CN104217907A - Preparation method for graphene field emitting cathode, and graphene field emitting cathode - Google Patents
Preparation method for graphene field emitting cathode, and graphene field emitting cathode Download PDFInfo
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- CN104217907A CN104217907A CN201410465528.6A CN201410465528A CN104217907A CN 104217907 A CN104217907 A CN 104217907A CN 201410465528 A CN201410465528 A CN 201410465528A CN 104217907 A CN104217907 A CN 104217907A
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Abstract
The application discloses a preparation method for a graphene field emitting cathode. The preparation method comprises the following steps of: adding graphene and metal soluble inorganic salts in an organic solvent in a preset ratio to prepare graphene electrophoresis solution with positive charges; using a conductive substrate as a cathode, placing an anode and the cathode in the graphene electrophoresis solution, externally adding an electric field to enable the graphene with positive charges to move towards the direction of the cathode, and deposit on the cathode, so as to obtain a graphene film doped with metal particles; drying the graphene film to obtain the graphene field emitting cathode. The application further discloses a graphene field emitting cathode. The preparation method and the graphene field emitting cathode disclosed by the application are capable of improving the electrical contact characteristic between graphene and a substrate, and improving conduction performance; meanwhile, due to the metal nano-particles, the roughness of the graphene surface is improved, the local electric field intensity of the graphene surface is enhanced, the turn-on electric field of the graphene field emitting cathode is remarkably reduced, and the field emitting current is increased.
Description
Technical field
The application relates to Flied emission technology, particularly relates to a kind of graphene field emission cathode preparation method and graphene field emission cathode.
Background technology
Graphene is a kind of Novel Carbon Nanomaterials, and it refers to the monolayer carbon atom of tightly packed one-tenth bi-dimensional cellular shape lattice structure, has the performance similar with CNT (carbon nano-tube), such as extremely excellent conductive characteristic and thermal conduction characteristic, highly stable mechanochemistry performance.Graphene has large dimensional thickness ratio and abundant flourishing marginal texture, is a kind of desirable field emmision material, is expected to be applied in Flied emission fields such as vacuum microwave device, Field Emission Display, x-ray sources.
In order to realize the application of Graphene transmitting aspect on the scene, first must graphene uniform deposition on a suitable substrate.At present, adoptable method comprises chemical vapour deposition technique (CVD) and electrophoretic deposition.CVD is placed in high temperature furnace by catalyst substrate, then passes into the gas as carbon matrix precursor, generates the method for Graphene.Graphene prepared by CVD growth method is parallel to substrate direction usually, and effective emission tip is few, causes emission current little.In addition, the Graphene of CVD growth needs, through complicated shifting process, to transfer on other substrates.These all seriously limit the practical application of graphene field emission cathode.Electrophoretic deposition is by Graphene and the metal inorganic salt of electric charge (charge additive) can be provided to be dispersed in water or organic solvent, under direct current or AC field effect, and charged Graphene anode or movable cathode, and deposit in conductive substrates.Compare with chemical vapour deposition technique, electrophoretic deposition technique is simple and easy to control, and manufacturing cycle is short, and on the substrate of any shape and size, can prepare graphene field emission cathode by Large-Area-Uniform, actual application prospect is wide.
But use electrophoretic deposition, the electric conductivity between Graphene and substrate is poor, causes Flied emission electric current little.Meanwhile, because contact resistance is large, serious from heating phenomena in negative electrode emission process on the scene, cause the structure of Graphene to be easily destroyed, Flied emission electric current is decayed rapidly.
Summary of the invention
The application provides a kind of graphene field emission cathode preparation method and graphene field emission cathode.
