四氟乙烯基热塑性含氟高分子流变行为与加工性能研究
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摘要
含氟高分子，特别是全氟离子聚合物，是太空、能源、国防等核心基础和战略尖端行业不可或缺的高性能材料，因此一直是各国重点开发和研究的对象。随着资源枯竭忧虑加深和能源供应日趋紧张，国际社会对含氟高分子的关注急剧升温，科研与工业部门迫切希望更充分、全面地掌握含氟高分子微观结构与宏观性能之间的关系（构效关系），为含氟高分子的生产、加工提供准确可靠指导，从而使其能更好地满足上述重要经济部门和行业的需要，也为含氟高分子成型及产品性能优化提供理论依据。
考察物质构效关系的手段众多，流变学即为其中重要、有力且操作方便的一种。流变学研究方法具有宏观统计的特征，材料流变行为与其内部结构、加工特性及宏观性能有着千丝万缕的联系，因此本论文通过线性粘弹性、傅里叶变换流变学（FTR）、加工流变学对四氟乙烯基热塑性含氟高分子（聚全氟乙丙烯（FEP）、乙烯-四氟乙烯交替共聚物（ETFE）和全氟磺酰氟树脂（全氟磺酸离子交换树脂前驱体，PFSF）的加工性能、流动行为和微观结构之间的关系进行了系统研究，以期为四氟乙烯基热塑性含氟高分子的加工成型和流动行为模拟及预测提供实验支持，从而为控制、优化此类含氟高分子的生产及调控终端产品性能提供指导依据。本论文主要研究内容如下：
1.研究了FEP、ETFE和PFSF的高速挤出流动行为。分别确定了上述三种含氟高分子的稳定流动区和粘度的剪切速率、温度、分子参数依赖性，同时对剪切粘度进行了模型拟合和数值分析；报道了上述三种含氟高分子的拉伸流变性质及其在稳定区外的流动和熔体破裂（及相应临界应力值）；考察了氟含量对直链（线形）四氟乙烯基含氟高分子加工性能的影响。结果发现：1）FEP高速挤出时稳定流动区非常窄（335°C下<86s-1），加工性能极差。证实了FEP加工性能“低劣”的深层原因是FEP分子链中F原子的大尺寸（相对于H原子）和C-F键的强极性（相对于C-H键）所引起的含氟分子链间独特的强相互作用，这使得FEP分子具有较强的链刚性，在剪切流动过程中应力难以耗散而迅速累积达到熔体破裂临界应力以致极早出现不稳定流动；2）与FEP相比，ETFE稳定流动区宽、加工性能优异。通过比较FEP、ETFE和PE（聚乙烯）等的高速挤出流动行为，发现氟含量增加将导致直链四氟乙烯基含氟高分子稳定流动区变窄、熔体破裂临界应力降低；3）加工流变学能灵敏、准确地评价PFSF的加工性能并反映PFSF分子参数对加工性能的影响——窄MWD（分子量分布）PFSF（nPFSF）剪切粘度高但随剪切速率增大而急剧下降；而宽MWD PFSF（wPFSF）剪切粘度低但粘度下降先慢后快；nPFSF熔体弹性大、临界应力极低（280°C时也仅为~0.07MPa，远低于通用高分子和其他含氟聚合物熔体的响应值），熔体破裂极早，而wPFSF的熔体弹性仅为nPFSF树脂的1/5，稳定流动区宽，加工性能好。
2.研究了FEP、ETFE和PFSF的动态振荡剪切流变性质（线性粘弹性）。发现各四氟乙烯基热塑性含氟高分子具热流变简单性，构建了各四氟乙烯基热塑性含氟高分子的动态模量主曲线，通过更具鲁棒性的数值方法——普适正则算法（generalized regularization method）获得了松弛时间谱。结果发现松弛时间谱能全面、准确地表征三种含氟高分子的流动行为，阐明分子结构对流动行为的影响。
3.首次研究了四氟乙烯基热塑性含氟高分子（FEP、ETFE和PFSF）的非线性动态流变学。非线性动态流变学能灵敏地区分含氟高分子结构，并跟踪其对外部流场的响应。研究表明含氟高分子的非线性动态流变行为与非氟高分子有许多不同。首次发现在本文实验条件下无论是全氟高分子（FEP、PFSF），还是部分含氟高分子（ETFE），其非线性条件下的I31（3次谐波相对强度）是应变的线性函数，而相应报道的非氟高分子的I31为应变的二次幂函数；基于Whilhelm非线性动态流变模型推出ETFE非线性粘弹性起始的临界应变为0.17，而PFSF-A、B和C树脂对应的临界应变分别为0.28、0.32和0.42。同种树脂较大的临界应变说明加工性好、抵抗破坏能力强，这从侧面说明非线性动态流变学可以用来评估含氟高分子的加工性能；实验显示PFSF的非线性强度与MW、MWD的关系与非氟高分子不同，当MW降低、MWD变窄时，非线性强度反而变大，具体原因尚在研究中。同时发现PFSF无应变Q系数（Q0系数）的频率函数在0.5Hz处有一个极大值，与线性粘弹模量函数的等模量（G’=G’’）交点频率不一致，这可能是PFSF的磺酰氟支链松弛或者测试过程中PFSF变质（交联或降解）所致，具体情形还有待进一步的实验验证。
Fluoropolymers, especially perfluorinated ionomers, are essential highperformance materials employed in fundamental basic industries and Hi-tech fieldssuch as aerospace exploration, energy utilization, and defense and securityapplications etc, and therefore attract continually intense and enormous attentionfrom all over the world. Moreover, with growing anxieties in resources exhaustingand insufficiency in energy support, fluoropolymers are a growing rapid hot focus ininternational scientists and engineers’ community and thus driving them to getinsight into the intrinsic relationship between microscopic structures andmacroscopic properties (the structures-properties relationship) of fluoropolymers.Understanding on such relationship not only guides synthesis, production, andprocess of fluoropolymers, and thus qualifies better application in the fundamentalbasic industries and Hi-tech fields above mentioned, but also set partially atheoretical basis for the further improvement and optimization of fluoropolymersperformance.
