CN109941988A - A kind of preparation method and application of graphene quantum dot and device or device comprising it - Google Patents
A kind of preparation method and application of graphene quantum dot and device or device comprising it Download PDFInfo
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- CN109941988A CN109941988A CN201910334317.1A CN201910334317A CN109941988A CN 109941988 A CN109941988 A CN 109941988A CN 201910334317 A CN201910334317 A CN 201910334317A CN 109941988 A CN109941988 A CN 109941988A
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Abstract
The present invention provides a kind of preparation method and application of graphene quantum dot and include its device or device.Preparation method of the present invention includes: will be after crystalline flake graphite and strong sulfuric acid response, and nitrate and potassium permanganate is added, and the reaction was continued, after reaction system is diluted with water, hydrogen peroxide is added, gained sediment is graphene quantum dot.For preparation method of the present invention is compared to conventional hydrothermal method, the required reaction time is greatly shortened, and is not necessarily to pyroreaction, reduces the operation difficulty and risk of reaction；Meanwhile reagent dosage needed for preparation method of the present invention is few, post-processing step is easy, is suitable for large-scale production graphene quantum dot.
Description
Technical field
The present invention relates to carbon based material fields, in particular to a kind of preparation method and application of graphene quantum dot
With device or device comprising it.
Background technique
As newest a member of graphene family, zero dimension graphene quantum dot (Graphene quantum dot, GQDs)
Other than the excellent properties with common graphite alkene material, due to its size in 10nm hereinafter, thus have stronger quantum limit
Domain effect and boundary effect, and a series of new characteristics can be shown.Graphene quantum dot is in solar energy electrical part, biology
There is more extensive application prospect in the fields such as medicine, light emitting diode and sensor.
GQDs is increasingly becoming the hot spot of each field scientist concern in recent years, but its development is still in infancy, synthesis
Technique is also just to start to be furtherd investigate for nearly 1 year.The synthetic method of GQDs mainly has hydro-thermal method, electrochemical process and change
Learn removing carbon fiber method etc..Hydro-thermal method is to prepare a kind of method more common in GQDs, and technique generally divides three steps: will aoxidize stone
Black alkene (GO) vacuum-thermal reduction is graphene nanometer sheet (Graphene nanosheets, GNSs), then in the concentrated sulfuric acid and concentrated nitric acid
Middle oxidation GNSs, the GNSs after oxidation are restored under thermal and hydric environment, obtain graphene quantum dot.
For other synthetic methods, the yield that hydro-thermal method prepares graphene quantum dot is higher.However, hydro-thermal method
It is disadvantageous in that, this method is carried out based on raw material GO and its reduzate, this not only needs to be oxidized a large amount of graphite
Powder also needs to carry out the redox reaction of a series of complex, and reduction process generally also needs to add to obtain GO
A large amount of reagent simultaneously expends time a couple of days.
In view of this, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of preparation method of graphene quantum dot, in preparation method of the present invention,
Using crystalline flake graphite as raw material, without carrying out graphene oxide reduction, can effectively shorten the reaction time, reduce reaction examination
The use of agent.
The second object of the present invention is to provide one kind by the obtained graphene quantum dot of preparation method of the present invention.
The third object of the present invention is to provide a kind of application of graphene quantum dot of the present invention, and includes stone of the present invention
The device or device of black alkene quantum dot.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
A kind of preparation method of graphene quantum dot, comprising: after crystalline flake graphite and strong sulfuric acid response, will be added nitrate and
The reaction was continued for potassium permanganate, after reaction system is diluted with water, hydrogen peroxide is added, gained sediment is graphene quantum dot；It is preferred that
, the nitrate includes at least one of potassium nitrate and sodium nitrate.
Preferably, in preparation method of the present invention, the ratio between quality grams and the volume ml of the concentrated sulfuric acid of crystalline flake graphite are
(0.8-2): 50；And/or the reaction time of crystalline flake graphite and the concentrated sulfuric acid is 25-35min.
Preferably, in preparation method of the present invention, the ratio between quality grams of crystalline flake graphite and nitrate is (0.8-2): (1-
2)；And/or the ratio between quality grams of crystalline flake graphite and potassium permanganate is (0.8-2): (5-8).
