拉伸下PET的取向诱导结晶

综述了PET在3种拉伸方式(单轴拉伸、平面拉伸和双轴拉伸)下的取向诱导结晶的最新进展。拉伸温度、应变速率和拉伸比是常用的3个宏观参数，它们对取向诱导结晶等微观参数有着最直接的影响。     

聚苯酯对聚醚醚酮结晶行为的影响

用模压法制备了聚苯酯(Ekonol)／聚醚醚酮(PEEK)复合材料，通过X射线衍射(XRD)、差示扫描量热分析(DSC)考察了PEEK的结晶行为，并测定了复合材料的熔点、结晶温度和玻璃化转变温度。结果表明：Ekonol含量的大小对PEEK的结晶行为产生了直接影响，PEEK的相对结晶度随着Ekonol含量的增加而提高；Ekonol含量小于30％时，对复合材料的熔点、结晶温度和玻璃化转变温度影响不大，但含量大于30％时，材料的结晶温度、熔融温度下降，玻璃化转变温度提高。     

聚醚醚酮纤维的拉伸定形后处理研究

通过熔融纺丝制得聚醚醚酮(PEEK)纤维,并采用差示扫描量热仪(DSC)、声速取向测量仪、热重分析仪、单纱电子强力仪分别研究了干热拉伸及热定形处理对PEEK纤维结晶和取向、热稳定性及力学性能的影响。结果表明:随着热拉伸倍数增大,PEEK纤维取向度、结晶度增加,纤维的断裂强度增加,断裂伸长减小;PEEK纤维的热拉伸温度应选在200～240℃,热定形温度应为220～260℃;PEEK纤维的重结晶主要是在热拉伸过程中完成,热定形则进一步完善纤维的结晶结构;经过后处理,PEEK纤维的断裂强度可达到6.12cN/dtex;且具有优异的热稳定性能,热分解温度高达505℃,后处理几乎不影响PEEK纤维的热稳定性。     

熔融条件对聚醚醚酮结晶熔融行为的影响

用ＤＳＣ法研究了熔融温度和熔融时间对聚醚醚酮地晶熔融行为的影响。实验表明，聚醚醚酮的结晶峰随熔融延长向高温移动，且峰形变窄，峰的强度增大，继续延长熔融时间，结晶峰降低，峰形变宽；熔融时间延长时，聚醚醚酮的玻璃化转变温度和冷结晶峰温度均提高，熔融峰强度减弱。熔融温度升高时，聚醚醚酮的结晶峰强度减弱，峰宽增强；而冷结晶温度提高。     

拉伸方式对聚醚醚酮纤维结构和性能的影响

采用进口聚醚醚酮(PEEK)树脂为原料,熔融纺丝制备了PEEK初生纤维,研究了一次拉伸和二次拉伸对PEEK纤维结构和力学性能的影响。结果表明:在150～270℃内,随着拉伸温度的提高,PEEK初生纤维的最大拉伸倍数增大,纤维的取向因子和力学性能提高;一次拉伸和二次拉伸时纤维的最大拉伸倍数相同,纤维的取向度、结晶度和力学性能基本相当,但二次拉伸纤维干热收缩率较低。二次拉伸时,总拉伸倍数相同,随着一段拉伸倍数的增大,纤维取向因子增大,力学性能提高;随着二段拉伸温度的提高,纤维结晶度增大,干热收缩率减小,取向因子基本相同,力学性能更优。     

聚醚醚酮的FDM工艺参数与结晶行为研究

采用熔融沉积成型技术(FDM)制备了聚醚醚酮(PEEK)试样,并应用试验设计(DOE)方法分析研究了打印层高、热台温度和打印速度对PEEK试样拉伸强度和结晶行为的影响。结果表明:当打印层高、热台温度和打印速度分别为0.10 mm、160℃、30 mm/s时试样的拉伸强度最大(82 MPa)。3个打印参数从试样的层间结合、缺陷与结晶行为等方面不同程度地影响着PEEK试样的拉伸强度;随着热台温度的提升,试样的结晶度提高。而在同一热台温度下,由于打印过程中存在的温度分布差异,试样存在着明显的结晶不均匀现象,从试样的中心到边缘、沿厚度增加方向,结晶度逐步降低。     

