全同立构聚丙烯诱导结晶行为研究
摘要
在全同聚丙烯(iPP)的附生结晶过程中，基底与附生晶体之间一定程度的晶格/几何结构匹配对附生结晶过程的作用是全同聚丙烯附生结晶研究领域内的重要理论问题。目前很多研究人员认为聚合物附生结晶需要在具有一定程度匹配关系的晶面内进行；而也有人认为结构的匹配性并不是聚合物间产生附生结晶作用的必要条件。本论文的一部分工作主要围绕几何尺寸匹配程度对全同聚丙烯附生结晶过程的影响展开；通过对α成核剂/iPP、β成核剂/iPP异质复合体系，以及iPP纤维/iPP基体均质复合体系的界面结晶形态研究，详细讨论了附生基底与iPP基体间不同晶格/几何结构匹配程度对于附生结晶过程的影响。
本论文的第一部分工作主要针对iPP纤维/iPP基体均质复合体系中iPP纤维对iPP基体的诱导结晶行为。由于高分子聚合物熔体在降温结晶过程中存在过冷态，因此通过向iPP过冷熔体中引入iPP纤维可以得到iPP纤维/iPP基体均质复合体系。对于iPP均质复合体系的偏光显微镜观察表明，由于iPP纤维和iPP基体之间化学组成相同、晶格匹配一致、表面润湿性好，iPP纤维表面对iPP基体有很强的成核能力。在较低的温度(远低于纤维熔点)下引入iPP纤维，纤维与基体界面处诱导形成纯α相的横穿晶层。扫描电镜观察刻蚀后的样品，结果证实在160℃的纤维引入温度下，固态iPP纤维能够诱导α-iPP片晶垂直于纤维表面生长。进一步的原位偏光显微镜观察发现，iPP纤维诱导α-iPP横穿晶生成的结晶过程中，iPP纤维的成核时间短，成核密度高。通过向iPP基体中共混入山梨醇类、磷酸酯盐类两种α成核剂以及芳酰胺类和庚二酸钙两种β成核剂，分别制备了α成核剂/iPP、β成核剂/iPP异质复合体系，并对相应成核剂诱导结晶过程中的成核时间、成核密度等进行研究。试验结果表明，iPP纤维的成核能力优于试验中使用的四种α、β成核剂。相关实验结果表明，在全同聚丙烯异相成核过程中，几何尺寸匹配程度对成核过程起到非常关键的作用。
本论文的另一部分工作围绕β-iPP诱导结晶机理展开。在β-iPP诱导结晶机理的研究中，除晶格匹配效应（例如β成核剂）诱导β-iPP生成机理外，有研究工作表明熔体中的剪切效应也可以诱导β-iPP生成：在剪切作用下形成的一定程度取向的分子链段诱导了β-iPP的生成。取向分子链段在β-iPP的诱导结晶机理中究竟扮演怎样的角色，其与晶格匹配效应下α、β成核剂的成核效率相比，哪种机理的成核效率更高是本论文研究的另一个重要研究内容。
在本论文的这部分工作中，首先通过改变纤维引入温度以及对于复合体系熔融重结晶过程的观察，研究了iPP纤维/iPP基体均质复合体系下，iPP纤维诱导β相晶体形成的机理。研究发现，当纤维引入温度略高于纤维熔点(170℃)时，在全同聚丙烯均质复合体系中观察到界面处部分熔融的iPP纤维诱导基体形成了纯β相的横穿晶层；而当纤维引入温度进一步提高时，纤维诱导的横穿晶层中β相减少，主要由α相组成。在实验过程中固定纤维引入温度，改变纤维引入过程中在过冷熔体中的松弛时间也得到类似的规律。相关实验结果表明β-iPP晶体的形成与iPP纤维取向分子链的松弛程度有关；iPP纤维中分子链的取向状态对于诱导β-iPP的形成起到重要作用。
在研究中，将纤维部分熔融重结晶诱导β-iPP横穿晶的结晶过程与α、β成核剂诱导基体的结晶过程对比。实验结果表明部分熔融iPP纤维与NB328、庚二酸钙两种β成核剂相比，部分熔融iPP纤维诱导β-iPP的成核时间比NB328成核剂短；而庚二酸钙由于表面独特结构对于iPP分子链的吸附和稳定能力，成为三者中成核效率最高的基底。另外，部分熔融iPP纤维与DBS、NA11两种α成核剂相比，iPP纤维熔融重结晶诱导β横穿晶的成核诱导时间比DBS、NA11两种α成核剂的成核诱导时间短，说明部分熔融纤维表面的有序结构微区对于iPP基体的成核效率与几何尺寸不完全匹配的成核剂相比仍具有优势。
此外，结晶温度的改变也会影响部分熔融的iPP纤维在界面处诱导α或β-iPP晶体的形成：当均质复合体系在105℃~137℃之间进行等温结晶时，可以在界面处得到β-iPP的横穿晶；当等温结晶温度超过141℃时，iPP纤维无法诱导β晶生成，而是得到纯α-iPP晶体；而在同一结晶温度下， β成核剂NB328仍然具有一定的β成核能力，并在143°C左右失去诱导β-iPP的能力。
In this work, iPP fiber/matrix homogeneious composite andnucleating agents/iPP heterogeneous composites were prepared, andtheir interfacial supermolecular structuress were investigated. The iPPfibers were introduced into the iPP matrices at the supercooled moltenstate.
