CN112574744A - 一种光致发光蓝光碳量子点的制备方法 - Google Patents
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Abstract
本发明公开了一种光致发光具有激发依赖性的蓝光碳点的制备方法，将催化剂氯盐，引发剂卤代烷烃与碳源溶解于四氢呋喃中，并加热至50‑90℃，反应12‑24小时，得到蓝光碳点粗产物。使用水和三氯甲烷混合液萃取得到光致光蓝光碳点，再通过旋转蒸发去除多余溶剂，最后干燥得到碳点粉末。采用本发明制备出的光致发光蓝光碳点，方法简单，成本低，收率高，制备工艺设备简易，且可大量生产，易于推广。
Description
技术领域
本发明涉及化学及纳米材料科学领域，尤其是一种光致发光蓝光碳量子点的制备方法。
背景技术
量子点(Quantum Dots，QDs)，通常是指半径小于或接近激光波尔半径的半导体纳米晶体，是具有独特的光特性和电特性的纳米尺寸粒子。作为一种纳米荧光材料，与传统的有机染料分子相比具有光化学稳定性强，激发光谱宽，且连续分布，且发光颜色可调等优点，在发光器件，生物标记、生物检测和生物传感器等领域均有应用价值。然而，传统的半导体量子点均由高毒性的金属元素组成，因此具有不可逾越的缺陷，人体健康和环境污染问题一直备受关注，从而限制了其广泛的应用。
近年来，继碳纳米管、石墨烯、纳米金刚石之后，碳纳米材料家族诞生了一位新成员—碳量子点(Carbon Quantum Dots，或称为碳点)，其核心为粒径为小于10nm的碳纳米颗粒，由于具有良好的荧光性能、优异的生物相容性、无毒和易于表面功能化，有望作为传统
半导体量子点的替代物，逐渐成为光致发光领域内的研究热点。目前碳量子点的制备方法很多，但是大多数的碳点的合成方法复杂，需要在高压的反应釜中进行，且温度较高，需要200℃以上，不能大规模生产。且碳量子点与传统的荧光材料相比，具有低毒性、良好的生物相容性和碳源丰富等特点。因此，一种操作简单、低温下大批量合成碳量子点的工艺的构筑显得十分重要。
发明内容
本发明解决的技术问题是提供了一种生物相容性好、制备过程简单、可以在较温和条件下合成且能够规模化生产的光致发光蓝光碳量子点的制备方法。
本发明的技术方案为：一种光致发光蓝光碳点的制备方法，其具体步骤如下：
1)称取催化剂氯盐、引发剂卤代烃和碳源于容器中，溶解于溶剂中，加热至50-90℃反应12-24小时，得到蓝色荧光碳点粗产物；
2)将步骤1)得到的蓝色荧光碳点粗产物混合萃取并旋蒸除去多余溶剂，经最后冷冻干燥或鼓风干燥得到碳点粉末。
优选所述的氯盐为InCl3或ZnCl2。优选所述的引发剂卤代烃为1,2-二氯乙烷或1,2-二溴乙烷。优选所述的碳源为2-羟基-2-甲基苯丙酮。优选所述的溶剂为四氢呋喃。
优选所述的催化剂与碳源的摩尔比为1：(1-2)；引发剂与催化剂的摩尔比为(2-3)：5。
优选萃取溶剂为三氯甲烷和水按体积比为1：(1-4)的混合溶剂。
优选所述的旋蒸温度为50～70℃。
优选所述的冷冻干燥温度为-30℃～-50℃；鼓风干燥温度为40～70℃。
有益效果：
采用本发明制备出的光致发光蓝光碳点，方法简单，成本低，收率高，制备工艺设备简易，且可大量生产，易于推广。
具体实施方式
为了使本技术领域的人员更好地理解本发明技术方案，下面结合附图和实施方式对本发明作进一步的详细说明。
实施例1
称取10mmol InCl3、15mmol 2-羟基-2-甲基苯丙酮(摩尔比为2:3)于装有30mL的四氢呋喃的四口烧瓶中，通氮气10min后加入4mmol的1，2-二氯乙烷(与InCl3摩尔比为2:5)，在通氮气10min加热至50℃，回流24h。反应结束冷却至室温，使用体积比为1:4的三氯甲烷和水进行萃取，60℃旋转蒸发后放到-30℃的冷冻干燥机干燥得到蓝光碳量子点固体，该蓝光碳量子点的PLQY为10.6％，得率为12％。本实施例所制得的荧光碳点在390nm激发波长下的荧光图普，如图1所示。
实施例2
