剪切作用下聚烯烃共混物的形态控制与性能
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摘要
研究高分子成型加工中的形态控制问题,在成型过程中引入特殊加工方法,
改变聚合物的凝聚态结构,从而改变其性能是优化材料性能和用途的经济而实
用的方法,是目前国际上高分子科学研究的热点之一,已成为我国高分子材料
科学与工程的一个重要研究课题。本论文采用在注射成型过程中引入剪切应力
场的作用,使聚合物及其共混物在往复剪切应力作用下逐渐冷却固化成型,通
过剪切应力的作用控制基体和分散相在成型过程中的形态发展,相容与相分离、
相转变、取向和结晶等凝聚态结构,并且通过熔体冷却固化将应力对共混物微
观形态结构的影响冻结下来,进而研究微观形态结构变化对共混物材料宏观力
学性能的影响。通过上述方法制备了几种聚烯烃共混物,系统研究了剪切应力
作用下聚烯烃及其共混物取向和结晶,相容与相分离、相转变等形态结构的变
化,以及共混体系性能的变化。本文还详细研究了剪切应力诱导橡胶粒子形变
和取向,及其共混物 PP/EPDM 在冲击断裂过程中的断裂行为。主要研究结果如
下:
(1)研究了剪切对注射成型制品各向异性的影响。发现在剪切应力作用下,熔
体经注塑机注射入模具型腔后,熔体遇到处于室温的模具,皮层首先快速冷却
固化;随后施加的剪切应力推动熔体在型腔中往复流动,受到持续的剪切应力
作用,熔体逐渐冷却固化成型,应力对形态结构的影响一并冻结下来,即形成
剪切层;剪切停止后,试样进一步冷却,应力的影响可以通过聚合物分子链的
松弛得以消除,形成明显的芯层结构。后续的实验证明,剪切作用下固化成型
的动态试样不同区域表现出不同的形态结构。
(2)对聚烯烃(HDPE、LDPE、LLDPE、PP 等)及其共混物(HDPE/LLDPE、
HDPE/LDPE、PP/LLDPE 等)的研究表明,剪切应力作用下固化成型的聚合物
及其共混物的拉伸强度、杨氏模量、缺口冲击强度等都有不同程度的提高,获
1
四川大学博士学位论文
得了具有高拉伸强度和高冲击强度的超级聚烯烃共混物。HDPE 和 PP 的拉伸强
度增加比较明显,而 LDPE 和 LLDPE 拉伸强度增加较弱,这主要是由于不同的
聚合物在相同的剪切应力作用下分子链结构的差异导致其运动能力不同,从而
导致不同的取向结果。2d-WAXD 研究结果表明,在相同的剪切应力条件下,
HDPE 和 PP 具有明显的取向行为,其取向度较大,而 LLDPE 和 LDPE 的取向
较弱。分散相对基体取向的影响不同,研究发现,在共混物 HDPE/LDPE 中,
分散相 LDPE 的增加,基体 HDPE 的取向程度减弱。而 PP/LLDPE 共混物中,
分散相 LLDPE 的增加,PP 的取向程度先增加而后降低。在 PP/EC 共混物中也
发现加入低含量的 EC,可以显著改善基体的取向程度,从而改善共混物的拉伸
性能。具有较低粘度和较好流动性的分散相的加入改善了共混物的熔体流动性
是造成基体取向程度增加的主要原因。进一步证明,拉伸强度主要与剪切层的
面积大小有关,即与共混物在熔体冷却过程中的取向程度的大小有关;而冲击
强度主要与剪切层和芯层有关。在冲击断裂过程中,动态样品不同区域表现出
不同的断裂模式,皮层和芯层产生的大量银纹和材料的拔出吸收大量能量,为
典型的韧性断裂;而剪切层断面平整光滑,为脆性断裂模式。
(3)采用半晶性聚合物研究了剪切应力对聚合物结晶形态和片晶取向的影响,
DSC、SEM、2d-SAXD 等结果表明在应力作用下,共混物不同区域形成不同的
结晶结构。HDPE 在应力作用下形成较多的 shish-kebab 结构,表现出力学性能
的显著增加;PP 在皮层以 shish 结构为主,剪切层中形成 shish-kebab 结构,而
芯层以 kebab 结构为主。共混物 PP/LLDPE 中,PP 在不同区域都形成 shish-kebab
结构,而 LLDPE 除了生成片晶取向方向垂直于剪切流动方向以外,还沿剪切流
动方向发生一定角度的偏转(450～500),这可能与片晶中晶块在剪切作用下沿
流动方向滑移有关。剪切作用下,聚合物所形成的 shish 伸直链晶体,在熔融重
结晶过程中,诱导基体在较低的过冷度下结晶。EC 的加入使 PP 在相同剪切条
件下生成更多的 shish 伸直链晶体。
(4)橡胶增韧塑料的研究由来已久,并在此基础上提出了许多增韧理论和判据,
其中最著名的就是 Wu 氏增韧理论,认为临界基体层厚度Tc 是橡胶增韧塑料的
唯一判据,即当橡胶粒子间距TTc ,共
混物表现为脆性断裂;当T =Tc 时,共混物发生脆韧转变。但需要注意的是,
2
四川大学博士学位论文
Wu 氏增韧理论最重要的一个前提就是作为分散相的橡胶粒子在基体中呈球形
简立方分布。因此为了进一步研究橡胶在塑料中的增韧行为,本文选择 EPDM
作为分散相,PP 作为基体,在注射成型过程中施加动态剪切应力场,控制基体
的取向、分散相的形变和取向、以及共混体系相分离行为。实验表明,随着橡
胶含量的增加,其形变和取向的程度增加,当这种形变达到一定程度时,共混
物的韧性明显降低,体系发生明显的韧-脆转变行为。通过对基体层厚度的测
量和计算表明,当共混物中橡胶粒子发生形变和取向时,Wu 氏增韧理论的临界
基体层厚度作为共混物韧性行为的判据不再适用,此时,当T 表现出明显的韧性降低
The morphology controlling of polymer blends during the process is one of the
hottest research topics in polymer science and engineering at present. The aim of
morphology controlling is to achieve the desired structure via special ways thus
