CN109294570B - 一种黄光油相碳点的制备方法 - Google Patents
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Abstract
本发明属于无机发光材料技术领域，具体涉及一种油相碳点的制备方法，其具体步骤如下：将无水柠檬酸、油胺、1‑十八烯置于三口瓶中，在N2气氛保护下，高温热解、碳化、自组装成碳点。本发明具有方法简单、原材料廉价的优点。所述的碳点具有优异的油相互溶性，解决了目前传统的水溶性碳点无法满足太阳能电池、LED/LCD显示、光电器件等领域有机相的难题，可以满足多个领域的应用要求。
Description
技术领域
本发明属于荧光纳米材料制备技术领域，具体涉及一种油相互溶性碳点的制备方法及其在WLED照明、显示等领域的应用。
背景技术
美国南卡罗莱纳大学的Walter A．Scrivens团队在2004年提纯单壁碳纳米管时偶然发现了一种具有荧光的纳米材料，经过进一步分离后，在365 nm紫外光激发下发出不同的荧光，并将其命名为“fluorescent carbon”（非专利文献1），随后证实该荧光纳米材料即是碳点。美国克莱姆森大学的Ya Ping Sun团队于2006年通过激光消融碳靶，成功合成出蓝光发射的 “carbon dots”（CDs），并首次将其命名为“碳点”（非专利文献2），自此，全世界范围内正式拉开了研究碳点的序幕。碳点是一种由内部碳核和包含丰富官能团（-COOH、-OH、-C=O-、-NH2等）及缺陷的无定形基质两部分组成的准球状纳米粒子，其内部碳核由sp2杂化的纳米碳结构（无定形或结晶）组成；碳点具有制备方法多样、制备过程简单、毒性小、光稳定性好、生物相容性优异、水溶性好等优点，近年来被广泛用于荧光标记、传感、生物医药、检测等领域，是继碳纳米管、富勒烯、石墨烯之后，最受关注的新型碳纳米材料之一（非专利文献3,4）。
碳点的制备方法多达数十种，如水热法、微波法、溶剂热法、等离子体法、电化学法、电弧放电法、激光消融法等，但是获得的碳点多为水溶性的（专利文献1-4），无法满足光电器件、光伏电池等领域的应用要求。目前虽然有少数关于油相互溶性碳点（以下简称为“油相碳点”）的报道（专利文献5-6），但是制备方法复杂，亟待制备出性能优异的油相碳点，使其满足更多领域的应用要求。
[非专利文献1] X.Y. Xu, R. Ray, Y.L. Gu, et al. Electrophoreticanalysis and purification of fluorescent single-walled carbon nanotubefragments [J]. Journal of the American Chemical Society, 2004, 126(40):12736-12737. [非专利文献2] Y.P. Sun, B. Zhou, Y. Lin, et al. Quantum-sizedcarbon dots for bright and colorful photoluminescence [J]. Journal of theAmerican Chemical Society, 2006, 128(24): 7756-7757.[非专利文献3] S.Y. Tao,S.J. Zhu, T.L. Feng, et al. The polymeric characteristics andphotoluminescence mechanism in polymer carbon dots: A review [J]. MaterialsToday Chemistry, 2017, 6:13-25.[非专利文献4] S.Y. Tao, S.J. Zhu, T.L. Feng,et al. The polymeric characteristics and photoluminescence mechanism inpolymer carbon dots: A review materials [J]. Materials Today Chemistry, 2017,6: 13-25.[专利文献1] CN201410005216.7，一种生物活性酶辅助微波法合成碳点的方法、由此制备的碳点及其应用。
[专利文献2] CN201410842186.5，一种发蓝光和绿光的碳量子点的快速制备方法。[专利文献3]CN201310487328.6，一种光致发光碳量子点的制备方法。[专利文献4]CN201610139530.3，一种有机废水制备碳量子点及其混凝回收方法。 专利文献5]CN201510822666.X，一种制备水相、油相碳点的方法。 [专利文献6] CN201410348124.9，一类离子液体修饰碳点的制备方法。
发明内容
本发明的目的在于提供一种适用于WLED、太阳能电池等领域的油相碳点的简单制备方法。
本发明方法包括如下步骤：
步骤一：将一定量的无水柠檬酸、油胺、1-十八烯置于三口瓶中；依次抽真空、通N2；在剧烈的磁力搅拌下逐渐升温至使无水柠檬酸完全熔化；随后，继续升温至200～250 °C，恒温保持0.5～5 h，得到澄清透明的淡黄色溶液；
步骤二：反应完成后，冷却至室温，在上述的淡黄色溶液中加入等体积的丙酮，对混合溶液进行离心清洗，获得纯化的油相碳点溶液；
本发明所述的无水柠檬酸前驱液的浓度为0.01～0.2 g/mL；反应温度为200～250°C；反应时间为0.5～5 h。
本发明所制备的碳点为无定型结构，粒径分布在5～8 nm，量子效率为38～56％。
