带球晶的生长，此时较低含量（10wt%）的HDPE足以使LLDPE发生由环带球晶向普通球晶的转变；而在冷却速率较高（如WAIM）时，LLDPE可与HDPE同时结晶，在此情况下，混入10wt%的HDPE并不足以扰乱LLDPE的结晶过程，需将HDPE含量提高至30wt%才能有效阻碍LLDPE的结晶过程而导致其发生由环带球晶向普通球晶的转变。
在探索如何调控WAIM PP制品结晶形态和结构的过程中，发现少量（6wt%）聚合物成核剂（苯乙烯-丙烯腈共聚物，SAN）的混入可实现在WAIM中通过改变工艺参数来调控PP基体的结晶形态和结构。在较低的熔体温度（如180或190℃）下，WAIM94/6PP/SAN共混物制品中可同时形成较高含量的晶型和横晶，例如制品外表层和芯层晶型的含量分别为30.7和18.4%，而靠近内表层的局部区域内则完全形成横晶。晶型的形成是由于SAN对PP具有较强的成核效应；横晶的形成则是由于高压水穿透引起的强剪切和快速冷却作用导致SAN液滴变形为纤维的同时也诱导PP分子链在SAN纤维表面形成大量的晶核，由于生长空间受限，晶片只能垂直于SAN纤维长度方向生长。此外，通过研究WAIM PP/SAN共混物制品的相形态和力学性能发现，在制品的整个壁厚方向上SAN几乎都变形为纤维状，而且WAIM PP/SAN共混物制品的冲击强度和拉伸强度较WAIM PP制品都有较明显的提高。因此，WAIM有望应用于一步成型原位微纤增强共混物制品。
通过研究WAIM PP/埃洛石纳米管（HNTs）纳米复合材料制品的微观结构发现，WAIM中的强剪切作用可使HNTs沿流动方向高度取向。此外，在WAIM中，HNTs可诱导PP形成晶型，提高PP制品的结晶度，例如加入8wt%的HNTs可将PP制品的结晶度由35.5提高至43.5%。研究还发现，加入少量（2wt%）的HNTs即可提高PP制品的热稳定性，如PP制品的T5%和T10%分别提高22和19℃，且HNTs表面对PP分子链直接的稳定作用是使PP热稳定性提高的主因，而HNTs的阻隔效应和HNTs空腔对降解产物的诱捕效应是次要因素。
Water-assisted injection molding (WAIM) is an efficient molding technology that can beused to mold hollow or partially hollow polymer parts with complicated profile. Due to thecomplexity of WAIM process, the researchers mainly focused on the optimization of WAIMequipment and processing parameters in the recent stage of its development, whereas littlework has been done on the mechanism of morphology and structure development duringWAIM. Thus, in this dissertation, the morphology and structure development mechanism ofpolyolefin during WAIM was investigated firstly, and then the mechanism of manipulating themorphology and structure via blending and nano-compositing during WAIM was revealed soas to provide theoretical guidence for molding light-weight and high-performance polyolefinparts via WAIM.
The crystal morphologies of both WAIM high-density polyethylene (HDPE) andpolypropylene (PP) parts were investigated. The results showed that both WAIM HDPE andPP parts showed unique “outer layer-core layer-inner layer” hierarchical crystal morphology,which was closely related to the stress and temperature fields that the melts experiencedduring WAIM. For the WAIM HDPE parts, the molecular weight of HDPE has a significantimpact on the crystal morphology. The WAIM part of the HDPE with higher molecular weightwas dominated by oriented lamellae in the outer layer, and spherulites in both core and innerlayers; whereas banded spherulites dominanted all three layers in the WAIM part of the HDPEwith lower molecular weight, despite that the sizes of banded spherulites in both outer andinner layers were smaller than those in the core layer. For the WAIM PP parts, oriented crystalstructures were observed in both outer and inner layers, but the thickness of these orientedareas was only2%of the whole residual wall thickness; spherulites with various sizes weredominant in the rest areas of the part, among which the core layer showed spherulites withlargest sizes (about45m in diameter). The processing parameters were not effective intailoring the crystalline morphology of the WAIM PP parts, despite that lowering the melttemperature was favorable for the formation of a small amount (lower than10%) of-formcrystal.