improve the properties of polymer blends. In this work, polyolefin and their blends
were cooled and solidified under the shear stress condition via the introduction of
shear stress field during the injection process. The morphology, miscibility and phase
separation, phase inversion, orientation and crystallization of polymer blends were
greatly affected under the effect of shear stress fields. The alteration of morphology
was kept by the way of solidification of melt blends. And then, the correlation
between the morphology and the mechanical properties could be established.
The main results are:
1.The effect of shear stress on anisotropic of injection-molded samples was studied.
After the melt was injected into the mold, the specimen was forced to move
repeatedly in a chamber by two pistons that moved reversibly with the same
frequency as the solidification progressively occurred from the mold wall to the
molding core part. During the cooling of the sample, three different structures were
formed, namely, the skin, the shear layer and the core. The further experiments
suggested that the morphologies among the three layers were different.
2. The study of the polyolefin (such as HDPE, LDPE, LLDPE and PP) and their
blends (such as HDPE/LLDPE, HDPE/LLDPE and PP/LLDPE) suggested that the
tensile strength, the elastic module and the Izod notched impact strength could be
improved at the different degree, depending on the molecular architecture and phase
morphology. And the super polyolefin blends, which had higher tensile properties
5
四川大学博士学位论文
and higher impact properties, were obtained. 2d-WAXD was adopted to study the
effect of shear stress on orientation of the polymers and their blends. The results
showed that different polymer had the different orientation behavior in the same
shear condition, and the orientation of HDPE and PP was easier than that of LLDPE
and LDPE. On the other hand, in the blends, the effect of dispersed phase on the
orientation of matrix was different. In HDPE/LDPE blends, the degree of orientation
of HDPE was decreased with the increasing of LDPE content, while in PP/LLDPE
blends, the degree of orientation of PP was increased firstly and then was decreased
with the increasing of LLDPE content. In PP/EC blends, the orientation ability of PP
was improved greatly when a few EC was added into PP. Further experiments
showed that the tensile strength was related to the area of shear layer, which further
proved that the orientation of polymers is a key to improve the mechanical properties.