称取5mmol InCl3、10mmol 2-羟基-2-甲基苯丙酮(摩尔比为1:2)于装有30mL的四氢呋喃的四口烧瓶中，通氮气10min后加入3mmol的1，2-二氯乙烷(与InCl3摩尔比为3:5)，在通氮气10min加热至60℃，回流12h。反应结束冷却至室温，使用体积比为1:1的三氯甲烷和水进行萃取，50℃旋转蒸发后放到60℃的鼓风干燥机中干燥得到蓝光碳量子点固体，该蓝光碳量子点的PLQY为12.9％，产率为16％。本实施例所制得的荧光碳点在390nm激发波长下的荧光图普，见图2。
实施例3
称取5mmol ZnCl2、10mmol 2-羟基-2-甲基苯丙酮(摩尔比为1:2)于装有30mL的四氢呋喃的四口烧瓶中，通氮气10min后加入2mmol的1，2-二氯溴烷(与ZnCl2摩尔比为2:5)，在通氮气10min加热至70℃，回流15h。反应结束冷却至室温，使用体积比为1:2的三氯甲烷和水进行萃取，65℃旋转蒸发后放到65℃的鼓风干燥机中干燥得到蓝光碳量子点固体，该蓝光碳量子点的PLQY为16.4％，产率为15％。本实施例所制得的荧光碳点在390nm激发波长下的荧光他图谱，见图3。
实施例4
称取10mmol ZnCl2、10mmol 2-羟基-2-甲基苯丙酮(摩尔比为1:1)于装有30mL的四氢呋喃的四口烧瓶中，通氮气10min后加入5mmol的1，2-二氯乙烷(与ZnCl2摩尔比为2:5)，在通氮气10min加热至80℃，回流18h。反应结束冷却至室温，使用体积比为1:1的三氯甲烷和水进行萃取，70℃旋转蒸发后放到-50℃的冷冻干燥机中干燥得到蓝光碳量子点固体，该蓝光碳量子点的PLQY为11.2％，产率为10％。本实施例所制得的荧光碳点在390nm激发波长下的荧光图谱，见图4。
实施例5
称取2.5mmol InCl3、10mmol 2-羟基-2-甲基苯丙酮(摩尔比为1:1)于装有30mL的四氢呋喃的四口烧瓶中，通氮气10min后加入1mmol的1，2-二溴乙烷(与InCl3摩尔比为2:5)，在通氮气10min加热至90℃，回流24h。反应结束冷却至室温，使用体积比为1:3的三氯甲烷和水进行萃取，60℃旋转蒸发后放到50℃的鼓风干燥机中干燥得到蓝光碳量子点固体，该蓝光碳量子点的PLQY为8.9％，得率为12％。本实施例所制得的荧光碳点在390nm激发波长下的荧光图谱，见图5。
以上实施例描述了本发明的基本原理、主要特征及优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明原理的范围下，本发明还会有各种变化和改进，这些变化和改进均落入本发明保护的范围内。
Claims (9)
1.一种光致发光蓝光碳点的制备方法，其具体步骤如下：
1)称取催化剂氯盐、引发剂卤代烃和碳源于容器中，溶解于溶剂中，加热至50-90℃反应12-24小时，得到蓝色荧光碳点粗产物；
2)将步骤1)得到的蓝色荧光碳点粗产物混合萃取并旋蒸，经最后冷冻干燥或鼓风干燥得到碳点粉末。
2.根据权利要求1所述的制备方法，其特征在于所述的氯盐为InCl3或ZnCl2。
3.根据权利要求1所述的制备方法，其特征在于所述的引发剂卤代烃为1,2-二氯乙烷或1,2-二溴乙烷。
4.根据权利要求1所述的制备方法，其特征在于所述的碳源为2-羟基-2-甲基苯丙酮。
5.根据权利要求1所述的制备方法，其特征在于所述的溶剂为四氢呋喃。
6.根据权利要求1所述的制备方法，其特征在于所述的催化剂与碳源的摩尔比为1：(1-2)；引发剂与催化剂的摩尔比为(2-3)：5。
7.根据权利要求1所述的制备方法，其特征在于萃取溶剂为三氯甲烷和水按体积比为1：(1-4)的混合溶剂。
8.根据权利要求1所述的制备方法，其特征在于所述的旋蒸温度为50～70℃。
9.根据权利要求1所述的制备方法，其特征在于所述的冷冻干燥温度为-30℃～-50℃；鼓风干燥温度为40～70℃。
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| CN111961237A (zh) * | 2019-05-20 | 2020-11-20 | 湖北大学 | 一种碳量子点基反蛋白石结构凝胶薄膜的制备方法及应用 |
| CN110885680A (zh) * | 2019-11-12 | 2020-03-17 | 中国矿业大学 | 一种无溶剂法制备多色荧光碳点的方法及其制备的多色荧光碳点 |
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