用原位聚合法制备的PA6/GO纳米复合材料的结构和性能

以己内酰胺(CL)和6-氨基己酸(ACA)为聚合反应单体,用Hummers法制备氧化石墨烯(GO),再以GO为纳米填料用原位开环聚合法制备了GO改性PA6纳米复合材料(PA6/GO),并对PA6/GO纳米复合材料的结构及性能进行了研究。结果表明,PA6的黏均分子量达到104数量级,但加入过多的GO使PA6的分子量降低。形貌分析表明,GO均匀地分散在PA6基体中,并诱导了PA6基体的晶型由α晶型转变成γ晶型。同时,GO作为异相成核剂促进了PA6/GO复合材料中PA6基体的结晶,提高了PA6/GO复合材料的结晶度。拉伸测试结果表明,随着GO的加入PA6/GO纳米复合材料的拉伸强度先提高后降低,GO加入量为0.4份时拉伸强度达到最大值61.72 MPa,比纯PA6(48.52 MPa)提高了27.21%。导热性能分析表明含1.0份GO的PA6/GO纳米复合材料其50℃和100℃的热导率分别为0.317 W/(m·K)和0.280 W/(m·K),较纯PA6分别提高了33.19%和33.23%。     

纳米有机蒙脱土对尼龙6/N-苯基马来酰亚胺-马来酸酐的结构及耐热性能影响EI北大核心CSCD

采用自制新型耐热改性剂N-苯基马来酰亚胺-马来酸酐二元共聚物(NMA)与纳米有机蒙脱土(OMMT)对尼龙6(PA6)进行熔融共混制备了PA6/NMA/OMMT纳米复合材料,并通过透射电镜、X射线衍射、差示扫描量热、旋转流变仪、热变形及力学性能测试等分析研究了纳米OMMT用量对PA6/NMA/OMMT纳米复合材料的结构及耐热性能的影响。结果表明:纳米OMMT剥离分散在PA6基体中,诱导了PA6由α晶型向γ晶型转变;且OMMT对PA6/NMA/OMMT纳米复合材料的异相成核作用提高了体系结晶度。此外,对比于PA6/NMA复合材料,PA6/NMA/OMMT纳米复合材料的动态复合黏度、储存模量、损耗模量均增大;且PA6/NMA/OMMT纳米复合材料热变形温度及力学性能随着OMMT添加量的增加呈增大趋势。     

纳米有机蒙脱土对尼龙6/N-苯基马来酰亚胺-马来酸酐的结构及耐热性能影响

采用自制新型耐热改性剂N-苯基马来酰亚胺-马来酸酐二元共聚物(NMA)与纳米有机蒙脱土(OMMT)对尼龙6(PA6)进行熔融共混制备了PA6/NMA/OMMT纳米复合材料,并通过透射电镜、X射线衍射、差示扫描量热、旋转流变仪、热变形及力学性能测试等分析研究了纳米OMMT用量对PA6/NMA/OMMT纳米复合材料的结构及耐热性能的影响。结果表明:纳米OMMT剥离分散在PA6基体中,诱导了PA6由α晶型向γ晶型转变;且OMMT对PA6/NMA/OMMT纳米复合材料的异相成核作用提高了体系结晶度。此外,对比于PA6/NMA复合材料,PA6/NMA/OMMT纳米复合材料的动态复合黏度、储存模量、损耗模量均增大;且PA6/NMA/OMMT纳米复合材料热变形温度及力学性能随着OMMT添加量的增加呈增大趋势。     

氧化石墨烯/苯甲酸钠复合成核剂协同改性PA6纳米复合材料的性能

先用水热法合成氧化石墨烯(GO)/苯甲酸钠(Sb)复合成核剂(GO-Sb),然后用熔融共混法制备尼龙6(PA6)/GO-Sb纳米复合材料,研究了分别添加GO和Sb、同时添加GO-Sb对PA6纳米复合材料的形态、力学和热性能的影响。结果表明：GO与Sb之间存在静电相互作用和π-π共轭,Sb的加入能促进PA6中γ晶的形成。GOSb作为异相成核剂均匀分散在PA6中,使PA6纳米复合材料的结晶温度、结晶度和热变形温度提高。PA6-GOSb(100/0.05/0.25)纳米复合材料的拉伸强度和冲击强度分别比纯PA6提高了69.9%和157.1%。PA6-GO-Sb(100/0.05/0.25)纳米复合材料的拉伸强度、冲击强度和弹性模量分别比PA6-GO-Sb(100/0.3/0)纳米复合材料提高了13.6%、186.4%和52.6%。与纯PA6(k=0.238 W/m·k)相比,PA6-GO-Sb(100/0.3/0)纳米复合材料(k=0.536 W/m·k)的热导率提高了125.2%,PA6-GO-Sb(100/0.05/0.25)纳米复合材料(k=0.854 W/m·k)的热导率提高了258...     