Among a great variety of techniques in exploring the structures-propertiesrelationship of polymers, rheology is one of such techniques with huge importance,applicability and easiness in operation. Rheology holds macroscopic statisticalcharacteristics, and rheological behaviors of materials are the mirror of their internalstructures, processability and other macroscopic performances, and herein therelationship between the processability, flow behaviors and molecular structures ofthree tetrafluoroethylene-based thermoplastic fluoropolymers, fluorinated ethylenepropylene copolymer (FEP), ethylene tetrafluoroethylene alternative copolymer(ETFE) and perfluorosulfonic acid ion exchange resin precursor (orperfluorosulfonyl fluoride resin, PFSF), was researched systematically and detailedly based on rheology, with aim to1) model, also predict, the processing and flowcharacteristics,2) control and optimize fluoropolymers forming and production, and3) tailor fluoropolymer products end performances. The outlines of this thesis are asfollowing:
1. Extrusion flow behaviors with high shear rates of FEP, ETFE and PFSF werepresented. The stable flow region and the temperature, shear rate dependence ofshear viscosity of the three fluoropolymers were determined, and modeling towardthe shear viscosities was also performed. Extensional viscosities, and flowperformance and melt fracture beyond stable flow region of the three fluoropolymerswere reported. Effect of fluorine substitution on processability of linearfluoropolymers was estimated. The results are listed below.1) FEPs possess quitenarrow stable flow region (<86s-1at335°C) and very poor processability; specialstrong interchain interaction of FEP originated from the bigger size of F atom than Hatom and stronger electronic polarity of C-F bond than C-H bond is the intrinsicdriving force of its poor processability. The bigger size of F atom and strongerelectronic polarity of C-F bond both cause strong chain stiffness of FEP. Duringshear flow, stress is cumulated quickly due to difficulty in energy dissipation withinhigh viscosity melt, and thus exceeds easily critical stress of melt fracture and thenmelt distortion occurs.2) Compared to FEP, ETFE holds wider stable region andsuperber processability. Researching on the high shear rate extrusion of FEP, ETFEand PE, it can be concluded tentatively that the more in fluorine substitution thenarrower steady flow region, the lower critical shear stress in melt fracture.3)Process rheology is adept enough in evaluation the processability of PFSFs andreflecting prompt the effect of microscopic structures of PFSFs on their processperformance. It appears that the PFSF with narrow molecular weight distribution(MWD)(nPFSF) possesses high shear viscosity and the viscosity sharply shifts downwhen shear rate increases. While the PFSF with wide MWD (wPFSF) holds lowshear viscosity and shear viscosity decreases slowly at the first and then the decreaseaccelerates with slower rate. At the same time, the nPFSF holds high melt elasticityand very low melt fracture critical shear stress (~0.07MPa within260~280°C), farlower than that of common polymers and other fluoropolymers, melt distortionappears extremely early. Contrary, the wPFSF, bears lower melt elasticity and widersteady flow region.
