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摘要
以富勒烯C60、4-(N,N-二甲基氨基)苯甲醛为原料,通过1,3-偶极环加成反应合成了N-甲基-2-[4-二甲基氨基]苯基-3,4-富勒烯基吡咯烷(NMDAPF)。首次采用表面活性剂协助自组装的方法制备出该C60衍生物的微米花状结构,通过扫描电子显微镜(SEM)、高分辨透射电子显微镜(HRTEM)、选区电子衍射(SAED)、拉曼光谱(Raman)、热重分析(TGA)和荧光光谱(PL)进行表征,考察了溶液浓度、醇与溶剂体积比、表面活性剂种类、表面活性剂浓度以及温度对其形貌和晶体结构的影响。结果表明:在CCl4溶剂中,该C60衍生物溶液浓度为1.0mg/mL,异丙醇与CCl4体积比为4∶1,以十六烷基三甲基溴化铵(CTAB)为表面活性剂,其浓度为5.0mmol/L,温度为20℃时,NMDAPF晶态形貌为规整的微米花状结构。
Abstract
N-methyl-2-[4-dimethyl-amido] phenyl-3,4-fulleropyrrolidine (NMDAPF) was synthesized by [60]fullerene and 4-(N,N-dimethylamino)benzaldehyde with 1,3-dipolar cycloaddition reaction.The morphology of microflowers was fabricated for the first time using the surfactant assisted self-assembly method.The crystalline structure was characterized by SEM,TEM,HRTEM,SAED,Raman,TGA and PL.The concentration,volume ratio of alcohol and solvent,the type of surfactant,surfactant concentration and temperature were explored on the crystalline structure and morphology.The results showed that:when carbon tetrachloride as solvent,the concentration was 1.0mg/mL,the volume ratio of isopropyl alcohol and carbon tetrachloride was 1∶4,the surfactant was CTAB and concentration was 5.0mmol/L,the temperature was 20℃,the morphology and crystal structure of NMDAPF with regular microflowers was obtained and controlled.
关键词
1,3-偶极环加成
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富勒烯C60衍生物
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微米花状结构
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性能研究
Key words
1,3-dipolar cycloaddition
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[60] fullerene derivative
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microflower structure
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property research
N-甲基-2-[4-二甲基氨基]苯基-3,4-富勒烯基吡咯烷微米花的控制合成及性能研究[J].
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基金资助
国家自然科学基金(21071005和21271006);安徽省高校自然科学一般项目(KJHS2016B06和KJHS2017B02);国家级大学生创新创业训练计划项目(201710375002和201710375011)