Preferably, in preparation method of the present invention, the reaction was continued includes: in ice bath item for the addition nitrate and potassium permanganate
Under part, nitrate and potassium permanganate reaction is added, is then transferred in water-bath and is reacted；It is furthermore preferred that potassium permanganate is point
Batch charge.
Preferably, in preparation method of the present invention, the reaction time under condition of ice bath is 1-3h；And/or water-bath
Temperature is 30-40 DEG C, and the time reacted in water-bath is 12-24h.
Preferably, in preparation method of the present invention, it includes: under condition of ice bath, to reaction that the reaction system, which is diluted with water,
System is once diluted with water, and after heating reaction, carries out secondary be diluted with water；It is furthermore preferred that being once diluted with water water used
The ratio between volume ml and the volume ml of the concentrated sulfuric acid be (1.1-1.5): 1；It is furthermore preferred that secondary be diluted with water water used
The ratio between volume ml and the volume ml of the concentrated sulfuric acid be (1-1.2): 1.
Preferably, in preparation method of the present invention, the heating reaction includes: to turn the reaction system after being once diluted with water
Move to progress heating stirring reaction in water-bath；It is furthermore preferred that the temperature of heating reaction is 80-90 DEG C, the time for heating reaction is
10-30min。
Further, the present invention also provides the graphene quantum dots obtained by the preparation method.
Likewise, the application the present invention also provides graphene quantum dot of the present invention in device or device preparation.
Meanwhile present invention provides devices or device comprising graphene quantum dot of the present invention.
For conventional hydrothermal method, the reaction time needed for preparation method of the present invention is greatly shortened, and is not necessarily to high temperature
Reaction, reduces the operation difficulty and risk of reaction；
Meanwhile reagent dosage needed for preparation method of the present invention is few, post-processing step is easy, is suitable for large-scale production graphene
Quantum dot.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described.
Fig. 1 is the XRD and Raman detection figure of graphene quantum dot prepared by embodiment 1；
Fig. 2 is the high power transmission electron microscope picture of graphene quantum dot prepared by embodiment 1；
Wherein, in Fig. 1, (a) is that the XRD of graphene quantum dot prepared by embodiment 1 detects figure；
It (b) is the Raman detection figure of graphene quantum dot prepared by embodiment 1.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Prepare shortcoming present in graphene quantum dot in view of existing hydro-thermal method, the present invention provides one kind to
Prepare the new method of graphene quantum dot.
Preparation method provided by the present invention is to prepare graphene quantum dot by raw material of crystalline flake graphite.In the prior art
In, the preparation of graphene quantum dot mostly using graphene oxide as raw material (for details, reference can be made to CN102807209A etc.), also has with richness
It strangles alkene (for details, reference can be made to CN104211050A) and is attempted to the related preparation that coal (for details, reference can be made to CN103803540A) is raw material.
However, the correlative study for preparing graphene quantum dot using this lamellar graphite of crystalline flake graphite as raw material is actually rare.Therefore, originally
The it is proposed of invention, can not only solve conventional hydrothermal method prepare graphene quantum dot it is existing reaction step it is more, when reacting
Between the consumption of long, reagent it is more the problems such as, while completely newly trying and exploring also for graphene quantum dot preparation.
Specifically, preparation method of the present invention includes the following steps:
(a) crystalline flake graphite is added in reaction vessel (such as beaker etc.), the concentrated sulfuric acid is then added, stirs under normal temperature conditions
Mix reaction；
Preferably, in this step, the concentrated sulfuric acid used is the concentrated sulfuric acid of concentration 98wt.%；
Preferably, in this step, the ratio between quality grams and the volume ml of the concentrated sulfuric acid of crystalline flake graphite are (0.8-2):
50, the mass volume ratio of two kinds of raw materials can be, but be not limited to 1:50,1.2:50,1.5:50 or 1.8:50 etc..
Preferably, in this step, the normal temperature condition is 15-35 DEG C and is stirred to react under room temperature.
Preferably, in this step, the time being stirred to react is 25-35min, and mixing time for example can be, but be not limited to,
27,30 or 32min etc..
