CN107117600B - A method of graphene quantum dot is prepared using 3D graphene as raw material - Google Patents
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- CN107117600B CN107117600B CN201710361600.4A CN201710361600A CN107117600B CN 107117600 B CN107117600 B CN 107117600B CN 201710361600 A CN201710361600 A CN 201710361600A CN 107117600 B CN107117600 B CN 107117600B
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Abstract
The present invention discloses one kind using 3D graphene as raw material, has the method for the graphene quantum dot of fluorescence property by solvent-thermal method preparation.Specifically includes the following steps: a) using CVD method to prepare 3D graphene under the high temperature conditions using tube furnace；B) in ethanol by the dispersion of 3D graphene powder, and a certain amount of lye is added, after ultrasonic dissolution, is put into reaction kettle and seals, under the high temperature conditions reaction a period of time；C) it is cooled to room temperature, collects filtrate after vacuum filtration, filtrate is dialysed in the bag filter of certain molecular cut off to neutrality, fluorescence graphene quantum dot is obtained.Preparation method simple process provided by the invention, easily operated, at low cost and environmentally friendly, obtained graphene quantum dot purity and yield is higher, has good dispersibility and stability and fluorescence intensity is high.There is potential application prospect in fields such as lithium ion battery, photocatalysis.
Description
Technical field
The present invention relates to a kind of methods for preparing graphene quantum dot as raw material using 3D graphene, belong to nano material technology
Field.
Background technique
With the development of science and technology, semiconductor-quantum-point is in biomedical imaging, medical diagnosis on disease, bio-sensing etc.
It is widely used in research.However, its heavy metal component contained is more toxic, to limit semiconductor-quantum-point
From zoopery to the conversion of clinical application.As the newcomer of graphene family, graphene quantum dot (Graphene
Quantum dots, GQDs), in addition to the excellent properties with graphene, also show because of quantum limitation effect and boundary effect
A series of new characteristics out obtain the extensive concern of each field scientist such as chemistry, physics, material and biology.
The research of GQDs starts from recent years, it has been found that two-dimensional graphene is passed through the means of some physics, chemistry
When being cut into zero-dimension structural, property not available for many two-dimensional structures is showed, this has also evoked both at home and abroad again
Research enthusiasm of the scientist for zero dimensional nanometer materials.Compared with traditional semiconductor-quantum-point and organic dyestuff, GQDs has
Highly-water-soluble, extensive chemical stability are easy to functionalization, anti-light Bleachability and excellent biological nature, good bio-compatible
Property, there is potential application prospect in biomedicine (bio-imaging, bio-sensing, drug delivery etc.).
Currently, the report for preparing graphene quantum dot using 3D graphene as raw material is also seldom.Ananthanarayanan etc.
People (" Facile Synthesis of Graphene Quantum Dots from 3D Graphene and their
Application for Fe3+ Sensing”Adv. Funct. Mater. 2014, 24, 3021-3026) and it reports for the first time
The 3D graphene prepared using CVD method prepares graphene quantum dot as raw material.They are by electrochemical stripping method, in ionic liquid
Effect, successfully obtain fluorescence graphene quantum dot, and be applied to Fe3+Specific detection.(" the One-step such as Zhu
synthesis of graphene quantum dots from defective CVD graphene and their
Application in IGZO UV thin film phototransistor " Carbon. 2016,100,20-207) benefit
Preparing graphene (non-3D graphene) with CVD method is raw material, prepares graphene quantum dot using ultrasonic method.Pass through above method
The graphene quantum dot with fluorescence property can successfully be prepared, but still remain the reaction time is long, experimentation is cumbersome,
The disadvantages of severe reaction conditions and expensive reaction reagent.The yield and fluorescence efficiency of graphene quantum dot prepared by existing report are still
It is so lower, also significantly limit its industrialized production and application.Therefore, it develops a kind of simple and environmentally-friendly and can be applied to
The method of large-scale production graphene quantum dot is still a challenge.