乙烯-乙烯醇共聚物/尼龙6复合材料的加工流变性能

采用熔融共混法制备了乙烯-乙烯醇共聚物/尼龙6(EVOH/PA6)复合材料,用高级毛细管流变仪和旋转流变仪研究了复合材料的加工流变特性.通过幂律模型对EVOH/PA6复合材料的黏度与剪切速率(?γ)的关系进行了拟合,并用Arrhenius方程描述了复合材料黏度与温度的关系.结果表明,EVOH/PA6复合材料为假塑性流体,复合材料的表观黏度(ηa)和非牛顿常数(n)随着EVOH添加量的增加而增大.在角频率(ω)扫描范围内,EVOH的加入提高了EVOH/PA6复合材料的储能模量(G')、损耗模量(G″)和复数黏度|η*|.用Han曲线、Cole-Cole曲线和扫描电子显微镜(SEM)等方法研究发现,EVOH和PA6之间具有较好的相容性.另外,EVOH/PA6复合材料在EVOH的添加量达到15％(质量分数)时形成了微观相分离结构.     

聚对苯二甲酸乙二醇酯-聚酰胺嵌段共聚物/聚酰胺6共混物的流变性能

通过熔融共混挤出的方法,制备了不同共聚比例的聚对苯二甲酸乙二醇酯-聚酰胺嵌段共聚物(PET-PA)与聚酰胺6(PA6)的共混物,采用毛细管流变仪对PET-PA/PA6共混物的流变性能进行了研究。结果表明,PET-PA/PA6共混物熔体为剪切变稀的非牛顿流体。随温度升高,PET-PA/PA6共混物熔体的表观黏度下降,非牛顿指数增大,表观黏度对剪切速率的敏感性减小,因此升高温度能改善共混物熔体的流动性能。随PET-PA中PA共聚比例的增加,PET-PA/PA6共混物的黏度减小,非牛顿指数增大,这为开发酸性染料可染聚酯纤维提供了参考。     

氧化石墨烯/尼龙6复合材料的等温结晶行为

采用液相共混法制备氧化石墨烯(GO)/尼龙6(PA6)复合材料,利用差示扫描量热(DSC)和偏光显微镜(POM)表征该体系的等温结晶行为。结果表明,Avrami方程可较好地描述PA6和GO/PA6复合材料的等温结晶行为,氧化石墨烯对尼龙6起到成核剂作用,使其结晶速率增大,结晶活化能减少。等温结晶温度升高,PA6和GO/PA6的绝对结晶度和结晶速率减少。偏光显微镜观察证实,添加氧化石墨烯后的尼龙球晶细化。     

制备工艺对纳米有机蒙脱土／聚酰胺6-聚丙烯复合材料分散相形态及力学性能的影响

通过熔融挤出法制备了纳米有机蒙脱土OMMT／聚酰胺6（PA6）母粒M1和OMMT／聚丙烯（PP）母粒M2,将这两种母粒分别与PA6-PP熔融共混,制备了不同OMMT含量的纳米OMMT／PA6-PP复合材料,同时采用直接共混法制备了相同配比的该纳米复合材料。利用TEM和SEM表征了OMMT在复合材料中的分散、分布和复合材...     

尼龙6/埃洛石纳米管纳米复合材料的制备与性能

通过熔融共混制备了尼龙-6(PA6)/埃洛石纳米管(HNTs)纳米复合材料.研究了HNTs含量对PA6/HNTs纳米复合材料微观形态、力学性能、结晶行为的影响.结果表明,在熔融共混条件下,HNTs不经过任何表面处理即可以纳米尺度均匀地分散于PA6基体中.随着HNTs含量的增加,纳米复合材料的弯曲强度和弯曲模量显著提高.DSC结果显示HNTs的存在起到了成核剂的作用,提高了PA6的结晶温度.HNTs份数少时能提高PA6/HNTs纳米复合材料的结晶度,份数多时会使其结晶度下降和生成不稳定的晶体.     