(b) step (a) reaction vessel is transferred in ice bath, nitrate and potassium permanganate is added under agitation, it is former
After the completion of material is added, the reaction was continued under condition of ice bath；
In certain embodiments of the present invention, the nitrate is one or both of potassium nitrate and sodium nitrate.
In certain embodiments of the present invention, the ratio between quality grams of crystalline flake graphite and nitrate is (0.8-2): (1-
2)；
Preferably, in this step, the ratio between quality grams of crystalline flake graphite and nitrate is (1-1.5): (1-1.5)；
It is furthermore preferred that the ratio between quality grams of crystalline flake graphite and nitrate is (1.2-1.3): (1.4- in this step
1.5)。
In certain embodiments of the present invention, in this step, nitrate is primary charging.
In certain embodiments of the present invention, the ratio between quality grams of crystalline flake graphite and potassium permanganate is (0.8-2):
(5-8)；
Preferably, in this step, the ratio between quality grams of crystalline flake graphite and potassium permanganate is (1-1.5): (6-7)；
It is furthermore preferred that the ratio between quality grams of crystalline flake graphite and nitrate is (1.2-1.3): (6-7) in this step.
In certain embodiments of the present invention, in this step, potassium permanganate is to be added in batches, for example, potassium permanganate
It can divide 3-5 times and be added portionwise, be divided into 8-15min between each feed time, optional each feeding quantity is identical or not
Together；
Preferably, in this step, for potassium permanganate for point 5 additions, the interval time to feed every time is 10min, is added every time
Doses is identical.
In certain embodiments of the present invention, in this step, after the completion of nitrate and potassium permanganate feed, it is also necessary to
The reaction was continued under condition of ice bath 1-3h (such as 1.5,2 or 2.5h etc.).
(c) reaction vessel after reacting under step (b) condition of ice bath is transferred in water-bath, continues to be stirred to react.
In certain embodiments of the present invention, the temperature of heating water bath is 30-40 DEG C, such as can be, but be not limited to
32,35,37 or 39 DEG C etc.；
The time reacted in water-bath is 12-24h, such as can be, but be not limited to 15,18 or 21h etc..
(d) reaction vessel after reacting under step (c) water bath condition is transferred in ice bath, then under agitation,
Add water (preferably distilled water) into reaction vessel, reaction system is once diluted with water；It, will be anti-after the completion of being diluted with water
It answers container to be again transferred in water-bath, carries out heating stirring reaction；
In certain embodiments of the present invention, volume ml and step (a) Central Plains of water used are once diluted with water
Expect that the ratio between volume ml of the concentrated sulfuric acid is (1.1-1.5): 1 (such as can be, but be not limited to 1.2:1,1.3:1 or 1.4:
1 etc.)；
In certain embodiments of the present invention, the temperature of heating reaction (water-bath), which is 80-90 DEG C, (such as can be but not
Be limited to 82,85,87 or 89 DEG C etc.), heat reaction time be 10-30min (such as can be, but be not limited to 15,20, or
Person 25min etc.).
(e) reaction vessel after step (d) reaction is taken out from water-bath, is placed in 20-25 DEG C of room temperature condition, then
Under agitation, add water (preferably distilled water) again into reaction vessel, carry out secondary is diluted with water；It is secondary to be diluted with water
After the completion, hydrogen peroxide is added into reaction vessel, will appear golden yellow precipitate object in reaction system, is product graphene quantum
Point；
Further, also purified to product graphene quantum dot by the method for dialysis.
In certain embodiments of the present invention, the secondary volume ml for being diluted with water water used and step (a) Central Plains
Expect that the ratio between volume ml of the concentrated sulfuric acid is (1-1.2): 1 (such as can be, but be not limited to 1.1:1 etc.).
In certain embodiments of the present invention, the concentration of hydrogen peroxide used is 10-35% (m/m)；Preferably, used double
The concentration of oxygen water is 15-30%；It is furthermore preferred that the concentration of hydrogen peroxide used is 20-25%.