The crystal morphologies and their development mechanism in both conventionalinjection molded (CIM) and WAIM LLDPE and LLDPE/HDPE parts were investigated. Theresults showed that banded spherulites dominated both CIM and WAIM LLDPE parts;however, the crystal morphology of LLDPE could be influenced by the HDPE. At low cooling rates (such as the situation in CIM), the heterogeneous nucleation effect of the HDPE on theLLDPE hindered the growth of banded spherulites, and a low concent (10wt%) of the HDPEcould result in the banding to nonbanding morphological transition of the LLDPE; whereas athigh cooling rates (such as the situation in WAIM), the HDPE and the LLDPE crystallizedsimultaneously, a content of10wt%HDPE is not high enough to hinder the crystallization ofthe LLDPE, but increased the HDPE content to30wt%could result in the banding tononbanding morphological transition of the LLDPE.
In the process of exploring an effective way to tailor the crystal morphology andstructure of the WAIM PP part, the presence of a low content (6wt%) of polymer nucleatingagent (acrylonitrile–styrene copolymer, SAN) was found to be favorable for tailoring thecrystal morphology and structure of PP matrix by varying the processing parameters duringWAIM. At a melt temperature of180or190°C, a WAIM94/6PP/SAN blend part with highcontent of-form and transcrystal can be molded. For example, the-form content in theouter and core layers were30.7and18.4%, respectively; and a totally transcrystallized matrixcan be seen near the inner layer. The formation of-form was ascribed to the-nucleatingeffect of the SAN on PP; whereas the formation of the transcrystals was ascribed to the in situfibrillation of the SAN resulted from high shear and cooling rates by high-pressure waterpenetration during WAIM. Moreover, it was found that the whole residual wall of the WAIMPP/SAN blend part was dominanted by SAN microfiber, and both impact and tensilestrengthes were improved compared to those of WAIM PP part. Consequently, the WAIMwould be expected to directly mold in-situ microfibrillar reinforced blend parts.
The microstructures of the WAIM PP/halloysite nanotube (HNTs) nanocomposite partswere investigated. The results showed that the high shear rates during WAIM resulted in thepreferential orientation of the HNTs in the flow direction. Moreover, during the WAIM, theHNTs could induce the-form of the PP, increasing the crystallinity of the WAIM PP part.For example, the addition of8wt%HNTs could incease the crystallinity from35.5to43.5%.Moreover, the addition of a low content (2wt%) of HNTs was enough to ehance the thermalstability of the WAIM PP/HNTs nanocomposite part. The T5%and T10%increased22and19°C,respectively. The direct stabilizing effect of HNTs on the PP contributed largely to theincreased thermal stability of the WAIM PP/HNTs nanocomposite parts rather than theirbarrier and entrapment effects on the volatile products.