PMB/GO纳米复合材料的制备及阻燃性能

用共混法制备甲基丙烯酸甲酯-丙烯酸丁酯共聚物(PMB)/氧化石墨(GO)纳米复合材料。采用X射线衍射(XRD)和透射电镜(TEM)对复合材料结构进行了表征,并采用热重分析法(TGA)和锥形量热分析(CONE)研究了其阻燃性能变化。XRD和TEM分析结果表明,复合物中添加GO形成剥离型结构的纳米复合材料。TGA研究发现复合材料的热稳定性得到提高。CONE的测试结果表明,GO极大地改善了体系的燃烧性能,其中加5%GO体系的pk-HRR降低了62.2%。     

Synthesis and characterization of polyamide-6/graphite oxide nanocomposites

Polyamide-6/graphite oxide (PA6/GO) nanocomposites were synthesized using delamination/absorption method. The morphologies of the composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Both XRD and TEM showed that the GO sheets were completely exfoliated and distributed uniformly in PA6 matrix. Differential scanning calorimetry results revealed that the crystallization temperatures of the composites increased compared to that of pristine PA6, which was due to the heterogeneous nucleating effect of GO. However, the half-time of crystallization of the composites were evidently longer than that of pristine PA6, indicating an apparent decrease in the crystallization rate when GO was loaded into the polymer matrix. This was due to the constraining effect of layered GO on PA6 chains. The temperature of maximum decomposition rate was increased by 53 °C only by adding 5 wt% GO, and the maximum decomposition rate of the nanocomposites reduced greatly. The storage modulus (G′) and loss modulus (G″) curves shifted to higher modulus upon addition of 1–5 wt% of GO. With increasing GO loading, the shear viscosity of the nanocomposites gradually increased compared with pure PA6.     

原位聚合尼龙11/石墨烯氧化物纳米复合材料的等温结晶和熔融行为

采用原位聚合法制备了尼龙11/石墨烯氧化物纳米复合材料,并利用差示扫描量热分析仪(DSC)研究了材料的等温结晶动力学和熔融行为。研究结果表明,Avrami方程能够较好地描述尼龙11及其纳米复合材料的等温结晶动力学;尼龙11结晶速率受晶体生长速率控制,而纳米复合材料的结晶速率在不同的结晶温度范围内分别受晶体生长速率或成核速率控制;与纯尼龙11相比较,复合材料具有较低的平衡熔点和表面折叠自由能。     

In situ thermal reduction of graphene oxide for high electrical conductivity and low percolation threshold in polyamide 6 nanocomposites

Electrically conductive and thermally stable polyamide 6 (PA 6) nanocomposites were prepared through one-step in situ polymerization of ε-caprolactam monomer in the presence of electrically insulating and thermally unstable graphene oxide (GO) nanosheets. These nanocomposites show a low percolation threshold of ∼0.41 vol.% and high electrical conductivity of ∼0.028 S/m with only ∼1.64 vol.% of GO. Thermogravimetric analysis and X-ray photoelectron spectroscopy results of GO before and after thermal treatment at the polymerization temperature indicate that GO was reduced in situ during the polymerization process. X-ray diffraction patterns and scanning electron microscopy observation confirm the exfoliation of the reduced graphene oxide (RGO) in the PA 6 matrix. The low percolation threshold and high electrical conductivity are attributed to the large aspect ratio, high specific surface area and uniform dispersion of the RGO nanosheets in the matrix. In addition, although GO has a poor thermal stability, its PA 6 nanocomposite is thermally stable with a satisfactory thermal stability similar to those of neat PA 6 and PA 6/graphene nanocomposite. Such a one-step in situ polymerization and thermal reduction method shows significant potential for the mass production of electrically conductive polymer/RGO nanocomposites.     

Unusual toughening effect of graphene oxide on the graphene oxide/nylon 11 composites prepared by in situ melt polycondensation

Graphene oxide/nylon 11 composites were prepared by in situ melt polycondensation. These composites displayed better mechanical properties including stiffness and toughness than the pure nylon 11 matrix. The enhanced toughness was ascribed to the change of crystal form of nylon 11, namely the triclinic α crystal form to the pseudo-hexagonal δ′ crystal form transition trend with the incorporation of GO. Scanning electron microscopy and transmission electron microscopy images showed that GO bundles and stacks with an average thickness of 20 nm are homogeneously dispersed over the nylon 11 matrix with almost no large agglomerates.     

