CN100437881C - Method of inproving nano-carbon tube electronic emitting performance of field emitting display - Google Patents
Method of inproving nano-carbon tube electronic emitting performance of field emitting display Download PDFInfo
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- CN100437881C CN100437881C CNB2005100538566A CN200510053856A CN100437881C CN 100437881 C CN100437881 C CN 100437881C CN B2005100538566 A CNB2005100538566 A CN B2005100538566A CN 200510053856 A CN200510053856 A CN 200510053856A CN 100437881 C CN100437881 C CN 100437881C
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Abstract
The present invention relates to a method for improving the performance of an electron emission source of a nanometer carbon pipe of an emission display, which firstly takes a cathode structure semi-product. The cathode structure and a metal panel are connected with a cathode of an electrophoresis electrode. After the cathode structure and the metal panel are connected with the cathode of an electrophoresis electrode, one side of the cathode structure to be in electrophoretic deposition and the metal panel keep a fixed distance and are arranged in parallel; the cathode structure and the metal panel after connection are arranged in solution of an electrophoresis tank, and a power supply device provides dc voltage of a cathode and an anode to form an electric field. The electrophoretic deposition of the nanometer carbon pipe is manufactured on the cathode electrode to form an electron emission source, and the cathode structure after deposition is taken out to make low temperature simple baking to remove redundant ethanol solution on the cathode structure. Auxiliary salt indium chloride and electrolytic hydroxyl ions form indium hydroxide which is sintered later, and the indium hydroxide on a cathode electrode layer is oxygenized into indium oxide again, and thereby, the electron conduction relationship of the nanometer carbon pipe and the cathode electrode layer is increased.
Description
Technical field
The present invention relates to a kind of method of improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display, relate in particular to a kind of electrophoretic deposition technique that utilizes, the CNT (carbon nano-tube) powder is deposited on cathode electrode to form electron emission source, and behind electrophoretic deposition, bake and can form the burning salt with conductivity, increase the method for the CNT (carbon nano-tube) electron emission source performance of improving Field Emission Display of the electronics output efficiency of CNT (carbon nano-tube) electron emission source layer.
Background technology
Known three-electrode field transmitting display device mainly comprises anode construction and cathode construction, between anode construction and cathode construction, be provided with eyelid retractor (spacer), provide the interval of vacuum area between anode construction and cathode construction and as the support between anode construction and cathode construction.This anode construction comprises anode substrate, anode electrode layer and fluorescent powder coating (phosphors layer); This cathode construction comprises cathode base, negative electrode layer, electron emission source layer, dielectric layer and gate layer; Wherein, this gate layer is applied in potential difference to draw the electronics ejaculation of drawing the electron emission source layer; , make electronics have fluorescent powder coating on enough kinetic energy bump (impinge) anode constructions to excite and make it luminous so that the acceleration of electron beam to be provided by high voltage that anode electrode layer provided.In view of the above, for electronics is moved in Field Emission Display, need display to be kept following vacuum degree of 10-5 holder (torr) at least, make electronics obtain good average free radius vector (mean free path), avoid the pollution in electron emission source and fluorescent material district simultaneously and poison with vacuum equipment.Therefore in addition, there are enough energy to remove to clash into fluorescent material, between two plates, appropriate gap need be arranged, make electronics have enough accelerating spaces to clash into fluorescent powder, reach and make the fluorescent material physical efficiency fully produce luminous effect for making electronics.
Wherein, this electron emission source layer is principal component with the CNT (carbon nano-tube), (Nature 354 because CNT (carbon nano-tube) (Carbonnanotubes) was proposed the back from 1991 by Iijima, 56 (1991)) possesses high characteristic electron, be applied in the multiple electronic building brick, and CNT (carbon nano-tube) can have very high length-width ratio (aspect ratio), greater than 500, and high rigidity, its young's modulus is many more than 1000GPn, and the tip of CNT (carbon nano-tube) or fault location are exposing of atom level scale, more than these characteristics therefore be considered to a kind of desirable field electron emission source (electron field emitter) material, for example electron emission source on a kind of cathode construction of Field Emission Display.Because CNT (carbon nano-tube) possesses above-described physical characteristic, therefore also can be designed to be applied in multiple manufacture process, as: wire mark or thin film manufacture process etc. uses at electronic building brick with totemization.
