CN108587616A - A kind of preparation method and applications of solid-state powdered graphite alkene quantum dot - Google Patents
A kind of preparation method and applications of solid-state powdered graphite alkene quantum dot Download PDFInfo
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- CN108587616A CN108587616A CN201810565538.5A CN201810565538A CN108587616A CN 108587616 A CN108587616 A CN 108587616A CN 201810565538 A CN201810565538 A CN 201810565538A CN 108587616 A CN108587616 A CN 108587616A
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 98
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 36
- 239000010439 graphite Substances 0.000 title claims abstract description 36
- -1 graphite alkene Chemical class 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 81
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 66
- 238000010438 heat treatment Methods 0.000 claims abstract description 56
- 239000011259 mixed solution Substances 0.000 claims abstract description 38
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 37
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 37
- 239000007787 solid Substances 0.000 claims abstract description 36
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 33
- 239000008103 glucose Substances 0.000 claims abstract description 33
- 238000000502 dialysis Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 14
- 238000007789 sealing Methods 0.000 claims abstract description 6
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 11
- 238000003801 milling Methods 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 239000000843 powder Substances 0.000 description 8
- 235000019795 sodium metasilicate Nutrition 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 102000004316 Oxidoreductases Human genes 0.000 description 1
- 108090000854 Oxidoreductases Proteins 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Optics & Photonics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biophysics (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
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- General Physics & Mathematics (AREA)
- Luminescent Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a kind of preparation method and applications of solid-state powdered graphite alkene quantum dot, include the following steps:1) glucose is completely dissolved in deionized water, obtains glucose solution, ammonium hydroxide is then added into glucose solution, obtains mixed solution A;2) mixed solution A is put into sealing container, then carries out microwave heating, obtains reaction solution;3) reaction solution is subjected to dialysis treatment, obtains graphene quantum dot solution;4) sodium silicate solids are completely dissolved in deionized water, obtain sodium silicate aqueous solution;5) graphene quantum dot solution is added in sodium silicate aqueous solution, obtains mixed solution B;6) foamed will be carried out after mixed solution B microwave heatings, obtains solid block graphene quantum dot;7) solid block graphene quantum dot is ground, obtains solid-state powdered graphite alkene quantum dot, the quantum dot reunion of solid-state powdered graphite alkene quantum dot prepared by this method is smaller, and can be applied in LED component.
Description
Technical field
The invention belongs to LED light fluorescent powder field, be related to a kind of solid-state powdered graphite alkene quantum dot preparation method and its
Using.
Background technology
Graphene quantum dot is as a kind of novel quantum dot, due to its quantum confinement and edge effect, shows very much
Unique physics, chemical property.In addition to this, graphene quantum dot also has that hypotoxicity, bio-compatibility be good, chemical stabilization
The advantages such as property, adjustable fluorescent characteristic, low cost, bleach-resistant so that have in photoelectric device, sensor, bio-imaging etc.
Prodigious application prospect.
The preparation method of graphene quantum dot is broadly divided into two classes at present:Method from top to bottom, by electrochemistry, acid oxidase,
The methods of hydro-thermal method is cut graphene or graphene oxide to prepare graphene quantum dot.Method from bottom to top, profit
With microwave synthesis, pyrolysis, the methods of hydro-thermal, organic molecule presoma is prepared into graphene by the reactions such as being pyrolyzed or being condensed
Quantum dot, such as open the dilute method of cage fowler and prepare the solution chemical method of the dilute quantum dot of graphite using glucose as presoma.
Based on the graphene quantum dot prepared by the above method mainly exists with solution state, this must be limited with regard to very big
Application of the graphene quantum dot in terms of photoelectric device is made.Graphene quantum dot in solution is prepared into solid graphite alkene amount
It is sub-, have great importance to the LED component based on graphene quantum dot.However, preparing solid graphite alkene quantum at present
It is exactly the fluorescent weakening phenomenon occurred because quantum dot is reunited there are a common problem during point.Therefore, it is badly in need of a kind of
The solid graphite alkene quantum dot preparation method of reunion can be reduced.