Results show that the fiber introduction temperature andcrystallization temperature significantly affect the interfacialsupermolecular structure between the nucleation surface and iPPmatrix, and the influences were studied in details.
When iPP fibers were introduced into the matrix at temperatureblow the fiber melting point, they remained in the solid state andexhibited rather high nucleation capacity towards the iPP matrix.Thenucleation behavior of iPP melt in the presence of its homogeneityfibers, DBS and NA11under various conditions was studied using anpolarized optical microscope equipped with a hot stage and thermalanalysis. The results show that the nucleation capacity of iPP fibers is stronger than that of NA11and DBS, due to better dimensionalmatching at lattice level. The iPP fibers have the same chemicalcomposition and crystalline structure with the α-phase iPP, and thusinduce the crystallization more efficiently than NA11and DBS, whoserepeated period does not exactly accord with structure of α-iPP. Thehigh-level dimensional matching is propitious to fast nucleationprocess, demonstrating that dimension matching is the control step ofheterogeneous nucleation for α-iPP isothermal crystallization.
When iPP fibers were introduced at higher temperature, theinterfacial transcrystalline iPP was composed of more β-iPP thanα-modification. When the introduction temperature was173°C, nearthe fiber melting point, the introduced mainly β-modificationtranscrystallization layers were obtained. However, when fiberintroduction were conducted at even higher temperature, thetranscrystalline goes back to α-modification again. Adjusting the fiberrelaxation time at a fixed fiber introduction temperature obtainedsimilar conclusions. Therefore, it can be concluded that the nucleationof the β-modification was strongly related to the partially melting stateof the iPP fibers.
The nucleation behavior of iPP in the presence of its partiallymelted homogeneity fibers, α nucleating agents (DBS and NA11) and βnucleating agents (NB328and calcium pimelate) under various conditions was compared using a polarized optical microscopeequipped with a hot stage and thermal analysis. Results show that theiPP fiber exhibited stronger nucleation capacity than the nucleatingagent NB328, but calcium pimelate shows the strongest nucleationcapacity because of its unique surface structure. And the iPP fiberexhibited stronger nucleation capacity than α nucleating agent DBSand NA11, demonstrating that dimensional matching is an importantfactor for nucleation and growth of iPP.
Moreover, the crystallization temperature could also affect theinterfacial morphology of iPP induced by its own fiber and nucleatingagents. It is found in the experiments that the transcrystalline structuresof β-iPP can only generate below141°C. While the β nucleating agentNB328remained some nucleation capacity to β-iPP at the sametemperature, but it lose it at the crystallization temperature of143°C.
本论文的第一部分工作主要针对iPP纤维/iPP基体均质复合体系中iPP纤维对iPP基体的诱导结晶行为。由于高分子聚合物熔体在降温结晶过程中存在过冷态，因此通过向iPP过冷熔体中引入iPP纤维可以得到iPP纤维/iPP基体均质复合体系。对于iPP均质复合体系的偏光显微镜观察表明，由于iPP纤维和iPP基体之间化学组成相同、晶格匹配一致、表面润湿性好，iPP纤维表面对iPP基体有很强的成核能力。在较低的温度(远低于纤维熔点)下引入iPP纤维，纤维与基体界面处诱导形成纯α相的横穿晶层。扫描电镜观察刻蚀后的样品，结果证实在160℃的纤维引入温度下，固态iPP纤维能够诱导α-iPP片晶垂直于纤维表面生长。进一步的原位偏光显微镜观察发现，iPP纤维诱导α-iPP横穿晶生成的结晶过程中，iPP纤维的成核时间短，成核密度高。通过向iPP基体中共混入山梨醇类、磷酸酯盐类两种α成核剂以及芳酰胺类和庚二酸钙两种β成核剂，分别制备了α成核剂/iPP、β成核剂/iPP异质复合体系，并对相应成核剂诱导结晶过程中的成核时间、成核密度等进行研究。试验结果表明，iPP纤维的成核能力优于试验中使用的四种α、β成核剂。相关实验结果表明，在全同聚丙烯异相成核过程中，几何尺寸匹配程度对成核过程起到非常关键的作用。
本论文的另一部分工作围绕β-iPP诱导结晶机理展开。在β-iPP诱导结晶机理的研究中，除晶格匹配效应（例如β成核剂）诱导β-iPP生成机理外，有研究工作表明熔体中的剪切效应也可以诱导β-iPP生成：在剪切作用下形成的一定程度取向的分子链段诱导了β-iPP的生成。取向分子链段在β-iPP的诱导结晶机理中究竟扮演怎样的角色，其与晶格匹配效应下α、β成核剂的成核效率相比，哪种机理的成核效率更高是本论文研究的另一个重要研究内容。
在本论文的这部分工作中，首先通过改变纤维引入温度以及对于复合体系熔融重结晶过程的观察，研究了iPP纤维/iPP基体均质复合体系下，iPP纤维诱导β相晶体形成的机理。研究发现，当纤维引入温度略高于纤维熔点(170℃)时，在全同聚丙烯均质复合体系中观察到界面处部分熔融的iPP纤维诱导基体形成了纯β相的横穿晶层；而当纤维引入温度进一步提高时，纤维诱导的横穿晶层中β相减少，主要由α相组成。在实验过程中固定纤维引入温度，改变纤维引入过程中在过冷熔体中的松弛时间也得到类似的规律。相关实验结果表明β-iPP晶体的形成与iPP纤维取向分子链的松弛程度有关；iPP纤维中分子链的取向状态对于诱导β-iPP的形成起到重要作用。