Wherein, the cathode construction manufacture craft is that the carbon pipe is risen material on negative electrode layer as electronics, its manufacture method can have utilizes chemical vacuum deposition (CVD) directly to form CNT (carbon nano-tube) on the negative electrode layer in this cathode pixels respectively, or a kind ofly be produced on the negative electrode layer in this pixel respectively with photosensitive type CNT (carbon nano-tube) solution totemization, also can be spraying CNT (carbon nano-tube) solution collocation guard makes, but according to the structure of the electron emission source of above-mentioned three-electrode field transmitting display device, desire is produced on CNT (carbon nano-tube) on the cathode electrode structure in each pixel, above-mentioned respectively this manufacture method still has the obstruction restriction of cost of manufacture and stereochemical structure, and the uniformity of especially large-sized electron emission source will more be difficult to reach.
Recent a kind of electrophoretic deposition EPD (Electrophoresis Deposition) technology is suggested successively, as U.S.'s application for a patent for invention US2003/0102222A1 number disclosed " nano structural material deposition process ", this application is formulated as the alcohols aaerosol solution with CNT (carbon nano-tube), and utilize magnesium, lanthanum, yttrium, aluminium plasma salt is as auxiliary salt (Charger), be made as electrophoresis solution, the cathode construction and the electrode of desire deposition are attached in this electrophoresis solution, direct current or alternating voltage are provided, in solution, form electric field, utilize auxiliary salt in solution electrolysis for ion with attached to the CNT (carbon nano-tube) powder, form with electrophoresis moving (Electrophoresis force) by electric field and to assist CNT (carbon nano-tube) to be deposited on special electrodes, thus can be on electrode with the CNT (carbon nano-tube) deposition patternsization, utilize the electrophoretic deposition technique of above-mentioned technology, can easily CNT (carbon nano-tube) be deposited on the electrode layer, and can avoid because of the restriction of three-electrode field transmitting display device on cathode construction, so this technology extensively is used in the structural making of minus plate.
Though but the electrophoretic deposition manufacturing technology is widely used, need be modified part but wherein still have, as, the ion of this auxiliary salt also will together be deposited on the electrode, and with regard to cation, usually with anionic reactive (hydroxide anion of part hydrone oxidation in the solution) the formation hydroxide salt of electrode surface, and with the same codeposition of CNT (carbon nano-tube).And must utilize high temperature to bake behind the electrophoresis process again to remove unnecessary solvent and organic substance, therefore this metalloid hydrogen-oxygen salt will be converted into burning salt through after baking simultaneously, be example with the known magnesium chloride that uses, then form magnesian salt and CNT (carbon nano-tube) common deposited on the electrode or on the CNT (carbon nano-tube) surface, and magnesium oxide is not good conductor material, though not high 0.1% weight concentration that is generally of electrophoresis process working concentration, the unlikely effect that influences CNT (carbon nano-tube) electron emission layer generation electron beam, but do not increase useful effect yet.
Other has a kind of " making low energy electrons fluorescence excitation curtain method " to be disclosed, and this method is to utilize a kind of metallic salt to cross manufacturing Cheng Houke at electrophoresis to form the metal oxide with conductive characteristic on phosphor powder layer, to improve the characteristics of luminescence of fluorescent powder.Thus, the inventor utilizes this characteristic, selects for use specific metallic salt to be dissolved in water or the alcohol solution, and bakes behind electrophoretic deposition and can form the burning salt with conductivity, to increase the electronics output efficiency of CNT (carbon nano-tube) electron emission source layer.
Content of the present invention
Main purpose of the present invention is to solve the defective that exists in the above-mentioned prior art.The present invention utilizes electrophoretic deposition technique, the CNT (carbon nano-tube) powder made from arc discharge is configured to electrophoresis solution, and select suitable auxiliary salt for use, ion after electrolysis can produce the ion dispersion effect, can make CNT (carbon nano-tube) powder dispersion effect in water or ethanol electrophoresis solution better, help the uniformity of electrophoretic deposition in cathode electrode surface.In addition, select for use suitable auxiliary salt behind electrophoretic deposition, to bake, can form burning salt, increased the electronics output efficiency of CNT (carbon nano-tube) electron emission source layer with conductivity.
