CN109941988B - Preparation method and application of graphene quantum dots, and device or apparatus containing graphene quantum dots - Google Patents
Preparation method and application of graphene quantum dots, and device or apparatus containing graphene quantum dots Download PDFInfo
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- CN109941988B CN109941988B CN201910334317.1A CN201910334317A CN109941988B CN 109941988 B CN109941988 B CN 109941988B CN 201910334317 A CN201910334317 A CN 201910334317A CN 109941988 B CN109941988 B CN 109941988B
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Abstract
The invention provides a preparation method and application of graphene quantum dots and a device or device comprising the graphene quantum dots. The preparation method comprises the following steps: reacting the crystalline flake graphite with concentrated sulfuric acid, adding nitrate and potassium permanganate to continue to react, adding water to dilute the reaction system, and adding hydrogen peroxide to obtain the precipitate which is the graphene quantum dots. Compared with the traditional hydrothermal method, the preparation method provided by the invention has the advantages that the required reaction time is greatly shortened, high-temperature reaction is not required, and the operation difficulty and danger of the reaction are reduced; meanwhile, the preparation method disclosed by the invention is low in reagent consumption, simple and convenient in post-treatment steps, and suitable for large-scale production of the graphene quantum dots.
Description
Technical Field
The invention relates to the field of carbon-based materials, in particular to a preparation method and application of graphene quantum dots and a device or device comprising the graphene quantum dots.
Background
As a latest member of Graphene family, zero-dimensional Graphene Quantum Dots (GQDs) have superior properties of common Graphene materials, and have stronger quantum confinement effect and boundary effect due to their size below 10nm, and can exhibit a series of new characteristics. The graphene quantum dots have wider application prospect in the fields of solar photoelectric devices, biomedicine, light-emitting diodes, sensors and the like.
GQDs have become a focus of scientific attention in various fields in recent years, but the development of the GQDs is still in the beginning stage, and the synthesis process is only studied deeply in two or three years. The GQDs are synthesized mainly by hydrothermal method, electrochemical method and chemical stripping carbon fiber method. The hydrothermal method is a commonly used method for preparing GQDs, and generally comprises three steps of carrying out vacuum thermal reduction on Graphene Oxide (GO) to obtain Graphene Nanosheets (GNSs), oxidizing the GNSs in concentrated sulfuric acid and concentrated nitric acid, and reducing the oxidized GNSs in a hydrothermal environment to obtain the Graphene quantum dots.
Compared with other synthesis methods, the yield of the graphene quantum dots prepared by the hydrothermal method is higher. However, the hydrothermal process has the disadvantage that it is carried out based on the starting material GO and its reduction products, which not only requires oxidation of a large amount of graphite powder to obtain GO, but also requires a series of complex redox reactions, and the reduction process typically requires addition of large amounts of reagents and takes several days.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the present invention is to provide a method for preparing graphene quantum dots, wherein in the preparation method of the present invention, crystalline flake graphite is used as a raw material, and steps such as graphene oxide reduction are not required, such that reaction time can be effectively shortened, and the use of reaction reagents can be reduced.
The second purpose of the invention is to provide the graphene quantum dot obtained by the preparation method.
The third purpose of the present invention is to provide an application of the graphene quantum dot of the present invention, and a device or apparatus comprising the graphene quantum dot of the present invention.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a preparation method of graphene quantum dots comprises the following steps: reacting the crystalline flake graphite with concentrated sulfuric acid, adding nitrate and potassium permanganate to continue to react, adding hydrogen peroxide after the reaction system is diluted by water, and obtaining a precipitate which is graphene quantum dots; preferably, the nitrate salt includes at least one of potassium nitrate and sodium nitrate.
Preferably, in the preparation method of the present invention, the ratio of the mass gram of the flake graphite to the volume milliliter of the concentrated sulfuric acid is (0.8-2): 50; and/or the reaction time of the crystalline flake graphite and concentrated sulfuric acid is 25-35 min.
