CN108359451A - Graphene quantum dot and preparation method thereof - Google Patents
Graphene quantum dot and preparation method thereof Download PDFInfo
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- CN108359451A CN108359451A CN201810030355.3A CN201810030355A CN108359451A CN 108359451 A CN108359451 A CN 108359451A CN 201810030355 A CN201810030355 A CN 201810030355A CN 108359451 A CN108359451 A CN 108359451A
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- 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
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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
Abstract
The present invention relates to quantum dot preparation fields, disclose a kind of preparation method of graphene quantum dot, and this method is included under oxidation reaction condition, so that graphene is carried out oxidation reaction in aoxidizing solution, obtain graphene quantum dot, wherein the oxidation solution contains H2SO4And HNO3, the H aoxidized in solution2SO4A concentration of 10 14mol/L, and H2SO4With HNO3Molar ratio be 1：0.20‑0.45.The graphene quantum dot that the preparation method of the present invention obtains has uniform carbon ratio, and has the regulatable property of spectrum, is suitable for the structure of bio-imaging, multi-color marking and fluorescence and electroluminescent chemiluminescence biosensor.
Description
Technical field
The present invention relates to quantum dot preparation fields, and in particular to a kind of graphene quantum dot and preparation method thereof.
Background technology
Graphene is the two-dimension nano materials for zero band gap being made of the graphite of individual layer laminated structure, opens the energy of graphene
Band is beneficial to its application in optics and electronic device etc..Graphene quantum dot (GQDs) is as the homologous of graphene
Body material, by controlling grain size and shape, the energy band of GQDs can be regulated and controled between 0eV to~6eV (phenyl ring).Cause
This, the carbon nanomaterial of this zero-bits of GQDs has received widespread attention.The preparation method of GQDs mainly has chemical oxidation, electrochemistry
Etching, microwave radiation, free-radical oxidation etc..It is being continuously increased about GQDs preparation methods, however, GQDs surface state can be regulated and controled
Method it is still to be developed.Wherein chemical oxidization method is a kind of more commonly used method, in some oxidising agents, such as H2SO4、
HNO3、H2O2、O3Deng to carbon source material progress oxide etch, you can obtain GQDs.After Pan etc. restores graphene oxide (GO)
Precursor material Sheet Graphite alkene is obtained, in H2SO4With HNO3Mixed acid system in oxidation obtain the GQDs with blue emission.
Peng etc. obtains the GQDs of polychrome by chemical oxidation carbon fiber.In addition, passing through six bandit of chemical oxidation macromolecular benzo, nanometer
The carbon source materials such as graphite and graphite powder can also obtain GQDs.It can be seen that the raw material sources of chemical oxidization method are extensive, and
And the polychrome that GQDs may be implemented is prepared with a large amount of, this provides preciousness to investigate the application of the fluorescence property and GQDs of GQDs
Material.But for how to obtain having the GQDs of uniform carbon ratio to have not been reported at present.
Invention content
The purpose of the invention is to overcome to be difficult to control oxygen in graphene quantum dot preparation process of the existing technology
Change degree problem, provides a kind of preparation method of graphene oxide, and the graphene quantum dot that this method is prepared has uniform
Degree of oxidation (carbon ratio) and extensive particle diameter distribution, and have the regulatable property of spectrum, be suitable for be based on graphene
Structure, bio-imaging, the multi-color marking etc. of quantum dot fluorescence and electrogenerated chemiluminescence performance biosensor.
To achieve the goals above, the present invention provides a kind of preparation method of graphene quantum dot, this method is included in
Under oxidation reaction condition, so that graphene is carried out oxidation reaction in aoxidizing solution, obtain graphene quantum dot, wherein the oxygen
Change solution and contains H2SO4And HNO3, the H aoxidized in solution2SO4A concentration of 10-14mol/L, and H2SO4With HNO3's
Molar ratio is 1：0.20-0.45.
Preferably, the H in the oxidation solution2SO4A concentration of 12-14mol/L, and H2SO4With HNO3Molar ratio
It is 1：0.30-0.35.