To achieve these goals, the invention provides a kind of method of improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display.This method is that the CNT (carbon nano-tube) electron emission source deposition that cathode construction carries out cathode construction is made, and the negative electrode layer of this cathode construction is connected with the negative electrode of iontophoretic electrode by cathode wire, and the anode of iontophoretic electrode is connected with metal decking;
After keeping a fixed range between the cathode construction that connects and metal decking, parallel be placed on electrophoresis tank and soak put the configuration electrophoresis solution in, utilize power supply unit to provide the anode and cathode direct voltage, carry out the deposition of this CNT (carbon nano-tube) electron emission source and make to form electric field;
Above-mentioned post-depositional cathode construction is taken out the back simply bake with low temperature earlier, to remove ethanolic solution unnecessary on cathode construction.At this moment, the hydroxyl ion of auxiliary salt inidum chloride and electrolysis forms indium hydroxide, carry out sintering process afterwards again, indium hydroxide on this negative electrode layer will reoxidize and be indium oxide, because indium oxide has conductive characteristic, therefore when making negative electrode layer, except CNT (carbon nano-tube), also comprise having conductivity indium oxide particle on the electron emission source, increased the electrical conductivity relation of CNT (carbon nano-tube) and negative electrode layer.
Brief description of drawings
Fig. 1 is that (a)～(g) cathode construction of the present invention is made schematic flow sheet;
Fig. 2 is that cathode construction of the present invention is made the electron emission source schematic flow sheet;
Fig. 3 is cathode construction of the present invention and metal decking connection diagram;
Fig. 4 is cathode construction of the present invention and the schematic diagram that carries out electrophoretic deposition after metal decking is connected;
Fig. 5 finishes schematic diagram for the present invention makes CNT (carbon nano-tube) with arc discharge method.
In the accompanying drawing, the list of parts of each label representative is as follows:
The 10-cathode construction
The 1-glass substrate
The 2-negative electrode layer
The 21-electron emission source
The 3-dielectric layer
The 4-gate layer
41,31-depressed area
5,6-protective layer
The 7-electrophoresis tank
The 101-cathode wire
The 8-iontophoretic electrode
The 81-negative electrode
The 82-anode
The 9-metal decking
Embodiment
Relevant technology contents of the present invention and detailed description, existing conjunction with figs. is described as follows:
Fig. 1 (a)～(g) is that cathode construction of the present invention is made schematic flow sheet.As shown in the figure: the method for improving the high-effect high uniformity CNT (carbon nano-tube) electron emission source of Field Emission Display of the present invention, mainly be to pass through electrophoretic techniques, select for use suitable auxiliary salt to deposit and make the CNT (carbon nano-tube) electron emission source, to improve the uniformity that CNT (carbon nano-tube) is deposited on cathode construction 10 surfaces, its effect is good.
At first; on the surface of glass substrate 1, form negative electrode layer 2; on negative electrode layer 2 surfaces, form dielectric layer 3; form gate layer 4 in dielectric layer 3 surfaces again; form the depressed area 41 that dielectric layer 3 is exposed by little shadow technology on gate layer 4 surfaces again; form protective layer 5 in gate layer 4 surfaces again; form the depressed area 31 that cathode electrode 2 is exposed by etching technique on dielectric layer 3 surfaces; after protective layer 5 is peeled off; again another protective layer 6 coatings are coated on dielectric layer 3 and the gate layer 4, promptly finish the making of cathode construction.