On the other hand, the impact strength was related to the shear layer and the core
layer. The skin and the core showed a typical ductile-fracture mode since the much
craze was formed and some materials were pulled out during the fracture propagation.
While for the shear layer, the fractured surface was very smooth, which is the typical
character of brittle-fracture mode.
3. The effect of shear stress on crystallization and lamellar orientation was studied
in the work. The results of DSC, SEM and 2d-SAXD proved that different crystal
structures were formed in the different zones of the prepared samples. Much more
shish-kebab structure was formed in HDPE and the mechanical properties were
proved greatly. While in PP, shish structure formed in the skin, shish-kebab structure
formed in the shear layer and kebab structure formed in the core zone. But in
PP/LLDPE blends, PP formed shish-kebab structure in each different zones, while a
very unique crystal morphology and lamellar orientation of LLDPE were obtained,
with the lamellar stack oriented either perpendicular or 45-500 away from the shear
flow direction. And the further study suggested that shish structure formed in th
改变聚合物的凝聚态结构,从而改变其性能是优化材料性能和用途的经济而实
用的方法,是目前国际上高分子科学研究的热点之一,已成为我国高分子材料
科学与工程的一个重要研究课题。本论文采用在注射成型过程中引入剪切应力
场的作用,使聚合物及其共混物在往复剪切应力作用下逐渐冷却固化成型,通
过剪切应力的作用控制基体和分散相在成型过程中的形态发展,相容与相分离、
相转变、取向和结晶等凝聚态结构,并且通过熔体冷却固化将应力对共混物微
观形态结构的影响冻结下来,进而研究微观形态结构变化对共混物材料宏观力
学性能的影响。通过上述方法制备了几种聚烯烃共混物,系统研究了剪切应力
作用下聚烯烃及其共混物取向和结晶,相容与相分离、相转变等形态结构的变
化,以及共混体系性能的变化。本文还详细研究了剪切应力诱导橡胶粒子形变
和取向,及其共混物 PP/EPDM 在冲击断裂过程中的断裂行为。主要研究结果如
下:
(1)研究了剪切对注射成型制品各向异性的影响。发现在剪切应力作用下,熔
体经注塑机注射入模具型腔后,熔体遇到处于室温的模具,皮层首先快速冷却
固化;随后施加的剪切应力推动熔体在型腔中往复流动,受到持续的剪切应力
作用,熔体逐渐冷却固化成型,应力对形态结构的影响一并冻结下来,即形成
剪切层;剪切停止后,试样进一步冷却,应力的影响可以通过聚合物分子链的
松弛得以消除,形成明显的芯层结构。后续的实验证明,剪切作用下固化成型
的动态试样不同区域表现出不同的形态结构。
(2)对聚烯烃(HDPE、LDPE、LLDPE、PP 等)及其共混物(HDPE/LLDPE、
HDPE/LDPE、PP/LLDPE 等)的研究表明,剪切应力作用下固化成型的聚合物
及其共混物的拉伸强度、杨氏模量、缺口冲击强度等都有不同程度的提高,获
1
四川大学博士学位论文
得了具有高拉伸强度和高冲击强度的超级聚烯烃共混物。HDPE 和 PP 的拉伸强
度增加比较明显,而 LDPE 和 LLDPE 拉伸强度增加较弱,这主要是由于不同的
聚合物在相同的剪切应力作用下分子链结构的差异导致其运动能力不同,从而
导致不同的取向结果。2d-WAXD 研究结果表明,在相同的剪切应力条件下,
HDPE 和 PP 具有明显的取向行为,其取向度较大,而 LLDPE 和 LDPE 的取向
较弱。分散相对基体取向的影响不同,研究发现,在共混物 HDPE/LDPE 中,
分散相 LDPE 的增加,基体 HDPE 的取向程度减弱。而 PP/LLDPE 共混物中,
分散相 LLDPE 的增加,PP 的取向程度先增加而后降低。在 PP/EC 共混物中也
发现加入低含量的 EC,可以显著改善基体的取向程度,从而改善共混物的拉伸
性能。具有较低粘度和较好流动性的分散相的加入改善了共混物的熔体流动性
