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 PDFInfo
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- 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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, 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
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)
- 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. 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. 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. 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.
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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)
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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 |
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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)
Title |
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