挤出型不同厚度聚醚醚酮膜的机械性能和取向性研究

对挤出型不同厚度的PEEK样品进行机械性能和取向性研究,并通过XRD和DSC进行了测试与表征。机械性能测试结果表明,PEEK最佳的拉伸速率为20mm/min;XRD分析结果表明不同厚度的试样,其晶体结构不同,说明不同度厚PEEK样品在挤出过程中受力而分子链发生取向,导致晶体变形或晶体缺陷;DSC测试结果表明,0.50mm样品取向性最大,因此初始熔融温度(onset)、最大熔融温度(peak)、结晶度等是最小的;而1.00mm厚度的样品由于取向性最小,因此初始熔融温度(onset)、最大熔融温度(peak)、结晶度等是最大的。     

碳纤维增强聚醚醚酮的非等温结晶行为与力学性能

利用聚酰亚胺(PI)作为碳纤维(CF)界面改性剂,制备了界面改性碳纤维增强聚醚醚酮(MCF/PEEK)复合材料。采用差示扫描量热仪(DSC)讨论了CF及其界面改性对PEEK非等温结晶行为的影响机制与作用规律,并基于莫志深法研究了MCF/PEEK的非等温结晶动力学;借助DSC和小角X射线散射仪(SAXS)表征不同降温速率下PEEK基体的结晶结构,采用万能试验机评价了MCF/PEEK的力学性能。结果发现:CF对PEEK的结晶有较为明显的异相成核促进作用,经过PI界面改性之后成核作用有所下降,但结晶行为仍较纯PEEK更容易发生,整体结晶速率更快;随冷却速率的增大,基体结晶度、片晶厚度与长周期均减小,MCF/PEEK的拉伸强度与模量也显著减小,层间断裂韧性提高。     

PEEK/PEI共混物的相容性和结晶行为研究

在380℃下熔融挤出制得聚醚醚酮（PEEK）与聚醚酰亚胺（PEI）共混物。采用差示扫描量热仪（DSC）和广角X射线衍射仪（WAXD）研究了共混物的相容性和结晶行为。结果表明,PEEK／PEI共混物完全相容．所有共混物均呈现一个玻璃化转变温度（Tg）,且与组分的关系符合Porch方程;随PEI含量的增加,共混体系的熔点、结晶度、整体结晶速率和结晶能力均降低：而PEEK的结晶度呈现先增加后减小的趋势,当PEI质量分数为50％时,达到最大。     

热致液晶聚酰胺对聚酰胺66结晶行为的影响

利用差示扫描量热仪（DSC）、广角X射线衍射（WAXD）和偏光显微镜（POM）等仪器研究了热致液晶聚酰胺（TLCP）对聚酰胺66（R％6）结晶行为的影响。结果表明：随TLCP的添加量从0增加到30％，共混物的结晶温度和结晶度分别从PA66的235．83℃和39．8％逐步下降为224．7℃和30．8％，PA66的结晶明显受到抑制；共混物中PA66衍射峰的强度随TLCP含量的增加而下降，（100）、（010）晶面间距分别从0．43667nm和0．37139nm增加到0．4414nm和0．37793nm；共混物球晶尺寸明显大于PA66，并且随TLCP含量增加PA66的球晶变得越来越不完善。     

Uniaxial Orientation and Crystallization Behavior of Amorphous Poly(ethylene terephthalate) Fibers

The effects of drawing conditions on the orientation and crystallinity of poly(ethylene terephthalate) (PET) fibers were investigated by using optical birefringence, sonic velocity, and wide-angle X-ray diffraction measurements, respectively. The preferred condition for preparation of uniaxially oriented amorphous PET fibers was suggested. The crystallization behavior of oriented PET fibers under relaxed and fixed length conditions was investigated by using differential scanning calorimetry (DSC). The multi-overlapping peaks were observed in the non-isothermal DSC curves of oriented PET fibers under relaxed condition. The kinetics of non-isothermal crystallization of oriented PET fibers under relaxed condition was analyzed by using an equation which takes the multi-crystallization processes into account. The kinetic parameters of every process were obtained and the crystallization mechanism was discussed. The crystallization behavior under fixed length condition differs from that under relaxed condition.     

CNFs的掺杂与取向对CNFs/LDPE纳米复合材料结晶性能的影响

通过微波法化学镀镍对纳米碳纤维(CNFs)进行表面改性,采用熔融共混法制备CNFs/低密度聚乙烯(LDPE)纳米复合材料,在模压硫化过程中施加磁场,实现表面镀镍CNFs在LDPE基体中的取向,研究了CNFs的掺杂对CNFs/LDPE纳米复合材料结晶性能的影响,采用场发射扫描电子显微镜(FE-SEM)观察刻蚀后样品中CNFs分散、取向情况和球晶形貌,采用X射线衍射仪(XRD)分析纳米复合材料结晶性能。研究发现,在LDPE基体中CNFs的掺杂对纳米复合材料结晶性能有着较大的影响;掺杂CNFs使LDPE的结晶度下降,且掺杂样品需较长时间的刻蚀才能看到清晰的球晶结构,LDPE的球晶结构较明显,其直径约6μm,CNTs的取向使纳米复合材料的结晶度增大。     

