CN104787756A - Macroscopic preparation method for graphene quantum dots - Google Patents
Macroscopic preparation method for graphene quantum dots Download PDFInfo
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- CN104787756A CN104787756A CN201510160014.4A CN201510160014A CN104787756A CN 104787756 A CN104787756 A CN 104787756A CN 201510160014 A CN201510160014 A CN 201510160014A CN 104787756 A CN104787756 A CN 104787756A
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Abstract
The invention discloses a macroscopic preparation method for graphene quantum dots. The macroscopic preparation method comprises the following steps: a, a dispersing agent of a nano metal catalyst is prepared; b, the dispersing agent containing the nano metal catalyst is applied to a substrate and solidified; c, the substrate coated with a dispersing agent film layer is arranged in a CVD (chemical vapor deposition) system, a reducing gas is introduced at a high temperature, and the solidified dispersing agent is removed; d, a carbon source and the reducing gas are introduced at the high temperature, and the graphene quantum dots located on the nano metal catalyst are prepared; e, the substrate is cooled to the room temperature in reducing atmosphere, then the substrate is taken out and placed in a nano metal etching liquid, and the quantum dots suspended in a solution are obtained. According to the method, the CVD method is adopted to prepare the graphene quantum dots, and macroscopic preparation of the quantum dots is realized; nano metal particles are taken as the catalyst, the size of the graphene quantum dots is accurate and controllable and can be controlled through the size of the metal catalyst particles, the productivity is improved, and the cost is reduced.
Description
Technical field
The present invention relates to a kind of graphene preparation method, particularly relate to a kind of graphene quantum dot preparation method, be applied to quantum dot synthesis technical field.
Background technology
Graphene quantum dot (Graphene quantum dot) is the nano material of accurate zero dimension, and the motion of its internal electron in all directions is all limited to, so quantum confinement effect is remarkable especially, has the character of many uniquenesses.This maybe will bring revolutionary change for electronics, photoelectricity and electromagnetism field.Be applied to the aspects such as solar cell, electronics, optical dye, biomarker and multiple microparticles system.Graphene quantum dot has important potential application in fields such as biology, medical science, material, semiconductor devices.Can monomolecular sensor be realized, also may expedite the emergence of subminiature transistor or the chip communication utilizing semiconductor laser to carry out and be used for making chemical sensor, solar cell, medical imaging apparatus or nanoscale circuit etc.
Due to rim condition and quantum confinement, the shape of graphene quantum dot and large young pathbreaker determine their electricity, optics, magnetic and chemical property.The graphene quantum dot of a large amount of acquisition particular edge shape and uniform-dimension is a difficult problem.The preparation method of usual graphene quantum dot is mainly divided into two large classes: from top to bottom and bottom-to-top method.Bottom-to-top method is, by the method for physics or chemistry, large-sized graphene platelet is cut into undersized graphene quantum dot, comprises hydrothermal method, electrochemical method and chemical method and peels off the methods such as carbon fiber; Bottom-to-top method prepares graphene quantum dot as precursor by series of chemical using small molecules, mainly contains ultrasonic method and microwave method, solution chemical method.Its carbon source of hydrothermal method is generally graphene oxide, and its preparation process is complicated and need more reagent; The carbon source of electrochemical method is generally graphite rod, makes process more complicated the early stage of graphite, the comparatively complicated and length consuming time of the purifying dialysis step of graphene quantum dot in subsequent experimental; The experimental procedure of chemical solution method is comparatively complicated, the more difficult control of experiment condition in experimentation.Therefore, a kind of simple graphene quantum dot preparation in macroscopic quantity method is found extremely urgent.
Summary of the invention
In order to solve prior art problem, the object of the invention is to the deficiency overcoming prior art existence, a kind of preparation in macroscopic quantity method of graphene quantum dot is provided, adopt nano metal particles as catalyzer, making it to be attached on substrate by simply applying, preparing graphene quantum dot by CVD, preparation is simple in the present invention, and the size of graphene quantum dot can be controlled by the yardstick of metal catalytic particles, improve productive rate, reduce cost.
