一步法合成N,S共掺杂荧光碳量子点及其检测汞离子性能.pdf
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1、文章编号:摇 1007鄄8827(2018)04鄄0333鄄08一步法合成 N,S 共掺杂荧光碳量子点及其检测汞离子性能魏居孟1,摇 刘碧桃2,摇 张摇 欣3,摇 宋常春1(1. 安徽科技学院 化学与材料工程学院, 安徽 凤阳 233100;2. 重庆文理学院 材料与化学工程学院, 重庆 402160;3. 西安科技大学 理学院, 陕西 西安 710054)摘摇 要:摇 采用简单一步水热法合成了高荧光量产率(FLQY, 12. 6%)的 N,S 共掺杂碳量子点(N, S鄄CQDs)。 该碳量子点具有小的粒径,无定型结构,独特的表面态和依赖于激发光的荧光特性。 N 和 S 的共掺杂促进了 N,
2、S鄄CQDs 和 Hg2+离子之间的电子传递和协调相互作用。 结果表明,该 N,S 共掺杂碳量子点在湖水中检测 Hg2+离子展现出了较高的灵敏度和选择性。 因此,该碳量子点作为荧光探针在环境监测中具有很好的应用前景。关键词:摇 碳量子点; L鄄半胱氨酸; 共掺杂; 荧光; Hg2+离子检测中图分类号: 摇 TQ127. 1+1文献标识码: 摇 A基金项目:安徽科技学院引进人才项目基金(ZRC2014448);安徽科技学院重点学科基金(AKZDXK2015A01);环境材料与修复技术重庆市重点实验室开放课题基金(CEK1502).通讯作者:宋常春. E鄄mail: lzu_alice163. c
3、omOne鄄pot synthesis of N, S co鄄doped photoluminescentcarbon quantum dots for Hg2+ion detectionWEI Ju鄄meng1,摇 LIU Bi鄄tao2,摇 ZHANG Xin3,摇 SONG Chang鄄chun1(1. College of Chemistry and Materials Engineering, Anhui Science and Technology of University, Fengyang233100, China;2. College of Materials and Ch
4、emical Engineering, Chongqing University of Arts and Sciences, Chongqing402160, China;3. College of Science, Xi爷an University of Science and Technology, Xi爷an710054, China)Abstract: 摇 N and S co鄄doped carbon quantum dots (N, S鄄CQDs) with a high fluorescence quantum yield (12. 6%) were synthe鄄sized b
5、y a one鄄pot hydrothermal method. Results indicate that the N, S鄄CQDs have a small particle size and an amorphous structure,exhibiting unique surface states and excitation wavelength鄄independent fluorescent properties. Co鄄doping of N and S increases theelectron鄄transfer rate and improves the coordina
6、tion interaction between the N, S鄄CQDs and Hg2+ions. The N, S鄄CQDs show a highsensitivity and selectivity in detecting Hg2+ions even for a lake water sample. They are promising fluorescence probes for environ鄄mental monitoring.Key words:摇 Carbon quantum dots; L鄄cysteine; Co鄄doped; Photoluminescent;
7、Hg2+ions detectionReceived date: 2018鄄04鄄02;摇 Revised date: 2018鄄06鄄06Foundation item: Talent Introduction Foundation of Anhui Science and Technology of University (ZRC2014448); Key DisciplineFoundation of Anhui Science and Technology of University (AKZDXK2015A01); Open Foundation of ChongqingKey La
8、boratory of Environmental &Remediation Technologies (CEK1502).Corresponding author: SONG Chang鄄chun. E鄄mail: lzu_alice163. comEnglish edition available online ScienceDirect (http:蛐蛐www. sciencedirect. com蛐science蛐journal蛐18725805).DOI: 10. 1016/ S1872鄄5805(18)60343鄄91摇 IntroductionHeavy鄄metal ions a
9、re greatly hazardous to humanhealth and ecological environments1鄄4. During thepast few decades, industrial and other anthropogenicprocesses have been constantly releasing heavy鄄metalions into the environment. Among them, the Hg2+ions are never away from our sight due to its extremetoxicity, wide dis
10、tribution and high industrial val鄄ue5,6. According to research data, approximate 940tons of Hg2+ions are released to lithosphere and hy鄄drosphere each year, which is seriously harmful tohuman and other organisms due to the hydrologic cy鄄cle and accumulation7. Conventional analytical tech鄄niques for
11、the determination of Hg2+ions have beensuccessfully developed such as chromatography, spec鄄trofluorimetry,andatomicabsorptionspectrome鄄try5,8. However, most of these methods are not con鄄摇第 33 卷摇 第 4 期2018 年 8 月新摇 型摇 炭摇 材摇 料NEW CARBON MATERIALSVol. 33摇 No. 4Aug. 2018摇venient due to the requirement of
12、 expensive equipmentand complicated sample pretreatment.Accordingly,the development of advanced analytical techniques forHg2+ion detection is highly desired.Comparedwithconventionalanalyticaltech鄄niques, the fluorescent probe method possess a seriesof merits such as high sensitivity, high selectivit
