CN102180459A - Method for preparing carbon quantum dots - Google Patents
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- CN102180459A CN102180459A CN 201110049051 CN201110049051A CN102180459A CN 102180459 A CN102180459 A CN 102180459A CN 201110049051 CN201110049051 CN 201110049051 CN 201110049051 A CN201110049051 A CN 201110049051A CN 102180459 A CN102180459 A CN 102180459A
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Abstract
The invention relates to the technical field of quantum dot preparation, in particular to a method for preparing carbon quantum dots, and solves the problems that mass production cannot be realized because raw materials are difficult to obtain, and the fluorescence quantum yield of the obtained carbon quantum dots is low in the conventional method for preparing the carbon quantum dots. The method for preparing the carbon quantum dots comprises the following steps of: heating dried plant stalks in a tubular electric heating furnace, introducing air through an air lead-in pipe of the tubular electric heating furnace, and leading flue gas generated by reaction in a water tank through a flue gas lead-out pipe to obtain soot; adding the obtained soot into nitric acid solution for refluxing and acid boiling, regulating the pH value of reaction solution to be between 6 and 8, and removing water to obtain a solid product; and mixing the solid product and polyethylene glycol in a mass ratio of 3:(2-1) in deionized water, and centrifuging to obtain the carbon quantum dots. The process is easy to operate and can be widely applied to the fields of biological detection, sensing, photoelectric conversion, catalysis, optical amplitude limiting and the like.
Description
Technical field
The present invention relates to the quantum dot preparing technical field, be specially a kind of preparation method of carbon quantum dot.
Background technology
The carbon quantum dot is another the novel carbon nanomaterial after soccerballene, carbon nanotube and Graphene, it is the spherical fluorescence carbon nano-particle that size is generally less than 10 nm and has good dispersion, it not only has the fluorescence quantum yield that compares favourably with conventional semiconductors quantum dot (as CdS, CdSe and nucleocapsid structure thereof), and have nontoxic (or low toxicity), excellent biological compatibility and be easy to many advantages such as surface-functionalized, so have important use at numerous areas such as biological detection, sensing, radiographies; The carbon quantum dot also can be used as electron donor(ED) or acceptor produces photic transfer transport, makes the efficiency light power conversion device thereby can be used as the interpolation component in organic semiconductor material; In addition, the carbon quantum dot has also shown very high potential using value in fields such as nonlinear optics, catalysis.
The method for preparing at present the carbon quantum dot has multiple, but can be divided into from top to bottom generally and two classes from bottom to up.Class methods are to utilize means such as arc-over, laser and electrochemistry directly to obtain from the carbon material of bulk or carbon nanotube from top to bottom, these class methods often need the strict experiment condition or the special energy, the cost height, and the fluorescence quantum yield of acquisition carbon quantum dot is less; Class methods are to obtain tiny from organism and dispersive carbon quantum dot by means such as chemical oxidation, microwave treatment, organic charings from bottom to up, but because the raw material that these class methods are selected for use all is Nonrenewable energy resources and the aftertreatment technology that needs strictness, so also be unfavorable for continuing and scale production carbon quantum dot.
Summary of the invention
The present invention be for solve existing carbon quantum dot preparation method because of raw material is difficult to obtain can't large-scale production and obtain the less problem of fluorescence quantum yield of carbon quantum dot, a kind of preparation method of carbon quantum dot has been proposed.
