X-射线衍射法测定尼龙1010结晶度

根据X-射线散射强度理论,使用图解多重峰方法对尼龙1010三个结晶峰及非晶峰的衍射强度进行校正,首次导出了尼龙1010结晶度计算公式,所得结果与密度及量热测定结果具有很好可比性。     

THE DEGREE OF CRYSTALLINITY OF NYLON-1010 BY WAXD

Based on the X-ray scattering intensity theory and using the atomic scattering factorapproximate expression,the correction factors for three main crystalline peaks and an amorphouspeak of Nylon-1010 were calculated and the formula of degree of crystallinity of Nylon-1010 wasderived by graphic multipeak resolution method. The results calculated are compatible with the density measurement and calorimetry.     

Microstructure Analysis of Nylon 66 by WAXD and SAXS

IntroductionNylon 66,one of the most successfulcommercial polyamides,has been widely usednowadays as an engineering plastic in many fields.The development of the structure of nylons is acontinuing area of their technological and scientificstudy.The structure of nylon 66 during thephotoinduced decomposition process has beenstudied by resonance Raman[1] ,and the effect oftranscrystalline layers have been investigated[2— 4] .Moreover,the crystallization and meltingbehavior[5] have been learned …     

THE DEGREE OF CRYSTALLINITY OF MULTICOMPONENT POLYMERS BY WAXD

Based on the X- ray scattering intensity theory, the correction factors of the degree ofcrystallinity formulae of the multicomponent polymers have been clearly defined. The formulae ofthe degree of crystallinity of the multicomponent polymers were derived in terms of WAXDtheory and improved graphic multipeak resolution methods. The results calculated aresatisfactory in comparison with the density measurement.     

Thermal,physical and mechanical properties of hydrogenated dimer acid-based Nylon 636/Nylon 66 copolymers

Hydrogenated dimer acid-based Nylon 636/NyIon 66 copolymers were synthesized by in situ polymerization.The effects of Nylon 66 contents on the copolymers were characterized by intrinsic viscosity measurements,attenuated total reflection-Fourier transform infrared spectroscopy,X-ray diffraction,differential scanning calorimetry,tliermogravimetric analysis and mechanical tests.The results showed that incorporation of Nylon 66 into hydrogenated dimer acid-based Nylon had no significant effect on the glass transition or melting temperatures.However,the crystallization temperature,crystallinity degree and the maximum rate of decomposition temperature from derivative thermogravimetry measurements vary.Mechanical testing data revealed that with increasing Nylon 66 concentrations,the tensile strength of copolymers increased,while the elongation at break point and notched izod impact strength decreased.The physical and mechanical properties of HN-40,HN-50 and HN-60 are similar to those of the current PA11,PA1212,and PA1111 Nylon products.     

MULTIPLE MELTING AND CRYSTALLIZATION BEHAVIOR OF NYLON 1212

The wide-angle X-ray diffraction (WAXD) patterns of isothermally crystallized Nylon 1212 show that γ-form crystals form below 90℃ and the α-form crystals can exist above 140℃. In the temperature range of 90-140℃, the α-form and γ-form crystals coexist. Variable-temperature WAXD exhibits that the nylon 1212 γ-form does not show crystal transition on heating, while α-form isothermally crystallized at 160℃ exhibits Brill transition at a little higher than 180℃ on heating. The multiple melting behaviors of Nylon 1212 isothermally crystallized from melt come from a complex mechanism of different crystal structures, dual lamellar population and melting-recrystallization. In polarized optical microscope (POM) observations, Nylon 1212 isothermally crystallized at 175℃ shows the ringed banded spherulites. However, at temperatures below 160℃ the ringed banded image disappears, and cross-extinct spherulites are formed.     

聚醚醚酮酮结晶度研究

聚醚醚酮酮结晶度研究刘天西，王尚尔，张宏放，莫志深（中国科学院长春应用化学研究所高分子物理联合开放研究实验室长春１３００２２）那辉，王军佐，吴忠文（吉林大学化学系长春）关键词聚醚醚酮酮，广角Ｘ射线衍射，结晶度新型特种工程塑料聚醚醚酮酮（ＰＥＥＫＫ）具...     

Crystal Transformation of Nylon 11 Using in situ WAXD

Nylon I I is a high-performance semicrystalline polymer which was used widely in manyfields. In recent years, the curious ferroelectric and piezoelectric propel'ties of nylon I Iwere foundl'2. It is well known that piezoelectricity is related to the crystal form ofNylon I 1.The sample was mounteds in a capillary (diameter was Zmm) within a small ovenwith mica windows. The scattered intensity was recorded from Q = 0.2 to 6.5 A-] (Q =ursine/~) using steps of AQ=o.o5A-'. The values of the p…     

