聚乙烯熔体在突变收敛流道挤出口模内流变行为双折射理论与实验研究
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摘要
挤出成型是塑料成型加工的重要方法之一，几乎所有的热塑性塑料都可以用挤出成型方法来加工，因此它在塑料成型加工中占有重要的地位。电磁动态塑化挤出机首次将振动力场引入到聚合物挤出全过程，振动力场的引入对聚合物塑化挤出过程和熔体流变行为产生了重大影响。
掌握聚合物熔体在挤出机口模内的流变行为，对于合理设计成型工艺参数、制备性能优异的制品具有重要指导意义。因而借助于可视化技术手段，真实的描述聚合物熔体在动态挤出成型条件下口模内的流动情况，了解聚合物熔体对振动力场的响应规律，对研究电磁动态塑化挤出机的成型机理具有重要的科学与现实意义。据此，本文主要作了以下几方面的工作：
首先，介绍了应用流动双折射方法研究聚合物熔体流变性能的基本原理，说明了应力光学系数的科学意义及其计算方法。在计算流场剪切应力方面，提出一种新的流动双折射测量方法。通过重新合理地布置装置中的光学元件，使得测量的条纹图中既有等差线信息，同时又包含取向角信息，从而根据应力光学定律对应力分布进行计算。
其次，对三种商业聚乙烯材料的流变性能进行了表征，分析了三种材料的流变响应特性。应用高压毛细管流变仪测量了熔体在不同长径比口模下稳态剪切流动时的流变特性，根据Cogswell模型计算了三种聚乙烯熔体的拉伸粘度；应用高温凝胶色谱仪测定了材料的相对分子量及其分布；应用旋转流变仪测量了三种商业聚乙烯材料的流变性能，并通过Matlab编程，运用非线性拟合方法计算了材料的离散松弛时间谱。
然后，根据熔体狭缝口模入口区的压力分布特点建立了入口长度模型，并根据稳态实验数据计算了不同条件下的入口长度；同时，应用双折射测量装置，在装有突变收缩流道口模的电磁振动塑化挤出机上进行了稳态挤出双折射实验，测量了不同加工条件的入口长度，验证了入口长度模型的可行性；应用粒子图像测速（PIV）技术测量了流场的速度分布，计算了熔体的表观拉伸粘度，并与Cogswell模型的计算结果进行了比较。
最后，对三种聚合物进行了动态挤出实验分析。应用压力传感器测量了熔体在挤出机口模内沿流动方向的压力降，通过即得即测的方法测量熔体挤出速率，计算了熔体在振动条件下的瞬时剪切粘度，讨论了振动条件对流场应力分布、挤出成型压力及挤出速率等参数的影响；应用流动双折射实验装置，测得聚合物熔体在振动挤出过程中的双折射条纹图，得到了在不同振动条件下的流动双折射图谱，分析了相应流场的应力状态，计算了流场对称轴上的拉伸应力，分析了振动条件对熔体拉伸应力的影响。
Extrusion molding, as one main method of plastic forming, plays an important role inplastic industry, by which almost all thermoplastics can be processed. Electromagneticdynamic plastics extruder introduces the vibration force field into the whole process ofpolymer extrusion for the first time, and the vibration force field has a significant impact onthe rheological behavior of polymer melts in the whole forming process.
It is instructive, for the reasonable decision of process parameters and the preparation ofproducts with excellent mechanical performance, to master the knowledge of the rheologicalbehavior of polymer melt in the die. So, to give a real characterization of the flow of polymermelts in the die, to master the knowledge of the response property of polymer melts to thevibration force field are of vital important scientific and practical significance to study theforming mechanism of the electromagnetic dynamic plastics extrusion.
First, the basic principles of the method of flow induced birefringence to study therheological properties of polymer melts are introduced, and the scientific significance of thestress-optic coefficient is introduced, the method to calculate the stress-optic coefficient isintroduced as well.
