CN110627049A - Preparation method and application of graphene-loaded black phosphorus quantum dot - Google Patents
Preparation method and application of graphene-loaded black phosphorus quantum dot Download PDFInfo
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 91
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 62
- 239000002096 quantum dot Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000006228 supernatant Substances 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
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- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 12
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 8
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000010411 electrocatalyst Substances 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
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- 238000006243 chemical reaction Methods 0.000 description 6
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- 239000002131 composite material Substances 0.000 description 5
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- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- -1 black phosphorus alkene Chemical class 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
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- 238000005406 washing Methods 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
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- 229910001626 barium chloride Inorganic materials 0.000 description 1
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- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
-
- B01J35/23—
-
- B01J35/33—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
Abstract
The invention provides a preparation method and application of graphene-loaded black phosphorus quantum dots, which comprises the steps of weighing black phosphorus, grinding the black phosphorus in a glove box, dissolving the black phosphorus in an organic solvent, crushing obtained liquid under an ice bath condition by an ultrasonic cell crusher, centrifuging the crushed liquid, taking supernate, centrifuging the supernate, taking supernate, and obtaining the centrifuged supernate to obtain the black phosphorus quantum dots; and adding graphene into the prepared supernatant, manually grinding to obtain a mixed solution, performing ultrasonic dispersion, centrifuging the obtained dispersed solution, removing the supernatant, and drying the obtained precipitate in a vacuum drying oven to obtain the graphene-loaded black phosphorus quantum dot. The preparation method is simple, convenient to operate, low in cost, beneficial to industrial production and has a certain use value.
Description
Technical Field
The invention relates to the field of materials science, and particularly relates to a preparation method and application of graphene-loaded black phosphorus quantum dots.
Background
The wide use of fossil energy brings convenience to the world and also causes adverse consequences such as environmental pollution and global warming. In order to find a new environment-friendly energy source which is efficient and clean, hydrogen energy is considered as the most ideal choice. Hydrogen is the basis of the field of hydrogen energy, and the research on the production and utilization of the related electrolyzed water and fuel cells naturally becomes the focus of attention of people. However, the key to the energy conversion efficiency of electrolyzed water and fuel cells is the catalyst. The catalysts used in the first study are mainly noble metals, but non-metal catalysts have to be found for replacing them due to their high price, limited resources, poor stability, etc.
Black phosphorus (black phosphorus) is a novel direct band gap two-dimensional material, and has attracted a great deal of interest in the field of electrocatalysis due to its unique electronic, optical and structural properties. In practical application, the black phosphorus needs to be stripped into a single layer, few layers or multiple layers of black phosphorus alkene to exert the excellent photoelectric and photo-thermal properties of the black phosphorus. In addition, the stability of the black phosphorus nanosheet and the black phosphorus quantum dot also becomes a difficult problem. Therefore, the BP nanosheet prepared by adopting a liquid phase stripping method has good electrocatalytic activity and structural stability as an electrocatalyst. Moreover, if the black phosphorus is prepared into quantum dots loaded on the graphene layer, the graphene composite material not only has larger specific surface area, proper band gap, good thermal stability, chemical stability and the like, but also can change the structure of pure black phosphorus, so that the number of chemical active sites on the surface of the composite material is increased. Therefore, the composite material of the black phosphorus graphene has a good development prospect in the field of electrochemistry.
Disclosure of Invention
The invention provides a preparation method and application of graphene-loaded black phosphorus quantum dots, and aims to solve the problems.
The technical scheme of the invention is realized as follows:
a preparation method of graphene-loaded black phosphorus quantum dots comprises the following steps:
(1) preparation of Black phosphorus Quantum dots
Weighing black phosphorus, grinding the black phosphorus in a glove box, dissolving the black phosphorus in an organic solvent, crushing the obtained liquid by an ultrasonic cell crusher under an ice bath condition, centrifuging the crushed liquid, taking the supernatant, centrifuging the supernatant, taking the supernatant, and taking the centrifuged supernatant to obtain black phosphorus quantum dots;
(2) preparation of graphene-loaded black phosphorus quantum dots
And (2) adding graphene into the supernatant prepared in the step (1), manually grinding to obtain a mixed solution, then carrying out ultrasonic dispersion, centrifuging the obtained dispersed solution, removing the supernatant, and placing the obtained precipitate in a vacuum drying oven for drying to obtain the graphene-loaded black phosphorus quantum dot.
Optionally, the black phosphorus is a black phosphorus crystal, and the graphene is prepared by preparing graphene oxide by a traditional Hummers method and performing thermal reduction on the graphene oxide.