本发明具有反应条件温和、方法简单易行，原材料绿色、廉价等优点。通过改变实验条件可以获得发光峰位分别为蓝光、绿光和黄光的油相碳点，获得的碳点可广泛用于光电显示、光电催化、太阳能电池等领域。
附图说明
图1. 本发明实施例1制备得到的蓝光油相碳点的荧光光谱。
图2. 本发明实施例1制备得到的蓝光油相碳点的紫外-可见光吸收光谱。
图3. 本发明实施例2制备得到的绿光油相碳点的荧光光谱。
图4. 本发明实施例2制备得到的绿光油相碳点的紫外-可见光吸收光谱。
图5. 本发明实施例3制备得到的黄光油相碳点的微观形貌（TEM）图。
图6. 本发明实施例3制备得到的黄光油相碳点的荧光光谱。
图7. 本发明实施例3制备得到的黄光油相碳点的紫外-可见光吸收光谱。
图8. 本发明实施例4制备得到的黄光油相碳点用于WLED器件的光学参数图。
具体实施方式
通过以下具体实施例来说明本发明，但并不用来限制本发明。
实施例1：
蓝光油相碳点溶液的制备：
步骤一：分别将0.1 g无水柠檬酸和9 mL 1-十八烯置于50 mL的三口瓶中；依次抽真空、通N2各10 min；
步骤二：在N2保护氛围和剧烈的磁力搅拌下，以1 °C/min的速率，逐渐升温至170°C并保持30 min，使无水柠檬酸完全熔化；
步骤三：将步骤二所述的溶液升温加热至200 °C，恒温保持3 h，得到澄清透明的淡黄色溶液。
碳点溶液的纯化：反应完成后，冷却至室温，在步骤三所述的淡黄色溶液中加入等体积的丙酮，对混合溶液进行离心清洗，获得纯化的碳点溶液。
碳点的光学性能表征：采用稳态荧光光谱仪测试碳点溶液在不同激发波长（330～ 430 nm）下的发射光谱（图1），所述碳点在370 nm的激发光下发出峰位为445 nm的明亮的蓝光。采用紫外-可见光荧光光谱仪测试本实施例所述的碳点的吸收光谱（图2），其在280nm左右有一个源于n-π*跃迁的明显的吸收带。
实施例2：
绿光油相碳点溶液的制备：
步骤一：分别将1 g无水柠檬酸、0.3 mL油胺、9 mL 1-十八烯置于50 mL的三口瓶中；依次抽真空、通N2各10 min；
步骤二：在N2保护氛围和剧烈的磁力搅拌下，以1 °C/min的速率，逐渐升温至170°C并保持30 min，使无水柠檬酸完全熔化；
步骤三：将步骤二所述的溶液升温加热至200 °C，恒温保持3 h，得到澄清透明的淡黄色溶液。
碳点溶液的纯化：反应完成后，冷却至室温，在步骤三所述的淡黄色溶液中加入等体积的丙酮，对混合溶液进行离心清洗，获得纯化的碳点溶液。
碳点的光学性能表征：采用稳态荧光光谱仪测试碳点溶液在不同激发波长（340 ~430 nm）下的发射光谱（图3），碳点在380 nm的激发光下发出峰位为517 nm的明亮的绿光。采用紫外-可见光荧光光谱仪测试本实施例所述的碳点的吸收光谱（图4），其位于400 ~500 nm的吸收带贡献了碳点的绿光发射。
实施例3：
黄光油相碳点溶液的制备：
步骤一：分别将2 g无水柠檬酸、1 mL油胺、9 mL 1-十八烯置于50 mL的三口瓶中；依次抽真空、通N2各10 min；
步骤二：在N2保护氛围和剧烈的磁力搅拌下，以1 °C/min的速率，逐渐升温至170°C并保持30 min，使无水柠檬酸完全熔化；
步骤三：将步骤二所述的溶液升温加热至250 °C，恒温保持5 h，得到澄清透明的淡黄色溶液。
黄光油相碳点的纯化：反应完成后，冷却至室温，在步骤三所述的淡黄色溶液中加入等体积的丙酮，对混合溶液进行离心清洗，获得纯化的碳点溶液。
黄光油相碳点的微观形貌表征：采用透射电子显微镜对本实施例所述的黄光油相碳点的微观形貌进行观察（图5），可以看出合成的黄光碳点平均粒径分布在 5 ~ 8 nm，是具有无定型结构的球形颗粒。
黄光油相碳点的荧光性能表征：采用稳态荧光光谱仪测试黄光碳点溶液在不同激发波长（350 ~ 490 nm）下的发射光谱（图6），碳点在460 nm的激发光下发出峰位为545 nm的明亮的黄光。采用紫外-可见光荧光光谱仪测试本实施例所述的黄光碳点的吸收光谱（图7），其位于400 ~ 510 nm的吸收带贡献了碳点的黄光发射。
实施例4：
将该发明制备的油相黄光碳点与发光峰值位于450 nm的蓝光芯片封装在一起，制备WLED器件。具体实施方法如下：分别取0. 5 mL该发明制备的黄色碳点溶液、0. 25 g光学专用胶加入玛瑙研钵中，研磨成均匀的浆料，然后将该浆料均匀的滴加到蓝光芯片的凹槽中，形成均匀的覆盖层；最后，将该芯片转移至真空干燥箱中，在160 ℃ 恒温环境下使涂覆层固化，得到WLED平面光源器件，测试得到该WLED器件在30 mA电流驱动下的电致发光谱（图8）。
Claims (1)
1. 一种包含黄光油相碳点的制备方法，其特征在于，黄光油相碳点粒径分布在5-8nm，是具有无定型结构的球形颗粒，黄光油相碳点在350-490nm的任一激发光下均能发出黄光；
具有包含以下步骤，
步骤一，分别将2 g无水柠檬酸、1 mL油胺、9 mL 1-十八烯置于50 mL的三口瓶中；依次抽真空、通N2各10 min；
步骤二，在N2保护氛围和剧烈的磁力搅拌下，以1 °C/min的速率，逐渐升温至170 °C并保持30 min，使无水柠檬酸完全熔化；
步骤三，将步骤二获得的溶液升温加热至250 °C，恒温保持5 h，得到澄清透明的淡黄色溶液；
步骤四，反应完成后，冷却至室温，在步骤三所述的淡黄色溶液中加入等体积的丙酮，对混合溶液进行离心清洗，获得纯化的黄色碳点溶液。
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