Summary of the invention
The purpose of the present invention is overcoming the shortcoming of the above method, a kind of simple and fast, Environmental Safety, high yield are provided
Graphene quantum dot production method.
Realization that the present invention adopts the following technical solutions: a kind of to prepare graphene quantum dot using 3D graphene as raw material
Method prepares graphene quantum dot as raw material, using solvent-thermal method using 3D graphene, comprising the following steps:
(1) preparation of 3D graphene:
Foam nickel base is cut to 50 × 50 mm first2Square, and it is each super in dehydrated alcohol and deionized water respectively
Sound cleans 30 min, with the greasy dirt for the nickel surface that defoams；The nickel foam that cleaning finishes is placed in vacuum tube furnace flat-temperature zone to exist
It is heated to 1000 DEG C in 500 sccm argon gas, 200 sccm atmosphere of hydrogen, gas flow and temperature-resistant 10 min are kept, to go
The oxide layer of foam-expelling nickel surface；Keep temperature and hydrogen argon flow constant later, after being passed through 10 min of methane gas holding
Stopping is passed through methane, then is cooled to room temperature with the cooling rate of 100-200 DEG C/min, closes all gas, can obtain 3D graphite
Alkene/nickel foam composite material.Finally by 3D graphene/foam nickel composite material two hours in 4M nitric acid solution, after taking-up
It is cleaned up with deionized water, obtains the 3D graphene for washing nickel foam；
(2) preparation of graphene quantum dot:
A. the 3D graphene powder that step (1) obtains is dispersed in alcohols solvent, dispersion liquid is made, configures to obtain
Dispersion liquid in 3D graphene concentration be 10 ~ 30 mg/L；100 ~ 500 mg/L sodium hydroxides are added into the dispersion liquid again,
Ultrasound, which mixes, is made mixed liquor；
B. the obtained mixed liquor of step A is uniformly transferred in reaction kettle by graduated cylinder, is sealed；Being placed on temperature is
6 ~ 24 h are reacted in 100 ~ 200 DEG C of baking oven, are cooled to room temperature, are collected after vacuum filtration and obtain flaxen filtrate；
C. the filtrate that step B is obtained dialysis in the bag filter that molecular cut off is 8000 ~ 14000 Da is removed to neutrality
Extra basic ion is removed, graphene quantum dot dispersion is obtained, obtains graphene quantum dot powder after dry.
Alcohols solvent described in the A of step (2) of the present invention can be dehydrated alcohol, can better disperse 3D Graphene powder
End；Sodium hydroxide saturated aqueous solution is less than spacing between graphene layer, can be effectively performed as saturation lye, ion size
Intercalation and removing.
Reaction kettle described in the B of step (2) of the present invention is polytetrafluoroethyllining lining reaction kettle；Used in the vacuum filtration
Filter membrane be organic filter membrane, aperture be 0.45 um, the complete residue of unreacted can be removed.
Dialysis time is 3 ~ 4 days in the C of step (2) of the present invention, until it is neutral, remove effectively extra basic ion.
It is -40 DEG C that drying means described in the C of step (2) of the present invention, which is in temperature, under conditions of air pressure is 20 Pa
Freeze-drying, obtains solid graphene quantum dot powder.
Compared with the prior art, the present invention has the following advantages:
1. the present invention prepares graphene quantum dot using solvent-thermal method, required ethyl alcohol and sodium hydroxide are all convenient in the market
The raw material being easy to get, and can effectively disperse and remove 3D graphene powder, graphene quantum dot purity obtained and production
Rate is relatively high, and has good dispersibility, water-soluble and stable fluorescence property.
2. production method of the present invention is environmentally protective, required experimental facilities is easy to operate, and production cost is low and the period is short,
There is potential application prospect in the fields such as lithium ion battery, micro super capacitor, bio-imaging and solar battery, it is expected to real
Existing industrial mass production.
