CN105714323B - The method that dc-pulse method quickly prepares fluorescent carbon quantum dot - Google Patents

The method that dc-pulse method quickly prepares fluorescent carbon quantum dot Download PDF

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Publication number
CN105714323B
CN105714323B CN201610116350.3A CN201610116350A CN105714323B CN 105714323 B CN105714323 B CN 105714323B CN 201610116350 A CN201610116350 A CN 201610116350A CN 105714323 B CN105714323 B CN 105714323B
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quantum dot
carbon quantum
preparation
carbon
deionized water
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CN105714323A (en
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陈智栋
许志刚
刘长海
王文昌
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Changzhou University
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Changzhou University
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00Nanooptics, e.g. quantum optics or photonic crystals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/65Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon

Abstract

The present invention relates to a kind of preparation method of fluorescent carbon quantum dot, belong to the preparation field of carbon quantum dot.Its preparation method is:Deionized water is placed in electrolytic cell, using graphite carbon rod as both positive and negative polarity, using direct current pulse power source, is electrolysed certain time, you can obtain the grey black aqueous solution, obtain water-solubility fluorescent carbon quantum dot solution after filtering.The preparation technology of carbon quantum dot is prepared simply using this method and substantially reduces the reaction time.

Description

The method that dc-pulse method quickly prepares fluorescent carbon quantum dot
Technical field
The invention belongs to fluorescent carbon quantum dot preparing technical field, and fluorescent carbon quantum dot is prepared more particularly to electrochemical process Method.
Background technology
Fluorescent carbon quantum dot is generally referred to as size and is less than 10nm, has the structure of torispherical, one kind of energy stabilized illumination Nano-sized carbon.Because its raw material resources is abundant and cheap, and there is excellent water solubility, chemical inertness, hypotoxicity, easy functional group Change and anti-light bleaching power, therefore carbon quantum dot is urged in fluorescence sense, bio-imaging, organic photovoltaic, Organic Light Emitting Diode, light The fields such as change obtain good application.The method for the synthesis carbon quantum dot developed, there is the method by chemistry, before small molecule The carbon quantum dot that body is converted into nano-scale is driven, this kind of method mainly includes arc discharge method, laser ablation method, hydro-thermal method, changed Oxidizing process etc. is learned, this kind of methods experiment condition requirement is strict, and cost is higher, complex process;In addition also by physically or chemically Method, large-sized carbon material is obtained into the carbon quantum dot of small size by oxidation, etching, this kind of method has pyrolysismethod, microwave Method, combustion method, solution chemical method etc., this kind of experiment need strict aftertreatment technology, production cycle length, are unfavorable for advising greatly mostly Mould produces.
At present, have been reported that using electrochemical process prepare carbon quantum dot, as fluorescence nano carbon point electrochemistry prepare and its Application [D] in biochemical analysis, Deng Jianhui, Hunan Normal University's master thesis, 2015, it was recently reported that in sodium hydroxide solution In, fluorescent carbon quantum dot is prepared for by electrode of graphite, electrolysis time is about 3 hours, and follow-up dialysis time is about 72 hours, From the point of view of the time used, this method post-processing is comparatively laborious.
The content of the invention
Need to dialyse to solve electrochemical process last handling process, its time length, the cumbersome technical problem of aftertreatment technology, The present invention uses direct current pulse power source, in deionized water, fluorescent carbon quantum dot, party's legal system is prepared by carbon source of graphite carbon rod Standby technique is simple, fast and easy.
Electrolyte is done less than 10 μ S/cm water using electrical conductivity, if the electrical conductivity of water is big, in order to further purify institute Obtained carbon quantum dot solution, subsequent treatment need also exist for carrying out the cumbersome operation such as dialyse.The present invention is using graphite carbon rod as carbon Source, fluorescent carbon quantum dot is prepared using the method for DC pulse, comprised the following steps, concrete operations are as follows:Power taking conductance is less than 10 μ S/cm deionized water, graphite electrode is placed in deionized water, is electrolysed about using direct current pulse power source at normal temperatures 24 hours, by resulting electrolyte filtering, that is, obtain required carbon quantum dot solution.
Further, the voltage that direct current pulse power source is applied is 50~1000V, and frequency is 50~500Hz, and dutycycle is 5%~95%.
Further optimum condition is that selected voltage is 100~500V, and frequency is 100~400Hz, and dutycycle is 20%~50%.
Further, using a diameter of 0.5cm graphite electrode as both positive and negative polarity, positive and negative anode-cathode distance is 5cm.
The beneficial effect of invention:Preparation method technique of the present invention is simple, with short production cycle, without post-processing, after electrolysis Solution only need to filter, not dialyse, obtained carbon quantum dot has preferably water-soluble and dispersiveness, chemical stability in water And good biocompatibility.It is also unlikely even if applying very high voltage on electrode and the present invention is due to using pulse dc power The preparation of carbon quantum dot is influenceed in the side reaction occurred on electrode.The carbon quantum dot can be in fluorescence sense, photocatalysis, You Jiguang The fields such as volt are widely used.
Brief description of the drawings
Fig. 1:In embodiment 2, the fluorescence spectrum of carbon quantum dot;
Fig. 2:Carbon quantum dot compares figure in embodiment 2 and comparative example.
Embodiment
The present invention is elaborated with reference to embodiment, embodiment gives detailed embodiment and specific behaviour Make process, but protection scope of the present invention is not limited to following embodiments.
Embodiment 1-8
350ml deionized water is taken to be placed in 500ml beaker, using a diameter of 0.5cm graphite electrode as both positive and negative polarity, just Negative anode-cathode distance is 5cm, and electrolysis 24 hours, the condition that direct current pulse power source is applied such as table 1 are carried out using direct current pulse power source It is shown, the carbon quantum dot with fluorescence can be obtained after filtering electrolyte.
Table 1 prepares the embodiment of carbon quantum dot
Embodiment Electrolyte Electrolyte volume (ml) Voltage (V) Frequency (Hz) Dutycycle (%)
1 Deionized water 350 50 400 95
2 Deionized water 350 100 400 80
3 Deionized water 350 300 300 75
4 Deionized water 350 500 300 50
5 Deionized water 350 700 200 30
6 Deionized water 350 750 200 20
7 Deionized water 350 800 100 10
8 Deionized water 350 1000 100 5
Comparative example 1
350ml deionized water is taken to be placed in 500ml beaker, using a diameter of 0.5cm graphite electrode as both positive and negative polarity, just Negative anode-cathode distance is 5cm, applies 100V voltages using dc source, carries out electrolysis 24 hours.Resulting carbon quantum dot solution In contain substantial amounts of Carbon deposition, filter out deposition carbon, the fluorescent emission peak intensity of gained carbon quantum dot solution is the 0.36 of embodiment 2 Times.
It by above contrast test, can prove to prepare carbon quantum dot using pulse dc power, be a kind of simple, efficient Method.