广角X-射线衍射对PET结晶度的研究

应用广角X-射线衍射(WAXD)来测定高聚物的结晶度可以分为相对法(CCI、ICI)与绝对法(HWM、CPRM、Ruland)两大类,但长期以来在文献上这些方法得出的结果往往差别很大,而且WAXD与其它的方法,如DSC、ρ、NMR、IR等往往也不相一致。本文就此两问题进行了系统的研究,不仅对WAXD与DSC、ρ测定结晶度的可靠性进行了讨论,更对WAXD的各种方法中,2θ应选的范围、是否应作校正、非晶散射如何扣除、相对法自身之间的关系、各种绝对法之间的关系、相对法与绝对法的关系等进行了仔细的研究。结论是:WAXD在可靠性与重复性方面优于DSC与ρ法,而且是其它方法的根据;绝对法优于相对法,各种绝对法有利有弊,而非晶散射的合理分离是最为关键的问题。     

尼龙1212/尼龙6共混体系的非等温结晶行为

用DSC研究了尼龙 12 12 ,尼龙 6及其共混体系的非等温结晶行为 .结果表明 ,加工历史对尼龙的结晶和熔融行为影响很大 .经双螺杆挤出机挤出的尼龙 12 12和尼龙 6 ,由于应力诱导分子链取向 ,其结晶温度都有不同程度的提高 ,且表现出多重熔融现象 .在共混体系中 ,尼龙 12 12分子在共混物的界面上异相成核结晶 ,提高了其结晶温度 ,但酸酐化SEBS的加入抑制了分子链的运动又使其结晶温度降低 .共混体系降低了尼龙12 12的熔融温度 ,并使得其高熔点的熔融峰逐渐消失 ;而尼龙 6的熔融行为基本上没有变化 .     

热处理对聚醚醚酮晶体结构参数及结晶度的影响

采用广角Ｘ射线衍射（ＷＡＸＤ）方法研究了不同热处理温度下聚醚醚酮（ＰＥＥＫ）的晶胞参数、微晶尺寸及结晶度的变化。根据Ｘ射线散射强度理论，运用图解多重峰方法导出了以ＷＡＸＤ方法计算ＰＥＥＫ结晶度的公式；用此公式对经不同热处理的ＰＥＥＫ样品进行计算，结果与由密度法及量热法测定的结果具有较好的可比性。     

热历史对尼龙1212熔融行为的影响

利用DSC方法研究了不同热历史条件对尼龙1212熔融行为的影响.不同的热历史条件下,在DSC曲线上,观察到尼龙1212产生2个或3个熔融峰,依据聚合物结晶理论,对各峰的来源进行了分析.在160℃下不同温度退火120 min的尼龙1212样品DSC曲线上,低温结晶熔融峰主要由低温结晶形成的一些微晶体或者片晶熔融产生,其晶体完善程度较差,熔融峰值较低,峰面积较小;主熔融峰是由样品在淬火过程中形成的晶体和升温过程中低温结晶形成的晶体的熔融重结晶形成较为完善的晶体熔融所产生,熔融峰值较高,峰面积较大.在不同的升温速率条件下,熔融峰温度有所移动,表明不同升温速率条件下产生的熔融峰的结晶晶型是相同的.在不同结晶时间下结晶,延长结晶时间对较高完善程度晶体的生长有利.在不同温度下依次退火处理的样品,熔融产生两个附加峰,这两个附加峰的峰温都比它们相应的退火温度高,而峰高和峰面积随退火温度降低而减小.根据等温结晶结果,由Hoffman方法确定了尼龙1212的平衡熔融温度为202.8℃.     

马来酸酐化SEBS对尼龙1212/尼龙6共混体系形态和性能的影响

研究了马来酸酐接枝氢化苯乙烯 丁二烯 苯乙烯嵌段共聚物 (MA SEBS)对尼龙 12 12 尼龙 6共混体系形态和性能影响 .结果表明 ,在以尼龙 6为连续相而尼龙 12 12为分散相时 ,MA SEBS加入大大提高了两相间的相容性 ,导致尼龙 12 12分散相的细化 .透射电镜观察表明 ,共混体系形成特殊的“核 壳”结构 ,处在分散相和连续相间的“壳”MA SEBS起到了很好的相容剂的作用 .在尼龙 12 12 尼龙 6为 30 70时 ,仅用 15 %的MA SEBS ,共混体系即获得超高韧性 .     

Thermogravimetric and wide angle X-ray diffraction analysis of thermoplastic elastomers from nylon copolymer and EPDM rubber

Nylon copolymer (PA6, 66) and ethylene propylene diene (EPDM) blends with and without compatibilizer were prepared by melt mixing using Brabender Plasticorder. The thermal stability of nylon copolymer (PA6, 66)/ethylene propylene diene rubber (EPDM) blends was studied using thermogravimetric analysis (TGA). The morphology of the blends was investigated using scanning electron microscopy (SEM). In this work, the effects of blend ratio and compatibilisation on thermal stability and crystallinity were investigated. The incorporation of EPDM rubber was found to improve the thermal stability of nylon copolymer. The kinetic parameters of the degradation process were also studied. A good correlation was observed between the thermal properties and phase morphology of the blends. By applying Coats and Redfern method, the activation energies of various blends were derived from the Thermogravimetric curves. The compatibilization of the blends using EPM-g-MA has increased the degradation temperature and decreased the weight loss. EPM-g-MA is an effective compatibilizer as it increases the decomposition temperature and thermal stability of the blends. Crystallinity of various systems has been studied using wide angle X-ray scattering (WAXS). The addition of EPDM decreases the crystallinity of the blend systems.     