Optionally, the black phosphorus and graphene are in an atomic stoichiometric molar ratio of 1:8 to 1: 10.
Optionally, the organic solvent is N-methylpyrrolidone (NMP), and the mass ratio of the black phosphorus, the graphene and the organic solvent is 1:2:4-1:2: 5.
Optionally, the power of the ultrasonic cell crusher is 600W, the temperature is 8-10 ℃, the crushing time is 1s-3s, the working interval is 2s-4s, and the working time is 20-30 min.
Optionally, the rotation speed of the centrifugation is 8000rpm-12000rpm, and the separation time is 10min-30 min.
Optionally, the power of ultrasonic dispersion is 100W-150W, and the time is 40-60 min.
Alternatively, the manually ground mortar is an agate mortar and the grinding time is 1-2 h.
Optionally, the drying time is 12h-24h, and the drying temperature is 50 ℃ -60 ℃.
The graphene-loaded black phosphorus quantum dot is prepared based on the preparation method.
The application of the graphene-based black phosphorus quantum dot in preparing the electrocatalyst is also within the protection scope of the invention.
The invention has the beneficial effects that: the black phosphorus quantum dots are prepared by adopting a liquid phase stripping method, so that the stability of the black phosphorus in the air is ensured in an NMP solution; in addition, the graphene is ground in the NMP solution containing the black phosphorus, so that the co-stripping of the graphene and the black phosphorus material is realized, and the composite material is formed due to favorable electrostatic surface interaction between the black phosphorus and the graphene material dispersed in the NMP solvent; the black phosphorus alkene is uniformly distributed on the surface of the graphene, and has good electrocatalytic oxygen evolution activity; the preparation method is simple, convenient to operate, low in cost, beneficial to industrial production and has a certain use value.
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, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is an XRD pattern of a graphene successfully loaded with black phosphorus quantum dots prepared by an embodiment of the present invention;
fig. 2 is a Raman test chart of the graphene-supported black phosphorus quantum dot prepared according to the embodiment of the present invention;
FIG. 3 is a TEM image of graphene-supported black phosphorus quantum dots prepared by an embodiment of the invention;
fig. 4 is a Linear Sweep Voltammetry (LSV) graph of the catalytic oxygen evolution reaction of the graphene-supported black phosphorus quantum dots in a 0.1M KOH solution.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
As shown in fig. 1 and fig. 2, the application discloses a preparation method of graphene-loaded black phosphorus quantum dots, which comprises the following steps:
(1) preparation of Black phosphorus Quantum dots
Weighing black phosphorus, grinding the black phosphorus in a glove box, dissolving the black phosphorus in an organic solvent, crushing the obtained liquid by an ultrasonic cell crusher under an ice bath condition, centrifuging the crushed liquid, taking the supernatant, centrifuging the supernatant, taking the supernatant, and taking the centrifuged supernatant to obtain black phosphorus quantum dots;
(2) preparation of graphene-loaded black phosphorus quantum dots
And (2) adding graphene into the supernatant prepared in the step (1), manually grinding to obtain a mixed solution, then carrying out ultrasonic dispersion, centrifuging the obtained dispersed solution, removing the supernatant, and placing the obtained precipitate in a vacuum drying oven for drying to obtain the graphene-loaded black phosphorus quantum dot.
Optionally, the black phosphorus is a black phosphorus crystal, and the graphene is prepared by preparing graphene oxide by a traditional Hummers method and performing thermal reduction on the graphene oxide.
Optionally, the black phosphorus and graphene are in an atomic stoichiometric molar ratio of 1:8 to 1: 10.
Optionally, the organic solvent is N-methylpyrrolidone, and the mass ratio of the black phosphorus to the graphene to the organic solvent is 1:2:4-1:2: 5.
Optionally, the power of the ultrasonic cell crusher is 600W, the temperature is 8-10 ℃, the crushing time is 1s-3s, the working interval is 2s-4s, and the working time is 20-30 min.
Optionally, the rotation speed of the centrifugation is 8000rpm-12000rpm, and the separation time is 10min-30 min.
Optionally, the power of ultrasonic dispersion is 100W-150W, and the time is 40-60 min.
Alternatively, the manually ground mortar is an agate mortar and the grinding time is 1-2 h.
Optionally, the drying time is 12h-24h, and the drying temperature is 50 ℃ -60 ℃.