Invention content
It is an object of the invention to overcome the above-mentioned prior art, a kind of solid-state powdered graphite alkene quantum dot is provided
Preparation method and applications, the quantum dot of solid-state powdered graphite alkene quantum dot prepared by this method reunite it is less, and can
Applied in LED component.
In order to achieve the above objectives, the preparation method of solid-state powdered graphite alkene quantum dot of the present invention includes following step
Suddenly:
1) glucose is completely dissolved in deionized water, obtains glucose solution, then added into glucose solution
Enter ammonium hydroxide, is uniformly mixed, obtains mixed solution A;
2) mixed solution A that step 1) obtains is put into sealing container, then carries out microwave heating, obtain reaction solution;
3) reaction solution for obtaining step 2) carries out dialysis treatment, obtains graphene quantum dot solution;
4) sodium silicate solids are completely dissolved in deionized water, obtain sodium silicate aqueous solution;
5) graphene quantum dot solution that step 3) obtains is added in the sodium silicate aqueous solution that step 4) obtains, must be mixed
Solution B;
6) foamed will be carried out after mixed solution B microwave heatings that step 5) obtains, obtains solid block graphene quantum dot;
7) the solid block graphene quantum dot that step 6) obtains is ground, obtains solid-state powdered graphite alkene quantum dot.
In step 1), the mass ratio of glucose and deionized water is 1:The body of (30~50), ammonium hydroxide and glucose solution
Product is than being 1:(40~150).
The heating power of microwave heating is 200~800W in step 2), and heating time is 1~12min.
Dialysis treatment is carried out to the reaction solution that step 2) obtains by bag filter in step 3), wherein bag filter is cut
It is 1000~3000 to stay molecular weight, and dialysis time is for 24 hours, substitutional solution twice to be replaced during dialysis treatment.
Sodium silicate solids and the mass ratio of deionized water are 1 in step 4):(1~5).
The volume ratio of sodium silicate aqueous solution and graphene quantum dot solution is 1 in step 5):(0.1~5).
The heating power of microwave heating is 600~800W in step 6), and heating time is 2~8min.
Milling time in step 7) is 0.5~4h.
Application of the prepared solid-state powdered graphite alkene quantum dot in LED component.
The invention has the advantages that:
The preparation method of solid-state powdered graphite alkene quantum dot of the present invention is when specific operation, by graphene quantum dot
Solution is mixed with sodium silicate aqueous solution, obtains mixed solution B, mixed solution B is then carried out microwave heating, wherein silicon
Acid sodium aqueous solution generates silicon-oxygen polymer network structure in microwave heating, to which graphene quantum dot is wrapped in silica polymerization
In object network structure, to reduce the reunion of graphene quantum dot, quantum dot fluorescence Quenching is effectively solved, improves solid state powder
The fluorescence intensity of graphene quantum dot is so that it can applied in LED component, in addition, it is necessary to which explanation, used in of the invention
Glucose, ammonium hydroxide and sodium metasilicate be cheap common chemical article, it is at low cost, it is nontoxic and pollution-free.
Description of the drawings
Fig. 1 is the pictorial diagram for the graphene quantum dot solution that embodiment one to embodiment three is prepared;
Fig. 2 is luminescent spectrum of the graphene quantum dot solution that is prepared of embodiment one under different wave length laser excitation
Figure;
Fig. 3 is luminescent spectrum of the graphene quantum dot solution that is prepared of embodiment two under different wave length laser excitation
Figure;
Fig. 4 is the luminous light of the graphene quantum dot fluorescent powder that is prepared under 405nm laser excitations in embodiment three
Spectrogram;
Fig. 5 is the pictorial diagram for the graphene quantum dot fluorescent powder that embodiment one to embodiment three is prepared;
Fig. 6 is the schematic diagram that LED component is prepared using graphene quantum dot fluorescent powder.