In currently preferred some embodiments, the preparation step of graphene quantum dot be may be summarized as follows:
After crystalline flake graphite and the concentrated sulfuric acid are stirred to react 25-35min, reaction system is transferred in ice bath, nitric acid is added
Salt and potassium permanganate, and 1-3h is stirred to react under condition of ice bath；
Then, reaction system is transferred in 30-40 DEG C of water-bath, is stirred to react 12-24h；
Then, reaction system is again transferred in ice bath, is once diluted with water, it, will be anti-after the completion of being diluted with water
Container is answered to be again transferred in 80-90 DEG C of water-bath, heating stirring reacts 10-30min；
Then, reaction system is transferred in normal temperature environment, progress is secondary to be diluted with water, and it is anti-that hydrogen peroxide stirring is then added
It answers, generates and be precipitated as product graphene quantum dot.
The feature of the graphene quantum dot obtained by as above method of the invention is obvious, and crystal form is complete, as shown in Figure 1, product
Graphene quantum dot has strong diffraction maximum in 2 θ=26.5 ° or so, and Raman spectrum is in 1350cm-1Nearby there is the obvious peak D, quantum dot
Partial size in 12nm or so.
Further, can also using the graphene quantum dot prepared by the present invention as raw material, for solar energy luminous device,
The preparation of the devices such as biology/medicine detection probe, light emitting diode and sensor or device.
Embodiment 1
(1) it takes 1.2g crystalline flake graphite to be put into 500 milliliters of beakers, the 50ml concentrated sulfuric acid, room temperature magnetic agitation 30min is added.
(2) have in the bucket of ice cube in placing the beaker, be placed on magnetic stirring apparatus, keep ice bath stirring, 1.5g is added
Sodium nitrate；Divide 5 addition potassium permanganate, be added within every 10 minutes once, 1.2g is added every time, and (control reaction temperature is no more than 3
℃)；Ice bath stirring is kept, is reacted 2 hours.
(3) beaker is taken out, is placed into heat collecting type water-bath, under 35 DEG C of water bath conditions, is stirred to react 24 hours.
(4) ice bath state is kept, 70ml distilled water is added into beaker and (is slowly added dropwise, temperature of charge is kept to be no more than
50 DEG C), beaker is again placed in heat collecting type water-bath after the completion of dilution, under 85 DEG C of water bath conditions, is stirred to react 15 minutes.
(5) beaker is taken out, the dilution of 50ml distilled water is added thereto again, 30% hydrogen peroxide is finally added dropwise into beaker
Solution, until no longer generating golden yellow precipitate.
Gained precipitating, as product graphene quantum dot are collected, prepared graphene quantum spot diameter is 12nm or so.
As shown in Figure 1, product graphene quantum dot has strong diffraction maximum in 2 θ=9 ° or so, Raman spectrum is in 1350cm-1Nearby occur bright
The aobvious peak D；
Meanwhile the high power transmission electron microscope picture of gained graphene quantum dot is as shown in Figure 2.
Embodiment 2
(1) it takes 2g crystalline flake graphite to be put into 500 milliliters of beakers, the 50ml concentrated sulfuric acid, room temperature magnetic agitation 30min is added.
(2) have in the bucket of ice cube in placing the beaker, be placed on magnetic stirring apparatus, keep ice bath stirring, 2g nitre is added
Sour sodium, point 5 times every 10 minutes addition 1.5g potassium permanganate；Ice bath stirring is kept, is reacted 2 hours.
(3) beaker is taken out, is placed into heat collecting type water-bath, under 35 DEG C of water bath conditions, is stirred to react 24 hours.
(4) ice bath state is kept, 70ml distilled water is added into beaker, beaker is again placed in heat collecting type after the completion of dilution
In water-bath, under 85 DEG C of water bath conditions, it is stirred to react 15 minutes.
(5) beaker is taken out, the dilution of 50ml distilled water is added thereto again, 30% hydrogen peroxide is finally added dropwise into beaker
Solution, until no longer generating golden yellow precipitate.
Embodiment 3
(1) it takes 1.2g crystalline flake graphite to be put into 500 milliliters of beakers, the 50ml concentrated sulfuric acid, room temperature magnetic agitation 30min is added.
(2) have in the bucket of ice cube in placing the beaker, be placed on magnetic stirring apparatus, keep ice bath stirring, 1.5g is added
Sodium nitrate, point 5 times every 10 minutes addition 1.2g potassium permanganate；Ice bath stirring is kept, is reacted 2 hours.