The present invention adopts following technical scheme to realize: a kind of preparation method of carbon quantum dot may further comprise the steps:
(1) with quality is
mG and be processed into and put into the tubular type electrical heater less than the dried plant stem stalk of the fritter of 10 mm or thinner powder and heat, temperature of reaction maintains 350 ~ 450 ℃, and the air leading-in conduit per minute by the tubular type electrical heater feeds volume and is simultaneously
VThe air of L makes
V:
m=0.5 ~ 6, the flue gas that reaction generates imports in the tank by the flue gas delivery line, can get soot;
(2) the above-mentioned soot that obtains is joined carry out returned acid in the salpeter solution of 2.5 ~ 3.6 mol/L and boil, the reaction times is 10 ~ 12 hours, and the pH value of reaction back solution is adjusted into 6 ~ 8, then obtains solid product except that after anhydrating;
(3) be that 3:2 ~ 1 is mixed in deionized water and put into thermostat container with the mass ratio with the above-mentioned solid product that obtains after anhydrating and the polyoxyethylene glycol of removing, temperature of reaction maintains 105 ~ 135 ℃, reaction times is 48 ~ 72 hours, centrifugal with 4500 ~ 6000 rev/mins centrifugation rate then, can get the carbon quantum dot.
The molecular weight of described polyoxyethylene glycol is 200 ~ 3000.
Described plant haulm comprises common poplar, ash, various fruit tree and cotton stalk etc.These raw materials all are renewable resourcess, and cost is low, and can scale operation.
The critical nature of the carbon quantum dot that the present invention is obtained is measured: make transmission electron microscope and detect, the result shows that the carbon quantum dot is dispersion state, and the grain size of carbon quantum dot mainly is distributed in 2 ~ 7 nm; Carry out Micro-Structure Analysis with transmission electron microscope, the result shows that carbon quantum dot provided by the invention has part to be crystalline structure; The fluorescent emission character of the carbon quantum dot that the present invention is obtained detects: the ultraviolet lamp that with wavelength is 365 nm shines carbon quantum dot aqueous sample, can obviously observe strong blue light; Detect with spectrophotofluorometer, the result shows the fluorescent emission wavelength of the carbon quantum dot wavelength affects that is stimulated, and has the characteristic of multiple VISIBLE LIGHT EMISSION.
The fluorescence quantum yield of carbon quantum dot provided by the invention adopts conventional reference method to measure, promptly under identical shooting conditions, measure the integration fluorescence intensity of reference fluorescence standard material of fluorescence sample to be measured, known quantum yield and the absorption of incident light degree of same excitation wavelength respectively, again with formula below these value substitutions:
In the formula,
Q x With
Q St Be respectively the fluorescence quantum yield of test substance and reference material;
I x With
I St Be respectively the fluorescence integrated intensity of test substance and reference material;
A x With
A St Be test substance and reference material absorption of incident light degree in this excitation wavelength;
η x With
η St Be respectively the specific refractory power of testing sample and standard model.
With Quinine Sulphate Di HC as reference substance, the fluorescence quantum yield of carbon quantum dot provided by the invention after measured is 20 ~ 36%, can be satisfied with biological detection, sensing, optical limiter spare and can be used as and add the application that component improves photoelectric transformation efficiency in the organic semiconductor material.
In a word; technological operation of the present invention is simple, need not any particular energy source; and the carbon quantum dot fluorescence quantum yield that obtains is higher; solved existing carbon quantum dot preparation method because of raw material is difficult to obtain can't large-scale production and obtain the less problem of fluorescence quantum yield of carbon quantum dot, can be widely used in fields such as biological detection, sensing, opto-electronic conversion, catalysis and light amplitude limit.
Description of drawings
Fig. 1 is a preparation soot device synoptic diagram.Among the figure: the 1-air leading-in conduit; 2-tubular type electrical heater; 3-vegetable stem stem; 4-flue gas delivery line; The 5-tank.
(a) is the low power transmission electron microscope photo among Fig. 2, and illustration is the high-resolution-ration transmission electric-lens photo of a carbon quantum dot; (b) be carbon quantum point grain diameter distribution plan.
Fig. 3 is carbon quantum dot aqueous solution sample photo before and after ultra violet lamp.Among the figure: the 1st, carbon quantum dot aqueous solution sample photo is white in color; The 2nd, the sample photo under the wavelength 365 nm wavelength ultra violet lamps is blue.