Specific implementation mode
The present invention is described in further detail with reference to embodiment:
Embodiment one
The preparation method of solid-state powdered graphite alkene quantum dot of the present invention includes the following steps:
The glucose of 1g is added in the deionized water of 40ml, so that it is fully dissolved, add the ammonium hydroxide of 0.7ml, mixed
Uniformly, mixed solution A is obtained, the mixed solution A of 2ml, which is put into 4ml, to be capped in closed vial, is then in heating power
3min is heated in the microwave of 640W, obtains reaction solution, takes the reaction solution of 10ml, it is 1000 dialysis to recycle molecular cut off
Bag carries out dialysis treatment, and substitutional solution is deionized water, and dialysis time is that for 24 hours, substitutional solution twice is replaced in centre, obtains graphene
Quantum dot solution;
1ml deionized waters are added fully after dissolving to the sodium metasilicate of 0.8g and sodium silicate aqueous solution are obtained, by graphene quantum
Sodium silicate aqueous solution is added in point solution 2.5ml, and glass bar stirs 10min, obtains mixed solution B, mixed solution B is placed in microwave
Microwave heating in stove, setting heating power are 640W, and heating time 5min further takes out postcooling, obtains graphene quantum solid point
Body.Graphene quantum dot solid is ground 2h using grinding alms bowl, obtains solid state powder graphene quantum dot.
Embodiment two
The preparation method of solid-state powdered graphite alkene quantum dot of the present invention includes the following steps:
The glucose of 1g is added in the deionized water of 40ml, so that it is fully dissolved, add the ammonium hydroxide of 0.7ml, mixed
Uniformly, mixed solution A is obtained, the mixed solution A of 2ml, which is put into 4ml, to be capped in closed vial, is then in heating power
5min is heated in the microwave of 640W, obtains reaction solution, takes the reaction solution of 10ml, it is 1000 dialysis to recycle molecular cut off
Bag carries out dialysis treatment, and substitutional solution is deionized water, and dialysis time is that for 24 hours, substitutional solution twice is replaced in centre, obtains graphene
Quantum dot solution;
1.5ml deionized waters are added fully after dissolving to the sodium metasilicate of 0.8g and sodium silicate aqueous solution are obtained, by graphene amount
Sodium silicate aqueous solution is added in son point solution 2ml, and glass bar stirs 10min, obtains mixed solution B, mixed solution B is placed in microwave
Microwave heating in stove, setting heating power are 640W, and heating time 5min further takes out postcooling, obtains graphene quantum solid point
Body.Graphene quantum dot solid is ground 1h using grinding alms bowl, obtains solid state powder graphene quantum dot.
Embodiment three
The preparation method of solid-state powdered graphite alkene quantum dot of the present invention includes the following steps:
The glucose of 1g is added in the deionized water of 40ml, so that it is fully dissolved, add the ammonium hydroxide of 0.7ml, mixed
Uniformly, mixed solution A is obtained, the mixed solution A of 2ml, which is put into 4ml, to be capped in closed vial, is then in heating power
3min is heated in the microwave of 480W, obtains reaction solution, takes the reaction solution of 10ml, it is 1000 dialysis to recycle molecular cut off
Bag carries out dialysis treatment, and substitutional solution is deionized water, and dialysis time is that for 24 hours, substitutional solution twice is replaced in centre, obtains graphene
Quantum dot solution;
2ml deionized waters are added fully after dissolving to the sodium metasilicate of 0.8g and sodium silicate aqueous solution are obtained, by graphene quantum
Sodium silicate aqueous solution is added in point solution 1.5ml, and glass bar stirs 10min, obtains mixed solution B, mixed solution B is placed in microwave
Microwave heating in stove, setting heating power are 640W, and heating time 5min further takes out postcooling, obtains graphene quantum solid point
Body.Graphene quantum dot solid is ground 0.5h using grinding alms bowl, obtains solid state powder graphene quantum dot.