According to the first aspect of the application, the application provides a kind of graphene field emission cathode preparation method, comprising:
Graphene, metal soluble inorganic salt are added in organic solvent according to predetermined ratio, obtained positively charged Graphene electrophoresis solution;
Use electrically-conductive backing plate as negative electrode, respectively anode and described negative electrode are placed in described Graphene electrophoresis solution, extra electric field, positively charged Graphene is moved to described cathode direction, and deposition on the cathode, obtains the graphene film of doping metals particle;
Described graphene film is dry, obtain graphene field emission cathode.
In said method, described metal soluble inorganic salt comprises one or more the mixture in the soluble inorganic salt of copper, silver, gold and platinum.
In said method, described metal soluble inorganic salt comprises copper nitrate, cuprous nitrate, silver nitrate, copper chloride, chlorauride and platinum chloride.
In said method, the weight ratio of described metal soluble inorganic salt and described Graphene is 0.01 ~ 1.
In said method, described Graphene comprises single-layer graphene and/or multi-layer graphene.
In said method, the concentration of described Graphene electrophoresis solution is 0.05 ~ 10mg/ml.
In said method, described graphene film is dry the vacuum environment of 60 ~ 120 DEG C.
In said method, described organic solvent comprises one or more the mixture in ethanol, acetone, normal propyl alcohol and isopropyl alcohol.
In said method, described electrically-conductive backing plate comprises the insulated substrate that plating has the electro-conductive glass of indium tin oxide coating or stainless steel, titanium, copper, chromium, nickel metal substrate or plating titanium, nickel, chromium, copper, gold, silver, platinum conductive coating, and described anode comprises iron plate, copper sheet, aluminium flake or nickel sheet.
According to the second aspect of the application, the application provides a kind of graphene field emission cathode using said method to prepare.
Owing to have employed above technical scheme, the beneficial effect that the application is possessed is:
In the embodiment of the application, owing to adding metal soluble inorganic salt, as the soluble inorganic salt of copper, silver, gold and platinum, the metal ion being adsorbed in graphenic surface is reduced into metal nanoparticle in Graphene deposition process, prepare the graphene film of Uniform Doped copper, silver, gold, platinum grain, improve the contact characteristics between Graphene and substrate, improve electric conductivity; On the other hand, metal nanoparticle improves the roughness of graphenic surface, enhances the local electric field intensity of graphenic surface, significantly reduces the threshold electric field of graphene field emission cathode, improves Flied emission electric current.Compared with conventional electrophoretic sedimentation, the present invention does not need to increase processing step, just can in graphene film evenly, doping metals nano particle efficiently, simple to operate, cost is low, and controllability is good.
Accompanying drawing explanation
Fig. 1 is the graphene field emission cathode preparation method flow chart in one embodiment of the application;
Fig. 2 is that the application uses current deposits legal system for the structural representation of the device of graphene field emission cathode;
Fig. 3 is the change curve of emission J with electric field E of the application's graphene field emission cathode and existing graphene field emission cathode.
Embodiment
By reference to the accompanying drawings the application is described in further detail below by embodiment.
As shown in Figure 1, the graphene field emission cathode preparation method of the application, its a kind of execution mode, comprises the following steps:
Step 102: preparation Graphene electrophoresis solution.
Graphene, metal soluble inorganic salt (charge additive) are added in organic solvent according to predetermined ratio, ultrasonic disperse, prepare uniform and stable Graphene electrophoresis solution.
Graphene comprises single-layer graphene, multi-layer graphene or single-layer graphene and multi-layer graphene mixture.The lateral dimension of Graphene is preferably 500nm-10 μm, can by chemical vapour deposition (CVD) or chemical stripping method (Hummer method) preparation.Metal soluble inorganic salt comprises one or more the mixture in the soluble inorganic salt of copper, silver, gold and platinum.In one embodiment, metal soluble inorganic salt specifically comprises copper nitrate, cuprous nitrate, silver nitrate, copper chloride, chlorauride, platinum chloride etc.
Dispersed in order to Graphene, the organic solvent selected can be one or more in ethanol, acetone, normal propyl alcohol, isopropyl alcohol and their mixed solution.