Secondly, the rheological properties of the three used commercial polyethylene materialsin the experiments were characterized. The melt rheological properties in steady shear floware measured by a high pressure capillary rheometer and the extensional viscosity of theLDPEs were calculated using the famous Cogswell model; the molecular weight and itsdistribution of the three materials are determined by the application of a high-temperature gelchromatography; the rheological properties of three in the small oscillatory shear flow aremeasured by the use of a rotational rheometer, the discrete relaxation time spectra of fivemodes are calculated through the nonlinear fitting method making use of the Matlab programpackage, which would be used in the next numerical simulation.
Thirdly, a mathematical model is built to calculate the entrance length and the entrancelengths are calculated from the steady extrusion experimental data. At the same time, theentrance length at different processing conditions are measured by the application ofbirefringence measurement equipment, useful data will be provide for the optimization of forming parameters and of the designation of the die lip. It is proved by the comparison of thecalculted and measured entrance length that, this mathematical model is able to be used topredict the entrance length from the data of flow rate and the relaxation time of the material.The transient extensional viscosities were obtained from the calculated extensional stress byflow birefringence fringes and the measured velocity by PIV along the symmetry axis of thecontraction die.
Subsequently, the flow induced birefringence experiments are performed on the vibrationextruder, which equipped with an abrupt contraction die. The flow birefringence fringes areobtained during the extrusion process, the pressure drops along the die symmetry axis aremeasured by applying pressure sensors, the flow rate are measured by catch and measuremethod. The birefringence fringes are obtained in a variation of vibration conditions, byswitching the vibration frequency and vibration amplitude, the corresponding stress state ofthe flow field are analyzed, including shear stress and first normal stress difference, theinfluence of vibration parameters on the stress distribution of the flow field, on the extrusionpressure and flow rate are discussed semi-quantitatively.
In the end, a novel flow induced birefringence method is proposed on the basis of theconventional equipment. The birefringence fringes obtained from the conventional equipmentcan not be used to calculate the shear stress of the flow field for the lack of the information ofthe orientation angle. Here the obtained pictures contain information not only of isoclinic butalso of isochromatic by rearranged the optic components, which can be used to calculate theshear stress directly.
掌握聚合物熔体在挤出机口模内的流变行为，对于合理设计成型工艺参数、制备性能优异的制品具有重要指导意义。因而借助于可视化技术手段，真实的描述聚合物熔体在动态挤出成型条件下口模内的流动情况，了解聚合物熔体对振动力场的响应规律，对研究电磁动态塑化挤出机的成型机理具有重要的科学与现实意义。据此，本文主要作了以下几方面的工作：
首先，介绍了应用流动双折射方法研究聚合物熔体流变性能的基本原理，说明了应力光学系数的科学意义及其计算方法。在计算流场剪切应力方面，提出一种新的流动双折射测量方法。通过重新合理地布置装置中的光学元件，使得测量的条纹图中既有等差线信息，同时又包含取向角信息，从而根据应力光学定律对应力分布进行计算。
其次，对三种商业聚乙烯材料的流变性能进行了表征，分析了三种材料的流变响应特性。应用高压毛细管流变仪测量了熔体在不同长径比口模下稳态剪切流动时的流变特性，根据Cogswell模型计算了三种聚乙烯熔体的拉伸粘度；应用高温凝胶色谱仪测定了材料的相对分子量及其分布；应用旋转流变仪测量了三种商业聚乙烯材料的流变性能，并通过Matlab编程，运用非线性拟合方法计算了材料的离散松弛时间谱。
然后，根据熔体狭缝口模入口区的压力分布特点建立了入口长度模型，并根据稳态实验数据计算了不同条件下的入口长度；同时，应用双折射测量装置，在装有突变收缩流道口模的电磁振动塑化挤出机上进行了稳态挤出双折射实验，测量了不同加工条件的入口长度，验证了入口长度模型的可行性；应用粒子图像测速（PIV）技术测量了流场的速度分布，计算了熔体的表观拉伸粘度，并与Cogswell模型的计算结果进行了比较。
最后，对三种聚合物进行了动态挤出实验分析。应用压力传感器测量了熔体在挤出机口模内沿流动方向的压力降，通过即得即测的方法测量熔体挤出速率，计算了熔体在振动条件下的瞬时剪切粘度，讨论了振动条件对流场应力分布、挤出成型压力及挤出速率等参数的影响；应用流动双折射实验装置，测得聚合物熔体在振动挤出过程中的双折射条纹图，得到了在不同振动条件下的流动双折射图谱，分析了相应流场的应力状态，计算了流场对称轴上的拉伸应力，分析了振动条件对熔体拉伸应力的影响。
Extrusion molding, as one main method of plastic forming, plays an important role inplastic industry, by which almost all thermoplastics can be processed. Electromagneticdynamic plastics extruder introduces the vibration force field into the whole process ofpolymer extrusion for the first time, and the vibration force field has a significant impact onthe rheological behavior of polymer melts in the whole forming process.