Detailed description of the invention
Fig. 1 is the high resolution transmission electron microscopy piece of graphene quantum dot prepared by embodiment 1.
Fluorescence spectra under the different excitation wavelengths for the graphene quantum dot that Fig. 2 is prepared for embodiment 1.
Fig. 3 is the Raman spectrogram of graphene quantum dot prepared by embodiment 1.
Fig. 4 is the X-ray diffractogram of graphene quantum dot prepared by embodiment 1.
Fig. 5 is the ultraviolet-visible absorption spectroscopy figure of graphene quantum dot prepared by embodiment 1.
Fig. 6 is the Fourier transform infrared spectroscopy figure of graphene quantum dot prepared by embodiment 1.
Specific embodiment
Combined with specific embodiments below, technical solution of the present invention is furtherd elucidate.It is worth mentioning that below
Involved 3D graphene powder is all in embodiment 1 prepared by the preparation method of 3D graphene powder in all embodiments.
Embodiment 1:
(1) preparation of 3D graphene powder
Foam nickel base is cut to 50 × 50 mm first2Square, and it is each super in dehydrated alcohol and deionized water respectively
Sound cleans 30 min, with the greasy dirt for the nickel surface that defoams；The nickel foam that cleaning finishes is placed in vacuum tube furnace flat-temperature zone to exist
It is heated to 1000 DEG C in 500 sccm argon gas, 200 sccm atmosphere of hydrogen, gas flow and temperature-resistant 10 min are kept, to go
The oxide layer of foam-expelling nickel surface；Keep temperature and hydrogen argon flow constant later, after being passed through 10 min of methane gas holding
Stopping is passed through methane, then is cooled to room temperature with the cooling rate of 100-200 DEG C/min, closes all gas, can obtain 3D graphite
Alkene/nickel foam composite material.Finally by 3D graphene/foam nickel composite material two hours in 4M nitric acid solution, after taking-up
It is cleaned up with deionized water, obtains the 3D graphene for washing nickel foam.
(2) preparation of graphene quantum dot
1 mg of 3D graphene powder in step (1) is distributed in 50 mL ethanol solutions, 20 mg hydrogen-oxygens are added
Change sodium, 5 min of ultrasonic mixing.Solution will be mixed to be transferred in reaction kettle, seal, be put into baking oven, be warming up to 180 DEG C, maintain
10 h, cooled to room temperature.It will treated that dispersion liquid filters collection by vacuum obtains pale yellow filtrate.Filtrate is packed into
It dialyses in the bag filter of 10000 Da, until neutral.Obtained dialyzate is freezed, is later -40 DEG C in temperature, air pressure is
Graphene quantum dot powder is freeze-dried to obtain under conditions of 20 Pa.
Fig. 1 is the high resolution TEM picture for the graphene quantum dot that embodiment 1 obtains, as can be seen from the figure
To quantum dot size be mainly distributed on 5 ~ 9 nm, interplanar distance is 0.21 nm.Fig. 2 is the graphene quantum that embodiment 1 obtains
The fluorescence spectra of point, it can be seen that with the variation of excitation wavelength, the launch wavelength of graphene quantum dot is also changing, explanation
The fluorescence emission spectrum of graphene quantum dot has wavelength dependency.Fig. 3 is the drawing for the graphene quantum dot that embodiment 1 obtains
Graceful spectrogram, ID/IG ratio is 0.42 as seen from the figure, illustrates graphene quantum dot degree of graphitization with higher.Fig. 4 is real
Apply the X-ray diffractogram for the graphene quantum dot that example 1 obtains, it is known that graphene quantum dot has a spike in 2 θ=28.1 °, according to
The spacing of lattice of lamella known to Bragg equation 2dsin θ=n λ is 0.32 nm.Fig. 5 is the graphene quantum that embodiment 1 obtains
The ultraviolet-visible absorption spectroscopy figure of point, it can be seen that absorption peak appears in 262 and 304 nm in figure.Fig. 6 is what embodiment 1 obtained
The Fourier transform infrared spectroscopy figure of graphene quantum dot, by figure it can be observed that C-O-C(1145 cm-1), C-OH(1380
cm-1) ,-C=O(1628 cm-1) stretching vibration peak, and-OH(3410 cm-1) stretching vibration peak, illustrate graphene quantum dot table
Face oxygen-containing functional group rich in.
