CN103545158B - Carbon nanotube cathod and preparation method thereof - Google Patents
Carbon nanotube cathod and preparation method thereof Download PDFInfo
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- CN103545158B CN103545158B CN201310514545.XA CN201310514545A CN103545158B CN 103545158 B CN103545158 B CN 103545158B CN 201310514545 A CN201310514545 A CN 201310514545A CN 103545158 B CN103545158 B CN 103545158B
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Abstract
The invention provides a kind of preparation method of carbon nanotube cathod, and obtain carbon nanotube cathod by the method.Described preparation method is included in electrophoretic deposition adhesive layer on electrically-conductive backing plate; Electrophoresis carbon nano-tube film depositing on the electrically-conductive backing plate of deposition adhesive layer; Under vacuum or protective atmosphere environment, hot pressed sintering is carried out to carbon nano-tube film and adhesive layer, obtains carbon nanotube cathod.The present invention adopts hot-pressing sintering technique, and carbon nano-tube root under pressure, is imbedded in binder substrate, is formed and firmly combines, reduce the contact resistance with matrix simultaneously, thus improve emission current and the current stability of carbon nano-tube.
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, compared with other materials existing, have excellent conductance, the features such as the outstanding electron emissivity produced by nano level tip and stable mechanochemistry characteristic are a kind of desirable field emmision materials, showing as can instant on switch, threshold electric field is low, and emission is large, is expected at flat-panel monitor, x-ray source, is used widely in the vacuum electronic fields such as microwave amplifier.
It is good that the key of carbon nano tube field-emission application is to prepare surface topography, can the carbon nanotube cathod of continous-stable electron emission.The method 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, and on the substrate of any shape and size, large area can prepare carbon nanotube cathod, actual application prospect is wide.It is dispersed in water or organic solvent by carbon nano-tube, dispersant, charge additive etc., and under direct current or AC field effect, carbon nano-tube anode or movable cathode, deposit on substrate, obtains carbon nanotube cathod.Electrophoresis Problems existing is, the adhesion of carbon nano-tube and substrate is more weak, and contact resistance is large, causes Flied emission electric current less, launches stable not.
Electrophoretic deposition prepares carbon nanotube cathod, improve the adhesion property of carbon nano-tube and substrate, conventional method comprises: one be by Homogeneous phase mixing such as carbon nano-tube, adhesive particle and metallic particles in solvent, then electrophoretic deposition is on substrate, form mixture layer, obtain carbon nanotube cathod through sintering; Two is adopt the methods such as electrophoretic deposition, spraying, spin coating, lift in advance at deposited on substrates adhesive layer, and then electrophoretic deposition carbon nanotube layer, obtains carbon nanotube cathod through sintering.But carbon nano-tube tip is easily covered by binder substrate in first method, makes the most advanced and sophisticated significantly minimizing of carbon nano-tube of effectively launching, reduce 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 improves effect.
Summary of the invention
Based on this, an object of the present invention is to provide a kind of preparation method improving the carbon nanotube cathod of carbon nano-tube and substrate adhesion energy in electrophoretic deposition process, and the carbon nanotube cathod emission of preparation is large, good stability.
The technical scheme realizing 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
Glass dust is mixed with conductive nano-particles and charge additive as inorganic binder, is dissolved in organic solvent, obtain the binding agent electrophoresis liquid mixed; Using two pieces of electrically-conductive backing plates as negative electrode and anode, put into described binding agent electrophoresis liquid, under the effect of DC electric field, carry out electrophoresis, obtain the electrically-conductive backing plate depositing adhesive layer;
(2) electrophoresis carbon nano-tube film depositing on the electrically-conductive backing plate of deposition adhesive layer
By carbon nano-tube and charge additive mixing, 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, puts 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, the electrically-conductive backing plate of described deposition of carbon nanotubes and adhesive layer is sintered under vacuum or protective atmosphere, obtains described 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 described glass dust, described charge additive is soluble metal inorganic salts, and its consumption is the 1-5wt% of described glass dust; In described carbon nano-tube electrophoretic liquid, the concentration of described carbon nano-tube is 0.01-0.03mg/ml, and the consumption of described charge additive is the 25-50wt% of described carbon nano-tube.
Wherein 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, nanometer tin indium oxide powder; Described charge additive is soluble metal inorganic salts; Described charge additive is Mg (NO
3)
2, MgCl
2, MgSO
4, Al (NO
3)
3, AlCl
3, NiCl
2, FeCl
3or AgNO
3.
Wherein in an embodiment, described organic solvent can be the one in methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, acetone and their mixed solution.
Wherein 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 carries out plating.
Wherein in an embodiment, the diameter of described conductive nano-particles is 10-100 nanometer.
Wherein in an embodiment, in step (1), the voltage of electrophoresis can be 50-100V, and electrophoresis time is 5-30s.Negative electrode and anode spacing are 0.1-1cm.