Create object for reaching foregoing invention, the present invention adopts following technical proposals:
A preparation in macroscopic quantity method for graphene quantum dot, comprises the steps:
A. adopt dispersion agent to prepare the dispersion liquid of metallic catalyst, the particle dia of the metallic catalyst of employing is 2-100nm, and the concentration of the nano metal particles of dispersion liquid is 0.01%-30wt%; In dispersion liquid preparation process, preferably adopt any one or the combinations several arbitrarily in the aid dispersion means such as mechanical stirring, ultrasonic disperse and heating; Metallic catalyst is preferably the alloy nano particle of any one or any several metal in Nanometer Copper, nano nickel, Platinum Nanoparticles and nanometer gold; Dispersion agent preferably adopts the mixture of any one or any several dispersion agent of fatty acid, aliphatic amide type, ester class, paraffin class, metal soap and low-molecular-weight wax class;
B. by prepare in step a containing the dispersion of metallic catalyst on substrate, then dry solidification, thus coating forms dispersion liquid film layer on substrate; The thickness preferably applying the dispersion liquid film layer of formation on substrate is less than 10 microns; Preferably by any one in spin-coating method, dip coated, printing, convex-concave coating and gravure coating method or combined methods several arbitrarily, by the dispersion containing metallic catalyst on substrate; The method of dry solidification preferably adopts spontaneous curing, be heating and curing or nonoxidizing atmosphere is heating and curing method; The substrate of preferred employing is sapphire, silicon chip GaN epitaxy sheet, silicon chip, sheet glass, alumina wafer, tin indium oxide sheet, mix fluorine oxidation zinc metal sheet or flexible substrate;
C. the substrate being coated with dispersion liquid film layer prepared in stepb is placed in chemical gas-phase deposition system, reducing gas is passed under 300-1100 DEG C of condition, remove the dispersion agent in the dispersion liquid film layer that substrate solidifies, substrate is formed the metallic catalyst particle be uniformly distributed in; Chemical gas-phase deposition system preferably adopts hot CVD stove, PECVD stove or microwave-assisted CVD stove; Chemical gas-phase deposition system preferably also includes preheating oven;
D. under 300-1100 DEG C of condition, carbon source and reducing gas is passed in chemical gas-phase deposition system, on the metallic catalyst particle prepared in step c, load generates graphene quantum dot, and the graphene quantum dot prepared by control has the monatomic graphite linings of 1-5 layer; As preferred technical scheme, carbon source adopts gaseous carbon sources, specifically preferably adopts methane, acetylene or ethene; Or carbon source adopts solid carbon source, specifically preferably adopts urea, grass or biscuit; Or carbon source at least preferably adopts stupid liquid carbon source;
E. the substrate attachment prepared in steps d being generated graphene quantum dot is cooled to room temperature in reducing atmosphere, take out substrate and be placed in nano metal etching liquid, after metal catalyst particles is dissolved completely, graphene quantum dot and substrate separation, obtain the graphene quantum dot be suspended in solution, again after separation and purification, i.e. obtained graphene quantum dot; Etching liquid preferably adopts any one or any one the mixed solution in hydrochloric acid, sulfuric acid, iron nitrate, ammonium persulphate, hydrofluoric acid, Glacial acetic acid and nitric acid, and etching technics is one or multi-channel etching.
The present invention compared with prior art, has following apparent outstanding substantive distinguishing features and remarkable advantage:
1. the present invention adopts CVD macroscopic preparation of graphene quantum dot after adopting coated with nano metal catalytic agent dispersing liquid, is controlled the size of graphene quantum dot by the particle diameter controlling nano metal catalysis, simply controlled;
2. the present invention adopts CVD to realize the preparation in macroscopic quantity of graphene quantum dot, and productive rate is high, and cost is low;
3. the present invention is different from conventional cvd method and prepares the coating processes that Graphene part is only to add nano metal particles dispersion liquid, simple for process, is easy to promote.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation in macroscopic quantity method of the embodiment of the present invention one graphene quantum dot.
Fig. 2 is the schematic diagram of the preparation in macroscopic quantity method of the embodiment of the present invention one graphene quantum dot.