尼龙11/蒙脱土纳米复合材料的结晶行为

用广角X射线衍射仪(W AXD)、差示扫描量热仪(DSC)、偏光显微镜等手段研究了尼龙11/蒙脱土(PA 11/m on t)纳米复合材料的结晶行为,结果表明,蒙脱土起到成核剂的作用,它的加入没有改变PA 11的晶型,但使PA 11的结晶温度升高,结晶速率增加,结晶活化能降低,使PA 11更易于结晶。A vra-m i方程可较好地描述PA 11及其纳米复合材料的等温结晶行为。     

生物基PA56/PA11的力学、结晶和流变性能研究

采用生物基PA56有望替代传统石油基尼龙,实现尼龙材料的减碳降碳,然而PA56韧性不足的问题限制其广泛应用。采用生物基PA11通过熔融共混增韧PA56,系统研究了PA56/PA11的相容性、结晶行为、热性能和力学性能。结果发现：共混物只有一个Tg,说明PA56和PA11在共混物中具有较好的相容性;PA11的加入使PA56的结晶度和结晶温度有所降低,但对其的熔融温度影响不大;PA11的加入能够有效提升混合材料的韧性,在PA11质量分数为40%时,共混物的断后伸长率由PA56的5.27%提高到了44.26%,提高了739.8%;PA11质量分数为20%时,冲击强度由PA56的4.519 MPa提高到5.569 MPa,提高了23.2%。PA11的加入可有效提高PA56的韧性,提升生物基尼龙材料的综合性能,拓宽其应用领域。     

Crystal form and phase structure of poly(vinylidene fluoride)/polyamide 11/clay nanocomposites by high-shear processing

Polyamide 11 (PA11)/clay, Poly(vinylidene fluoride) (PVDF)/clay and PVDF/PA11/clay nanocomposites were prepared by melt processing using a high shear extruder. Two types of organoclay with different modified alkyl tails and different polarities were used for PA11 and PVDF nanocomposites. PA11 nanocomposites derived from an organoclay having one alkyl tail show a well-exfoliated morphology but no crystal form transformation, whereas those derived from an organoclay having two alkyl tails give a little worse clay dispersion with the clear alpha to gamma crystal form transition with the addition of the clay. In contrast, the PVDF composites derived from the two organoclays result in a poor dispersion. In addition, PVDF/PA11 blend nanocomposites with a novel morphology have been fabricated using the high-shear extruder. It was found that the clay platelets were selectively dispersed in the PA11 phase with the size of larger than 200 nm, while no clay platelets were located in the PVDF phase and in the PA11 nanodomains with the size of smaller than 200 nm. Moreover, the addition of organoclay shows significant effects on the phase structure of PVDF/PA11 blends.     

Mechanical,thermal, and flame-retardant performance of polyamide 11–halloysite nanotube nanocomposites

This study focused on the influence of different filler loadings on the elongation at break and flammability properties of the PA11/FR/HNTs nanocomposites. Polyamide 11 (PA11)/flame-retardant (FR) additives/halloysite nanotubes (HNTs) nanocomposites were melt compounded via twin-screw extrusion for all the compositions. Three FR additive loadings (15, 20, and 25 wt%) and three HNTs loadings (2.5, 5, and 10 wt%) were selected. The formula with 25 % FR and 2.5 % HNT had the lowest additives content and the highest elongation at break of 10.22 % among all UL-94 V-0 rated formulas. A homogeneous dispersion of HNTs in PA11 matrix was observed by transmission electron microscopy. Differential scanning calorimeter measurements indicated that HNTs behaved as nucleating agents by accelerating the rate of crystallization, thus increasing crystallization temperature. The young’s modulus of the PA11 nanocomposites was enhanced with the addition of HNTs. Micro-scale combustion calorimeter results demonstrated that the addition of HNTs also decreased the peak heat release rate of the nanocomposites. These results indicate the effectiveness of HNTs on the mechanical, thermal, and flame-retardant performance of PA11/FR/HNTs nanocomposites.