Preferably, this method further includes that obtained graphene quantum dot is carried out ultrafiltration.It is highly preferred that making in the ultrafiltration
It is 100kDa, 50kDa, 30kDa, 10kDa or 3kDa with the molecular cut off of ultrafiltration membrane.
Preferably, the oxidation reaction condition includes：Temperature is 70-90 DEG C, time 20-180min.
Preferably, relative to the graphene of 10mg, the oxidation solution of 8-15mL is used.
Preferably, this method further includes reaction being terminated after the completion of oxidation reaction, and the pH that alkali adjusts acquired solution is added
Value is 6-8；It is highly preferred that terminating reaction by the way that deionized water is added, and the pH value that NaOH adjusts acquired solution is added.
Preferably, this method further includes that the solution that will be obtained concentrates.
The present invention also provides the graphene quantum dots being prepared according to above-mentioned preparation method, wherein the graphite
The ratio of oxygen element and carbon is 0.38-0.76, preferably 0.58-0.71 in alkene quantum dot.
Preferably, the electrogenerated chemiluminescence peak of the graphene quantum dot is located at 450-645nm, is more preferably located at 528-
610nm。
Preferably, the fluorescence emission wavelengths of the graphene quantum dot are 450-630nm, more preferably 521-606nm.
The present invention also provides above-mentioned graphene quantum dots to send out in bio-imaging, multi-color marking and fluorescence and electroluminescent chemistry
Application in the structure of optical biosensor.
Through the above technical solutions, the preparation method of the present invention may be implemented relatively to accurately control graphene quantum dot oxidation journey
Degree can regulate and control the fluorescence emission wavelengths of graphene quantum dot by controlling grain size, to investigate dimensional effect to graphene amount
The influence of son point luminescent properties provides preferable material.The present invention graphene quantum dot have abundant oxygen-containing functional group,
Good water-soluble, regulatable fluorescence property and electrogenerated chemiluminescence performance, are suitable for multi-color marking, bio-imaging and base
Built in graphene quantum dot fluorescence and the biosensor of electrogenerated chemiluminescence performance etc..
Description of the drawings
Fig. 1 is that the graphene quantum dot aqueous solution of the present invention is shone in visible light (above) at 365nm ultraviolet lamps (figure below)
Picture under penetrating；
Fig. 2 is that different-grain diameter graphene quantum dot normalizes fluorescence emission spectrum in the present invention.
Specific implementation mode
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
According to the preparation method of graphene quantum dot in the present invention, this method is included under oxidation reaction condition, makes graphite
Alkene carries out oxidation reaction in aoxidizing solution, obtains graphene quantum dot, wherein the oxidation solution contains H2SO4And HNO3,
H in the oxidation solution2SO4A concentration of 10-14mol/L, and H2SO4With HNO3Molar ratio be 1：0.20-0.45.
Preferably, the H2SO4With HNO3Molar ratio be 0.25-0.45；It is highly preferred that the H2SO4With HNO3Rub
You are than being 1：0.31-0.44.
Preferably, the H in the oxidation solution2SO4A concentration of 12-14mol/L, and H2SO4With HNO3Molar ratio
It is 1：0.30-0.35.
According to the present invention, in order to preferably control the degree of oxidation of gained graphene quantum dot, in the oxidation solution
HNO3A concentration of 2.0-6.0mol/L, preferably 3.0-4.5mol/L, more preferably 4.0-4.5mol/L.
The present inventor passes through the study found that by selecting oxidation solution appropriate, so as to realize to graphite
The control of alkene aoxidizes, and the ratio for obtaining oxygen element and carbon is that having for 0.38-0.76 (preferably 0.58-0.71) provides oxygen
The graphene quantum dot of change degree, while the graphene quantum dot has extensive particle diameter distribution, so as to further pass through
The modes such as ultrafiltration prepare the graphene quantum dot of required grain size；And only graphene quantum dot can be controlled by controlling grain size
Fluorescence emission wavelengths, be convenient for fit applications demand.The electrogenerated chemiluminescence peak of the graphene quantum dot of the present invention is located at
450-645nm is preferably placed at 528-610nm, fluorescence emission wavelengths 450-630nm, more preferably 521-606nm, Neng Gouman
The sides such as biosensor structure, multi-color marking bio-imaging of the foot based on graphene quantum dot fluorescence and electrogenerated chemiluminescence performance
The demand in face.