With the above examples, the preferred specific preparation steps are as follows:
(1) preparation of graphene
A. Preoxidation
Pretreating GO (graphene oxide), and taking 12mL of concentrated H2SO42.5g of potassium persulfate, 2.5g of P2O5Heating to 80 ℃ in a round-bottom flask; dissolving, adding 3g of natural crystalline flake graphite, and stirring at constant temperature for reaction for 4.5 h. After the reaction is finished, cooling the solution to room temperature; diluting with 50ml of deionized water, filtering, washing for 3 times with deionized water, and drying a filter cake at normal temperature;
B. complete oxidation
Adding the pre-oxidized graphite into 120ml of concentrated sulfuric acid, carrying out ice bath, and then slowly adding 15g K2MnO4Controlling the temperature of the solution in the whole process to be lower than 10 ℃; after the addition, the temperature is raised to 35 ℃, and the mixture is stirred for 2.5 hours at constant temperature; after the reaction was complete, the reaction mixture was diluted with 1L of deionized water, the solution was allowed to boil with water, the temperature rose suddenly, stirred at high temperature for a period of time, and then 20mL of 30% H was added2O2The solution turns golden yellow by adding hydrogen peroxide, and a large amount of bubbles are generated; filtering the mixed solution while the solution is hot, washing the filter cake with 10% hydrochloric acid and deionized water to remove metal ions and acid in the mixed solution, and finally adding BaCl2Filtrate was tested for SO42-If the filter cake is not completely removed, placing the filter cake at 50 ℃; drying in a vacuum drying oven, sealing and storing for later use.
C. Reduced graphene oxide
Reducing graphene oxide by a thermal reduction method; putting a certain amount of the prepared graphene oxide into a quartz boat and a tube furnace, heating to 800 ℃ at a heating rate of 5 ℃/min under the argon atmosphere, keeping for 2 hours, and finally naturally cooling to room temperature to obtain a graphene sample;
(2) preparation of Black phosphorus Quantum dots
Weighing 5mg of block-shaped black phosphorus by adopting a liquid phase stripping method, grinding the block-shaped black phosphorus into powder in a glove box, adding the ground black phosphorus into 10ml of N-methyl pyrrolidone, carrying out cell crushing under an ice bath condition, keeping the temperature at 8-10 ℃, centrifuging the obtained solution for 30min at the rotating speed of 8000rpm, taking out supernatant, centrifuging for 20min at the rotating speed of 12000rpm, and taking the supernatant to obtain black phosphorus quantum dots;
(3) preparation of graphene-loaded black phosphorus quantum dots
Putting 20mg of graphene into about 8ml of the supernatant of the black phosphorus quantum dots prepared in the step (2), manually grinding for 1-2h, performing ultrasonic dispersion on the obtained solution for 1h, centrifuging for 10min at 10000rpm under a centrifugal machine, removing the supernatant, and drying the obtained precipitate in a vacuum drying oven for 24h at 60 ℃; and obtaining the graphene-loaded black phosphorus quantum dot composite material.
The XRD pattern of the obtained graphene-supported black phosphorus quantum dot is shown in fig. 1. The strong diffraction peak at 24.2 at 2 θ is consistent with the (002) plane of hexagonal crystalline graphite, indicating that GO has been thermally reduced. In addition, two additional diffraction peaks with a 2 θ of 16.6 and 34 were consistent with the (002) and (004) planes of black phosphorus, indicating successful loading of black phosphorus on graphene.
The Raman graph of the obtained graphene-supported black phosphorus quantum dot is shown in fig. 2. From the figure, it can be seen that the characteristic peaks of D and G of the black phosphorus-loaded graphene are shifted to the low wavenumber direction, indicating that the black phosphorus loading on the graphene is successful.
A TEM image of the graphene-supported black phosphorus quantum dot obtained above is shown in fig. 3. It can be seen from the figure that the black phosphorus is uniformly distributed on the graphene layer.
An LSV diagram of the obtained graphene-supported black phosphorus quantum dot in a 0.1M KOH solution for catalyzing an oxygen evolution reaction is shown in fig. 4. From fig. 4 it can be seen that the initial potential is 1.21V, comparable to some metal oxide based materials, indicating that the material has good catalytic activity.
The graphene-loaded black phosphorus quantum dot prepared based on the preparation method of the embodiment has the advantages of high specific surface area and good stability.