本文首先研究WAIM高密度聚乙烯（HDPE）和聚丙烯（PP）制品的结晶形态。发现，两种WAIM聚烯烃制品都呈现独特的“外表层-芯层-内表层”的多层次结晶形态，这与熔体在WAIM中所经历的应力场和温度场密切相关。对WAIM HDPE制品，HDPE分子量对其结晶形态有明显的影响。WAIM高分子量HDPE制品外表层以取向片晶为主，芯层和内表层以球晶为主；而WAIM低分子量HDPE制品外表层、芯层和内表层都以环带球晶为主，差别在于内、外表层环带球晶的尺寸比芯层的小。对WAIM PP制品，其外表层和内表层都形成了取向的晶体结构，但取向区域的厚度仅约占制品残留厚度的2%，而除取向区域外的其它区域都以球晶为主，其中芯层球晶的尺寸最大，平均约为45m。通过改变熔体温度、注水压力和注水延迟时间等加工参数并不能有效调控WAIMPP制品的结晶形态，仅是降低熔体温度有利于制品中形成少量（低于10%）的晶型。
通过对比研究普通注塑（CIM）和WAIM线性低密度聚乙烯（LLDPE）及LLDPE/HDPE共混物制品结晶形态的演变机理发现，CIM和WAIM LLDPE制品都以环带球晶为主，但HDPE的混入会影响LLDPE的结晶形态。在冷却速率较低（如CIM）时，HDPE先于LLDPE结晶，其晶片可诱导LLDPE发生异相成核而阻碍环带球晶的生长，此时较低含量（10wt%）的HDPE足以使LLDPE发生由环带球晶向普通球晶的转变；而在冷却速率较高（如WAIM）时，LLDPE可与HDPE同时结晶，在此情况下，混入10wt%的HDPE并不足以扰乱LLDPE的结晶过程，需将HDPE含量提高至30wt%才能有效阻碍LLDPE的结晶过程而导致其发生由环带球晶向普通球晶的转变。
在探索如何调控WAIM PP制品结晶形态和结构的过程中，发现少量（6wt%）聚合物成核剂（苯乙烯-丙烯腈共聚物，SAN）的混入可实现在WAIM中通过改变工艺参数来调控PP基体的结晶形态和结构。在较低的熔体温度（如180或190℃）下，WAIM94/6PP/SAN共混物制品中可同时形成较高含量的晶型和横晶，例如制品外表层和芯层晶型的含量分别为30.7和18.4%，而靠近内表层的局部区域内则完全形成横晶。晶型的形成是由于SAN对PP具有较强的成核效应；横晶的形成则是由于高压水穿透引起的强剪切和快速冷却作用导致SAN液滴变形为纤维的同时也诱导PP分子链在SAN纤维表面形成大量的晶核，由于生长空间受限，晶片只能垂直于SAN纤维长度方向生长。此外，通过研究WAIM PP/SAN共混物制品的相形态和力学性能发现，在制品的整个壁厚方向上SAN几乎都变形为纤维状，而且WAIM PP/SAN共混物制品的冲击强度和拉伸强度较WAIM PP制品都有较明显的提高。因此，WAIM有望应用于一步成型原位微纤增强共混物制品。
通过研究WAIM PP/埃洛石纳米管（HNTs）纳米复合材料制品的微观结构发现，WAIM中的强剪切作用可使HNTs沿流动方向高度取向。此外，在WAIM中，HNTs可诱导PP形成晶型，提高PP制品的结晶度，例如加入8wt%的HNTs可将PP制品的结晶度由35.5提高至43.5%。研究还发现，加入少量（2wt%）的HNTs即可提高PP制品的热稳定性，如PP制品的T5%和T10%分别提高22和19℃，且HNTs表面对PP分子链直接的稳定作用是使PP热稳定性提高的主因，而HNTs的阻隔效应和HNTs空腔对降解产物的诱捕效应是次要因素。
Water-assisted injection molding (WAIM) is an efficient molding technology that can beused to mold hollow or partially hollow polymer parts with complicated profile. Due to thecomplexity of WAIM process, the researchers mainly focused on the optimization of WAIMequipment and processing parameters in the recent stage of its development, whereas littlework has been done on the mechanism of morphology and structure development duringWAIM. Thus, in this dissertation, the morphology and structure development mechanism ofpolyolefin during WAIM was investigated firstly, and then the mechanism of manipulating themorphology and structure via blending and nano-compositing during WAIM was revealed soas to provide theoretical guidence for molding light-weight and high-performance polyolefinparts via WAIM.