Embodiment 2
The 3D graphene powder that (1) the step of 1.5mg embodiment 1 obtains is distributed in 50 mL ethanol solutions, is added
Enter 10 mg sodium hydroxides, 5 min of ultrasonic mixing.The solution of mixing is transferred in reaction kettle, seals, is put into baking oven, is heated up
To 200 DEG C, 9 h, cooled to room temperature are maintained.Treated dispersion liquid by being filtered by vacuum to collect is obtained into faint yellow filter
Liquid.Filtrate is fitted into 10000 Da bag filters and is dialysed, until neutral.Obtained dialyzate is freezed, is later -40 in temperature
DEG C, freeze-drying obtains solid graphite alkene quantum dot under conditions of air pressure is 20 Pa.
Embodiment 3
It disperses the 3D graphene powder that (1) the step of 0.5 mg embodiment 1 obtains in 30 mL ethanol solutions,
15 mg sodium hydroxides, 5 min of ultrasonic mixing is added.The dispersion liquid of mixing is transferred in reaction kettle, seals, is put into baking oven,
120 DEG C are warming up to, 12 h, cooled to room temperature are maintained.Will treated dispersion liquid by be filtered by vacuum collect obtain it is yellowish
Color filtrate.Filtrate is fitted into 10000 Da bag filters, until neutral.Obtained dialyzate is freezed, is later -40 in temperature
DEG C, freeze-drying obtains solid graphite alkene quantum dot under conditions of air pressure is 20 Pa.
Embodiment 4
It disperses the 3D graphene powder that (1) the step of 1 mg embodiment 1 obtains in 40 mL ethanol solutions, adds
Enter 12 mg sodium hydroxides, 5 min of ultrasonic mixing.The solution of mixing is transferred in reaction kettle, seals, is put into baking oven, is heated up
To 100 DEG C, 20 h, cooled to room temperature are maintained.Treated dispersion liquid by being filtered by vacuum to collect is obtained into faint yellow filter
Liquid.Filtrate is fitted into 10000 Da bag filters and is dialysed, until neutral.Obtained dialyzate is freezed, is later -40 in temperature
DEG C, freeze-drying obtains solid graphite alkene quantum dot under conditions of air pressure is 20 Pa.
Above embodiments merely illustrate several ways of the invention, are served only for further having done in detail the technical solution
Elaboration, not invention is imposed any restrictions, it is noted that those skilled in the art is not departing from present inventive concept
Under the premise of, the nonessential modifications and adaptations made belong to the protection scope of technical solution of the present invention.
Claims (5)
1. a kind of method for preparing graphene quantum dot as raw material using 3D graphene, which comprises the following steps:
(1) preparation of 3D graphene:
Foam nickel base is cut to 50 × 50 mm first2Square, and each ultrasound is clear in dehydrated alcohol and deionized water respectively
30 min are washed, with the greasy dirt for the nickel surface that defoams；The nickel foam that cleaning finishes is placed in vacuum tube furnace flat-temperature zone 500
It is heated to 1000 DEG C in sccm argon gas, 200 sccm atmosphere of hydrogen, gas flow and temperature-resistant 10 min are kept, to go de-bubble
The oxide layer of foam nickel surface；It keeps temperature and hydrogen and argon flow constant later, is passed through after methane gas keeps 10 min and stops
Only be passed through methane, then be cooled to room temperature with the cooling rate of 100-200 DEG C/min, close all gas, can obtain 3D graphene/
The composite material of nickel foam；Finally 3D graphene/foam nickel composite material is placed two hours in 4M nitric acid solution, after taking-up
It is cleaned up with deionized water, obtains the 3D graphene for washing nickel foam；
(2) preparation of graphene quantum dot:
A. dispersion liquid, the dispersion liquid configured is made in alcohols solvent in 3D graphene dispersion step (1) obtained
The concentration of middle 3D graphene is 10 ~ 30 mg/L；100 ~ 500 mg/L sodium hydroxides are added into the dispersion liquid again, ultrasound mixes
Mixed liquor is made；
B. the obtained mixed liquor of step A is uniformly transferred in reaction kettle by graduated cylinder, is sealed；Be placed on temperature be 100 ~
6 ~ 24 h are reacted in 200 DEG C of baking oven, are cooled to room temperature, are collected after vacuum filtration and obtain flaxen filtrate；
C. the filtrate that step B is obtained dialysis in the bag filter that molecular cut off is 8000 ~ 14000 Da removes more to neutrality
Remaining basic ion obtains graphene quantum dot dispersion, obtains solid graphite alkene quantum dot after dry.