Graphene electrophoretic liquid concentration used can be 0.05-10mg/ml, in order to improve Graphene dispersiveness in the solution, is preferably 0.05-1mg/ml.The weight ratio of metal soluble inorganic salt addition and Graphene is 0.01 ~ 1, is preferably 0.1 ~ 0.5.
Ultrasonic disperse equipment use supersonic cleaning machine or biomixer, ultrasonic power 50-1000W, ultrasonic time 30min ~ 2h.
Step 104: electrophoresis deposited graphite alkene film on electrically-conductive backing plate
As shown in Figure 2, wherein 1 is negative electrode, and 2 is anode, and 3 is Graphene electrophoresis solution, and 4 is container.Use electrically-conductive backing plate as negative electrode, respectively anode and negative electrode are placed in Graphene electrophoresis solution, extra electric field, positively charged Graphene are moved to cathode direction, and is deposited on negative electrode, obtain the graphene film of doping metals particle.
There is provided electrically-conductive backing plate as negative electrode; negative electrode and anode are put into Graphene electrophoresis liquid, and under the effect of direct voltage, positively charged Graphene moves to cathode direction; be deposited in order on electrically-conductive backing plate, obtain the graphene film of copper doped particle, Argent grain, gold grain or platinum grain.
Electrically-conductive backing plate can be the electro-conductive glass that plating has indium tin oxide (ITO) coating, or the metal substrate such as stainless steel, titanium, copper, chromium, nickel, or the insulated substrate of the metallic conduction coating such as plating titanium, nickel, chromium, copper, gold, silver, platinum.Insulated substrate can be glass, pottery, silicon chip etc.Metal coating can adopt magnetron sputtering, electron beam evaporation, and at least one in vapour deposition process or electroless plating method carries out plating.In one embodiment, anode also can be electrically-conductive backing plate, can be specifically iron plate, copper sheet, aluminium flake, the wherein one in nickel sheet.These metals have than copper, silver, gold, reproducibility that platinum is stronger, can ensure the realization of course of reaction of the present invention.
When charged Graphene moves to the electrically-conductive backing plate surface as negative electrode under electric field action, because Graphene has good conductivity, be adsorbed in the electronics that the copper ion of graphenic surface, silver ion, gold ion or platinum ion easily obtain from anode, be reduced into copper, silver, gold or Pt nanoparticle, simultaneously, metal on anode, owing to losing electronics, becomes corresponding metal ion, enters into solution.The reduction reaction formula that negative electrode occurs is (being described for copper, silver):
Cu
2+ + 2e
- → Cu
Ag
+ + e
- → Ag
Owing to there is above-mentioned reduction reaction, after electrophoretic deposition completes, just obtain the graphene film of Uniform Doped copper particle or Argent grain.
The thickness of graphene film and density can be controlled by electrophoretic voltage and electrophoresis time.Electrophoretic deposition applied voltage is 20 ~ 500V, is preferably 100 ~ 200V.The electrophoretic deposition time can be 10s ~ 30min, is preferably 30s ~ 5min.The spacing of negative electrode and anode can be 0.1 ~ 10cm, in order to reduce the edge effect that exists between anode and cathode, is preferably 0.1 ~ 1cm.
Step 106: graphene film is dry, obtains graphene field emission cathode.
Graphene film is dry, obtain graphene field emission cathode.In one embodiment, by graphene film 60 ~ 120 DEG C of vacuumizes, organic solvent residual in film can be removed, improve the adhesion between Graphene and substrate.Drying time is 10min ~ 2h.