Wherein in an embodiment, carbon nano-tube can be Single Walled Carbon Nanotube, multi-walled carbon nano-tubes, at least one in the single wall of modification or 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 nanotube diameter 1-20nm, length can be 1-100 μm, preferably 1-20 μm.
Wherein in an embodiment, in step (2), electrophoretic voltage is 100-200V, electrophoresis time 1-5min; Described negative electrode and anode spacing are 0.1-1cm.
Wherein in an embodiment, in step (3), the electrically-conductive backing plate of described deposition of carbon nanotubes and adhesive layer is put into vacuum or protective atmosphere sintering furnace sinters, in sintering process, on the surface of the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer, certain pressure is applied by pressure head, pressure size is 0.5-1MPa, and sintering temperature is 400-600 DEG C; Glass dust heat fused, parcel carbon nano-tube root and conductive nano-particles, form composite material, thus improve adhesive force and the conductivity of carbon nano-tube and substrate.During sintering, vacuum degree is 10
-1-10
-5pa, 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 cools with sintering furnace.
Wherein in an embodiment, after step (3) sintering, adopt tape-stripping; carbon nano-tube described in alignment, obtains carbon nanotube cathod, and the one side sticky by low viscous wafer with protection adhesive tape contacts with described carbon nano-tube; then tear off, obtain described 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 obtained by above-mentioned preparation method.
Advantage of the present invention and beneficial effect are:
(1) the present invention is by a large amount of experiments, optimizes 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, is formed and firmly combines, reduce the contact resistance with matrix simultaneously, thus improve emission current and the current stability of carbon nano-tube.
(2) ordinary sinter method is adopted, in adhesive layer, partial particulate is in conjunction with bad, easy emission process on the scene flies out, cause sparking, damage is caused to vacuum device, and in the present invention, through hot pressed sintering, form the combination of close and firm in adhesive layer between particle, significantly reduce the generation of spark phenomenon, improve the stability of carbon nanotube cathod vacuum device.
Accompanying drawing explanation
Fig. 1 is the change curve of carbon nanotube cathod Flied emission electric current I along with electric field strength E of embodiment 1 preparation; Fig. 2 is the change curve of carbon nanotube cathod Flied emission electric current I along with electric field strength E of embodiment 2 preparation; Fig. 3 is the change curve of carbon nanotube cathod Flied emission electric current I along with electric field strength E of embodiment 3 preparation.
Embodiment
Below in conjunction with specific embodiment and accompanying drawing, further explaination is done to the present invention.
Embodiment 1
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 nanometer) and 5%MgCl
2(with glass dust weighing scale) adds in 100ml absolute ethyl alcohol, and ultrasonic disperse 1h obtains binding agent electrophoresis liquid;
(1b) select stainless steel substrates and anaerobic copper sheet as electrode, priority acetone, EtOH Sonicate cleaning 10min, N before using
2dry up; Then, using stainless steel substrates as negative electrode, 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, stainless steel substrates form adhesive layer, obtain the electrically-conductive backing plate depositing 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, the multi-walled carbon nano-tubes of length 10-20 μm and 50%MgCl
2(in carbon nanotubes) adds in 100ml absolute ethyl alcohol, and ultrasonic disperse 5h, obtains carbon nano-tube electrophoretic liquid;
(2b) to deposit the stainless steel substrates of adhesive layer 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, forms the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer;
(3) hot-pressing sintering technique is adopted, the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer is put into protective atmosphere sintering furnace, in sintering process, apply certain pressure by pressure head at the electrically-conductive backing plate upper surface of carbon nano-tube and adhesive layer, sintering pressure size is 0.5MPa, sintering temperature is 400 DEG C, sintering time 2h, glass dust heat fused, parcel carbon nano-tube root and conductive nano-particles, form composite material, thus 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; be removed in conjunction with bad carbon nano-tube with binder substrate on a small quantity; make carbon nano-tube erect along the direction vertical with substrate simultaneously, thus optimize surface topography and the density of carbon nano-tube, obtain the carbon nanotube cathod with excellent field emission performance.
The carbon nanotube cathod prepared for embodiment 1 adopts diode structure to carry out electron field emission property test, as shown in Figure 1.(current density is 10 μ A/cm to carbon nanotube cathod threshold electric field
2) and threshold field (current density is 10mA/cm
2) be respectively 1.8V/ μm and 3.1V/ μm, show excellent field emission performance.
Embodiment 2
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 nanometer) and 1%AlCl
3(with glass dust weighing scale) adds in 250ml absolute ethyl alcohol, and ultrasonic disperse 2h obtains binding agent electrophoresis liquid;
(1b) select nickel sheet and anaerobic copper sheet as electrode, priority acetone, EtOH Sonicate cleaning 10min, N before using
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, nickel sheet forms adhesive layer, obtains the electrically-conductive backing plate depositing adhesive layer;
(2) electrophoresis carbon nano-tube film depositing on the electrically-conductive backing plate of deposition adhesive layer
(2a) by 1mg diameter be multi-walled carbon nano-tubes and the 25%AlCl of 2-8nm, length 5-15 μm
3(in carbon nanotubes) adds in 100ml absolute ethyl alcohol, and ultrasonic disperse 2h, obtains carbon nano-tube electrophoretic liquid;
(2b) to deposit the nickel sheet of adhesive layer 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, forms the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer;
(3) hot-pressing sintering technique is adopted, the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer is put into vacuum sintering furnace, in sintering process, certain pressure is applied at electrically-conductive backing plate upper surface by pressure head, pressure size is 1MPa, and sintering temperature is 600 DEG C, sintering time 1h, and naturally cool with sintering furnace, during sintering, 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 the carbon nanotube cathod with excellent field emission performance.
