CN103545158A - Carbon nano tube cathode and preparation method thereof - Google Patents
Carbon nano tube cathode and preparation method thereof Download PDFInfo
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- CN103545158A CN103545158A CN201310514545.XA CN201310514545A CN103545158A CN 103545158 A CN103545158 A CN 103545158A CN 201310514545 A CN201310514545 A CN 201310514545A CN 103545158 A CN103545158 A CN 103545158A
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Abstract
The invention provides a preparation method of a carbon nano tube cathode and the carbon nano tube cathode obtained through the method. The preparation method includes the steps that a bonding agent layer is arranged on an electric conduction substrate in an electrophoretic deposition mode; a carbon nano tube thin film is arranged on the electric conduction substrate in an electrophoretic deposition mode, wherein the bonding agent layer is also deposited on the electric conduction substrate; in a vacuum or protective atmosphere environment, hot pressed sintering is conducted on the carbon nano tube thin film and the bonding agent layer, so that the carbon nano tube cathode is obtained. According to the carbon nano tube cathode and the preparation method thereof, the hot pressed sintering technology is adopted, the root portion of a carbon nano tube is embedded into a base body of a bonding agent under the action of pressure, so that firm combination is formed, meanwhile, the contact resistance of the carbon nano tube and the base body is lowered, hence, emission currents of the carbon nano tube are increased, and the current stability of the carbon nano tube is improved.
Description
Technical field
The invention belongs to Material Field, particularly relate to carbon nanotube cathod and preparation method thereof.
Background technology
Carbon nano-tube is a kind of Novel Carbon Nanomaterials, compare with existing other materials, have excellent conductance, the outstanding electron emissivity being produced by nano level tip and the stable features such as mechanochemistry characteristic, be a kind of desirable field emmision material, showing as can instant on switch, unlatching electric field is low, and emission is large, is expected at flat-panel monitor, x-ray source, microwave amplifier equal vacuum electronic applications is used widely.
It is good that the key of carbon nano tube field-emission application is to prepare surface topography, carbon nanotube cathod that can continous-stable electron emission.The method of preparing carbon nanotube field emission cathode in prior art has chemical vapour deposition technique (CVD), silk screen print method and electrophoretic deposition etc.Wherein, electrophoretic deposition technique is simple and easy to control, and manufacturing cycle is short, can on the substrate of any shape and size, large area prepare carbon nanotube cathod, and actual application prospect is wide.It is that carbon nano-tube, dispersant, charge additive etc. are dispersed in water or organic solvent, and under direct current or AC field effect, carbon nano-tube anode or movable cathode, deposit on substrate, obtains carbon nanotube cathod.The problem that electrophoresis exists is, the adhesion of carbon nano-tube and substrate a little less than, contact resistance is large, causes an emission current less, launches stable not.
Electrophoretic deposition is prepared carbon nanotube cathod, improve the adhesion property of carbon nano-tube and substrate, conventional method comprises: the one, carbon nano-tube, adhesive particle and metallic particles etc. are evenly mixed in solvent, then electrophoretic deposition is on substrate, form mixture layer, through sintering, obtain carbon nanotube cathod; The 2nd, method deposits adhesive layer in advance on substrate to adopt electrophoretic deposition, spraying, spin coating, lift etc., and then electrophoretic deposition carbon nanotube layer, obtains carbon nanotube cathod through sintering.Yet carbon nano-tube tip is easily covered by binder substrate in first method, make the most advanced and sophisticated significantly minimizing of carbon nano-tube of effectively transmitting, reduced field emission performance; Nonwetting or wetability due to carbon nano-tube and binding agent in second method is poor, and it is unsatisfactory that tack is improved effect.
Summary of the invention
Based on this, one of object of the present invention is to provide a kind of preparation method who improves the carbon nanotube cathod of carbon nano-tube and substrate adhesion property in electrophoretic deposition process, and the carbon nanotube cathod emission of preparation is large, good stability.