The crystal morphologies of both WAIM high-density polyethylene (HDPE) andpolypropylene (PP) parts were investigated. The results showed that both WAIM HDPE andPP parts showed unique “outer layer-core layer-inner layer” hierarchical crystal morphology,which was closely related to the stress and temperature fields that the melts experiencedduring WAIM. For the WAIM HDPE parts, the molecular weight of HDPE has a significantimpact on the crystal morphology. The WAIM part of the HDPE with higher molecular weightwas dominated by oriented lamellae in the outer layer, and spherulites in both core and innerlayers; whereas banded spherulites dominanted all three layers in the WAIM part of the HDPEwith lower molecular weight, despite that the sizes of banded spherulites in both outer andinner layers were smaller than those in the core layer. For the WAIM PP parts, oriented crystalstructures were observed in both outer and inner layers, but the thickness of these orientedareas was only2%of the whole residual wall thickness; spherulites with various sizes weredominant in the rest areas of the part, among which the core layer showed spherulites withlargest sizes (about45m in diameter). The processing parameters were not effective intailoring the crystalline morphology of the WAIM PP parts, despite that lowering the melttemperature was favorable for the formation of a small amount (lower than10%) of-formcrystal.
The crystal morphologies and their development mechanism in both conventionalinjection molded (CIM) and WAIM LLDPE and LLDPE/HDPE parts were investigated. Theresults showed that banded spherulites dominated both CIM and WAIM LLDPE parts;however, the crystal morphology of LLDPE could be influenced by the HDPE. At low cooling rates (such as the situation in CIM), the heterogeneous nucleation effect of the HDPE on theLLDPE hindered the growth of banded spherulites, and a low concent (10wt%) of the HDPEcould result in the banding to nonbanding morphological transition of the LLDPE; whereas athigh cooling rates (such as the situation in WAIM), the HDPE and the LLDPE crystallizedsimultaneously, a content of10wt%HDPE is not high enough to hinder the crystallization ofthe LLDPE, but increased the HDPE content to30wt%could result in the banding tononbanding morphological transition of the LLDPE.
In the process of exploring an effective way to tailor the crystal morphology andstructure of the WAIM PP part, the presence of a low content (6wt%) of polymer nucleatingagent (acrylonitrile–styrene copolymer, SAN) was found to be favorable for tailoring thecrystal morphology and structure of PP matrix by varying the processing parameters duringWAIM. At a melt temperature of180or190°C, a WAIM94/6PP/SAN blend part with highcontent of-form and transcrystal can be molded. For example, the-form content in theouter and core layers were30.7and18.4%, respectively; and a totally transcrystallized matrixcan be seen near the inner layer. The formation of-form was ascribed to the-nucleatingeffect of the SAN on PP; whereas the formation of the transcrystals was ascribed to the in situfibrillation of the SAN resulted from high shear and cooling rates by high-pressure waterpenetration during WAIM. Moreover, it was found that the whole residual wall of the WAIMPP/SAN blend part was dominanted by SAN microfiber, and both impact and tensilestrengthes were improved compared to those of WAIM PP part. Consequently, the WAIMwould be expected to directly mold in-situ microfibrillar reinforced blend parts.
The microstructures of the WAIM PP/halloysite nanotube (HNTs) nanocomposite partswere investigated. The results showed that the high shear rates during WAIM resulted in thepreferential orientation of the HNTs in the flow direction. Moreover, during the WAIM, theHNTs could induce the-form of the PP, increasing the crystallinity of the WAIM PP part.For example, the addition of8wt%HNTs could incease the crystallinity from35.5to43.5%.Moreover, the addition of a low content (2wt%) of HNTs was enough to ehance the thermalstability of the WAIM PP/HNTs nanocomposite part. The T5%and T10%increased22and19°C,respectively. The direct stabilizing effect of HNTs on the PP contributed largely to theincreased thermal stability of the WAIM PP/HNTs nanocomposite parts rather than theirbarrier and entrapment effects on the volatile products.
引文
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