The application prepares graphene field emission cathode by electrophoretic deposition, in electrophoretic deposition process, be adsorbed in the copper of graphenic surface, silver, gold or platinum ion and be reduced into copper, silver, gold or Pt nanoparticle, and be dispersed in graphene film, on the one hand, these nano particles improve the contact characteristics between Graphene and substrate, improve electric conductivity; On the other hand, copper, silver, gold or Pt nanoparticle improve the roughness of graphenic surface, enhance the local electric field intensity of graphenic surface, thus, significantly reduce the threshold electric field of graphene field emission cathode, improve Flied emission electric current.Compared with conventional electrophoretic sedimentation, the present invention does not need to increase processing step, just can in graphene film evenly, doping metals nano particle efficiently, simple to operate, cost is low, and controllability is good.
Embodiment one:
By lateral dimension 0.5-3 μm standby for chemical stripping legal system, the Graphene of thickness 0.5-3.7nm adds in absolute ethyl alcohol, add 10% Cu (NO3) 2(with Graphene weighing scale), Graphene concentration is 0.05mg/ml, use ultrasonic cell-break machine ultrasonic disperse 30min, obtain even, stable Graphene electrophoresis solution;
Select ITO electro-conductive glass and anaerobic copper sheet as electrode, dry up with acetone, EtOH Sonicate cleaning 10min, N2 respectively before using.Then, using ITO electro-conductive glass as negative electrode, anaerobic copper sheet is as anode, and insert in graphene solution, negative electrode and anode spacing 1cm, direct current electrophoretic voltage 100V, electrophoresis time 5min, ITO substrate is prepared the graphene film of doped with Cu nano particle.
By graphene film vacuumize 30min at 60 DEG C, obtain graphene field emission cathode.
Embodiment two:
By lateral dimension 0.5-3 μm standby for chemical stripping legal system, the Graphene of thickness 0.5-3.7nm adds in isopropyl alcohol, add 50% AgNO3(with Graphene weighing scale), Graphene concentration is 1mg/ml, use ultrasonic cell-break machine ultrasonic disperse 2h, obtain even, stable Graphene electrophoresis solution;
Select ITO electro-conductive glass and nickel sheet as electrode, dry up with acetone, EtOH Sonicate cleaning 10min, N2 respectively before using.Then, using ITO electro-conductive glass as negative electrode, nickel sheet is as anode, and insert in graphene solution, negative electrode and anode spacing 0.1cm, direct current electrophoretic voltage 200V, electrophoresis time 30s, ITO substrate is prepared the graphene film of Ag doped nano particle.
By graphene film vacuumize 2h at 120 DEG C, obtain graphene field emission cathode.
Comparative example
By lateral dimension 0.5-3 μm standby for chemical stripping legal system, the Graphene of thickness 0.5-3.7nm adds in absolute ethyl alcohol, add 50% Mg (NO3) 2(with Graphene weighing scale), Graphene concentration is 0.1mg/ml, use ultrasonic cell-break machine ultrasonic disperse 1h, obtain even, stable Graphene electrophoresis solution;
Select ITO electro-conductive glass and anaerobic copper sheet as electrode, dry up with acetone, EtOH Sonicate cleaning 10min, N2 respectively before using.Then, using ITO electro-conductive glass as negative electrode, anaerobic copper sheet is as anode, and insert in graphene solution, negative electrode and anode spacing 1cm, direct current electrophoretic voltage 150V, electrophoresis time 2min, ITO substrate is prepared the graphene film of non-impurity-doped nano particle.
By graphene film vacuumize 30min at 60 DEG C, obtain graphene field emission cathode.
Diode structure is adopted to carry out electron field emission property test for above-mentioned prepared graphene field emission cathode, as shown in Figure 3, wherein, A and B comes from the graphene field emission cathode sample of embodiment one and embodiment two preparation respectively, and C comes from graphene field emission cathode sample prepared by comparative example.Graphene field emission cathode (curve A and B) threshold electric field prepared by embodiment one and embodiment two is respectively 3.1V/ μm and 2.5V/ μm, compared with the graphene field emission cathode (curve C) prepared with comparative example (threshold electric field 4.1 V/ μm), have dropped 24% and 39% respectively.When obtaining the current density of 1mA/cm2, needed for negative electrode prepared by embodiment 1 and embodiment 2, electric field strength is respectively 4.7 V/ μm and 4V/ μm, obvious reduction compared with the negative electrode prepared with comparative example (required electric field strength 6.4V/ μm).Result shows, graphene field emission cathode prepared by the application's method, and between Graphene and substrate, electric conductivity significantly improves, and thus threshold electric field obviously reduces, and emission current enlarges markedly.