是造成基体取向程度增加的主要原因。进一步证明,拉伸强度主要与剪切层的
面积大小有关,即与共混物在熔体冷却过程中的取向程度的大小有关;而冲击
强度主要与剪切层和芯层有关。在冲击断裂过程中,动态样品不同区域表现出
不同的断裂模式,皮层和芯层产生的大量银纹和材料的拔出吸收大量能量,为
典型的韧性断裂;而剪切层断面平整光滑,为脆性断裂模式。
(3)采用半晶性聚合物研究了剪切应力对聚合物结晶形态和片晶取向的影响,
DSC、SEM、2d-SAXD 等结果表明在应力作用下,共混物不同区域形成不同的
结晶结构。HDPE 在应力作用下形成较多的 shish-kebab 结构,表现出力学性能
的显著增加;PP 在皮层以 shish 结构为主,剪切层中形成 shish-kebab 结构,而
芯层以 kebab 结构为主。共混物 PP/LLDPE 中,PP 在不同区域都形成 shish-kebab
结构,而 LLDPE 除了生成片晶取向方向垂直于剪切流动方向以外,还沿剪切流
动方向发生一定角度的偏转(450～500),这可能与片晶中晶块在剪切作用下沿
流动方向滑移有关。剪切作用下,聚合物所形成的 shish 伸直链晶体,在熔融重
结晶过程中,诱导基体在较低的过冷度下结晶。EC 的加入使 PP 在相同剪切条
件下生成更多的 shish 伸直链晶体。
(4)橡胶增韧塑料的研究由来已久,并在此基础上提出了许多增韧理论和判据,
其中最著名的就是 Wu 氏增韧理论,认为临界基体层厚度Tc 是橡胶增韧塑料的
唯一判据,即当橡胶粒子间距T
混物表现为脆性断裂;当T =Tc 时,共混物发生脆韧转变。但需要注意的是,
2
四川大学博士学位论文
Wu 氏增韧理论最重要的一个前提就是作为分散相的橡胶粒子在基体中呈球形
简立方分布。因此为了进一步研究橡胶在塑料中的增韧行为,本文选择 EPDM
作为分散相,PP 作为基体,在注射成型过程中施加动态剪切应力场,控制基体
的取向、分散相的形变和取向、以及共混体系相分离行为。实验表明,随着橡
胶含量的增加,其形变和取向的程度增加,当这种形变达到一定程度时,共混
物的韧性明显降低,体系发生明显的韧-脆转变行为。通过对基体层厚度的测
量和计算表明,当共混物中橡胶粒子发生形变和取向时,Wu 氏增韧理论的临界
基体层厚度作为共混物韧性行为的判据不再适用,此时,当T
The morphology controlling of polymer blends during the process is one of the
hottest research topics in polymer science and engineering at present. The aim of
morphology controlling is to achieve the desired structure via special ways thus
improve the properties of polymer blends. In this work, polyolefin and their blends
were cooled and solidified under the shear stress condition via the introduction of
shear stress field during the injection process. The morphology, miscibility and phase
separation, phase inversion, orientation and crystallization of polymer blends were
greatly affected under the effect of shear stress fields. The alteration of morphology
was kept by the way of solidification of melt blends. And then, the correlation
between the morphology and the mechanical properties could be established.
The main results are:
1.The effect of shear stress on anisotropic of injection-molded samples was studied.
After the melt was injected into the mold, the specimen was forced to move
repeatedly in a chamber by two pistons that moved reversibly with the same
frequency as the solidification progressively occurred from the mold wall to the
molding core part. During the cooling of the sample, three different structures were
formed, namely, the skin, the shear layer and the core. The further experiments
suggested that the morphologies among the three layers were different.