The technical scheme that realizes above-mentioned purpose is as follows.
A preparation method for carbon nanotube cathod, comprises the following steps:
(1) electrophoretic deposition adhesive layer on electrically-conductive backing plate
Using glass dust as inorganic binder, mix with conductive nano-particles and charge additive, be dissolved in organic solvent, the binding agent electrophoresis liquid that obtains mixing; Two electrically-conductive backing plates, respectively as negative electrode and anode, are put into described binding agent electrophoresis liquid, under the effect of DC electric field, carry out electrophoresis, obtain depositing the electrically-conductive backing plate of adhesive layer;
(2) electrophoresis carbon nano-tube film depositing on the electrically-conductive backing plate of deposition adhesive layer
Carbon nano-tube and charge additive are mixed, be dissolved in organic solvent, obtain carbon nano-tube electrophoretic liquid, using the electrically-conductive backing plate of described deposition adhesive layer as negative electrode, another electrically-conductive backing plate, as anode, is put into described carbon nano-tube electrophoretic liquid, under the effect of DC electric field, carry out electrophoresis, form the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer;
(3) adopt hot-pressing sintering technique, by the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer sintering under vacuum or protective atmosphere, obtain carbon nanotube cathod.
In one of them embodiment, in described binding agent electrophoresis liquid, the concentration of described glass dust is 1-2mg/ml, and the consumption of described conductive nano-particles is the 30-60wt% of glass dust, described charge additive is soluble metal inorganic salts, and its consumption is the 1-5wt% of glass dust; In described carbon nano-tube electrophoretic liquid, the concentration of described carbon nano-tube is 0.01-0.03mg/ml, the 25-50wt% that the consumption of described charge additive is carbon nano-tube.
In an embodiment, described conductive nano-particles is at least one in nanometer iron powder, nano titanium powder, nano-silver powder, nano-nickel powder, copper nanoparticle, nano indium oxide powder, nano oxidized glass putty, nano indium oxide glass putty therein; Described charge additive is soluble metal inorganic salts; Described charge additive is for being Mg (NO
3)
2, MgCl
2, MgSO
4, Al (NO
3)
3, AlCl
3, NiCl
2, FeCl
3or AgNO
3.
Therein in an embodiment, described organic solvent can be a kind of in methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, acetone and their mixed solution.
Therein in an embodiment, described electrically-conductive backing plate can be the metal substrates such as stainless steel, titanium, copper, aluminium, chromium or nickel, or plating has the insulated substrate of the metal coatings such as tungsten, molybdenum, titanium, nickel, chromium, gold, silver or platinum, or plating has the electro-conductive glass of indium tin oxide (ITO) coating.Insulated substrate can be at least one of 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 carried out plating.
In an embodiment, the diameter of described conductive nano-particles is 10-100 nanometer therein.
In an embodiment, in step (1), the voltage of electrophoresis can be 50-100V therein, and electrophoresis time is 5-30s.Negative electrode and anode spacing are 0.1-1cm.
In an embodiment, carbon nano-tube can be Single Walled Carbon Nanotube therein, multi-walled carbon nano-tubes, the single wall of modification or at least one in multi-walled carbon nano-tubes.Described carbon nano-tube can adopt universal method as preparations such as arc discharge method, chemical vapour deposition technique, laser ablation methods.Carbon nano-tube diameter 1-20nm, length can be 1-100 μ m, preferably 1-20 μ m.
In an embodiment, in step (2), electrophoretic voltage is 100-200V, electrophoresis time 1-5min therein; Described negative electrode and anode spacing are 0.1-1cm.
Therein in an embodiment, in step (3), the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer is put into vacuum or protective atmosphere sintering furnace, in sintering process, by pressure head, on the surface of the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer, apply certain pressure, pressure size is 0.5-1MPa, and sintering temperature is 400-600 ℃; Glass dust heat fused, parcel carbon nano-tube root and conductive nano-particles, form composite material, thereby improve adhesive force and the conductivity of carbon nano-tube and substrate.During vacuum annealing, vacuum degree is 10
-1-10
-5pa, during protective atmosphere annealing, protective gas can be N
2, H
2or at least one in the inert gases such as Ar, described sintering time is 1h-2h, and naturally cooling with stove.
