以无水柠檬酸为碳源,以三羟甲基氨基甲烷(Tris)为氮源,采用一步水热法制备高荧光量子产率掺氮碳量子点(N-CQDs)。在单因素实验的基础上通过研究反应温度、反应时间和Tris质量及其交互作用对荧光量子产率(QY)的影响。利用透射电镜(HRTEM)、红外光谱(FT-IR)、紫外-可见光(UV-Vis)等分析手段对所制备的N-CQDs的形貌、表面官能团、荧光特征进行分析。结果表明:高荧光量子产率N-CQDs的最佳制备工艺条件为反应温度160℃,反应时间5h,Tris质量0.6g,获得的N-CQDs荧光量子产率达73.51%。N-CQDs直径分布约在5～25nm范围内,在365nm紫外光照射下发出蓝紫色荧光,表面含有大量含氮及含氧官能团(如—NH、CO、C—O等)。
The synthesis of highly photoluminescent quantum yield (QY) nitrogen doped carbon quantum dots (N-CQDs) by hydrothermal carbonization from Anhydrous citric acid as the carbon source and trishydroxymethyl aminomethane (Tris) as the nitrogen source was studied.Based on a single factor test,the effects of variables including reaction temperature,reaction time,Tris weight and the interactions of two factors on QY were investigated.The morphology,surface functional groups and fluorescence characteristics of the N-CQDs were explored by HRTEM,FT-IR,UV-Vis and other analytical methods.The results revealed that the obtained optimum synthesized conditions for the parameters i.e.reaction temperature,reaction time,and Tris weight were 160℃,5h and 0.6g respectively,with QY up to 73.51%.The diameter distribution of N-CQDs was around 5～25nm,emitted blue-violet fluorescence under 365nm UV light.The surface of N-CQDs contained a large number of nitrogen-containing and oxygen-containing functional groups (such as —NH,CO,C—O,etc.).
[1] Cao Xiaotong,Ma Jie,Lin Yanping,et al.A facile microwave-assisted fabrication of fluorescent carbon nitride quantum dots and their application in the detection of mercury ions[J].Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy,2015,151(5):875-880.
[2] Qian Zhaosheng,Chai Lujing,Tang Cong,et al.A fluorometric assay for acetylcholinesterase activity and inhibitor screening with carbon quantum dots[J].Sensors and Actuators B:Chemical,2016,222:879-886.
[3] Wang Qin,Zhang Shengrui,Ge Hongguang,et al.A fluorescent turn-off/on method based on carbon dots as fluorescentprobes for the sensitive determination of Pb2+ and pyrophosphate in an aqueous solution[J].Sensors and Actuators B:Chemical,2015,207:25-33.
[4] Bourlinos A B,Karakassides M A,Kouloumpis A,et al.Synthesis,characterization and non-linear optical response of organophilic carbon dots[J].Carbon,2013,61:640-649.
[5] Barati A,Shamsipur M,Arkan E,et al.Synthesis of biocompatible and highly photoluminescent nitrogen doped carbon dots from lime:analytical applications and optimization using response surface methodology[J].Materials Science and Engineering C,2015,47(47):325-332.
[6] Jahanbakhshi M,Habibi B.A novel and facile synthesis of carbon quantum dots via salep hydrothermal treatment as the silver nanoparticles support:application to electroanalytical determination of H2O2 in fetal bovine serum[J].Biosensors and Bioelectronics,2016,81:143-150.
[7] Yan Zhengyu,Zhang Zhengwei,Chen Jianqiu.Biomass-based carbon dots:synthesis and application in imatinib determination[J].Sensors and Actuators B:Chemical,2016,225:469-473.
[8] Campos B B,Abellan C,Zougagh M,et al.Fluorescent chemosensor for pyridine based on N-doped carbon dots[J].Journal of Colloid and Interface Science,2015,458:209-216.
[9] Borse V,Thakur M,Sengupta S,et al.N-doped multi-fluorescent carbon dots for ‘turn off-on’ silver-biothiol dual sensing and mammalian cell imaging application[J].Sensors and Actuators B:Chemical,2017,248:481-492.
[10] Li Hao,Kong Weiqian,Liu Juan,et al.Fluorescent N-doped carbon dots for both cellular imaging and highly-sensitive catechol detection[J].Carbon,2015,91:66-75.
[11] Liu Pengpeng,Zhang Changchang,Liu Xiang,et al.Preparation of carbon quantum dots with a high quantum yield and the application in labeling bovine serum albumin[J].Applied Surface Science,2016,368:122-128.
[12] 刘清浩.罗丹明、荧光素、尼罗红及尼罗兰衍生物的合成及应用[D].天津:天津大学,2009.
[13] Li Linbo,Wang Chao,Luo Jingxuan,et al.Fe3+-functionalized carbon quantum dots:a facile preparation strategy and detection for ascorbic acid in rat brain microdialysates[J].Talanta,2015,144(1):1301-1307.
[14] 高小龙.硫杂蒽酮合成与应用研究[D].杭州:浙江理工大学,2010.
[15] 高东,张煜亮,孙静,等.一步法合成特异性pH响应碳量子点及其发光机理研究[J].无机材料学报,2019,34(12):1309-1315.
[16] 鲍晓宇,张婷婷,黄飞飞,等.以甘蔗渣为基质的碳量子点的制备及表征[J].化工新型材料,2019,47(5):114-116.
[17] 王子儒,张光华,郭明媛.N掺杂碳量子点光稳定剂的制备及光学性能[J].发光学报,2016,37(6):655-661.