Preferably, in the preparation method of the invention, the mass gram ratio of the crystalline flake graphite to the nitrate is (0.8-2): (1-2); and/or the mass gram ratio of the crystalline flake graphite to the potassium permanganate is (0.8-2): (5-8).
Preferably, in the preparation method of the present invention, the adding nitrate and potassium permanganate to continue the reaction includes: under the ice bath condition, adding nitrate and potassium permanganate for reaction, and then transferring to a water bath for reaction; more preferably, the potassium permanganate is added in batches.
Preferably, in the preparation method, the reaction time under the ice bath condition is 1-3 h; and/or the temperature of the water bath is 30-40 ℃, and the reaction time in the water bath is 12-24 h.
Preferably, in the preparation method of the present invention, the diluting of the reaction system with water comprises: under the ice bath condition, diluting the reaction system by adding water for the first time, and after the heating reaction, diluting by adding water for the second time; more preferably, the ratio of the volume milliliters of water used for one-time water dilution to the volume milliliters of concentrated sulfuric acid is (1.1-1.5): 1; more preferably, the ratio of the volume milliliters of water used for the second water dilution to the volume milliliters of the concentrated sulfuric acid is (1-1.2): 1.
preferably, in the preparation method of the present invention, the heating reaction includes: transferring the reaction system diluted by adding water for the first time into a water bath for heating and stirring reaction; more preferably, the heating reaction temperature is 80-90 deg.C, and the heating reaction time is 10-30 min.
Further, the invention also provides the graphene quantum dot obtained by the preparation method.
Similarly, the invention also provides application of the graphene quantum dot in preparation of devices or devices.
Meanwhile, the invention also provides a device or a device comprising the graphene quantum dot.
Compared with the traditional hydrothermal method, the preparation method disclosed by the invention has the advantages that the reaction time is greatly shortened, high-temperature reaction is not needed, and the operation difficulty and the danger of the reaction are reduced;
meanwhile, the preparation method disclosed by the invention is low in reagent consumption, simple and convenient in post-treatment steps, and suitable for large-scale production of the graphene quantum dots.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
Fig. 1 is an XRD and raman detection graph of the graphene quantum dot prepared in example 1;
fig. 2 is a high power transmission electron micrograph of the graphene quantum dot prepared in example 1;
in fig. 1, (a) is an XRD detection diagram of the graphene quantum dot prepared in example 1;
(b) raman detection map of graphene quantum dots prepared for example 1.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In view of the defects of the existing hydrothermal method for preparing the graphene quantum dots, the invention provides a novel method for preparing the graphene quantum dots.
The preparation method provided by the invention is used for preparing the graphene quantum dots by taking the crystalline flake graphite as a raw material. In the prior art, graphene oxide is mostly used as a raw material for preparing graphene quantum dots (see CN102807209A, for example), and related preparation attempts are also made for preparing fullerenes (see CN104211050A, for example) and coals (see CN103803540A, for example). However, the research on preparing graphene quantum dots by using flake graphite, i.e., layered graphite, as a raw material is rare. Therefore, the method provided by the invention can solve the problems of more reaction steps, long reaction time, more reagent consumption and the like in the traditional hydrothermal method for preparing the graphene quantum dots, and is a brand-new attempt and exploration for preparing the graphene quantum dots.
Specifically, the preparation method comprises the following steps:
(a) adding the crystalline flake graphite into a reaction container (such as a beaker), adding concentrated sulfuric acid, and stirring for reaction at normal temperature;
preferably, in this step, the concentrated sulfuric acid used is concentrated sulfuric acid with a concentration of 98 wt.%;
preferably, in this step, the ratio of the mass gram of the flake graphite to the volume milliliter of the concentrated sulfuric acid is (0.8-2): 50, the mass-to-volume ratio of the two raw materials can be, but is not limited to, 1:50, 1.2:50, 1.5:50, or 1.8:50, etc.
Preferably, in this step, the reaction is carried out under stirring at room temperature of 15 to 35 ℃.