Claims (4)

  1. A kind of 1. preparation method of carbon quantum dot, it is characterised in that:The preparation method is:Using direct current pulse power source, with stone Black carbon-point is both positive and negative polarity, is electrolysed in deionized water, filters electrolyte, you can obtain having the carbon quantum dot of fluorescence molten Liquid, wherein, the deionized water electrical conductivity is less than 10 μ S/cm.
  2. 2. the preparation method of carbon quantum dot as claimed in claim 1, it is characterised in that:Described pulse dc power, voltage For 50~1000V, frequency is 50~500Hz, dutycycle 5%~95%.
  3. 3. the preparation method of carbon quantum dot as claimed in claim 1, it is characterised in that:Described pulse dc power, voltage For 100~500V, frequency is 100~400Hz, and dutycycle is 20%~50%.
  4. 4. the preparation method of carbon quantum dot as claimed in claim 1, it is characterised in that:The a diameter of 0.5cm of graphite carbon rod, The positive and negative anode-cathode distance of graphite electrode is 5cm.
CN201610116350.3A 2016-03-01 2016-03-01 The method that dc-pulse method quickly prepares fluorescent carbon quantum dot Active CN105714323B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106270836A (en) * 2016-09-05 2017-01-04 常州大学 Spark discharge prepares the method for fluorescent carbon quantum dot
CN106947475B (en) * 2017-03-30 2020-01-10 皖西学院 Preparation method of fluorescent carbon quantum dots and detection of Al in water by using fluorescent carbon quantum dots3+Ion application
CN108033437A (en) * 2017-12-08 2018-05-15 中国矿业大学 A kind of quick method for preparing carbon dots of salt auxiliary
CN108085711B (en) * 2017-12-21 2019-07-16 西安科技大学 A kind of preparation method of the carbon quantum dot to glow

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103981531A (en) * 2014-06-03 2014-08-13 哈尔滨工业大学 Preparation method of fluorescent carbon dots
CN104792844A (en) * 2015-04-01 2015-07-22 常州大学 Preparation of chitosan-carbon quantum dot composite film modified electrode and application of chitosan-carbon quantum dot composite film modified electrode to electrochemical identification of tryptophan enantiomer
CN105181660A (en) * 2015-06-24 2015-12-23 中国科学院宁波材料技术与工程研究所 Method for preparing graphene fluorescence quantum dots through electrochemical pulse

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103981531A (en) * 2014-06-03 2014-08-13 哈尔滨工业大学 Preparation method of fluorescent carbon dots
CN104792844A (en) * 2015-04-01 2015-07-22 常州大学 Preparation of chitosan-carbon quantum dot composite film modified electrode and application of chitosan-carbon quantum dot composite film modified electrode to electrochemical identification of tryptophan enantiomer
CN105181660A (en) * 2015-06-24 2015-12-23 中国科学院宁波材料技术与工程研究所 Method for preparing graphene fluorescence quantum dots through electrochemical pulse

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Large scale electrochemical synthesis of high quality carbon nanodots and their photocatalytic property;Hai Ming等;《Dalton Transactions》;20120601(第41期);第9526-9531页 *

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