Fig. 4 is the photoluminescence spectrum of carbon quantum dot.Among the figure: 1 is that 400 nm wavelength excite down the fluorescence spectrum of collecting; 2 is that 440 nm wavelength excite down the fluorescence spectrum of collecting; 3 is fluorescence spectrums of collecting under the 480 nm wavelength lasers; 4 is fluorescence spectrums of collecting under the 520 nm wavelength lasers; 5 is fluorescence spectrums of collecting under the 560 nm wavelength lasers.
Embodiment
Embodiment 1: a kind of preparation method of carbon quantum dot may further comprise the steps: with quality be
mThe dry poplar wood chip of=500 g is put into the tubular type electrical heater and is heated, and temperature of reaction is 350 ℃, and the air leading-in conduit per minute feeding volume by the tubular type electrical heater is simultaneously
VThe air of=250 L makes
V:
m=0.5, the flue gas that reaction generates imports in the tank by the flue gas delivery line, can get soot; The above-mentioned soot that obtains is joined carry out returned acid in the salpeter solution of 2.5 mol/L and boil, the reaction times is 10 hours, and the pH value of reaction back solution is adjusted into 6 ~ 8, then obtains solid product except that after anhydrating; With the above-mentioned solid product that obtains after anhydrating and the molecular weight of removing is that 200 polyoxyethylene glycol is that 3:2 mixes in deionized water and puts into thermostat container with the mass ratio, temperature of reaction maintains 105 ℃, reaction times is 48 hours, then with the centrifugal carbon quantum dot that gets of 4500 rev/mins centrifugation rate.As shown in Figure 2, the carbon quantum dot is dispersion state and size distribution is 2 ~ 7 nm, and part carbon quantum dot is crystalline structure; As shown in Figure 3, the ultra violet lamp of 365 nm wavelength can produce strong blue emission down; As shown in Figure 4, photoluminescence spectrum shows the wavelength size influence that is stimulated of carbon quantum dot fluorescence emission wavelength, has the characteristic of multiple VISIBLE LIGHT EMISSION.
Embodiment 2: a kind of preparation method of carbon quantum dot may further comprise the steps: with quality be
mThe dry ash wood chip of=600 g is put into the tubular type electrical heater and is heated, and temperature of reaction is 450 ℃, and the air leading-in conduit per minute feeding volume by the tubular type electrical heater is simultaneously
VThe air of=3600 L makes
V:
m=6, the flue gas that reaction generates imports in the tank by the flue gas delivery line, can get soot; The above-mentioned soot that obtains is joined carry out returned acid in the salpeter solution of 3.6 mol/L and boil, the reaction times is 12 hours, and the pH value of reaction back solution is adjusted into 6 ~ 8, then obtains solid product except that after anhydrating; With the above-mentioned solid product that obtains after anhydrating and the molecular weight of removing is that 3000 polyoxyethylene glycol is that 3:1 mixes in deionized water and puts into thermostat container with the mass ratio, temperature of reaction maintains 135 ℃, reaction times is 72 hours, then with the centrifugal carbon quantum dot that gets of 6000 rev/mins centrifugation rate.The carbon quantum dot is dispersion state and size distribution is 3 ~ 7 nm, and part carbon quantum dot is crystalline structure; The ultra violet lamp of 365 nm wavelength can produce strong blue emission down; Photoluminescence spectrum shows the wavelength size influence that is stimulated of carbon quantum dot fluorescence emission wavelength, has the characteristic of multiple VISIBLE LIGHT EMISSION.
