磁场作用下聚合物的凝固组织研究
摘要
本论文以高密度聚乙烯(HDPE)、等规聚丙烯(iPP)、间规聚苯乙烯(sPS)、聚甲醛(POM)以及聚对苯二甲酸乙二醇酯(PET)为研究对象,采用0.1T～0.3T的直流磁场、交流磁场、10T脉冲磁场及12T强磁场,考察聚合物凝固过程中结晶形态及取向的变化。采用金相显微镜、差示扫描量热法(DSC)、X射线衍射法(XRD)和红外光谱法(FT-IR)对磁场改性前后的结晶聚合物的结构变化进行了系统地观察和分析讨论,研究结果如下：
高密度聚乙烯(HDPE)在磁场下凝固的组织形貌发生了明显的变化,并且结晶度和结晶取向随着施加磁场强度的增加而增加。在直流磁场下凝固的聚乙烯的片晶厚度明显增大,片晶间距有小幅增加,形成的球晶尺寸增加；施加交流磁场后,片晶厚度变小,片晶间距也明显减小。
等规聚丙烯(iPP)在直流、交流和脉冲三种磁场下凝固时分子链易受外磁场的作用而产生诱导偶极,凝固时分子链构象规整性提高,晶粒沿外加磁场方向择优取向。直流磁场和脉冲磁场下凝固的聚丙烯熔点提高,凝固组织有生成串晶的趋势；交流磁场方向的周期变化,阻碍了聚丙烯形成完整的串晶结构,导致了聚丙烯的结晶度下降,熔点降低。
间规聚苯乙烯(sPS)在直流磁场下凝固的晶型仍为β晶型,晶粒尺寸变小,片晶沿顺磁场方向排列,熔点提高以及晶体中β晶型结晶度增加。这一结果的产生是由于sPS分子链在磁场环境下改变了堆砌方式,分子链沿顺磁场方向排列,阻碍了分子链折叠弯曲,晶粒的生长方向受到限制,片晶尺寸减小,形成了漩涡状的球晶形态。
聚甲醛(POM)的分子链在磁场下克服空间位阻效应而更有利于C—O—-C对称伸缩振动,减弱了C—O—C弯曲振动,从而减小晶片间增厚阻力,使片晶的厚度和间距增大,晶粒也沿磁场方向取向排列。随着施加磁场的强度增加,聚甲醛晶体的球晶尺寸、熔点以及晶粒沿磁场方向排列的取向比率都呈上升趋势,当磁场强度达到12T时,在聚甲醛晶体的横截面上发现明显的片晶类似漩涡排列的现象。
聚对苯二甲酸乙二醇酯(PET)在直流磁场中分子链更易于形成反式构象,苯环振动增强,熔体更易于结晶。随着施加磁场的强度增加,聚甲醛晶体的球晶尺寸以及晶粒沿磁场方向排列的取向比率都呈上升趋势,在强磁场的环境下生成的一排排串晶结构,这一现象未见报道。
综合本文所研究的聚合物结晶形貌发现：聚合物的片晶形貌是与分子链的结构性质有关的。柔性分子链的聚合物结晶时,分子链没有空间位阻可以自由排列,形成了自由弯曲的片晶形貌；而由刚性分子链构成的聚合物,由于较大的空间位阻效应,分子链按一定的形式规则排列,结晶形成了具有一定的刚性平直结构片晶。
比较本文所研究的聚合物在磁场下凝固组织发现：聚合物凝固组织在磁场作用前后的变化程度是由分子链的结构决定的。随着分子链基团的偶极距增大,磁场的作用就越明显。分子链上没有支链的聚合物,在整个分子链的折叠结晶过程中没有空间位阻的影响而依靠主链上的分子偶极距来感应外界环境的变化,外加磁场对主链产生一个拉伸的作用力,增大了片晶的厚度,使球晶的尺寸增加；而那些带有侧链的聚合物在结晶过程中受到磁场作用而产生构象变化,新的构象会产生空间位阻效应,限制了片晶的自由生长方向,片晶在某些特定的方向上易于生长,在其它生长方向上受到阻碍,凝固得到特定形貌的晶粒。
HDPE, iPP, sPS, POM, and PET were selected in this study to investigate the effects of magnetic fields on morphology, crystal orientation of polymers solidified in the magnetic fields with different types and intensities (including0.1T,0.2T,0.3T DC and AC fields,10T pulse field and12T high field). The microstructures of the polymers solidified with or without the magnetic fields were observed and analyzed by the optics microscope (OP), scanning electronic microscope (SEM), differential scanning calorimeter (DSC), X-ray diffraction (XRD) and infrared spectrometer (FT-IR) respectively. The results are as followings:
The obviouse change takes place in morphology of HDPE solidified in the magnetic fields, which shows increase in crystal degree and orientation with increase in magntic field intensity. The lamel thickness increases greatly, lamel space increases a little, and globe crystal size increases when HDPE solidified under DC magnetic field. However, the lamel thickness and the lamel space decreased abviously when it solidified under AC magnetic field.