2. Dynamic oscillatory shear rheological characteristics of FEP, ETFE and PFSF were evaluated. Experiments justify that the three fluoropolymers havethermorheological simplicity. Corresponding dynamic modulus master curves ofeach the fluoropolymer were constructed and relaxation time spectra extracted fromdynamic modulus were obtained based on a more robust numeric analysis technique,Generalized regularization algorithm. Results confirm that relaxation time spectracan characterize the molecular motion and relaxation of the fluoropolymersaccurately, and also map molecular structure dependence of the fluoropolymers meltflow.
3. Nonlinear dynamic rheological properties of FEP, ETFE and PFSF wereexplored for the first time. It is found that nonlinear dynamic rheology can mapsensitively effect of oscillatory shear force field on the rheological behaviors of thefluoropolymers and differentiate their molecular structures. Compared withpolyolefins, some novel nonlinear dynamic rheological phenomena occur influoropolymers. It is the first discovery and report that I31(the third harmoniccomponent) value of fluoropolymers scale up in proportion with strain acted, ratherthan with the square of strain like non-fluoropolymers reported by Hyun et al. ViaWhilhelm model on nonlinear dynamic rheology, critical strain, which nonlinearviscoelasticity of polymer melts initiates, of ETFE is0.17and critical strains ofPFSF-A, PFSF-B and PFSF-C are0.28,0.32and0.42, respectively. Larger criticalstrain of the same resin means better processability and stronger resistance todeformation and structure breakage, which means that nonlinear dynamic rheologycan estimate processability of fluoropolymers. It is found that MW and MWDdependence of I31value of PFSF is not the same as that of polyolefins. When MWdecreases and MWD narrowens, I31of PFSF increases, while that of polyolefinsreported shifts down.There exists a local maximum in the frequency function of Q0coefficient (vanishing strain Q coefficient) of PFSF, which means have molecularrelaxation or network disentanglement corresponding to this maximum. Thefrequency corresponding to this local maximum is0.5Hz, not equal to the crossfrequency of equal modulus (G’=G’’) in the dynamic modulus master curves ofPFSF. Consequently, the maximum may correlate with sulfonyl fluoride branchrelaxation or crosslinking (and/or degradation) of PFSF during measuring whichneeds further experiments.
考察物质构效关系的手段众多，流变学即为其中重要、有力且操作方便的一种。流变学研究方法具有宏观统计的特征，材料流变行为与其内部结构、加工特性及宏观性能有着千丝万缕的联系，因此本论文通过线性粘弹性、傅里叶变换流变学（FTR）、加工流变学对四氟乙烯基热塑性含氟高分子（聚全氟乙丙烯（FEP）、乙烯-四氟乙烯交替共聚物（ETFE）和全氟磺酰氟树脂（全氟磺酸离子交换树脂前驱体，PFSF）的加工性能、流动行为和微观结构之间的关系进行了系统研究，以期为四氟乙烯基热塑性含氟高分子的加工成型和流动行为模拟及预测提供实验支持，从而为控制、优化此类含氟高分子的生产及调控终端产品性能提供指导依据。本论文主要研究内容如下：