Crystallization kinetics of a PEEK/LCP blend

The crystallization kinetics of a polyetheretherketone (PEEK)/liquid crystalline polymer (LCP) blend was studied by using differential scanning calorimetry. Nonisothermal runnings were performed on heating and on cooling at different rates. Isothermal crystallization experiments at 315, 312, 310, and 307°C, from the melt state (380°C) were performed in order to calculate the Avrami parameters n and k and the fold surface free energy, σ_e. Polarized light optical micrographs were also obtained to confirm the Avrami predictions. It was observed that the LCP retarded the PEEK crystallization process and that the PEEK melting temperature decreased with the amount of LCP, but the LCP melting temperature increased with the amount of PEEK. Probably the PEEK improves the perfection of the LCP crystalline domains. A spherulitic morphology in pure PEEK and its blends was predicted by the Avrami analysis; however this morphology was only observed for pure PEEK and for the 80/20 composition. The other compositions presented a droplet and fibrillar-like morphology. The overall crystallization rate was observed to decrease with the crystallization temperature for all compositions. Finally, σ_e was found to decrease with the increase of LCP in the blends, having unrealistic negative values. Thus, calculations were made assuming σ_e constant at all compositions. It was observed that δ, the interfacial lateral free energy, decreased but still remained positive. It was concluded that in these blends neither σ_e nor σ could be considered constant. © 1995 John Wiley & Sons, Inc.     

非晶态合金FeNiVSiB的晶化过程研究

本文利用差示扫描量热法(DSC)对非晶态合金FeNiVSiB的晶化过程进行了研究。结果表明随热处理温度的增高晶化过程加快;随热处理时间的延长,晶化程度增大。     

溶液中的结晶和沉降行为的实验研究

在亚氨基二乙腈(IDAN)溶液中,对不同的停留时间晶体的沉降和分级行为、晶体的平均粒径以及粒度分布、晶体的形貌特征进行了分析.实验结果表明,随着停留时间的延长,在残余过饱和度已趋于稳定不变的情况下,沉积底部的晶体的质量逐渐增加,平均粒径不断增大,晶体形貌不断改善、结构更加完整.这种结晶成长和沉降行为对结晶过程和设备的设计和操作都有重要意义.     

Crystallization of Amorphous Components in Spray-Dried Powders

Spray-dried powders are typically produced as amorphous particles. Long storage of the particles tends to crystallize the powders, a reaction affected by moisture, time, and temperature. This work has examined partial crystallization from amorphous spray-dried powders by moisture sorption. Powders of citrus fiber with hibiscus extract, maltodextrin, coffee, tea, skim milk, and sucrose were produced with a laboratory-scale spray dryer. The powders were exposed to ambient temperature and various relative humidities, with weight measurements recorded over time. It has been found that, in different materials, the amorphous to crystalline state change is observed at varying rates depending on the relative humidities and molecular weights. This observation may be associated with all amorphous spray-dried materials.     

Crystallization of Amorphous Components in Spray-Dried Powders

Spray-dried powders are typically produced as amorphous particles. Long storage of the particles tends to crystallize the powders, a reaction affected by moisture, time, and temperature. This work has examined partial crystallization from amorphous spray-dried powders by moisture sorption. Powders of citrus fiber with hibiscus extract, maltodextrin, coffee, tea, skim milk, and sucrose were produced with a laboratory-scale spray dryer. The powders were exposed to ambient temperature and various relative humidities, with weight measurements recorded over time. It has been found that, in different materials, the amorphous to crystalline state change is observed at varying rates depending on the relative humidities and molecular weights. This observation may be associated with all amorphous spray-dried materials.     

磷对化学沉积Ni－P非晶态镀层晶化过程的影响

通过示差扫描热分析（ＤＳＣ）、Ｘ射线衍射（ＸＲＤ）和硬度测试研究了不同磷含量的Ｍ－Ｐ合金镀层的晶化过程。结果表明，随着镀层晶化的进行，硬度提高。当热处理温度达４２０℃时，镀层全部转化为晶态结构，主要为弥散分布的Ｎｉ３Ｐ产相，硬度大到峰值，高磷镀层的硬度高于低磷镀层。但在镀态，则低磷镀层的硬度高于高磷镀层。