在研究中，将纤维部分熔融重结晶诱导β-iPP横穿晶的结晶过程与α、β成核剂诱导基体的结晶过程对比。实验结果表明部分熔融iPP纤维与NB328、庚二酸钙两种β成核剂相比，部分熔融iPP纤维诱导β-iPP的成核时间比NB328成核剂短；而庚二酸钙由于表面独特结构对于iPP分子链的吸附和稳定能力，成为三者中成核效率最高的基底。另外，部分熔融iPP纤维与DBS、NA11两种α成核剂相比，iPP纤维熔融重结晶诱导β横穿晶的成核诱导时间比DBS、NA11两种α成核剂的成核诱导时间短，说明部分熔融纤维表面的有序结构微区对于iPP基体的成核效率与几何尺寸不完全匹配的成核剂相比仍具有优势。
此外，结晶温度的改变也会影响部分熔融的iPP纤维在界面处诱导α或β-iPP晶体的形成：当均质复合体系在105℃~137℃之间进行等温结晶时，可以在界面处得到β-iPP的横穿晶；当等温结晶温度超过141℃时，iPP纤维无法诱导β晶生成，而是得到纯α-iPP晶体；而在同一结晶温度下， β成核剂NB328仍然具有一定的β成核能力，并在143°C左右失去诱导β-iPP的能力。
In this work, iPP fiber/matrix homogeneious composite andnucleating agents/iPP heterogeneous composites were prepared, andtheir interfacial supermolecular structuress were investigated. The iPPfibers were introduced into the iPP matrices at the supercooled moltenstate.
Results show that the fiber introduction temperature andcrystallization temperature significantly affect the interfacialsupermolecular structure between the nucleation surface and iPPmatrix, and the influences were studied in details.
When iPP fibers were introduced into the matrix at temperatureblow the fiber melting point, they remained in the solid state andexhibited rather high nucleation capacity towards the iPP matrix.Thenucleation behavior of iPP melt in the presence of its homogeneityfibers, DBS and NA11under various conditions was studied using anpolarized optical microscope equipped with a hot stage and thermalanalysis. The results show that the nucleation capacity of iPP fibers is stronger than that of NA11and DBS, due to better dimensionalmatching at lattice level. The iPP fibers have the same chemicalcomposition and crystalline structure with the α-phase iPP, and thusinduce the crystallization more efficiently than NA11and DBS, whoserepeated period does not exactly accord with structure of α-iPP. Thehigh-level dimensional matching is propitious to fast nucleationprocess, demonstrating that dimension matching is the control step ofheterogeneous nucleation for α-iPP isothermal crystallization.
When iPP fibers were introduced at higher temperature, theinterfacial transcrystalline iPP was composed of more β-iPP thanα-modification. When the introduction temperature was173°C, nearthe fiber melting point, the introduced mainly β-modificationtranscrystallization layers were obtained. However, when fiberintroduction were conducted at even higher temperature, thetranscrystalline goes back to α-modification again. Adjusting the fiberrelaxation time at a fixed fiber introduction temperature obtainedsimilar conclusions. Therefore, it can be concluded that the nucleationof the β-modification was strongly related to the partially melting stateof the iPP fibers.
The nucleation behavior of iPP in the presence of its partiallymelted homogeneity fibers, α nucleating agents (DBS and NA11) and βnucleating agents (NB328and calcium pimelate) under various conditions was compared using a polarized optical microscopeequipped with a hot stage and thermal analysis. Results show that theiPP fiber exhibited stronger nucleation capacity than the nucleatingagent NB328, but calcium pimelate shows the strongest nucleationcapacity because of its unique surface structure. And the iPP fiberexhibited stronger nucleation capacity than α nucleating agent DBSand NA11, demonstrating that dimensional matching is an importantfactor for nucleation and growth of iPP.
Moreover, the crystallization temperature could also affect theinterfacial morphology of iPP induced by its own fiber and nucleatingagents. It is found in the experiments that the transcrystalline structuresof β-iPP can only generate below141°C. While the β nucleating agentNB328remained some nucleation capacity to β-iPP at the sametemperature, but it lose it at the crystallization temperature of143°C.
引文
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