(3) beaker is taken out, is placed into heat collecting type water-bath, under 45 DEG C of water bath conditions, is stirred to react 24 hours.
(4) ice bath state is kept, 70ml distilled water is added into beaker, beaker is again placed in heat collecting type after the completion of dilution
In water-bath, under 80 DEG C of water bath conditions, it is stirred to react 15 minutes.
(5) beaker is taken out, the dilution of 50ml distilled water is added thereto again, 30% hydrogen peroxide is finally added dropwise into beaker
Solution, until no longer generating golden yellow precipitate.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from of the invention
Many other change and modification can be made in the case where spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of preparation method of graphene quantum dot characterized by comprising
After crystalline flake graphite and strong sulfuric acid response, the reaction was continued for addition nitrate and potassium permanganate, after reaction system is diluted with water,
Hydrogen peroxide is added, gained sediment is graphene quantum dot；
Preferably, the nitrate includes: at least one of potassium nitrate and sodium nitrate.
2. preparation method according to claim 1, which is characterized in that the quality grams of crystalline flake graphite and the volume of the concentrated sulfuric acid
Ml the ratio between be (0.8-2): 50；
And/or the reaction time of crystalline flake graphite and the concentrated sulfuric acid is 25-35min.
3. preparation method according to claim 1, which is characterized in that the ratio between crystalline flake graphite and the quality grams of nitrate are
(0.8-2): (1-2)；
And/or the ratio between quality grams of crystalline flake graphite and potassium permanganate is (0.8-2): (5-8).
4. preparation method according to claim 1, which is characterized in that the reaction was continued for the addition nitrate and potassium permanganate
Include:
System after crystalline flake graphite and strong sulfuric acid response is transferred in ice bath, nitrate and potassium permanganate reaction is added, then turns
Move in water-bath that the reaction was continued；
Preferably, potassium permanganate is to feed in batches.
5. the preparation method according to claim 4, which is characterized in that the reaction time under condition of ice bath is 1-3h；
And/or the temperature of water-bath is 30-40 DEG C, the time reacted in water-bath is 12-24h.
6. preparation method according to claim 1, which is characterized in that the reaction system, which is diluted with water, includes:
Under condition of ice bath, reaction system is once diluted with water, after heating reaction, reaction system is carried out at normal temperature
It is secondary to be diluted with water；
Preferably, the ratio between the volume ml of water used in being once diluted with water and the volume ml of the concentrated sulfuric acid are (1.1-1.5):
1；
Preferably, the ratio between the secondary volume ml for being diluted with water water used and the volume ml of the concentrated sulfuric acid are (1-1.2): 1.
7. preparation method according to claim 6, which is characterized in that the heating, which is reacted, includes:
Reaction system after being once diluted with water is transferred to progress heating stirring reaction in water-bath；
Preferably, the temperature for heating reaction is 80-90 DEG C, and the time for heating reaction is 10-30min.
8. the graphene quantum dot obtained by preparation method of any of claims 1-7.
9. application of the graphene quantum dot according to any one of claims 8 in device or device preparation.
10. device or device comprising graphene quantum dot described in claim 8.
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| CN106744913A (en) * | 2017-03-28 | 2017-05-31 | 上海理工大学 | A kind of method that utilization cryptocrystalline graphite largely prepares graphene oxide quantum dot |
| CN107033885A (en) * | 2017-04-18 | 2017-08-11 | 南昌航空大学 | A kind of preparation method of graphene quantum dot and its utilization in photoluminescent diode |
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| CN102660270A (en) * | 2012-05-03 | 2012-09-12 | 吉林大学 | Method for preparing fluorescent graphene quantum dots by solvothermal method |
| KR20130123477A (en) * | 2012-05-03 | 2013-11-13 | 한국에너지기술연구원 | Method of manufacturing coating agent of dye-sensitive solar cell surface, coating agent thereof and dye-sensitive solar cell coated with coating agent |
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| CN104261386A (en) * | 2014-10-15 | 2015-01-07 | 中国人民解放军防化学院 | Method for preparing carbon dots with hydrothermal process on basis of plant leaves |
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