Embodiment
Details are as follows for the preferred embodiments of the present invention:
embodiment one:
In the present embodiment, see Fig. 1 and Fig. 2, a kind of preparation in macroscopic quantity method of graphene quantum dot, comprises the steps:
A. adopt copper powder as metallic catalyst 1, it is the ethanolic soln that copper nanoparticle 0. 05 g of 15nm puts into 50 mL by median size, add the PVP dispersion agent 5 of 5wt.%, disperse in 300 W supersonic cleaning machines, the dispersion liquid of obtained copper nanoparticle;
B. spin coating one deck dispersion liquid on sapphire substrate after cleaning, 180 DEG C of 1min are dried, thus on sapphire substrate 3, coating forms dispersion liquid film layer 2, is uniform-distribution with nano copper particle in dispersion liquid film layer 2;
C. sapphire substrate is placed in hot CVD stove, to be evacuated in reaction chamber below pressure drop to 0.1 pascal, pass into hydrogen, flow is 20sccm, is warming up to 500 DEG C, is incubated 20 minutes under pressure 100 pascal, keep gas flow rate constant, be heated to 300 DEG C, pass into hydrogen, thoroughly remove ethanol and PVP;
D. passing into methane flow is 10sccm, and hydrogen 10sccm, is warming up to 1000 DEG C, is incubated 10 minutes under pressure 200 pascal, cuts off methane, under the condition that hydrogen flowing quantity is constant, is cooled to room temperature, and on copper nanoparticle particle, load generates graphene quantum dot 4;
E. adopt in iron nitrate nano metal etching liquid 6, take out the combination of steps d gained sapphire/copper/graphene quantum dot, be placed in the iron nitrate solution that concentration is 0.1g/ml, after metal catalyst copper dissolves completely, in extraction graphene quantum dot 4 to target dispersion.
In the present embodiment, adopt copper nanoparticle as the catalyzer of graphene quantum dot preparation in macroscopic quantity, achieved the simple preparation in macroscopic quantity of graphene quantum dot 4 by the chemical vapour deposition of common CVD, adopt nano metal particles as catalyzer, the size controllable precise of graphene quantum dot.
embodiment two:
The present embodiment is substantially identical with embodiment one, and special feature is:
In the present embodiment, the preparation in macroscopic quantity method of graphene quantum dot, comprises the steps:
A. adopt nickel powder as metallic catalyst 1, the nano nickel particle 0.01g of median size 50nm is adopted to be distributed in 100ml ethanol solution, add the polyoxyethylene glycol dispersion agent of 2wt%, in KQ-700DE type supersonic cleaning machine, carry out the dispersion of 10 minutes, obtained nano nickel dispersion liquid;
B. spin coating one deck dispersion liquid on silicon chip after cleaning, 2000 DEG C of 1min are dried, thus on silicon chip, coating forms dispersion liquid film layer 2, is uniform-distribution with nano nickle granules in dispersion liquid film layer 2;
C. silicon substrate is placed in PECVD stove, to be evacuated in reaction chamber below pressure drop to 0.1 pascal, pass into hydrogen, flow is 20sccm, is warming up to 500 DEG C, is incubated 20 minutes under pressure 100 pascal, keep gas flow rate constant, be heated to 300 DEG C, pass into hydrogen, thoroughly remove ethanol and polyoxyethylene glycol;
D. radio-frequency (RF) energy 200W, passing into acetylene flow is 10sccm, hydrogen 10sccm, be warming up to 400 DEG C, under pressure 100 pascal, be incubated 10 minutes, cut off acetylene and radio-frequency power supply, under the condition that hydrogen flowing quantity is constant, be cooled to room temperature, on nano nickle granules, load generates graphene quantum dot 4;
E. take out the combination of steps d gained silicon chip/nickel/graphene quantum dot, be placed in the dilute nitric acid solution that concentration is 0.1g/ml 100ml, after metal catalyst nickel dissolves completely, separation and purification obtains Graphene quantum 4 point.
In the present embodiment, adopt nano-nickel powder as the catalyzer of graphene quantum dot preparation in macroscopic quantity, achieve the simple preparation in macroscopic quantity of graphene quantum dot at low temperature by PECVD.
By reference to the accompanying drawings the embodiment of the present invention is illustrated above; but the invention is not restricted to above-described embodiment; multiple change can also be made according to the object of innovation and creation of the present invention; change, the modification made under all spirit according to technical solution of the present invention and principle, substitute, combination, to simplify; all should be the substitute mode of equivalence; as long as goal of the invention according to the invention; only otherwise deviate from know-why and the inventive concept of the preparation in macroscopic quantity method of graphene quantum dot of the present invention, all protection scope of the present invention is belonged to.