In order to further obtain the graphene quantum dot of appropriate grain size, this method will may further include the stone that will be obtained
Black alkene quantum dot carries out ultrafiltration.Ultrafiltration membrane, the graphene amount that molecular cut off can be as needed may be used in the ultrafiltration
Son point grain size is specifically chosen, such as 100kDa, 50kDa, 30kDa, 10kDa or 3kDa etc., by using different retentions point
The ultrafiltration membrane of son amount carries out ultrafiltration, can obtain the graphene quantum dot for needing range.
In the present invention, in the graphene quantum dot that the condition of the oxidation reaction can obtain as needed oxygen element with
The ratio of carbon specifically determines that the oxidation reaction condition may include：Temperature is 70-90 DEG C, time 20-180min；
Preferably, temperature is 70-90 DEG C, time 30-180min；It is highly preferred that temperature is 75-85 DEG C, time 100-160min.
By selecting the condition of above-mentioned oxidation reaction, it can more accurately regulate and control the degree of oxidation of graphene quantum dot.
In the present invention, in order to make graphene by suitable oxidizing, the graphene quantum dot of required degree of oxidation is obtained, relatively
In the graphene of 10mg, using 8-15mL oxidation solution, it is preferable to use 9-12mL oxidation solution.
According to the present invention, in order to control the degree of oxidation reaction progress, this method is further preferably included in oxidation reaction completion
Reaction is terminated afterwards, and it is 6-8, preferably 6.5-7.5 that alkali, which is added, to adjust the pH value of acquired solution.As terminate reaction method,
Such as reaction can be terminated by the way that deionized water is added, and the pH value that NaOH adjusts acquired solution is added.Oxidation relative to 1mL
Solution, the deionized water used can be 180-300mL, preferably 220-270mL.PH value is adjusted in order to prevent acutely to put in the process
Heat influences the progress of oxidation reaction, and the process that alkali is added preferably carries out under condition of ice bath.
, according to the invention it is preferred to the salt contained in the graphene quantum dot solution removed, such as dialysis may be used
The methods of carry out.As the method for dialysis, can use commonly used in removing the dialysis of the inorganic salts small molecule in nano material
The molecular cut off of method, the dialysis membrane used can be determined according to the size of graphene quantum dot to be dialysed, such as
Can be 0.2-5kDa, preferably 0.5-2kDa, more preferably 0.9-1.1kDa.
According to the present invention, the graphene quantum dot of higher concentration, this method can also include molten by what is obtained in order to obtain
Liquid is concentrated.Preferably, the concentration is carried out using the method for rotary evaporation.As the condition of rotary evaporation, such as can be with
Including：Temperature is 60-90 DEG C, and pressure (in terms of gauge pressure, similarly hereinafter) is 1-20kPa；Preferably, temperature is 65-80 DEG C, pressure 2-
10kPa.The time of rotary evaporation can be selected according to required concentration, such as 20-40min, preferably 25-30min.
As the preferred embodiment of the present invention, the grain size of graphene quantum dot is preferably 1.8-6.0nm, more excellent
It is selected as 2.2-5.2nm, particularly preferably 2.6-4.6nm.
The present invention also provides the graphene quantum dots that above-mentioned preparation method is prepared, wherein the graphene quantum
The ratio of oxygen element and carbon is 0.38-0.76, preferably 0.58-0.71 in point.Preferably, the graphene quantum dot
Electrogenerated chemiluminescence peak is located at 450-645nm, is more preferably located at 528-610nm.Preferably, the fluorescence of the graphene quantum dot
Launch wavelength is 450-630nm, more preferably 521-606nm.By making graphene quantum dot that there is above-mentioned property, can be used for
Multi-color marking, the biosensor of bio-imaging and structure based on graphene quantum dot fluorescence Yu electrogenerated chemiluminescence performance.