Preferably, in this step, the stirring time for the reaction is 25-35min, and the stirring time may be, but is not limited to, 27, 30, or 32 min.
(b) Transferring the reaction container in the step (a) into an ice bath, adding nitrate and potassium permanganate under the stirring condition, and continuing to react under the ice bath condition after the raw material is added;
in some embodiments of the invention, the nitrate salt is one or both of potassium nitrate and sodium nitrate.
In some embodiments of the invention, the ratio of the flake graphite to the nitrate in grams by mass is (0.8-2): (1-2);
preferably, in the step, the mass gram ratio of the crystalline flake graphite to the nitrate is (1-1.5): (1-1.5);
more preferably, in the step, the mass gram ratio of the crystalline flake graphite to the nitrate is (1.2-1.3): (1.4-1.5).
In some embodiments of the invention, the nitrate is added in one portion during this step.
In some embodiments of the invention, the ratio of the weight grams of flake graphite to potassium permanganate is (0.8-2): (5-8);
preferably, in the step, the mass gram ratio of the crystalline flake graphite to the potassium permanganate is (1-1.5): (6-7);
more preferably, in the step, the mass gram ratio of the crystalline flake graphite to the nitrate is (1.2-1.3): (6-7).
In some embodiments of the invention, the potassium permanganate is added in portions in this step, for example, potassium permanganate can be added in portions of 3 to 5 times, each addition time interval is 8 to 15min, and the addition amounts can optionally be the same or different;
preferably, in the step, the potassium permanganate is added in 5 times, the interval time of each feeding is 10min, and the feeding amount is the same.
In some embodiments of the invention, in this step, after the addition of the nitrate and potassium permanganate is completed, the reaction is further continued for 1-3h (e.g., 1.5, 2, or 2.5h, etc.) under ice bath conditions.
(c) And (c) transferring the reaction container after the reaction in the step (b) under the ice bath condition into a water bath, and continuously stirring for reaction.
In some embodiments of the invention, the temperature of the water bath heating is 30-40 ℃, for example, but not limited to, 32, 35, 37, or 39 ℃, etc.;
the reaction time in the water bath is 12-24h, and may be, but is not limited to, 15, 18, 21h, or the like.
(d) Transferring the reaction vessel reacted under the water bath condition in the step (c) into an ice bath, adding water (preferably distilled water) into the reaction vessel under the stirring condition, and adding water into the reaction system for dilution once; after the water is added for dilution, the reaction vessel is transferred into the water bath again for heating and stirring reaction;
in some embodiments of the present invention, the ratio of the volume ml of water used for one dilution with water to the volume ml of the raw concentrated sulfuric acid in step (a) is (1.1-1.5): 1 (e.g., can be, but is not limited to, 1.2:1, 1.3:1, or 1.4:1, etc.);
in some embodiments of the invention, the temperature of the heating reaction (water bath) is 80-90 ℃ (such as but not limited to 82, 85, 87, or 89 ℃, etc.), and the time of the heating reaction is 10-30min (such as but not limited to 15, 20, or 25min, etc.).
(e) Taking the reaction vessel after the reaction in the step (d) out of the water bath, placing the reaction vessel at the room temperature of 20-25 ℃, adding water (preferably distilled water) into the reaction vessel again under the stirring condition, and adding water for the second time for dilution; after the secondary water addition is finished, adding hydrogen peroxide into the reaction vessel, wherein a golden yellow precipitate appears in a reaction system, and the product is the graphene quantum dot;
further, purifying the product graphene quantum dots by a dialysis method.
In some embodiments of the present invention, the ratio of the volume milliliters of water used for the second dilution with water to the volume milliliters of the raw concentrated sulfuric acid in step (a) is (1-1.2): 1 (e.g., can be, but is not limited to, 1.1: 1, etc.).
In some embodiments of the invention, the concentration of hydrogen peroxide used is 10-35% (m/m); preferably, the concentration of the hydrogen peroxide is 15-30%; more preferably, the concentration of the hydrogen peroxide is 20-25%.