2. The study of the polyolefin (such as HDPE, LDPE, LLDPE and PP) and their
blends (such as HDPE/LLDPE, HDPE/LLDPE and PP/LLDPE) suggested that the
tensile strength, the elastic module and the Izod notched impact strength could be
improved at the different degree, depending on the molecular architecture and phase
morphology. And the super polyolefin blends, which had higher tensile properties
5
四川大学博士学位论文
and higher impact properties, were obtained. 2d-WAXD was adopted to study the
effect of shear stress on orientation of the polymers and their blends. The results
showed that different polymer had the different orientation behavior in the same
shear condition, and the orientation of HDPE and PP was easier than that of LLDPE
and LDPE. On the other hand, in the blends, the effect of dispersed phase on the
orientation of matrix was different. In HDPE/LDPE blends, the degree of orientation
of HDPE was decreased with the increasing of LDPE content, while in PP/LLDPE
blends, the degree of orientation of PP was increased firstly and then was decreased
with the increasing of LLDPE content. In PP/EC blends, the orientation ability of PP
was improved greatly when a few EC was added into PP. Further experiments
showed that the tensile strength was related to the area of shear layer, which further
proved that the orientation of polymers is a key to improve the mechanical properties.
On the other hand, the impact strength was related to the shear layer and the core
layer. The skin and the core showed a typical ductile-fracture mode since the much
craze was formed and some materials were pulled out during the fracture propagation.
While for the shear layer, the fractured surface was very smooth, which is the typical
character of brittle-fracture mode.
3. The effect of shear stress on crystallization and lamellar orientation was studied
in the work. The results of DSC, SEM and 2d-SAXD proved that different crystal
structures were formed in the different zones of the prepared samples. Much more
shish-kebab structure was formed in HDPE and the mechanical properties were
proved greatly. While in PP, shish structure formed in the skin, shish-kebab structure
formed in the shear layer and kebab structure formed in the core zone. But in
PP/LLDPE blends, PP formed shish-kebab structure in each different zones, while a
very unique crystal morphology and lamellar orientation of LLDPE were obtained,
with the lamellar stack oriented either perpendicular or 45-500 away from the shear
flow direction. And the further study suggested that shish structure formed in th
引文
[1] 瞿金平,胡汉杰,聚合物成型原理及成型技术,化学工业出版社,2001
[2] Allan P.S., Bevis M.J., Multiple live-feed injection-molding, Plastics. Rubber.
Process. Appl., 1987, 7, 3
[3] Allan P.S., Bevis M.J., Composites Manufacturing, 1990, 1, 79
[4] Allan P.S., Bevis M.J., British Patent 2170-140-B
[5] Kalay G., Allan P.S., Bevis M.J., |?phase in injection moulded isotactic
polypropylene, Polymer, 1994, 35, 2480
[6] Kalay G., Allan P., Bevis M.J., in Proc. of The International Polypropylene
Conference, The Institute of Materials, London, 24-25 October 1994, pp. 109
[7] Kalay G., Allan P.S., Bevis M.J., Plastics, Rubber Compos. Process. Applicat.,
1995, 23, 71
[8] Ogbonna C.I., Kalay G., Allan P., Bevis M.J., The self-reinforcement of
polyolefins produced by shear controlled orientation in injection molding, J. Appl.
Polym. Sci., 1995, 58, 2131
[9] Kalay G., Ogbonna C., Allan P.S., Bevis M.J., The management of microstructure
in semicrystalline polymers, Trans. IchemE., Part A, 1995, 73, 798
[10] Kalay G., Zhong Z., Allan P., Bevis M.J., The occurrence of the |?-phase in
injection moulded polypropylene in relation to the processing conditions, Polymer,
1996, 37, 2077
[11] Kalay G., Allan P.S., Bevis M.J., Shear controlled orientation, Kunststoffe, 1997,
87. 768
[12] Kalay G., Bevis M.J., J. Polym. Sci. Part B: Polym. Phys., Processing and
physical property relationships in injection-molded isotactic polypropylene. 1.
mechanical properties, 1997, 35, 241
[13] Kalay G., Bevis M.J., J. Polym. Sci. Part B: Polym. Phys., Processing and
physical property relationships in injection-molded isotactic polypropylene. 2.
morphology and crystallinity, 1997, 35, 265
[14] Kalay G., Bevis M.J., J. Polym. Sci. Part B: Polym. Phys., The effect of shear
44
四川大学博士学位论文
controlled orientation in injection moulding on the mechanical properties of an
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