The present invention will be described in detail by way of examples below.In following embodiment, graphene is Nanjing Xian Fengna
The commercially available product that the rice material Science and Technology Ltd. trade mark is XF001H.
Embodiment 1
Containing H2SO4And HNO310mL oxidations solution (wherein H2SO4A concentration of 13.25mol/L, HNO3It is a concentration of
The graphene of 10mg is added in three-necked flask 4.03mol/L), and 120min is reacted under uniform stirring, and temperature is controlled at 80 DEG C.Body
System eventually becomes dark brown.Then, 250mL deionized waters are added into reaction system and terminate reaction, and be added in ice bath
It is 7.0 that NaOH, which is neutralized to pH value,.The salt in solution is removed by dialysis, the dialysis bag retention molecular weight used is 1kDa.Pass through
After Rotary Evaporators concentrate dialyzate, use successively molecular cut off for 100,50,30,10 with the super filter tube of 3KDa into
Row separation, obtain molecular weight be (50-100kDa), (30-50kDa), (10-30kDa), (3-10kDa) and<3kDa's
GQDs is respectively labeled as 1-GQDs@(50-100k), 1-GQDs@(30-50k), 1-GQDs@(10-30k), 1-GQDs@(3-
10k) with 1-GQDs@(<3k).
Embodiment 2
Graphene quantum dot is prepared according to the method for embodiment 1, unlike, H2SO4A concentration of 12.88mol/L,
HNO3A concentration of 4.32mol/L.
Be prepared graphene quantum dot 2-GQDs@(50-100k), 2-GQDs@(30-50k), 2-GQDs@(10-30k),
2-GQDs@(3-10k) and 2-GQDs@(<3k).
Embodiment 3
Graphene quantum dot is prepared according to the method for embodiment 1, unlike, H2SO4A concentration of 11.96mol/L,
HNO3A concentration of 5.04mol/L.
Be prepared graphene quantum dot 3-GQDs@(50-100k), 3-GQDs@(30-50k), 3-GQDs@(10-30k),
3-GQDs@(3-10k) and 3-GQDs@(<3k).
Embodiment 4
Graphene quantum dot is prepared according to the method for embodiment 1, unlike, H2SO4A concentration of 13.80mol/L,
HNO3A concentration of 3.60mol/L.
Be prepared graphene quantum dot 4-GQDs@(50-100k), 4-GQDs@(30-50k), 4-GQDs@(10-30k),
4-GQDs@(3-10k) and 4-GQDs@(<3k).
Comparative example 1
Graphene quantum dot is prepared according to the method for embodiment 1, unlike, H2SO4A concentration of 15.04mol/L,
HNO3A concentration of 2.88mol/L.
Be prepared graphene quantum dot D-GQDs@(50-100k), D-GQDs@(30-50k), D-GQDs@(10-30k),
D-GQDs@(3-10k) and D-GQDs@(<3k).
Test case 1
This test case is used to illustrate the relative amount of carbon in graphene quantum dot, nitrogen and oxygen element.
The stone that silent winged generation that science and technology VG Multilab 2000 measure above-described embodiment and comparative example obtains is matched using the U.S.
The x-ray photoelectron spectroscopy of black alkene quantum dot.By the integral area to C 1s and the x-ray photoelectron spectroscopy figure of O 1s into
The relative amount of carbon and oxygen element in graphene quantum dot is calculated in row, acquires ratio (the i.e. oxygen member of oxygen element and carbon
Plain relative amount/carbon relative amount), it is specifically shown in the following table 1.
Table 1
Test case 2
This test case is used to illustrate the photoluminescent property of graphene quantum dot.