Example IV
The preparation method of solid-state powdered graphite alkene quantum dot of the present invention includes the following steps:
1) glucose is completely dissolved in deionized water, obtains glucose solution, then added into glucose solution
Enter ammonium hydroxide, is uniformly mixed, obtains mixed solution A;
2) mixed solution A that step 1) obtains is put into sealing container, then carries out microwave heating, obtain reaction solution;
3) reaction solution for obtaining step 2) carries out dialysis treatment, obtains graphene quantum dot solution;
4) sodium silicate solids are completely dissolved in deionized water, obtain sodium silicate aqueous solution;
5) graphene quantum dot solution that step 3) obtains is added in the sodium silicate aqueous solution that step 4) obtains, must be mixed
Solution B;
6) foamed will be carried out after mixed solution B microwave heatings that step 5) obtains, obtains solid block graphene quantum dot;
7) the solid block graphene quantum dot that step 6) obtains is ground, obtains solid-state powdered graphite alkene quantum dot.
In step 1), the mass ratio of glucose and deionized water is 1:50, the volume ratio of ammonium hydroxide and glucose solution is
1:40
The heating power of microwave heating is 800W, heating time 1min in step 2).
Dialysis treatment is carried out to the reaction solution that step 2) obtains by bag filter in step 3), wherein bag filter is cut
It is 3000 to stay molecular weight, and dialysis time is for 24 hours, substitutional solution twice to be replaced during dialysis treatment.
Sodium silicate solids and the mass ratio of deionized water are 1 in step 4):1.
The volume ratio of sodium silicate aqueous solution and graphene quantum dot solution is 1 in step 5):5.
The heating power of microwave heating is 600W, heating time 8min in step 6).
Milling time in step 7) is 0.5h.
Embodiment five
The preparation method of solid-state powdered graphite alkene quantum dot of the present invention includes the following steps:
1) glucose is completely dissolved in deionized water, obtains glucose solution, then added into glucose solution
Enter ammonium hydroxide, is uniformly mixed, obtains mixed solution A;
2) mixed solution A that step 1) obtains is put into sealing container, then carries out microwave heating, obtain reaction solution;
3) reaction solution for obtaining step 2) carries out dialysis treatment, obtains graphene quantum dot solution;
4) sodium silicate solids are completely dissolved in deionized water, obtain sodium silicate aqueous solution;
5) graphene quantum dot solution that step 3) obtains is added in the sodium silicate aqueous solution that step 4) obtains, must be mixed
Solution B;
6) foamed will be carried out after mixed solution B microwave heatings that step 5) obtains, obtains solid block graphene quantum dot;
7) the solid block graphene quantum dot that step 6) obtains is ground, obtains solid-state powdered graphite alkene quantum dot.
In step 1), the mass ratio of glucose and deionized water is 1:30, the volume ratio of ammonium hydroxide and glucose solution is
1:150.
The heating power of microwave heating is 200W, heating time 12min in step 2).
Dialysis treatment is carried out to the reaction solution that step 2) obtains by bag filter in step 3), wherein bag filter is cut
It is 1000 to stay molecular weight, and dialysis time is for 24 hours, substitutional solution twice to be replaced during dialysis treatment.
Sodium silicate solids and the mass ratio of deionized water are 1 in step 4):5.
The volume ratio of sodium silicate aqueous solution and graphene quantum dot solution is 1 in step 5):0.1.
The heating power of microwave heating is 800W, heating time 2min in step 6).
Milling time in step 7) is 4h.
Embodiment six
The preparation method of solid-state powdered graphite alkene quantum dot of the present invention includes the following steps:
1) glucose is completely dissolved in deionized water, obtains glucose solution, then added into glucose solution
Enter ammonium hydroxide, is uniformly mixed, obtains mixed solution A;
2) mixed solution A that step 1) obtains is put into sealing container, then carries out microwave heating, obtain reaction solution;
3) reaction solution for obtaining step 2) carries out dialysis treatment, obtains graphene quantum dot solution;
4) sodium silicate solids are completely dissolved in deionized water, obtain sodium silicate aqueous solution;
5) graphene quantum dot solution that step 3) obtains is added in the sodium silicate aqueous solution that step 4) obtains, must be mixed
Solution B;
6) foamed will be carried out after mixed solution B microwave heatings that step 5) obtains, obtains solid block graphene quantum dot;
7) the solid block graphene quantum dot that step 6) obtains is ground, obtains solid-state powdered graphite alkene quantum dot.