In some preferred embodiments of the present invention, the preparation steps of the graphene quantum dots can be summarized as follows:
stirring and reacting the crystalline flake graphite and concentrated sulfuric acid for 25-35min, transferring a reaction system into an ice bath, adding nitrate and potassium permanganate, and stirring and reacting for 1-3h under the ice bath condition;
then, transferring the reaction system to a water bath at 30-40 ℃, and stirring for reaction for 12-24 h;
then, transferring the reaction system into an ice bath again, adding water for dilution once, transferring the reaction container into a water bath with the temperature of 80-90 ℃ again after the water dilution is completed, and heating and stirring for reaction for 10-30 min;
and then, transferring the reaction system to a normal temperature environment, adding water for dilution for the second time, adding hydrogen peroxide, stirring and reacting, and obtaining the product graphene quantum dot by the generated precipitate.
The graphene quantum dots obtained by the method have obvious characteristics and complete crystal forms, as shown in figure 1, the product graphene quantum dots have strong diffraction peaks at about 26.5 degrees 2 theta, and the Raman spectrum is 1350cm-1An obvious D peak appears nearby, and the particle size of the quantum dot is about 12 nm.
Furthermore, the graphene quantum dots prepared by the method can be used as raw materials for preparing devices or devices such as solar luminescent devices, biological/medical detection probes, light emitting diodes, sensors and the like.
Example 1
(1) 1.2g of flake graphite is put into a 500 ml beaker, 50ml of concentrated sulfuric acid is added, and magnetic stirring is carried out for 30min at normal temperature.
(2) Placing the beaker in a bucket with ice blocks, placing the beaker on a magnetic stirrer, keeping ice bath stirring, and adding 1.5g of sodium nitrate; adding potassium permanganate for 5 times, adding the potassium permanganate once every 10 minutes, and adding 1.2g (controlling the reaction temperature to be not more than 3 ℃) each time; the ice bath was kept under stirring and the reaction was continued for 2 hours.
(3) Taking out the beaker, putting the beaker into a heat collection water bath kettle, and stirring and reacting for 24 hours under the condition of 35 ℃ water bath.
(4) Keeping the ice bath state, adding 70ml of distilled water into a beaker (slowly dropwise adding, keeping the temperature of the reactant not more than 50 ℃), placing the beaker into a heat collection water bath kettle again after dilution is finished, and stirring and reacting for 15 minutes under the condition of water bath at 85 ℃.
(5) The beaker was taken out, 50ml of distilled water was added thereto again for dilution, and finally a 30% hydrogen peroxide solution was added dropwise to the beaker until no more golden yellow precipitate was produced.
And collecting the obtained precipitate to obtain the product graphene quantum dot, wherein the diameter of the prepared graphene quantum dot is about 12 nm. As shown in fig. 1, the product graphene quantum dot has a strong diffraction peak at about 2 θ ═ 9 °, and the raman spectrum is 1350cm-1A distinct D peak appears nearby;
meanwhile, a high-power transmission electron microscope image of the obtained graphene quantum dot is shown in fig. 2.
Example 2
(1) 2g of flake graphite is put into a 500 ml beaker, 50ml of concentrated sulfuric acid is added, and magnetic stirring is carried out for 30min at normal temperature.
(2) Placing the beaker in a bucket with ice blocks, placing the beaker on a magnetic stirrer, keeping ice bath stirring, adding 2g of sodium nitrate, and adding 1.5g of potassium permanganate every 10 minutes at 5 times; the ice bath was kept under stirring and the reaction was continued for 2 hours.
(3) Taking out the beaker, putting the beaker into a heat collection water bath kettle, and stirring and reacting for 24 hours under the condition of 35 ℃ water bath.
(4) Keeping the ice bath state, adding 70ml of distilled water into the beaker, putting the beaker into the heat collection water bath again after the dilution is finished, and stirring and reacting for 15 minutes under the condition of water bath at 85 ℃.