The fluorescence radiation situation of the graphene quantum dot obtained in above-described embodiment 2 is measured, Fig. 1 is graphene quantum dot 2-
GQDs@(50-100k), 2-GQDs@(30-50k), 2-GQDs@(10-30k), 2-GQDs@(3-10k) and 2-GQDs@(<3k)
Aqueous solution is in visible light (above) and the picture under 365nm ultraviolet lamps (figure below) irradiation；Fig. 2 is normalized fluorescence emission
Spectrum.
By Fig. 1-2 as can be seen that the graphene quantum dot of the present invention has the ratio of 0.38-0.76 oxygen elements and carbon
Value, wherein the embodiment 1-2 graphene quantum dots in most preferred range of the present invention have the oxygen element and carbon of 0.58-0.71
The ratio of element has more uniform surface oxidation degree, this is the shadow for investigating dimensional effect to graphene quantum dot luminescent properties
Sound provides good material；The fluorescence emission wavelengths of graphene quantum dot can be regulated and controled by grain size, realize unitary excitation
Polynary transmitting is conducive to application of the graphene quantum dot in biomedical imaging and multi-color marking field；The graphite of the present invention
Alkene quantum dot also has abundant oxygen-containing functional group, good water-soluble, regulatable fluorescence property and electrogenerated chemiluminescence
Can, this is conducive to application of the graphene quantum dot in field of biosensors.Above-mentioned property is all substantially better than the stone of comparative example
Black alkene quantum dot.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In the skill of the present invention
In art conception range, technical scheme of the present invention can be carried out a variety of simple variants, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, belongs to
Protection scope of the present invention.
Claims (10)
1. a kind of preparation method of graphene quantum dot, which is characterized in that this method is included under oxidation reaction condition, makes graphite
Alkene carries out oxidation reaction in aoxidizing solution, obtains graphene quantum dot,
Wherein, the oxidation solution contains H2SO4And HNO3, the H aoxidized in solution2SO4A concentration of 10-14mol/L, and
And H2SO4With HNO3Molar ratio be 1：0.20-0.45.
2. preparation method according to claim 1, wherein the H in the oxidation solution2SO4A concentration of 12-14mol/
L, and H2SO4With HNO3Molar ratio be 1：0.30-0.35.
3. preparation method according to claim 1 or 2, wherein this method further includes clicking through obtained graphene quantum
Row ultrafiltration；
Preferably, the use of the molecular cut off of ultrafiltration membrane is 100kDa, 50kDa, 30kDa, 10kDa or 3kDa in the ultrafiltration.
4. preparation method according to claim 1 or 2, wherein the oxidation reaction condition includes：Temperature is 70-90 DEG C,
Time is 20-180min.
5. preparation method according to claim 1 or 2, wherein relative to the graphene of 10mg, use the oxidation of 8-15mL
Solution.
6. preparation method according to claim 1 or 2, wherein this method further includes being terminated anti-after the completion of oxidation reaction
It answers, and it is 6-8 that alkali, which is added, to adjust the pH value of acquired solution；
Preferably, reaction is terminated by the way that deionized water is added, and the pH value that NaOH adjusts acquired solution is added.
7. preparation method according to claim 1 or 2, wherein this method further includes that the solution that will be obtained concentrates.
8. the graphene quantum dot that the preparation method described in any one of claim 1-7 is prepared, wherein the graphite
The ratio of oxygen element and carbon is 0.38-0.76, preferably 0.58-0.71 in alkene quantum dot.
9. graphene quantum dot according to claim 8, wherein the electrogenerated chemiluminescence peak position of the graphene quantum dot
In 450-645nm, it is preferably placed at 528-610nm；
Preferably, the fluorescence emission wavelengths of the graphene quantum dot are 450-630nm, preferably 521-606nm.
10. the graphene quantum dot described in claim 8 or 9 is sent out in bio-imaging, multi-color marking and fluorescence and electroluminescent chemistry
Application in the structure of optical biosensor.
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| CN111384267A (en) * | 2018-12-29 | 2020-07-07 | Tcl集团股份有限公司 | Preparation method of graphene quantum dot film, light-emitting diode and preparation method of light-emitting diode |
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