While iPP were solidified in AC, DC and PC magnetic field, molecule chain were induced by magnetic fields and induced dipole were produced, conformation order of molecule chain was improved and grain orientation trended to the direction of magnetic field. In DC and PC magnetic field, melting point (Tm) of iPP increased and shish-kebab was formed from the melt favourably. Alternating direction change of AC magnetic field stunts the perfect shish-kebab solidified from the iPP melt, which resulted in the decrease of crystal degree and Tm of the samples.
The crystal type of sPS solidified in the DC magnetic field was still β-crystal. The grain size decrease, lamel arranged along the direction of magnetic field, Tm and crystal degree of β-crystal increased when solidified in DC magnetic field,.which was result from transformation in the molecule chain stack modes of sPS solidified under DC magnetic field. When solidified in DC magnetic field, the circinate sphere shape grains emerged and lamel size decreases because molecule chain arranged along direction of magnetic field, right-angled bend was holden back, growth direction of grain was restricted.
In DC and high magnetic field, lamels thickness and space of POM were enhanced, grain orientation trended to the direction of magnetic field. Sphere size, Tm and grain tropism increased with increase in intensity of the magnetic field. While intensity of magnetic field reached12T, similar circinate sphere shape was observed in the cross section of POM samples. During the course of solidification in magneic field, the molecule chain of POM could conquer steric hindrance, symmetric stretching vibration of C-O-C bond was enhanced, and bending vibration of C-O-C bond was weakened, and resistance of lamels incrassation was reduced.
In the course of solidification in DC magneic field, molecule chain of PET favored reverse conformation, benzene vibration was enhanced, and PET melt crystallized more availably. With the increase in intensities of magnetic field, sphere size and grain orientation along with the direction of magnetic field increased. In the12T high magnetic, a row of shish-kebab emerged. This result was not be reported in publications.
According to above results it can be found that lamel shape was related with the structure of molecule chain. During solidification, flexible chain can arrange freely without any steric hindrance and crystal lamel can be bend freely. Moreover, rigid chain needs to arrange on principle due to steric hindrance, even rigid lamels formed in the polymers, which were made up of rigid chain.
Comparing the microstructure of polymer solidified in the magnetic field in this paper, it was found that the structure of molecule chain decided the crystal shape of polymer solidified in the magnetic fields. The more the dipole of molecule chain, the stronger the effects of the magnetic fields on the microstrucutres. The molecule chain of polymer without side group was not affected by steric hindrance and the molecule dipole was influenced by magnetic field. The magnetic field produced a extended force to main chain so that the lamel thickness and sphere dimension were increased. The molecule chain of polymer with side group was influenced by magnetic field and conformation was transformed. The new conformation brought steric hindrance and hindered growth of lamel with freedom. Thus, growth direction of lamel follow certain orientation, other growth direction was restricted, and special shape of grains formed.
高密度聚乙烯(HDPE)在磁场下凝固的组织形貌发生了明显的变化,并且结晶度和结晶取向随着施加磁场强度的增加而增加。在直流磁场下凝固的聚乙烯的片晶厚度明显增大,片晶间距有小幅增加,形成的球晶尺寸增加；施加交流磁场后,片晶厚度变小,片晶间距也明显减小。
等规聚丙烯(iPP)在直流、交流和脉冲三种磁场下凝固时分子链易受外磁场的作用而产生诱导偶极,凝固时分子链构象规整性提高,晶粒沿外加磁场方向择优取向。直流磁场和脉冲磁场下凝固的聚丙烯熔点提高,凝固组织有生成串晶的趋势；交流磁场方向的周期变化,阻碍了聚丙烯形成完整的串晶结构,导致了聚丙烯的结晶度下降,熔点降低。
间规聚苯乙烯(sPS)在直流磁场下凝固的晶型仍为β晶型,晶粒尺寸变小,片晶沿顺磁场方向排列,熔点提高以及晶体中β晶型结晶度增加。这一结果的产生是由于sPS分子链在磁场环境下改变了堆砌方式,分子链沿顺磁场方向排列,阻碍了分子链折叠弯曲,晶粒的生长方向受到限制,片晶尺寸减小,形成了漩涡状的球晶形态。
聚甲醛(POM)的分子链在磁场下克服空间位阻效应而更有利于C—O—-C对称伸缩振动,减弱了C—O—C弯曲振动,从而减小晶片间增厚阻力,使片晶的厚度和间距增大,晶粒也沿磁场方向取向排列。随着施加磁场的强度增加,聚甲醛晶体的球晶尺寸、熔点以及晶粒沿磁场方向排列的取向比率都呈上升趋势,当磁场强度达到12T时,在聚甲醛晶体的横截面上发现明显的片晶类似漩涡排列的现象。
聚对苯二甲酸乙二醇酯(PET)在直流磁场中分子链更易于形成反式构象,苯环振动增强,熔体更易于结晶。随着施加磁场的强度增加,聚甲醛晶体的球晶尺寸以及晶粒沿磁场方向排列的取向比率都呈上升趋势,在强磁场的环境下生成的一排排串晶结构,这一现象未见报道。
综合本文所研究的聚合物结晶形貌发现：聚合物的片晶形貌是与分子链的结构性质有关的。柔性分子链的聚合物结晶时,分子链没有空间位阻可以自由排列,形成了自由弯曲的片晶形貌；而由刚性分子链构成的聚合物,由于较大的空间位阻效应,分子链按一定的形式规则排列,结晶形成了具有一定的刚性平直结构片晶。
比较本文所研究的聚合物在磁场下凝固组织发现：聚合物凝固组织在磁场作用前后的变化程度是由分子链的结构决定的。随着分子链基团的偶极距增大,磁场的作用就越明显。分子链上没有支链的聚合物,在整个分子链的折叠结晶过程中没有空间位阻的影响而依靠主链上的分子偶极距来感应外界环境的变化,外加磁场对主链产生一个拉伸的作用力,增大了片晶的厚度,使球晶的尺寸增加；而那些带有侧链的聚合物在结晶过程中受到磁场作用而产生构象变化,新的构象会产生空间位阻效应,限制了片晶的自由生长方向,片晶在某些特定的方向上易于生长,在其它生长方向上受到阻碍,凝固得到特定形貌的晶粒。