The carbon nanotube cathod prepared for embodiment 2 adopts diode structure to carry out electron field emission property test, as shown in Figure 2.(current density is 10 μ A/cm to carbon nanotube cathod threshold electric field
2) and threshold field (current density is 10mA/cm
2) be respectively 1.2V/ μm and 2.5V/ μm, show excellent field emission performance.
Embodiment 3
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 nanometer) and 2.5%NiCl
2(with glass dust weighing scale) adds in 100ml absolute ethyl alcohol, and ultrasonic disperse 2h obtains binding agent electrophoresis liquid;
(1b) select titanium sheet and anaerobic copper sheet as electrode, priority acetone, EtOH Sonicate cleaning 10min, N before using
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, titanium sheet forms adhesive layer, obtains the electrically-conductive backing plate depositing 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, the Single Walled Carbon Nanotube of length 1-10 μm and 40%NiCl
2(in carbon nanotubes) adds in 100ml absolute ethyl alcohol, and ultrasonic disperse 3h, obtains carbon nano-tube electrophoretic liquid;
(2b) to deposit the titanium sheet of adhesive layer 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, forms the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer;
(3) hot-pressing sintering technique is adopted, the electrically-conductive backing plate of deposition of carbon nanotubes and adhesive layer is put into vacuum sintering furnace, in sintering process, certain pressure is applied at the electrically-conductive backing plate upper surface of deposition of carbon nanotubes and adhesive layer by pressure head, sintering pressure size is 0.8MPa, and sintering temperature is 500 DEG C, sintering time 1h, and naturally cool with sintering furnace, during sintering, 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 the carbon nanotube cathod with excellent field emission performance.
The carbon nanotube cathod prepared for embodiment 3 adopts diode structure to carry out electron field emission property test, as shown in Figure 3.(current density is 10 μ A/cm to carbon nanotube cathod threshold electric field
2) and threshold field (current density is 10mA/cm
2) be respectively 1.7V/ μm and 2.9V/ μm, show excellent field emission performance.
The above embodiment only have expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but therefore can not 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 (9)
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
Glass dust is mixed with conductive nano-particles and charge additive as inorganic binder, is dissolved in organic solvent, obtain the binding agent electrophoresis liquid mixed; Using two pieces of electrically-conductive backing plates as negative electrode and anode, put into described binding agent electrophoresis liquid, under the effect of DC electric field, carry out electrophoresis, obtain the electrically-conductive backing plate depositing adhesive layer;
(2) electrophoresis carbon nano-tube film depositing on the electrically-conductive backing plate of deposition adhesive layer
By carbon nano-tube and charge additive mixing, 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, puts 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) electrically-conductive backing plate of described deposition of carbon nanotubes and adhesive layer is put into vacuum or protective atmosphere sintering furnace sinters; in sintering process; the surface of the electrically-conductive backing plate of described deposition of carbon nanotubes and adhesive layer applies pressure; pressure size is 0.5-1MPa; sintering temperature is 400-600 DEG C; sintering time is 1h-2h, and naturally cools with sintering furnace, and vacuum degree during sintering is 10
-1-10
-5pa, described protective atmosphere is N
2, H
2or at least one in Ar inert gas, obtains described 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 described glass dust, described charge additive is soluble metal inorganic salts, and its consumption is the 1-5wt% of described glass dust;
In described carbon nano-tube electrophoretic liquid, the concentration of described carbon nano-tube is 0.01-0.03mg/ml, and the consumption of described charge additive is the 25-50wt% of described carbon nano-tube.
3. preparation method according to claim 1, is characterized in that, after step (3) sintering, also adopts tape-stripping, carbon nano-tube described in alignment, obtains described carbon nanotube cathod.
4. the preparation method according to any one of claim 1-3, 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, nanometer tin indium oxide powder, 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.
5. the preparation method according to any one of claim 1-3, is characterized in that, described organic solvent is at least one in methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, acetone.
6. the preparation method according to any one of claim 1-3, 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.
7. the preparation method according to any one of claim 1-3, 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.
8. the preparation method according to any one of claim 1-3, is characterized in that, described carbon nano-tube is Single Walled Carbon Nanotube, multi-walled carbon nano-tubes, at least one in the single wall of modification or multi-walled carbon nano-tubes; The diameter of described carbon nano-tube is 1-20nm, and length is 1-20 μm.
9. according to the carbon nanotube cathod that preparation method described in claim 1-8 obtains.
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