The application of the graphene-based black phosphorus quantum dot in preparing the electrocatalyst is also within the protection scope of the invention.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of graphene-loaded black phosphorus quantum dots is characterized by comprising the following steps:
(1) preparation of Black phosphorus Quantum dots
Weighing black phosphorus, grinding in a glove box, dissolving in an organic solvent, and subjecting the obtained liquid to ice bath
Crushing the mixture by an ultrasonic cell crusher, centrifuging the crushed mixture, taking the supernatant, centrifuging the supernatant, taking the centrifuged supernatant, and obtaining the black phosphorus quantum dots;
(2) preparation of graphene-loaded black phosphorus quantum dots
And (2) adding graphene into the supernatant prepared in the step (1), manually grinding to obtain a mixed solution, then carrying out ultrasonic dispersion, centrifuging the obtained dispersed solution, removing the supernatant, and placing the obtained precipitate in a vacuum drying oven for drying to obtain the graphene-loaded black phosphorus quantum dot.
2. The method for preparing the graphene-supported black phosphorus quantum dot according to claim 1, wherein the black phosphorus is a black phosphorus crystal, and the graphene is prepared by preparing graphene oxide by a traditional Hummers method and performing thermal reduction on the graphene.
3. The method for preparing the graphene-supported black phosphorus quantum dot according to claim 1, wherein the organic solvent is N-methylpyrrolidone, and the mass ratio of the black phosphorus to the graphene to the organic solvent is 1:2:4-1:2: 5.
4. The preparation method of the graphene-loaded black phosphorus quantum dot according to claim 1, wherein the power of an ultrasonic cell crusher is 600W, the temperature is 8-10 ℃, the crushing time is 1s-3s, the working interval is 2s-4s, and the working time is 20-30 min.
5. The method for preparing the graphene-loaded black phosphorus quantum dot according to claim 1, wherein the rotation speed of centrifugation is 8000rpm to 12000rpm, and the separation time is 10min to 30 min.
6. The preparation method of the graphene-loaded black phosphorus quantum dot as claimed in claim 1, wherein the power of ultrasonic dispersion is 100W-150W, and the time is 40-60 min.
7. The preparation method of the graphene-supported black phosphorus quantum dot according to claim 6, wherein a mortar for manual grinding is an agate mortar, and the grinding time is 1-2 h.
8. The preparation method of the graphene-loaded black phosphorus quantum dot as claimed in claim 1, wherein the drying time is 12h-24h, and the drying temperature is 50 ℃ -60 ℃.
9. The preparation method according to any one of claims 1 to 8, wherein the graphene-supported black phosphorus quantum dot is prepared.
10. Use of the graphene-supported black phosphorus quantum dot of claim 9 in the preparation of an electrocatalyst.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111420052A (en) * | 2020-01-14 | 2020-07-17 | 深圳瀚光科技有限公司 | DSPE-PEG-FA modified BP/rGO photothermal agent and preparation method thereof |
| CN112103485A (en) * | 2020-08-29 | 2020-12-18 | 温州玖源锂电池科技发展有限公司 | Preparation method of 0D/2D quantum dot/graphene nanocolloid heterostructure electrode material |
| CN114479985A (en) * | 2022-01-27 | 2022-05-13 | 西安建筑科技大学 | Composite material coated with black phosphorus quantum dots and preparation method and application thereof |
| CN114572946A (en) * | 2022-03-30 | 2022-06-03 | 贵州民族大学 | Preparation method for rapidly preparing high-brightness black phosphorus quantum dot by ball milling method and black phosphorus quantum dot |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108394879A (en) * | 2018-04-04 | 2018-08-14 | 青岛大学 | A kind of black phosphorus alkene and its preparation method and application |
| CN108529578A (en) * | 2018-04-26 | 2018-09-14 | 昆明理工大学 | A kind of preparation method of high stable nanometer black phosphorus/three-dimensional graphene composite material |
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| CN108394879A (en) * | 2018-04-04 | 2018-08-14 | 青岛大学 | A kind of black phosphorus alkene and its preparation method and application |
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| CN111420052A (en) * | 2020-01-14 | 2020-07-17 | 深圳瀚光科技有限公司 | DSPE-PEG-FA modified BP/rGO photothermal agent and preparation method thereof |
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| CN114479985A (en) * | 2022-01-27 | 2022-05-13 | 西安建筑科技大学 | Composite material coated with black phosphorus quantum dots and preparation method and application thereof |
| CN114572946A (en) * | 2022-03-30 | 2022-06-03 | 贵州民族大学 | Preparation method for rapidly preparing high-brightness black phosphorus quantum dot by ball milling method and black phosphorus quantum dot |
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Application publication date: 20191231 |