Embodiment 3: a kind of preparation method of carbon quantum dot may further comprise the steps: with quality be
mThe dried cotton bar bits of=650 g are put into the tubular type electrical heater and are heated, and temperature of reaction is 400 ℃, and the air leading-in conduit per minute feeding volume by the tubular type electrical heater is simultaneously
VThe air of=1950 L makes
V:
m=3, the flue gas that reaction generates imports in the tank by the flue gas delivery line, can get soot; The above-mentioned soot that obtains is joined carry out returned acid in the salpeter solution of 3 mol/L and boil, the reaction times is 11 hours, and the pH value of reaction back solution is adjusted into 6 ~ 8, then obtains solid product except that after anhydrating; With the above-mentioned solid product that obtains after anhydrating and the molecular weight of removing is that 1500 polyoxyethylene glycol is that 3:1.5 mixes in deionized water and puts into thermostat container with the mass ratio, temperature of reaction maintains 120 ℃, reaction times is 60 hours, then with the centrifugal carbon quantum dot that gets of 5250 rev/mins centrifugation rate.The carbon quantum dot is dispersion state and size distribution is 3 ~ 6 nm, and part carbon quantum dot is crystalline structure; The ultra violet lamp of 365 nm wavelength can produce strong blue emission down; Photoluminescence spectrum shows the wavelength size influence that is stimulated of carbon quantum dot fluorescence emission wavelength, has the characteristic of multiple VISIBLE LIGHT EMISSION.
Embodiment 4: a kind of preparation method of carbon quantum dot may further comprise the steps: with quality be
mThe dry apple bar bits of=400 g are put into the tubular type electrical heater and are heated, and temperature of reaction is 420 ℃, and the air leading-in conduit per minute feeding volume by the tubular type electrical heater is simultaneously
VThe air of=800 L makes
V:
m=2, the flue gas that reaction generates imports in the tank by the flue gas delivery line, can get soot; The above-mentioned soot that obtains is joined carry out returned acid in the salpeter solution of 2.8mol/L and boil, the reaction times is 11.5 hours, and the pH value of reaction back solution is adjusted into 6 ~ 8, then obtains solid product except that after anhydrating; With the above-mentioned solid product that obtains after anhydrating and the molecular weight of removing is that 2000 polyoxyethylene glycol is that 3:1.2 mixes in deionized water and puts into thermostat container with the mass ratio, temperature of reaction maintains 115 ℃, reaction times is 55 hours, then with the centrifugal carbon quantum dot that gets of 5500 rev/mins centrifugation rate.The carbon quantum dot is dispersion state and size distribution is 2 ~ 6 nm, and part carbon quantum dot is crystalline structure; The ultra violet lamp of 365 nm wavelength can produce strong blue emission down; Photoluminescence spectrum shows the wavelength size influence that is stimulated of carbon quantum dot fluorescence emission wavelength, has the characteristic of multiple VISIBLE LIGHT EMISSION.
Embodiment 5: a kind of preparation method of carbon quantum dot may further comprise the steps: with quality be
mThe dry shaddock bar bits of=350 g are put into the tubular type electrical heater and are heated, and temperature of reaction is 400 ℃, and the air leading-in conduit per minute feeding volume by the tubular type electrical heater is simultaneously
VThe air of=1350 L makes
V:
m=4.5, the flue gas that reaction generates imports in the tank by the flue gas delivery line, can get soot; The above-mentioned soot that obtains is joined carry out returned acid in the salpeter solution of 3.3 mol/L and boil, the reaction times is 10.5 hours, and the pH value of reaction back solution is adjusted into 6 ~ 8, then obtains solid product except that after anhydrating; With the above-mentioned solid product that obtains after anhydrating and the molecular weight of removing is that 1000 polyoxyethylene glycol is that 3:1.7 mixes in deionized water and puts into thermostat container with the mass ratio, temperature of reaction maintains 130 ℃, reaction times is 66 hours, then with the centrifugal carbon quantum dot that gets of 4900 rev/mins centrifugation rate.The carbon quantum dot is dispersion state and size distribution is 3 ~ 6 nm, and part carbon quantum dot is crystalline structure; The ultra violet lamp of 365 nm wavelength can produce strong blue emission down; Photoluminescence spectrum shows the wavelength size influence that is stimulated of carbon quantum dot fluorescence emission wavelength, has the characteristic of multiple VISIBLE LIGHT EMISSION.