HDPE, iPP, sPS, POM, and PET were selected in this study to investigate the effects of magnetic fields on morphology, crystal orientation of polymers solidified in the magnetic fields with different types and intensities (including0.1T,0.2T,0.3T DC and AC fields,10T pulse field and12T high field). The microstructures of the polymers solidified with or without the magnetic fields were observed and analyzed by the optics microscope (OP), scanning electronic microscope (SEM), differential scanning calorimeter (DSC), X-ray diffraction (XRD) and infrared spectrometer (FT-IR) respectively. The results are as followings:
The obviouse change takes place in morphology of HDPE solidified in the magnetic fields, which shows increase in crystal degree and orientation with increase in magntic field intensity. The lamel thickness increases greatly, lamel space increases a little, and globe crystal size increases when HDPE solidified under DC magnetic field. However, the lamel thickness and the lamel space decreased abviously when it solidified under AC magnetic field.
While iPP were solidified in AC, DC and PC magnetic field, molecule chain were induced by magnetic fields and induced dipole were produced, conformation order of molecule chain was improved and grain orientation trended to the direction of magnetic field. In DC and PC magnetic field, melting point (Tm) of iPP increased and shish-kebab was formed from the melt favourably. Alternating direction change of AC magnetic field stunts the perfect shish-kebab solidified from the iPP melt, which resulted in the decrease of crystal degree and Tm of the samples.
The crystal type of sPS solidified in the DC magnetic field was still β-crystal. The grain size decrease, lamel arranged along the direction of magnetic field, Tm and crystal degree of β-crystal increased when solidified in DC magnetic field,.which was result from transformation in the molecule chain stack modes of sPS solidified under DC magnetic field. When solidified in DC magnetic field, the circinate sphere shape grains emerged and lamel size decreases because molecule chain arranged along direction of magnetic field, right-angled bend was holden back, growth direction of grain was restricted.
In DC and high magnetic field, lamels thickness and space of POM were enhanced, grain orientation trended to the direction of magnetic field. Sphere size, Tm and grain tropism increased with increase in intensity of the magnetic field. While intensity of magnetic field reached12T, similar circinate sphere shape was observed in the cross section of POM samples. During the course of solidification in magneic field, the molecule chain of POM could conquer steric hindrance, symmetric stretching vibration of C-O-C bond was enhanced, and bending vibration of C-O-C bond was weakened, and resistance of lamels incrassation was reduced.
In the course of solidification in DC magneic field, molecule chain of PET favored reverse conformation, benzene vibration was enhanced, and PET melt crystallized more availably. With the increase in intensities of magnetic field, sphere size and grain orientation along with the direction of magnetic field increased. In the12T high magnetic, a row of shish-kebab emerged. This result was not be reported in publications.
According to above results it can be found that lamel shape was related with the structure of molecule chain. During solidification, flexible chain can arrange freely without any steric hindrance and crystal lamel can be bend freely. Moreover, rigid chain needs to arrange on principle due to steric hindrance, even rigid lamels formed in the polymers, which were made up of rigid chain.
Comparing the microstructure of polymer solidified in the magnetic field in this paper, it was found that the structure of molecule chain decided the crystal shape of polymer solidified in the magnetic fields. The more the dipole of molecule chain, the stronger the effects of the magnetic fields on the microstrucutres. The molecule chain of polymer without side group was not affected by steric hindrance and the molecule dipole was influenced by magnetic field. The magnetic field produced a extended force to main chain so that the lamel thickness and sphere dimension were increased. The molecule chain of polymer with side group was influenced by magnetic field and conformation was transformed. The new conformation brought steric hindrance and hindered growth of lamel with freedom. Thus, growth direction of lamel follow certain orientation, other growth direction was restricted, and special shape of grains formed.
引文
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