In an embodiment, after step (3) sintering, adopt tape-stripping therein; carbon nano-tube described in alignment, obtains carbon nanotube cathod, is about to the sticky one side of low viscous wafer with protection adhesive tape and contacts with described carbon nano-tube; then tear off, obtain carbon nanotube cathod.
It is large that another object of the present invention is to provide emission, the carbon nanotube cathod of good stability.
Concrete technical scheme is: the carbon nanotube cathod being obtained by above-mentioned preparation method.
Advantage of the present invention and beneficial effect are:
(1) the present invention, by a large amount of experiments, has optimized the preparation technology of carbon nanotube cathod.The present invention adopts hot-pressing sintering technique, and carbon nano-tube root under pressure, is imbedded in adhesive layer matrix, forms firmly combination, has reduced the contact resistance with matrix simultaneously, thereby has improved emission current and the current stability of carbon nano-tube.
(2) adopt ordinary sinter method, in adhesive layer, part particle is in conjunction with bad, easy emission process on the scene flies out, cause sparking, vacuum device is caused to damage, and in the present invention, through hot pressed sintering, in adhesive layer, between particle, form the combination of close and firm, significantly reduced the generation of spark phenomenon, improved the stability of carbon nanotube cathod vacuum device.
Accompanying drawing explanation
Fig. 1 is that the carbon nanotube cathod field emission current I of embodiment 1 preparation is along with the change curve of electric field strength E; Fig. 2 is that the carbon nanotube cathod field emission current I of embodiment 2 preparations is along with the change curve of electric field strength E; Fig. 3 is that the carbon nanotube cathod field emission current I of embodiment 3 preparations is along with the change curve of electric field strength E.
Embodiment
Below in conjunction with specific embodiment and accompanying drawing, the present invention is done to further explaination.
The preparation method of the carbon nanotube cathod described in the present embodiment, comprises the following steps:
(1) electrophoretic deposition adhesive layer on electrically-conductive backing plate
(1a) by 100mg glass powder particles, 30mg nano titanium powder (diameter 10 nanometers) and 5%MgCl
2(with glass dust weighing scale) adds in 100ml absolute ethyl alcohol, and ultrasonic dispersion 1h, obtains binding agent electrophoresis liquid;
(1b) select stainless steel substrates and anaerobic copper sheet as electrode, before using, successively use acetone, ethanol ultrasonic cleaning 10min, N
2dry up; Then, using stainless steel substrates as negative electrode, and anaerobic copper sheet, as anode, inserts in binding agent electrophoresis liquid solution, negative electrode and anode spacing 1cm, under the effect of DC electric field, carry out electrophoresis, electrophoretic voltage 50V, electrophoresis time 30s, described glass dust and conductive nano-particles, to movable cathode, form adhesive layer on stainless steel substrates, obtain depositing the electrically-conductive backing plate of adhesive layer;
(2) electrophoresis carbon nano-tube film depositing on the electrically-conductive backing plate of deposition adhesive layer
(2a) by 3mg diameter 10-20nm, multi-walled carbon nano-tubes and the 50%MgCl of length 10-20 μ m
2(with carbon nano-tube weighing scale) adds in 100ml absolute ethyl alcohol, and ultrasonic dispersion 5h, obtains carbon nano-tube electrophoretic liquid;
(2b) using deposit adhesive layer stainless steel substrates as negative electrode, anaerobic copper sheet is as anode, insert in described carbon nano-tube electrophoretic liquid, negative electrode and anode spacing 1cm, under the effect of DC electric field, carry out electrophoresis, electrophoretic voltage 100V, electrophoresis time 5min, with the carbon nano-tube of electric charge to movable cathode, deposition, the electrically-conductive backing plate of formation deposition of carbon nanotubes and adhesive layer;
(3) adopt hot-pressing sintering technique, the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer is put into protective atmosphere sintering furnace, in sintering process, by pressure head, at the electrically-conductive backing plate upper surface of carbon nano-tube and adhesive layer, apply certain pressure, sintering pressure size is 0.5MPa, sintering temperature is 400 ℃, sintering time 2h, glass dust heat fused, parcel carbon nano-tube root and conductive nano-particles, form composite material, thereby improve adhesive force and the conductivity of carbon nano-tube and substrate; The protective atmosphere of the present embodiment is N
2inert gas;
(4) last; use low viscous wafer with protection tape-stripping carbon nano tube surface; the one side that adhesive tape is sticky contacts with carbon nano-tube; then tear off; the bad carbon nano-tube of being combined with binder substrate is on a small quantity removed; make carbon nano-tube erect along the direction vertical with substrate simultaneously, thereby optimized surface topography and the density of carbon nano-tube, obtain having the carbon nanotube cathod of excellent field emission performance.