Claims (3)
1. the preparation method of a carbon quantum dot is characterized in that may further comprise the steps:
(1) with quality is
mG and be processed into and put into the tubular type electrical heater less than the dried plant stem stalk of the fritter of 10 mm or thinner powder and heat, temperature of reaction maintains 350 ~ 450 ℃, and the air leading-in conduit per minute by the tubular type electrical heater feeds volume and is simultaneously
VThe air of L makes
V:
m=0.5 ~ 6, the flue gas that reaction generates imports in the tank by the flue gas delivery line, can get soot;
(2) the above-mentioned soot that obtains is joined carry out returned acid in the salpeter solution of 2.5 ~ 3.6 mol/L and boil, the reaction times is 10 ~ 12 hours, and the pH value of reaction back solution is adjusted into 6 ~ 8, then obtains solid product except that after anhydrating;
(3) be that 3:2 ~ 1 is mixed in deionized water and put into thermostat container with the mass ratio with the above-mentioned solid product that obtains after anhydrating and the polyoxyethylene glycol of removing, temperature of reaction maintains 105 ~ 135 ℃, reaction times is 48 ~ 72 hours, centrifugal with 4500 ~ 6000 rev/mins centrifugation rate then, can get the carbon quantum dot.
2. the preparation method of a kind of carbon quantum dot according to claim 1 is characterized in that: the molecular weight of described polyoxyethylene glycol is 200 ~ 3000.
3. the preparation method of a kind of carbon quantum dot according to claim 1 and 2 is characterized in that: described plant haulm comprises common poplar, ash, various fruit tree and cotton stalk etc.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102675565A (en) * | 2012-05-09 | 2012-09-19 | 天津大学 | Carbon quantum dot-poly N-isopropylacrylamide composite material and preparation method thereof |
| CN102816567A (en) * | 2012-08-21 | 2012-12-12 | 中国人民解放军军事医学科学院卫生装备研究所 | Method for preparing high-yield carbon quantum dots |
| CN102911664A (en) * | 2012-11-09 | 2013-02-06 | 吉林大学 | Fluorescent polymer dot, hydrothermal synthesis method through linear non-conjugated polymers and application thereof |
| CN102942170A (en) * | 2012-10-22 | 2013-02-27 | 上海交通大学 | Preparation method of carbon quantum dots based on atmospheric pressure micro-plasma technology |
| CN103086356A (en) * | 2013-02-19 | 2013-05-08 | 复旦大学 | Method for preparing carbon quantum dots |
| CN103100725A (en) * | 2013-02-28 | 2013-05-15 | 江苏大学 | Preparation method of silver/carbon quantum dot composite nanometer materials |
| CN103160279A (en) * | 2011-12-12 | 2013-06-19 | 中国科学院大连化学物理研究所 | Functional carbon dots, and preparation and application thereof |
| CN103332676A (en) * | 2013-07-07 | 2013-10-02 | 上海科润光电技术有限公司 | Preparation method of carbon quantum dot fluorescent material |
| CN103344756A (en) * | 2013-07-15 | 2013-10-09 | 中南大学湘雅二医院 | Preparation method of carbon quantum dot test paper strip for detecting P24 antigen |
| CN103447058A (en) * | 2013-09-18 | 2013-12-18 | 中北大学 | Preparation method for chlorine element modified carbon quantum dot |
| WO2014023097A1 (en) * | 2012-08-06 | 2014-02-13 | 中国科学院理化技术研究所 | Preparation method of heteroatom doped multifunctional carbon quantum dot and application thereof |
| CN105236386A (en) * | 2015-11-10 | 2016-01-13 | 东华大学 | Method for preparing carbon nanoparticles through corncob |