Claims (12)
1. a preparation in macroscopic quantity method for graphene quantum dot, is characterized in that, comprise the steps:
A. adopt dispersion agent to prepare the dispersion liquid of metallic catalyst, the particle dia of the metallic catalyst of employing is 2-100nm, and the concentration of the nano metal particles of dispersion liquid is 0.01%-30wt%;
B. by prepare in described step a containing the dispersion of metallic catalyst on substrate, then dry solidification, thus coating forms dispersion liquid film layer on substrate;
C. the substrate being coated with dispersion liquid film layer prepared in described step b is placed in chemical gas-phase deposition system, reducing gas is passed under 300-1100 DEG C of condition, remove the dispersion agent in the dispersion liquid film layer that substrate solidifies, substrate is formed the metallic catalyst particle be uniformly distributed in;
D. under 300-1100 DEG C of condition, carbon source and reducing gas is passed in chemical gas-phase deposition system, on the metallic catalyst particle prepared in described step c, load generates graphene quantum dot, and the graphene quantum dot prepared by control has the monatomic graphite linings of 1-5 layer;
E. the substrate attachment prepared in described steps d being generated graphene quantum dot is cooled to room temperature in reducing atmosphere, take out substrate and be placed in nano metal etching liquid, after metal catalyst particles is dissolved completely, graphene quantum dot and substrate separation, obtain the graphene quantum dot be suspended in solution, again after separation and purification, i.e. obtained graphene quantum dot.
2. the preparation in macroscopic quantity method of graphene quantum dot according to claim 1, it is characterized in that: in described step b, the thickness that substrate applies the dispersion liquid film layer of formation is less than 10 microns.
3. the preparation in macroscopic quantity method of graphene quantum dot according to claim 1 or 2, is characterized in that: in described steps d, and described carbon source adopts gaseous carbon sources, specifically adopts methane, acetylene or ethene; Or described carbon source adopts solid carbon source, specifically adopts urea, grass or biscuit; Or described carbon source at least adopts stupid liquid carbon source.
4. the preparation in macroscopic quantity method of graphene quantum dot according to claim 1 or 2, it is characterized in that: in described step a, in dispersion liquid preparation process, adopt any one or the combinations several arbitrarily in the aid dispersion means such as mechanical stirring, ultrasonic disperse and heating.
5. the preparation in macroscopic quantity method of graphene quantum dot according to claim 1 or 2, it is characterized in that: in described step a, described metallic catalyst is the alloy nano particle of any one or any several metal in Nanometer Copper, nano nickel, Platinum Nanoparticles and nanometer gold.
6. the preparation in macroscopic quantity method of graphene quantum dot according to claim 1 or 2, it is characterized in that: in described step a, dispersion agent is the mixture of any one or any several dispersion agent of fatty acid, aliphatic amide type, ester class, paraffin class, metal soap and low-molecular-weight wax class.
7. the preparation in macroscopic quantity method of graphene quantum dot according to claim 1 or 2, it is characterized in that: in described step b, by any one in spin-coating method, dip coated, printing, convex-concave coating and gravure coating method or combined methods several arbitrarily, by the dispersion containing metallic catalyst on substrate.
8. the preparation in macroscopic quantity method of graphene quantum dot according to claim 1 or 2, is characterized in that: in described step b, and the method for dry solidification adopts spontaneous curing, be heating and curing or nonoxidizing atmosphere is heating and curing method.
9. the preparation in macroscopic quantity method of graphene quantum dot according to claim 1 or 2, it is characterized in that: in described step b, the described substrate of employing is sapphire, silicon chip GaN epitaxy sheet, silicon chip, sheet glass, alumina wafer, tin indium oxide sheet, mix fluorine oxidation zinc metal sheet or flexible substrate.
10. the preparation in macroscopic quantity method of graphene quantum dot according to claim 1 or 2, is characterized in that: in described step c, and described chemical gas-phase deposition system adopts hot CVD stove, PECVD stove or microwave-assisted CVD stove.
The preparation in macroscopic quantity method of 11. graphene quantum dots according to claim 10, is characterized in that: described chemical gas-phase deposition system also includes preheating oven.
