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 PDF

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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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quantum dot
solution
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graphite alkene
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丁文
云峰
宋晓娟
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Xian Jiaotong University
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    • C09K11/65Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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    • B82NANOTECHNOLOGY
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    • H01L33/502Wavelength conversion materials

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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

A kind of preparation method and applications of solid-state powdered graphite alkene quantum dot
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.
CN201810565538.5A 2018-06-04 2018-06-04 A kind of preparation method and applications of solid-state powdered graphite alkene quantum dot Pending CN108587616A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ZHEN TIAN ET AL.,: ""Full-Color Inorganic Carbon Dot Phosphors for White-Light-Emitting Diodes"", 《ADVANCED OPTICAL MATERIALS》 *

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