(5) The beaker was taken out, 50ml of distilled water was added thereto again for dilution, and finally a 30% hydrogen peroxide solution was added dropwise to the beaker until no more golden yellow precipitate was produced.
Example 3
(1) 1.2g of flake graphite is put into a 500 ml beaker, 50ml of concentrated sulfuric acid is added, and magnetic stirring is carried out for 30min at normal temperature.
(2) Placing the beaker in a bucket with ice blocks, placing the beaker on a magnetic stirrer, keeping ice bath stirring, adding 1.5g of sodium nitrate, and adding 1.2g of potassium permanganate every 10 minutes for 5 times; the ice bath was kept under stirring and the reaction was continued for 2 hours.
(3) Taking out the beaker, putting the beaker into a heat collection water bath kettle, and stirring and reacting for 24 hours under the condition of water bath at 45 ℃.
(4) Keeping the ice bath state, adding 70ml of distilled water into the beaker, putting the beaker into the heat collection water bath kettle again after the dilution is finished, and stirring and reacting for 15 minutes under the condition of 80 ℃ water bath.
(5) The beaker was taken out, 50ml of distilled water was added thereto again for dilution, and finally a 30% hydrogen peroxide solution was added dropwise to the beaker until no more golden yellow precipitate was produced.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (1)
1. A preparation method of graphene quantum dots is characterized by comprising the following steps:
reacting the crystalline flake graphite with concentrated sulfuric acid, adding nitrate and potassium permanganate to continue to react, adding hydrogen peroxide after the reaction system is diluted by water, and obtaining a precipitate which is graphene quantum dots;
the nitrate salt comprises: at least one of potassium nitrate and sodium nitrate;
the ratio of the mass gram of the flake graphite to the volume milliliter of concentrated sulfuric acid is (0.8-2): 50;
and/or the reaction time of the crystalline flake graphite and concentrated sulfuric acid is 25-35 min;
the mass gram ratio of the crystalline flake graphite to the nitrate is (0.8-2): (1-2);
and/or the mass gram ratio of the crystalline flake graphite to the potassium permanganate is (0.8-2): (5-8);
the continuous reaction by adding the nitrate and the potassium permanganate comprises the following steps:
transferring the system after the reaction of the crystalline flake graphite and concentrated sulfuric acid into an ice bath, adding nitrate and potassium permanganate for reaction, and then transferring into a water bath for continuous reaction;
adding potassium permanganate in batches;
the reaction time is 1-3h under the ice bath condition;
and/or the temperature of the water bath is 30-40 ℃, and the reaction time in the water bath is 12-24 h;
the water dilution of the reaction system comprises the following steps:
under the ice bath condition, diluting the reaction system by adding water for the first time, and after heating reaction, diluting the reaction system by adding water for the second time at normal temperature;
the ratio of the volume milliliter number of water used for diluting by adding water once to the volume milliliter number of concentrated sulfuric acid is (1.1-1.5): 1;
the ratio of the volume milliliter number of water used for the second time of water addition and the volume milliliter number of concentrated sulfuric acid is (1-1.2): 1;
the heating reaction comprises the following steps:
transferring the reaction system diluted by adding water for the first time into a water bath for heating and stirring reaction;
the heating reaction temperature is 80-90 deg.C, and the heating reaction time is 10-30 min.
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| KR101347198B1 (en) * | 2012-05-03 | 2014-01-10 | 한국에너지기술연구원 | Method of manufacturing coating agent of dye-sensitive solar cell surface, coating agent thereof and dye-sensitive solar cell coated with coating agent |
| CN102660270A (en) * | 2012-05-03 | 2012-09-12 | 吉林大学 | Method for preparing fluorescent graphene quantum dots by solvothermal method |
| CN103803540B (en) * | 2014-02-19 | 2015-12-02 | 上海交通大学 | A kind of preparation method of coal-based graphene quantum dot |
| 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 |
| 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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