Carbon nanotube cathod for embodiment 1 preparation adopts diode structure to carry out electron field emission property test, as shown in Figure 1.Carbon nanotube cathod is opened electric field, and (current density is 10 μ A/cm
2) and threshold field (current density is 10mA/cm
2) be respectively 1.8V/ μ m and 3.1V/ μ m, show excellent field emission performance.
The preparation method of the carbon nanotube cathod described in the present embodiment, comprises the following steps:
(1) electrophoretic deposition adhesive layer on electrically-conductive backing plate
(1a) by 500mg glass dust, 300mg nanometer iron powder (diameter 50 nanometers) and 1%AlCl
3(with glass dust weighing scale) adds in 250ml absolute ethyl alcohol, and ultrasonic dispersion 2h, obtains binding agent electrophoresis liquid;
(1b) select nickel sheet and anaerobic copper sheet as electrode, before using, successively use acetone, ethanol ultrasonic cleaning 10min, N
2dry up.Then, using nickel sheet as negative electrode, anaerobic copper sheet, as anode, inserts in binder solution, negative electrode and anode spacing 0.1cm, under the effect of DC electric field, carry out electrophoresis, electrophoretic voltage 100V, electrophoresis time 5s forms adhesive layer on nickel sheet, obtains depositing the electrically-conductive backing plate of adhesive layer;
(2) electrophoresis carbon nano-tube film depositing on the electrically-conductive backing plate of deposition adhesive layer
(2a) by 1mg diameter, be 2-8nm, multi-walled carbon nano-tubes and the 25%AlCl of length 5-15 μ m
3(with carbon nano-tube weighing scale) adds in 100ml absolute ethyl alcohol, and ultrasonic dispersion 2h, obtains carbon nano-tube electrophoretic liquid;
(2b) using deposit adhesive layer nickel sheet as negative electrode, anaerobic copper sheet is as anode, insert in carbon nano-tube solution, negative electrode and anode spacing 0.1cm, under the effect of DC electric field, carry out electrophoresis, electrophoretic voltage 200V, electrophoresis time 1min, with the carbon nano-tube of electric charge to movable cathode, deposition, the electrically-conductive backing plate of formation deposition of carbon nanotubes and adhesive layer;
(3) adopt hot-pressing sintering technique, the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer is put into vacuum sintering furnace, in sintering process, by pressure head, at electrically-conductive backing plate upper surface, apply certain pressure, pressure size is 1MPa, and sintering temperature is 600 ℃, sintering time 1h, and naturally cooling with stove, annealing vacuum degree is 10
-5pa;
(4) last, as described in Example 1, use low viscous wafer with protection tape-stripping carbon nano tube surface, obtain having the carbon nanotube cathod of excellent field emission performance.
