Crystallization Behavior of Polyamide 1010-Single-Walled Carbon Nanotube Nanocomposites under High Pressure
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摘要: 采用XKY-61200MN型六面顶压机,在不同温度、压力条件下处理30 min后制备了尼龙1010(PA1010)-单壁碳纳米管(SWCNT)复合材料的高压结晶样品,通过X射线衍射(XRD)、差热分析仪(DSC)、扫描电子显微镜(SEM)、透射电子显微镜(TEM),研究了高压处理样品的结晶行为、结构变化及形貌特征。结果表明:在1.0~2.5 GPa压力下,属于高压熔体结晶;在3.0和4.5 GPa压力下属于高压退火处理;高压结晶或高压退火均有助于聚合物片层晶体的增厚,并且高压熔体结晶的增厚效果优于高压退火处理。XRD结果表明,PA1010的三斜晶型在高压处理后保持不变,高压熔体结晶或高压退火都可以使(100)晶面和(010)晶面间距减小,即高压处理致使聚合物分子链紧密堆积。DSC结果表明:在高压熔体结晶过程中,升高压力和温度可以得到片层厚度较大的PA1010晶体;在2.0 GPa、350 ℃下获得的高压结晶样品的熔点和结晶度最高,分别达到208.5 ℃和64.6%。SEM和TEM结果表明:与常压结晶样品相比,高压结晶样品内部出现c轴厚度超过150 m的大尺寸晶体;SWCNT与PA1010基体之间形成相互穿插的网络结构,刚性的SWCNT作为高压成核剂促进PA1010晶体生长和增厚。Abstract: The PA1010 (polyamide 1010)-SWCNT (single-walled carbon nanotube) nanocomposites crystallized at different temperatures and pressures for 30 min are prepared by an XKY-61200MN type high-pressure apparatus. The structure, crystallization behavior and morphological feature of high-pressure crystallized samples are studied by XRD (X-ray diffraction), DSC (differential scanning calorimetry), SEM (scanning electron microscope) and TEM (transmission electron microscope). The results show that high-pressure melt crystallization occurs in the pressure range of 1.0-2.5 GPa, while high-pressure annealing occurs in 3.0 and 4.5 GPa. Both melt crystallization and annealing under high pressure contribute to the thickening of polymer lamellar crystals, and moreover, the effect of high pressure melt crystallization is superior to that of high-pressure annealing. XRD results show that the triclinic form of PA1010 remains unchanged after high-pressure treatment, and both melt crystallization and annealing under high pressure can decrease (100) and (010) crystal plane spacing, and namely the high-pressure treatment results in close packing of polymer molecular chains. DSC results show that elevating the pressure and temperature during melt crystallization under high pressure can lead to the formation of crystals with larger lamella thickness, and the highest value of melting point and crystallinity obtained in the sample crystallized at 2.0 GPa and 350 ℃ are 208.5 ℃ and 64.6%, respectively. The large-sized crystals with c axis thickness exceeding 150 m are detected by SEM and TEM in the sample crystallized at high pressure. The interpenetrating network structure between the SWCNT and PA1010 matrix is formed, and the rigid SWCNT as high pressure nucleating agent can promote growth and thickening of PA1010 crystals under high pressure.
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