| CN106167256A (en) * | 2016-07-07 | 2016-11-30 | 中北大学 | Utilize the method that ature of coal Colophonium prepares multicolor luminous adjustable carbon point |
| CN106497562A (en) * | 2016-10-20 | 2017-03-15 | 广西壮族自治区林业科学研究院 | A kind of preparation method of carbon quantum dot |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973541A (en) * | 2010-10-11 | 2011-02-16 | 福州大学 | Method for extracting carbon quantum dots from activated carbon |
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2011
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973541A (en) * | 2010-10-11 | 2011-02-16 | 福州大学 | Method for extracting carbon quantum dots from activated carbon |
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| CN103160279A (en) * | 2011-12-12 | 2013-06-19 | 中国科学院大连化学物理研究所 | Functional carbon dots, and preparation and application thereof |
| CN102675565A (en) * | 2012-05-09 | 2012-09-19 | 天津大学 | Carbon quantum dot-poly N-isopropylacrylamide composite material and preparation method thereof |
| WO2014023097A1 (en) * | 2012-08-06 | 2014-02-13 | 中国科学院理化技术研究所 | Preparation method of heteroatom doped multifunctional carbon quantum dot and application thereof |
| CN102816567A (en) * | 2012-08-21 | 2012-12-12 | 中国人民解放军军事医学科学院卫生装备研究所 | Method for preparing high-yield carbon quantum dots |
| CN102816567B (en) * | 2012-08-21 | 2014-10-22 | 中国人民解放军军事医学科学院卫生装备研究所 | Method for preparing high-yield carbon quantum dots |
| CN102942170A (en) * | 2012-10-22 | 2013-02-27 | 上海交通大学 | Preparation method of carbon quantum dots based on atmospheric pressure micro-plasma technology |
| CN102911664A (en) * | 2012-11-09 | 2013-02-06 | 吉林大学 | Fluorescent polymer dot, hydrothermal synthesis method through linear non-conjugated polymers and application thereof |
| CN103086356A (en) * | 2013-02-19 | 2013-05-08 | 复旦大学 | Method for preparing carbon quantum dots |
| CN103100725A (en) * | 2013-02-28 | 2013-05-15 | 江苏大学 | Preparation method of silver/carbon quantum dot composite nanometer materials |
| CN103100725B (en) * | 2013-02-28 | 2015-03-04 | 江苏大学 | Preparation method of silver/carbon quantum dot composite nanometer materials |
| CN103332676B (en) * | 2013-07-07 | 2015-01-28 | 上海科润光电技术有限公司 | Preparation method of carbon quantum dot fluorescent material |
| CN103332676A (en) * | 2013-07-07 | 2013-10-02 | 上海科润光电技术有限公司 | Preparation method of carbon quantum dot fluorescent material |
| CN103344756A (en) * | 2013-07-15 | 2013-10-09 | 中南大学湘雅二医院 | Preparation method of carbon quantum dot test paper strip for detecting P24 antigen |
| CN103344756B (en) * | 2013-07-15 | 2015-09-09 | 中南大学湘雅二医院 | A kind of preparation method of the carbon quantum dot test strips for detecting P24 antigen |
| CN103447058A (en) * | 2013-09-18 | 2013-12-18 | 中北大学 | Preparation method for chlorine element modified carbon quantum dot |
| CN105236386A (en) * | 2015-11-10 | 2016-01-13 | 东华大学 | Method for preparing carbon nanoparticles through corncob |
| CN106167256A (en) * | 2016-07-07 | 2016-11-30 | 中北大学 | Utilize the method that ature of coal Colophonium prepares multicolor luminous adjustable carbon point |
| CN106167256B (en) * | 2016-07-07 | 2018-06-01 | 中北大学 | The method that multicolor luminous adjustable carbon dots is prepared using coal quality pitch |
| CN106497562A (en) * | 2016-10-20 | 2017-03-15 | 广西壮族自治区林业科学研究院 | A kind of preparation method of carbon quantum dot |
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