It is instructive, for the reasonable decision of process parameters and the preparation ofproducts with excellent mechanical performance, to master the knowledge of the rheologicalbehavior of polymer melt in the die. So, to give a real characterization of the flow of polymermelts in the die, to master the knowledge of the response property of polymer melts to thevibration force field are of vital important scientific and practical significance to study theforming mechanism of the electromagnetic dynamic plastics extrusion.
First, the basic principles of the method of flow induced birefringence to study therheological properties of polymer melts are introduced, and the scientific significance of thestress-optic coefficient is introduced, the method to calculate the stress-optic coefficient isintroduced as well.
Secondly, the rheological properties of the three used commercial polyethylene materialsin the experiments were characterized. The melt rheological properties in steady shear floware measured by a high pressure capillary rheometer and the extensional viscosity of theLDPEs were calculated using the famous Cogswell model; the molecular weight and itsdistribution of the three materials are determined by the application of a high-temperature gelchromatography; the rheological properties of three in the small oscillatory shear flow aremeasured by the use of a rotational rheometer, the discrete relaxation time spectra of fivemodes are calculated through the nonlinear fitting method making use of the Matlab programpackage, which would be used in the next numerical simulation.
Thirdly, a mathematical model is built to calculate the entrance length and the entrancelengths are calculated from the steady extrusion experimental data. At the same time, theentrance length at different processing conditions are measured by the application ofbirefringence measurement equipment, useful data will be provide for the optimization of forming parameters and of the designation of the die lip. It is proved by the comparison of thecalculted and measured entrance length that, this mathematical model is able to be used topredict the entrance length from the data of flow rate and the relaxation time of the material.The transient extensional viscosities were obtained from the calculated extensional stress byflow birefringence fringes and the measured velocity by PIV along the symmetry axis of thecontraction die.
Subsequently, the flow induced birefringence experiments are performed on the vibrationextruder, which equipped with an abrupt contraction die. The flow birefringence fringes areobtained during the extrusion process, the pressure drops along the die symmetry axis aremeasured by applying pressure sensors, the flow rate are measured by catch and measuremethod. The birefringence fringes are obtained in a variation of vibration conditions, byswitching the vibration frequency and vibration amplitude, the corresponding stress state ofthe flow field are analyzed, including shear stress and first normal stress difference, theinfluence of vibration parameters on the stress distribution of the flow field, on the extrusionpressure and flow rate are discussed semi-quantitatively.
In the end, a novel flow induced birefringence method is proposed on the basis of theconventional equipment. The birefringence fringes obtained from the conventional equipmentcan not be used to calculate the shear stress of the flow field for the lack of the information ofthe orientation angle. Here the obtained pictures contain information not only of isoclinic butalso of isochromatic by rearranged the optic components, which can be used to calculate theshear stress directly.
引文
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