In step 1), the mass ratio of glucose and deionized water is 1:40, the volume ratio of ammonium hydroxide and glucose solution is
1:100.
The heating power of microwave heating is 400W, heating time 8min in step 2).
Dialysis treatment is carried out to the reaction solution that step 2) obtains by bag filter in step 3), wherein bag filter is cut
It is 1500 to stay molecular weight, and dialysis time is for 24 hours, substitutional solution twice to be replaced during dialysis treatment.
Sodium silicate solids and the mass ratio of deionized water are 1 in step 4):4.
The volume ratio of sodium silicate aqueous solution and graphene quantum dot solution is 1 in step 5):3.
The heating power of microwave heating is 700W, heating time 5min in step 6).
Milling time in step 7) is 3h.
The present invention takes the solid-state powdered graphite alkene quantum dot being prepared to obtain graphene quantum dot fluorescent glue with glue, by stone
Black alkene quantum dot fluorescence glue is coated on ultraviolet, blue-light LED chip and excites LED light to get ultraviolet, blue light.
Claims (9)
1. a kind of preparation method of solid-state powdered graphite alkene quantum dot, which is characterized in that include the following steps:
1) glucose is completely dissolved in deionized water, obtains glucose solution, ammonia is then added into glucose solution
Water is uniformly mixed, obtains mixed solution A;
2) mixed solution A that step 1) obtains is put into sealing container, then carries out microwave heating, obtain reaction solution;
3) reaction solution for obtaining step 2) carries out dialysis treatment, obtains graphene quantum dot solution;
4) sodium silicate solids are completely dissolved in deionized water, obtain sodium silicate aqueous solution;
5) graphene quantum dot solution that step 3) obtains is added in the sodium silicate aqueous solution that step 4) obtains, obtains mixed solution
B;
6) foamed will be carried out after mixed solution B microwave heatings that step 5) obtains, obtains solid block graphene quantum dot;
7) the solid block graphene quantum dot that step 6) obtains is ground, obtains solid-state powdered graphite alkene quantum dot.
2. the preparation method of solid-state powdered graphite alkene quantum dot according to claim 1, which is characterized in that its feature exists
In in step 1), the mass ratio of glucose and deionized water is 1:The volume ratio of (30~50), ammonium hydroxide and glucose solution is
1:(40~150).
3. the preparation method of solid-state powdered graphite alkene quantum dot according to claim 1, which is characterized in that its feature exists
In the heating power of microwave heating is 200~800W in step 2), and heating time is 1~12min.
4. the preparation method of solid-state powdered graphite alkene quantum dot according to claim 1, which is characterized in that lead in step 3)
It crosses the reaction solution that bag filter obtains step 2) and carries out dialysis treatment, wherein the molecular cut off of bag filter is 1000~
3000, dialysis time is for 24 hours, substitutional solution twice to be replaced during dialysis treatment.
5. the preparation method of solid-state powdered graphite alkene quantum dot according to claim 1, which is characterized in that silicon in step 4)
Sour sodium solid and the mass ratio of deionized water are 1:(1~5).
6. the preparation method of solid-state powdered graphite alkene quantum dot according to claim 1, which is characterized in that silicon in step 5)
The volume ratio of acid sodium aqueous solution and graphene quantum dot solution is 1:(0.1~5).
7. the preparation method of solid-state powdered graphite alkene quantum dot according to claim 1, which is characterized in that micro- in step 6)
The heating power of Wave heating is 600~800W, and heating time is 2~8min.
8. the preparation method of solid-state powdered graphite alkene quantum dot according to claim 1, which is characterized in that in step 7)
Milling time is 0.5~4h.
9. application of the solid-state powdered graphite alkene quantum dot in LED component as prepared by claim any one of 1-8.
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2018
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CN103910492A (en) * | 2014-04-09 | 2014-07-09 | 福州大学 | Graphene compound glass as well as preparation method and application of compound glass |
CN107502348A (en) * | 2017-08-18 | 2017-12-22 | 复旦大学 | A kind of method by carbohydrate presoma low temperature preparation graphene quantum dot |
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Title |
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