Carbon nanotube cathod for embodiment 2 preparations adopts diode structure to carry out electron field emission property test, as shown in Figure 2.Carbon nanotube cathod is opened electric field, and (current density is 10 μ A/cm
2) and threshold field (current density is 10mA/cm
2) be respectively 1.2V/ μ m and 2.5V/ μ m, show excellent field emission performance.
The preparation method of the carbon nanotube cathod described in the present embodiment, comprises the following steps:
(1) electrophoretic deposition adhesive layer on electrically-conductive backing plate
(1a) by 150mg glass dust, 67.5mg nano-silver powder (diameter 100 nanometers) and 2.5%NiCl
2(with glass dust weighing scale) adds in 100ml absolute ethyl alcohol, and ultrasonic dispersion 2h, obtains binding agent electrophoresis liquid;
(1b) select titanium sheet and anaerobic copper sheet as electrode, before using, successively use acetone, ethanol ultrasonic cleaning 10min, N
2dry up; Then, using titanium sheet as negative electrode, anaerobic copper sheet, as anode, inserts in binder solution, negative electrode and anode spacing 0.5cm, under the effect of DC electric field, carry out electrophoresis, electrophoretic voltage 70V, electrophoresis time 20s forms adhesive layer on titanium sheet, obtains depositing the electrically-conductive backing plate of adhesive layer;
(2) electrophoresis carbon nano-tube film depositing on the electrically-conductive backing plate of deposition adhesive layer
(2a) by 2mg diameter 1-2nm, Single Walled Carbon Nanotube and the 40%NiCl of length 1-10 μ m
2(with carbon nano-tube weighing scale) adds in 100ml absolute ethyl alcohol, and ultrasonic dispersion 3h, obtains carbon nano-tube electrophoretic liquid;
(2b) using deposit adhesive layer titanium sheet as negative electrode, anaerobic copper sheet is as anode, insert in carbon nano-tube solution, negative electrode and anode spacing 0.5cm, under the effect of DC electric field, carry out electrophoresis, electrophoretic voltage 150V, electrophoresis time 2min, with the carbon nano-tube of electric charge to movable cathode, deposition, the electrically-conductive backing plate of formation deposition of carbon nanotubes and adhesive layer;
(3) adopt hot-pressing sintering technique, the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer is put into vacuum sintering furnace, in sintering process, by pressure head, at the electrically-conductive backing plate upper surface of deposition of carbon nanotubes and adhesive layer, apply certain pressure, sintering pressure size is 0.8MPa, and sintering temperature is 500 ℃, sintering time 1h, and naturally cooling with stove, annealing vacuum degree is 10
-1pa;
(4) last, as described in Example 1, use low viscous wafer with protection tape-stripping carbon nano tube surface, obtain having the carbon nanotube cathod of excellent field emission performance.
Carbon nanotube cathod for embodiment 3 preparations adopts diode structure to carry out electron field emission property test, as shown in Figure 3.Carbon nanotube cathod is opened electric field, and (current density is 10 μ A/cm
2) and threshold field (current density is 10mA/cm
2) be respectively 1.7V/ μ m and 2.9V/ μ m, show excellent field emission performance.
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a preparation method for carbon nanotube cathod, is characterized in that, comprises the following steps:
(1) electrophoretic deposition adhesive layer on electrically-conductive backing plate
Using glass dust as inorganic binder, mix with conductive nano-particles and charge additive, be dissolved in organic solvent, the binding agent electrophoresis liquid that obtains mixing; Two electrically-conductive backing plates, respectively as negative electrode and anode, are put into described binding agent electrophoresis liquid, under the effect of DC electric field, carry out electrophoresis, obtain depositing the electrically-conductive backing plate of adhesive layer;
(2) electrophoresis carbon nano-tube film depositing on the electrically-conductive backing plate of deposition adhesive layer
Carbon nano-tube and charge additive are mixed, be dissolved in organic solvent, obtain carbon nano-tube electrophoretic liquid, using the electrically-conductive backing plate of described deposition adhesive layer as negative electrode, another electrically-conductive backing plate, as anode, is put into described carbon nano-tube electrophoretic liquid, under the effect of DC electric field, carry out electrophoresis, form the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer;
(3) adopt hot-pressing sintering technique, by the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer sintering under vacuum or protective atmosphere, obtain carbon nanotube cathod.