The application proves feasible through many experiments, test result shows, graphene field emission cathode threshold electric field prepared by the application obviously reduces, and emission current enlarges markedly, and shows that between graphene field emission cathode and substrate, electric conductivity significantly improves.
Above content is the further description done the application in conjunction with concrete execution mode, can not assert that the concrete enforcement of the application is confined to these explanations.For the application person of an ordinary skill in the technical field, under the prerequisite not departing from the application's design, some simple deduction or replace can also be made.
Claims (10)
1. a graphene field emission cathode preparation method, is characterized in that, comprising:
Graphene, metal soluble inorganic salt are added in organic solvent according to predetermined ratio, obtained positively charged Graphene electrophoresis solution;
Use electrically-conductive backing plate as negative electrode, respectively anode and described negative electrode are placed in described Graphene electrophoresis solution, extra electric field, positively charged Graphene is moved to described cathode direction, and deposition on the cathode, obtains the graphene film of doping metals particle;
Described graphene film is dry, obtain graphene field emission cathode.
2. graphene field emission cathode preparation method as claimed in claim 1, it is characterized in that, described metal soluble inorganic salt comprises one or more the mixture in the soluble inorganic salt of copper, silver, gold and platinum.
3. graphene field emission cathode preparation method as claimed in claim 2, it is characterized in that, described metal soluble inorganic salt comprises copper nitrate, cuprous nitrate, silver nitrate, copper chloride, chlorauride and platinum chloride.
4. graphene field emission cathode preparation method as claimed in claim 1, it is characterized in that, the weight ratio of described metal soluble inorganic salt and described Graphene is 0.01 ~ 1.
5. graphene field emission cathode preparation method as claimed in claim 1, it is characterized in that, described Graphene comprises single-layer graphene and/or multi-layer graphene.
6. graphene field emission cathode preparation method as claimed in claim 1, it is characterized in that, the concentration of described Graphene electrophoresis solution is 0.05 ~ 10mg/ml.
7. graphene field emission cathode preparation method as claimed in claim 1, is characterized in that, described graphene film is dry the vacuum environment of 60 ~ 120 DEG C.
8. graphene field emission cathode preparation method as claimed in claim 1, it is characterized in that, described organic solvent comprises one or more the mixture in ethanol, acetone, normal propyl alcohol and isopropyl alcohol.
9. graphene field emission cathode preparation method as claimed in claim 1, it is characterized in that, described electrically-conductive backing plate comprises the insulated substrate that plating has the electro-conductive glass of indium tin oxide coating or stainless steel, titanium, copper, chromium, nickel metal substrate or plating titanium, nickel, chromium, copper, gold, silver, platinum conductive coating, and described anode comprises iron plate, copper sheet, aluminium flake or nickel sheet.
10. the graphene field emission cathode using the graphene field emission cathode preparation method according to any one of claim 1 to 9 to prepare.
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| CN113838725A (en) * | 2021-09-03 | 2021-12-24 | 深圳先进技术研究院 | Graphene field emission cathode and preparation method thereof |
| CN114318468A (en) * | 2021-12-29 | 2022-04-12 | 哈尔滨工业大学 | Graphene surface enhanced heat transfer composite material and preparation method thereof |
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| CN114318468A (en) * | 2021-12-29 | 2022-04-12 | 哈尔滨工业大学 | Graphene surface enhanced heat transfer composite material and preparation method thereof |
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Application publication date: 20141217 |