2. according to a kind of method for preparing graphene quantum dot as raw material using 3D graphene described in claim 1, it is characterised in that:
Alcohols solvent described in the A of step (2) is dehydrated alcohol, can better disperse 3D graphene powder.
3. a kind of method for preparing graphene quantum dot as raw material using 3D graphene according to claim 1, feature exist
In: reaction kettle described in the B of step (2) is polytetrafluoroethyllining lining reaction kettle；Filter membrane used in the vacuum filtration is to have
Machine filter film, aperture are 0.45 um, can remove the complete residue of unreacted.
4. a kind of method for preparing graphene quantum dot as raw material using 3D graphene according to claim 1 or 2, feature
Be: dialysis time is 3 ~ 4 days in the C of step (2), until it is neutral, remove effectively extra basic ion.
5. a kind of method for preparing graphene quantum dot as raw material using 3D graphene according to claim 1 or 2, feature
Be: it is -40 DEG C that drying means described in the C of step (2), which is in temperature, and air pressure is freeze-dried under conditions of being 20 Pa, is obtained
To solid graphene quantum dot powder.
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| CN108855040A (en) * | 2018-06-29 | 2018-11-23 | 江苏弗瑞仕环保科技有限公司 | The preparation method of the Dy doping ZnO catalysis material of modified by graphene quantum dot |
| US11718531B2 (en) * | 2018-09-07 | 2023-08-08 | Dxome Co., Ltd. | Method for producing graphene quantum dots |
| CN109650382B (en) * | 2019-02-27 | 2020-05-05 | 厦门理工学院 | Large-size graphene and preparation method thereof |
| CN109704313A (en) * | 2019-03-06 | 2019-05-03 | 泉州师范学院 | A kind of high efficiency preparation method of hyperfluorescence graphene quantum dot |
| CN109971470A (en) * | 2019-03-19 | 2019-07-05 | 集美大学 | A method of preparing nitrogen, sulphur, phosphorus, chlorine co-doped graphene quantum dot |
| CN110197909B (en) * | 2019-06-17 | 2021-05-25 | 中国科学院大连化学物理研究所 | Nickel-iron catalytic material, preparation method thereof and application thereof in hydrogen production by electrolyzing water and preparation of liquid solar fuel |
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| CN102674321B (en) * | 2011-03-10 | 2015-02-25 | 中国科学院金属研究所 | Graphene foam with three dimensional fully connected network and macroscopic quantity preparation method thereof |
| CN102660270A (en) * | 2012-05-03 | 2012-09-12 | 吉林大学 | Method for preparing fluorescent graphene quantum dots by solvothermal method |
| CN102807209B (en) * | 2012-08-02 | 2014-04-16 | 清华大学 | Method for preparing graphene quantum dots |
| US9688540B2 (en) * | 2013-01-15 | 2017-06-27 | Solan, LLC | Segmented graphene growth on surfaces of a patterned substrate layer and devices thereof |
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