12. according to claim 1 or 2 the preparation in macroscopic quantity method of graphene quantum dot, it is characterized in that: in described step e, described etching liquid adopts any one or any one the mixed solution in hydrochloric acid, sulfuric acid, iron nitrate, ammonium persulphate, hydrofluoric acid, Glacial acetic acid and nitric acid, and etching technics is one or multi-channel etching.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098340A (en) * | 2017-06-16 | 2017-08-29 | 青岛河澄知识产权有限公司 | A kind of preparation method of graphene quantum dot dispersion |
| CN107556510A (en) * | 2017-08-29 | 2018-01-09 | 浙江理工大学 | A kind of preparation method of flexible sensor electrode |
| CN109824039A (en) * | 2019-03-26 | 2019-05-31 | 宁波大学 | A method of doped graphene is prepared using doped graphene quantum dot as nucleation point |
| CN110590173A (en) * | 2019-10-18 | 2019-12-20 | 北京大学 | Method for preparing graphene glass with assistance of metal nanoparticles, graphene glass and defogging glass |
| CN110817851A (en) * | 2018-08-08 | 2020-02-21 | 福建海峡石墨烯产业技术研究院有限公司 | Preparation method of multi-edge graphene and aluminum ion battery prepared by same |
| KR20210046431A (en) | 2019-10-18 | 2021-04-28 | 한국원자력연구원 | Method for preparing of graphene quantum dot using ion beam irradiaiton |
| CN113912050A (en) * | 2020-07-09 | 2022-01-11 | Tcl科技集团股份有限公司 | Graphene quantum dot and processing method thereof |
| KR102352572B1 (en) | 2020-07-21 | 2022-01-18 | 한국원자력연구원 | Graphene quantum dot pattern and preparing method thereof |
| CN115401963A (en) * | 2022-08-23 | 2022-11-29 | 江苏理工学院 | Preparation method of nonmetal quantum dot reinforced magnesium-lithium alloy based composite material |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098340B (en) * | 2017-06-16 | 2019-04-19 | 青岛大学 | A kind of preparation method of graphene quantum dot dispersion |
| CN107098340A (en) * | 2017-06-16 | 2017-08-29 | 青岛河澄知识产权有限公司 | A kind of preparation method of graphene quantum dot dispersion |
| CN107556510A (en) * | 2017-08-29 | 2018-01-09 | 浙江理工大学 | A kind of preparation method of flexible sensor electrode |
| CN107556510B (en) * | 2017-08-29 | 2020-06-05 | 浙江理工大学 | Preparation method of flexible sensor electrode |
| CN110817851A (en) * | 2018-08-08 | 2020-02-21 | 福建海峡石墨烯产业技术研究院有限公司 | Preparation method of multi-edge graphene and aluminum ion battery prepared by same |
| CN109824039A (en) * | 2019-03-26 | 2019-05-31 | 宁波大学 | A method of doped graphene is prepared using doped graphene quantum dot as nucleation point |
| CN110590173A (en) * | 2019-10-18 | 2019-12-20 | 北京大学 | Method for preparing graphene glass with assistance of metal nanoparticles, graphene glass and defogging glass |
| KR20210046431A (en) | 2019-10-18 | 2021-04-28 | 한국원자력연구원 | Method for preparing of graphene quantum dot using ion beam irradiaiton |
| KR102304783B1 (en) | 2019-10-18 | 2021-09-24 | 한국원자력연구원 | Method for preparing of graphene quantum dot using ion beam irradiaiton |
| CN113912050A (en) * | 2020-07-09 | 2022-01-11 | Tcl科技集团股份有限公司 | Graphene quantum dot and processing method thereof |
| CN113912050B (en) * | 2020-07-09 | 2023-11-14 | Tcl科技集团股份有限公司 | Graphene quantum dot and processing method thereof |
| KR102352572B1 (en) | 2020-07-21 | 2022-01-18 | 한국원자력연구원 | Graphene quantum dot pattern and preparing method thereof |
| CN115401963A (en) * | 2022-08-23 | 2022-11-29 | 江苏理工学院 | Preparation method of nonmetal quantum dot reinforced magnesium-lithium alloy based composite material |
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