2. preparation method according to claim 1, it is characterized in that, in described binding agent electrophoresis liquid, the concentration of described glass dust is 1-2mg/ml, the consumption of described conductive nano-particles is the 30-60wt% of glass dust, described charge additive is soluble metal inorganic salts, and its consumption is the 1-5wt% of glass dust;
In described carbon nano-tube electrophoretic liquid, the concentration of described carbon nano-tube is 0.01-0.03mg/ml, the 25-50wt% that the consumption of described charge additive is carbon nano-tube.
3. preparation method according to claim 1; it is characterized in that; step (3) is: the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer is put into vacuum or protective atmosphere sintering furnace; in sintering process, on the surface of the electrically-conductive backing plate of described deposition of carbon nanotubes and adhesive layer, exert pressure, pressure size is 0.5-1MPa; sintering temperature is 400-600 ℃; sintering time is 1h-2h, and naturally cooling with stove, and the vacuum degree of vacuum annealing is 10
-1-10
-5pa; Described protective atmosphere is N
2, H
2or at least one in Ar inert gas.
4. preparation method according to claim 1, is characterized in that, after step (3) sintering, also adopts tape-stripping, and carbon nano-tube described in alignment, obtains carbon nanotube cathod.
5. according to the preparation method described in claim 1-4 any one, it is characterized in that, described conductive nano-particles is at least one in nanometer iron powder, nano titanium powder, nano-silver powder, nano-nickel powder, copper nanoparticle, nano indium oxide powder, nano oxidized glass putty, nano indium oxide glass putty, and the diameter of described conductive nano-particles is 10-100 nanometer; Described charge additive is Mg (NO
3)
2, MgCl
2, MgSO
4, Al (NO
3)
3, AlCl
3, NiCl
2, FeCl
3or AgNO
3.
6. according to the preparation method described in claim 1-4 any one, it is characterized in that, described organic solvent is at least one in methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, acetone.
7. according to claim, ask the preparation method described in 1-4 any one, it is characterized in that, described electrically-conductive backing plate is the metal substrate of stainless steel, titanium, copper, aluminium, chromium or nickel, or plating has the insulated substrate of the metal coating of tungsten, molybdenum, titanium, nickel, chromium, gold, silver or platinum, or plating has the electro-conductive glass of indium tin oxide coating.
8. according to claim, ask the preparation method described in 1-4 any one, it is characterized in that, in step (1), electrophoretic voltage is 50-100V, and electrophoresis time is 5-30s, and described negative electrode and anode spacing are 0.1-1cm; In step (2), electrophoretic voltage is 100-200V, and electrophoresis time is 1-5min, and described negative electrode and anode spacing are 0.1-1cm.
9. according to the preparation method described in claim 1-4 any one, it is characterized in that, described carbon nano-tube is Single Walled Carbon Nanotube, multi-walled carbon nano-tubes, the single wall of modification or at least one in multi-walled carbon nano-tubes; The diameter of described carbon nano-tube is 1-20nm, and length is 1-20 μ m.
10. the carbon nanotube cathod obtaining according to preparation method described in claim 1-9.
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| CN104157791A (en) * | 2014-08-05 | 2014-11-19 | 京东方科技集团股份有限公司 | OLED (Organic Light Emitting Diode) display device and manufacturing method thereof as well as display device |
| CN105513921A (en) * | 2015-12-25 | 2016-04-20 | 深圳先进技术研究院 | Carbon nano field emission cathode, preparation method and application thereof |
| CN106653520A (en) * | 2016-12-08 | 2017-05-10 | 中国科学院深圳先进技术研究院 | Field emission cold cathode and manufacturing method thereof |
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