Structural investigation of polyaniline/Nylon 6 blends by small-angle neutron scattering and small- and wide-angle X-ray scattering

The structure of blends of Nylon 6 with deuterated polyaniline emeraldine base (D-PANI-EB) and fully doped D-PANI salts (D-PANI-ES) formed from camphorsulfonic acid (CSA), methanesulfonic acid (MSA), or dodecyl benzenesulfonic acid (DBSA) were investigated by small-angle neutron (SANS) and X-ray scattering. The blends were formed from hexafluoro-2-propanol solutions and had volume fractions of 0.038, 0.20, and 0.40 for D-PANI/CSA, 0.20 and 0.40 for D-PANI/MSA, 0.24 and 0.44 for D-PANI/DBSA, and 0.07, 0.14, and 0.31 for D-PANI-EB. The SANS results are compared with a number of standard models for two-phase systems. No evidence was found for significant molecular mixing. In some cases the inverse power law model is in reasonable agreement with observations, and in the case of the lowest concentration of D-PANI/CSA there is an indication of mass fractal structure. This was not found at the higher concentrations. The results establish that the blends with the smaller more polar dopants CSA and MSA behave similarly and are unlike either the D-PANI/DBSA blends or those with D-PANI-EB. There is evidence that the simple picture of two pure phases is inadequate for these materials. With the exception of the D-PANI/DBSA blend which has a relatively low scattering contrast, the results indicate that the lower limit of volume fraction for application of SANS is a few percent D-PANI-ES in Nylon 6. X-ray scattering was used to demonstrate the presence of Nylon 6 lamellae and residual peaks attributable to the pure components. © 1997 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 35: 2765–2774, 1997     

热处理对尼龙6及其与聚酰胺嵌段共聚物共混体系晶体熔融行为和结晶结构的影响

采用溶液共混-共沉淀的办法获得尼龙6及聚酰胺嵌段共聚物/尼龙6共混体系粉末,样品在260℃下熔融之后经程序降温的方法得到非淬火样品,然后分别在190℃下高温退火不同时间(0~48 h),采用示差扫描量热仪(DSC)、广角X射线衍射仪(WAXD)、偏光显微镜(POM)等表征手段研究热处理对体系晶体熔融行为和结晶结构的影响.结果表明,(1)在相同的热历史条件下,嵌段共聚物的存在影响了尼龙6的结晶行为及结晶结构;(2)退火处理对两种样品有着不同的影响,对于尼龙6体系,退火处理促进了非晶相向晶相的转变,大大提高样品的结晶完善程度和结晶度;对于共混体系,退火处理同样促进了非晶相向晶相的转变,同时形成新的α型和γ型结晶,体系的结晶完善程度明显提高,退火48 h后,结晶度比原始样品提高约84%.     

STUDY ON PET-PA66 COPOLYMER

In this work the PET-PA 66 copolymers are obtained. The characterization of chemical structure of copolymer chain by NMR method is also given. It is shown that when the 66 Nylon salt is added in the copolycondensation, the adipic acid and hexamethylenediamine reacted mainly by itself and the obtained copolymer is a random copolymer, and when the Nylon 66 oligomer is added, the obtained copolymer is a block copolymer. The result of NMR analysis is demonstrated by properties investigation.     

尼龙6/蒙脱土纳米复合材料的等温结晶动力学研究

用ＤＳＣ法研究了熔体插层制备的尼龙６／蒙脱土纳米复合材料的等温结晶行为．结果表明,加入少量的蒙脱土可明显提高尼龙６的结晶速率,降低球晶径向生长的单位面积表面自由能．从Ａｖｒａｍｉ方程和Ｈｏｆｍａｎ理论出发,得出蒙脱土纳米粒子的存在可明显改变尼龙６的结晶行为     

熔体插层制备尼龙6/蒙脱土纳米复合材料的性能表征

通过熔体插层成功地制备了尼龙６／蒙脱土纳米复合材料，测试了力学性能、耐热性能和耐溶剂性．通过ＴＥＭ、ＷＡＸＤ、ＤＳＣ等手段，研究了结构与结晶行为，并与插层聚合的尼龙６／蒙脱土纳米复合材料进行了对比．实验表明通过熔体插层可使尼龙６基体插层于蒙脱土中，所得到的复合物的性能较尼龙６有很大提高，且与插层聚合的尼龙６／蒙脱土纳米复合材料的性能相当．     

Dual-mode sorption of nonionic azo dyes by Nylon 6

Sorption isotherms of 2,4-dinitroaniline and three 4-amino-azobenzene derivatives (nonionic dyes with adequate solubility in water) on Nylon 6 (film and fiber) from water were determined at various temperatures. The observed isotherms were curved, not linear. They were very well described in terms of the dual-mode sorption model, Nernst-type partitioning, plus Langmuir sorption. The contribution of the Langmuir sorption to the total dye sorption decreased with increasing temperature. The saturation value for the Langmuir sorption increased with the crystallinity of Nylon 6 film, suggesting that the Langmuir sorption is associated with the crystalline phase.