1.研究了FEP、ETFE和PFSF的高速挤出流动行为。分别确定了上述三种含氟高分子的稳定流动区和粘度的剪切速率、温度、分子参数依赖性，同时对剪切粘度进行了模型拟合和数值分析；报道了上述三种含氟高分子的拉伸流变性质及其在稳定区外的流动和熔体破裂（及相应临界应力值）；考察了氟含量对直链（线形）四氟乙烯基含氟高分子加工性能的影响。结果发现：1）FEP高速挤出时稳定流动区非常窄（335°C下<86s-1），加工性能极差。证实了FEP加工性能“低劣”的深层原因是FEP分子链中F原子的大尺寸（相对于H原子）和C-F键的强极性（相对于C-H键）所引起的含氟分子链间独特的强相互作用，这使得FEP分子具有较强的链刚性，在剪切流动过程中应力难以耗散而迅速累积达到熔体破裂临界应力以致极早出现不稳定流动；2）与FEP相比，ETFE稳定流动区宽、加工性能优异。通过比较FEP、ETFE和PE（聚乙烯）等的高速挤出流动行为，发现氟含量增加将导致直链四氟乙烯基含氟高分子稳定流动区变窄、熔体破裂临界应力降低；3）加工流变学能灵敏、准确地评价PFSF的加工性能并反映PFSF分子参数对加工性能的影响——窄MWD（分子量分布）PFSF（nPFSF）剪切粘度高但随剪切速率增大而急剧下降；而宽MWD PFSF（wPFSF）剪切粘度低但粘度下降先慢后快；nPFSF熔体弹性大、临界应力极低（280°C时也仅为~0.07MPa，远低于通用高分子和其他含氟聚合物熔体的响应值），熔体破裂极早，而wPFSF的熔体弹性仅为nPFSF树脂的1/5，稳定流动区宽，加工性能好。
2.研究了FEP、ETFE和PFSF的动态振荡剪切流变性质（线性粘弹性）。发现各四氟乙烯基热塑性含氟高分子具热流变简单性，构建了各四氟乙烯基热塑性含氟高分子的动态模量主曲线，通过更具鲁棒性的数值方法——普适正则算法（generalized regularization method）获得了松弛时间谱。结果发现松弛时间谱能全面、准确地表征三种含氟高分子的流动行为，阐明分子结构对流动行为的影响。
3.首次研究了四氟乙烯基热塑性含氟高分子（FEP、ETFE和PFSF）的非线性动态流变学。非线性动态流变学能灵敏地区分含氟高分子结构，并跟踪其对外部流场的响应。研究表明含氟高分子的非线性动态流变行为与非氟高分子有许多不同。首次发现在本文实验条件下无论是全氟高分子（FEP、PFSF），还是部分含氟高分子（ETFE），其非线性条件下的I31（3次谐波相对强度）是应变的线性函数，而相应报道的非氟高分子的I31为应变的二次幂函数；基于Whilhelm非线性动态流变模型推出ETFE非线性粘弹性起始的临界应变为0.17，而PFSF-A、B和C树脂对应的临界应变分别为0.28、0.32和0.42。同种树脂较大的临界应变说明加工性好、抵抗破坏能力强，这从侧面说明非线性动态流变学可以用来评估含氟高分子的加工性能；实验显示PFSF的非线性强度与MW、MWD的关系与非氟高分子不同，当MW降低、MWD变窄时，非线性强度反而变大，具体原因尚在研究中。同时发现PFSF无应变Q系数（Q0系数）的频率函数在0.5Hz处有一个极大值，与线性粘弹模量函数的等模量（G’=G’’）交点频率不一致，这可能是PFSF的磺酰氟支链松弛或者测试过程中PFSF变质（交联或降解）所致，具体情形还有待进一步的实验验证。
Fluoropolymers, especially perfluorinated ionomers, are essential highperformance materials employed in fundamental basic industries and Hi-tech fieldssuch as aerospace exploration, energy utilization, and defense and securityapplications etc, and therefore attract continually intense and enormous attentionfrom all over the world. Moreover, with growing anxieties in resources exhaustingand insufficiency in energy support, fluoropolymers are a growing rapid hot focus ininternational scientists and engineers’ community and thus driving them to getinsight into the intrinsic relationship between microscopic structures andmacroscopic properties (the structures-properties relationship) of fluoropolymers.Understanding on such relationship not only guides synthesis, production, andprocess of fluoropolymers, and thus qualifies better application in the fundamentalbasic industries and Hi-tech fields above mentioned, but also set partially atheoretical basis for the further improvement and optimization of fluoropolymersperformance.