13、y,and easy operation9鄄11. As an outstanding fluores鄄cence probe material, carbon quantum dots (CQDs)have attracted growing interest owing to their distinctadvantages such as low cost, simple synthesis route,good biocompatibility, low cytotoxicity, high photoand chemical stability, no blinking fluore
14、scence, andtunable excitation and emission spectra. Up to date,the CQDs have been developed for the detection ofHg2+, Cu2+, Cr4+, Fe3+, et al. by monitoring thechanges of their fluorescence intensities12鄄15. Amongthem, the doped, especially co鄄doped CQDs with dif鄄ferent heteroatoms such as nitrogen
15、and sulfur intro鄄duced more active sites and improved the fluorescentquantum yield (FLQY), leading to outstanding sens鄄ing performance16鄄20. Therefore, the investigation onco鄄doped CQDs with peculiar properties for use asfluorescent probes have never been stopped. Wang etal. used citric acid and dit
16、hiooxamide to fabricate N,S鄄CQDs and investigated the Hg2+ion detection prop鄄erties21. Xu爷 s group employed heparin sodium toobtain N, S鄄CQDs and studied the performance forFe3+detection22. Nevertheless, it is still a challengeto prepare N, S鄄CQDs with novel properties via a fac鄄ile and effective ro
17、ute.In this work, a facile and simple strategy is de鄄veloped for the hydrothermal synthesis of N, S鄄CQDsby using L鄄cysteine as the single precursor.It isfound that both N and S atoms are doped in theCQDs. As鄄prepared N, S鄄CQDs exhibit a small parti鄄cle size, good fluorescence performance, relatively
18、high quantum yield up to 12. 6%, and have been suc鄄cessfully applied in Hg2+ion detection.2摇 Experimental2. 1摇 Chemicals and reagentsL鄄cysteine (L鄄cys) with a purity of 99% waspurchased from Aladdin Ltd.( Shanghai, China).All the other chemicals were purchased from AladdinLtd. (Shanghai, China) and
19、used as received withoutfurther purification. All solutions were prepared usingMilli鄄Q deionized water (18. 2 M赘 cm鄄1, Millipore)as the solvent throughout the experiments.2. 2摇 Synthesis of the N, S鄄CQDsThe N, S鄄CQDs were prepared by hydrothermaltreatment of L鄄cys. The typical experimental proce鄄dur
20、e is shown in Scheme 1. Typically, 1. 0 g L鄄cyswas dissolved in 30 mL deionized (DI) water underagitation at room temperature, and then the solutionwas transferred to a stainless steel autoclave with a50 mL Teflon liner and heated at 180 益 for 12 h.After cooled to room temperature naturally, the res
21、ul鄄ting yellow aqueous solution was centrifuged at 12000rpm for 20 min to remove the non鄄fluorescent depos鄄it. The resultant supernate containing fluorescent N,S鄄CQDs was dialyzed (MWCO: 3500) against DIwater for two days to remove inorganic ions and mol鄄ecules. Finally, a clear and transparent N, S
22、鄄CQDsolution without any precipitation was obtained. Onexposure to UV light (365 nm), the obtained solu鄄tion shows a bright blue color.Scheme 1摇 Schematic of the preparation procedure of N, S鄄CQDs and the photograph of the N,S鄄CQDs solution excited by daylight and a 365 nm UV lamp.2. 3摇 Characteriza
23、tionTransmission electron microscopy (TEM) ima鄄ges, high resolution TEM (HRTEM) images and se鄄lected area electron diffraction ( SAED) were ac鄄quired by using a Tecnai鄄G2F30 transmission electronmicroscope operating at an acceleration voltage of 300kV. X鄄Ray diffraction (XRD) measurements wereperfor
24、med on a Rigaku D/ Max鄄2400 X鄄ray diffrac鄄tometer using Cu K琢 radiation. The Fourier transforminfrared (FTIR) spectra were measured by a ThermoNicolet Nexus FTIR model 670 spectrometer. X鄄rayphotoelectron spectroscopic (XPS) analysis was car鄄ried on an ESCALAB 250 xi photoelectron spectrome鄄ter.UV鄄V
25、is spectroscopic studies were performedwith a TU鄄1901 dual beam UV鄄Vis spectrophotome鄄ter. Photoluminescent (PL) measurements were car鄄ried out with a FLs920 steadystate/ transientstate spec鄄tro xsort.433摇新摇 型摇 炭摇 材摇 料第 33 卷2. 4摇 Metal ion detectionThe obtained N, S鄄CQD solution was diluted 20times
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