Among a great variety of techniques in exploring the structures-propertiesrelationship of polymers, rheology is one of such techniques with huge importance,applicability and easiness in operation. Rheology holds macroscopic statisticalcharacteristics, and rheological behaviors of materials are the mirror of their internalstructures, processability and other macroscopic performances, and herein therelationship between the processability, flow behaviors and molecular structures ofthree tetrafluoroethylene-based thermoplastic fluoropolymers, fluorinated ethylenepropylene copolymer (FEP), ethylene tetrafluoroethylene alternative copolymer(ETFE) and perfluorosulfonic acid ion exchange resin precursor (orperfluorosulfonyl fluoride resin, PFSF), was researched systematically and detailedly based on rheology, with aim to1) model, also predict, the processing and flowcharacteristics,2) control and optimize fluoropolymers forming and production, and3) tailor fluoropolymer products end performances. The outlines of this thesis are asfollowing:
1. Extrusion flow behaviors with high shear rates of FEP, ETFE and PFSF werepresented. The stable flow region and the temperature, shear rate dependence ofshear viscosity of the three fluoropolymers were determined, and modeling towardthe shear viscosities was also performed. Extensional viscosities, and flowperformance and melt fracture beyond stable flow region of the three fluoropolymerswere reported. Effect of fluorine substitution on processability of linearfluoropolymers was estimated. The results are listed below.1) FEPs possess quitenarrow stable flow region (<86s-1at335°C) and very poor processability; specialstrong interchain interaction of FEP originated from the bigger size of F atom than Hatom and stronger electronic polarity of C-F bond than C-H bond is the intrinsicdriving force of its poor processability. The bigger size of F atom and strongerelectronic polarity of C-F bond both cause strong chain stiffness of FEP. Duringshear flow, stress is cumulated quickly due to difficulty in energy dissipation withinhigh viscosity melt, and thus exceeds easily critical stress of melt fracture and thenmelt distortion occurs.2) Compared to FEP, ETFE holds wider stable region andsuperber processability. Researching on the high shear rate extrusion of FEP, ETFEand PE, it can be concluded tentatively that the more in fluorine substitution thenarrower steady flow region, the lower critical shear stress in melt fracture.3)Process rheology is adept enough in evaluation the processability of PFSFs andreflecting prompt the effect of microscopic structures of PFSFs on their processperformance. It appears that the PFSF with narrow molecular weight distribution(MWD)(nPFSF) possesses high shear viscosity and the viscosity sharply shifts downwhen shear rate increases. While the PFSF with wide MWD (wPFSF) holds lowshear viscosity and shear viscosity decreases slowly at the first and then the decreaseaccelerates with slower rate. At the same time, the nPFSF holds high melt elasticityand very low melt fracture critical shear stress (~0.07MPa within260~280°C), farlower than that of common polymers and other fluoropolymers, melt distortionappears extremely early. Contrary, the wPFSF, bears lower melt elasticity and widersteady flow region.
2. Dynamic oscillatory shear rheological characteristics of FEP, ETFE and PFSF were evaluated. Experiments justify that the three fluoropolymers havethermorheological simplicity. Corresponding dynamic modulus master curves ofeach the fluoropolymer were constructed and relaxation time spectra extracted fromdynamic modulus were obtained based on a more robust numeric analysis technique,Generalized regularization algorithm. Results confirm that relaxation time spectracan characterize the molecular motion and relaxation of the fluoropolymersaccurately, and also map molecular structure dependence of the fluoropolymers meltflow.
3. Nonlinear dynamic rheological properties of FEP, ETFE and PFSF wereexplored for the first time. It is found that nonlinear dynamic rheology can mapsensitively effect of oscillatory shear force field on the rheological behaviors of thefluoropolymers and differentiate their molecular structures. Compared withpolyolefins, some novel nonlinear dynamic rheological phenomena occur influoropolymers. It is the first discovery and report that I31(the third harmoniccomponent) value of fluoropolymers scale up in proportion with strain acted, ratherthan with the square of strain like non-fluoropolymers reported by Hyun et al. ViaWhilhelm model on nonlinear dynamic rheology, critical strain, which nonlinearviscoelasticity of polymer melts initiates, of ETFE is0.17and critical strains ofPFSF-A, PFSF-B and PFSF-C are0.28,0.32and0.42, respectively. Larger criticalstrain of the same resin means better processability and stronger resistance todeformation and structure breakage, which means that nonlinear dynamic rheologycan estimate processability of fluoropolymers. It is found that MW and MWDdependence of I31value of PFSF is not the same as that of polyolefins. When MWdecreases and MWD narrowens, I31of PFSF increases, while that of polyolefinsreported shifts down.There exists a local maximum in the frequency function of Q0coefficient (vanishing strain Q coefficient) of PFSF, which means have molecularrelaxation or network disentanglement corresponding to this maximum. Thefrequency corresponding to this local maximum is0.5Hz, not equal to the crossfrequency of equal modulus (G’=G’’) in the dynamic modulus master curves ofPFSF. Consequently, the maximum may correlate with sulfonyl fluoride branchrelaxation or crosslinking (and/or degradation) of PFSF during measuring whichneeds further experiments.
引文
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