Fig. 2 to Fig. 4 for cathode construction of the present invention make electron emission source flow process and cathode construction be connected with metal decking be connected after carry out the schematic diagram of electrophoretic deposition.As shown in the figure, treat that above-mentioned cathode construction is finished after, carry out the CNT (carbon nano-tube) electron emission source deposition of cathode construction and make;
At first, carrying out the electrophoresis solution modulation, is solvent with ethanol, adds about 1%～10% pure water (being preferably 5%), adds the CNT (carbon nano-tube) powder again.The present invention selects the CNT (carbon nano-tube) made from arc discharge for use, it is below the average carbon length of tube 5 μ m, the CNT (carbon nano-tube) structure of the average a kind of multiple wall of carbon pipe caliber below 100nm, about 0.1%～0.005% (being preferably 0.02%) of its weight concentration, add auxiliary salt (Charger) class of about 0.1%～0.005% (being preferably 0.01%) of weight concentration again, should assist salt to select for use and behind electrophoresis, can form burning salt with electroconductive oxide, as inidum chloride, and indium nitrate, or other is as any salt of tin, and the solution that above-mentioned modulation is finished is poured in the electrophoresis tank 7;
After above-mentioned electrophoresis solution modulation is finished, carry out electrophoretic deposition.The negative electrode layer 2 of field emission cathode structure 10 is connected with the negative electrode 81 of iontophoretic electrode 8 by cathode wire 101, and the anode 82 of iontophoretic electrode 8 is connected with metal decking 9, and metal decking 9 can be platinum or titanium panel;
When cathode construction 10 be connected with metal decking 9 finish after, kept a fixed range to be arranged in parallel desiring by a side of the cathode construction 10 of electrophoretic deposition and metal decking 9, and the cathode construction after will connecting 10 is placed in the electrophoresis tank 7 with metal decking 9, utilize power supply unit to provide the anode and cathode direct voltage to form electric field, this electric field strength is 2V/cm, can be 0.5～10V/cm, with the CNT (carbon nano-tube) electrophoretic deposition at negative electrode layer 2 to form electron emission source 21 (as shown in Figure 5);
Above-mentioned post-depositional cathode construction is taken out the back simply bake for 80 ℃ with low temperature earlier, to remove the unnecessary ethanolic solution on cathode construction 10.The auxiliary salt inidum chloride of this moment and the hydroxyl ion of electrolysis form indium hydroxide; carry out 400 ℃ of sintering process afterwards again with burn off protection stratification 6; and the indium hydroxide on the negative electrode layer 2 will reoxidize and be indium oxide; because indium oxide has conductive characteristic; therefore when making negative electrode layer 2; except CNT (carbon nano-tube), also comprise indium oxide particle on the electron emission source 21 with conductivity; the magnesium salts of the auxiliary salt of using can provide the moving function of electrophoresis in having processes well known, has also increased the electrical conductivity relation of CNT (carbon nano-tube) and negative electrode layer.
Further, because the present invention adopts the CNT (carbon nano-tube) electron emission source layer of electrophoretic deposition, CNT (carbon nano-tube) is easy to level and pastes in cathode electrode surface, therefore easily form uniform CNT (carbon nano-tube) layer, average thickness can be controlled in below the 2 μ m, and the salt common deposited of CNT (carbon nano-tube) behind the sintering and indium oxide and form good adhesion effect, difficult drop-off.
Further, the dispersion effect of CNT (carbon nano-tube) electrophoresis solution of the present invention is good.With the electrophoresis solution of known magnesium chloride auxiliary salt at average unit are 250 μ m
2In, its dispersing characteristic relatively can find still more than 15% that greater than the CNT (carbon nano-tube) nodule of 10 μ m, the CNT (carbon nano-tube) electrophoresis solution of using inidum chloride auxiliary salt of the present invention instead then can be controlled at the CNT (carbon nano-tube) nodule of 10 μ m below 5%.
The above only is the preferred embodiments of the present invention, be not so promptly limit claim of the present invention, the equivalent structure transformation that every utilization specification of the present invention and accompanying drawing content are done, or directly or indirectly be used in other relevant technical field, all in like manner be included in the claim of the present invention.
Claims (17)
1. method of improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display is characterized in that described method comprises:
A) get cathode construction earlier;
B) described cathode construction is carried out electrophoretic deposition, described cathode construction and metal decking are connected with iontophoretic electrode;
C) described cathode construction be connected with metal decking finish after, kept a fixed range to be arranged in parallel desiring by cathode construction one side of electrophoretic deposition and described metal decking, and the cathode construction after will connecting and metal decking are placed in the solution of electrophoresis tank, utilize power supply unit to provide the anode and cathode direct voltage, make electron emission source to carry out the CNT (carbon nano-tube) electrophoretic deposition to form electric field;
D) described post-depositional cathode construction being taken out the back bakes with low temperature earlier, to remove ethanolic solution unnecessary on cathode construction, the hydroxyl ion of this moment auxiliary salt inidum chloride and hydrolysis forms indium hydroxide, carry out sintering afterwards again, indium hydroxide on the negative electrode layer in the described cathode construction will reoxidize and be indium oxide, to increase the electrical conductivity relation of described CNT (carbon nano-tube) and negative electrode layer.
2. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 1 is characterized in that described method for making cathode structure comprises:
A) on glass baseplate surface, form described negative electrode layer, on described cathode electrode laminar surface, form dielectric layer, form gate layer in described dielectric layer surface again, form the depressed area that described dielectric layer is exposed by little shadow technology on described gate layer surface again;
B) form protective layer in described gate layer surface again, form the depressed area that described negative electrode layer is exposed on described dielectric layer surface, more described protective layer is peeled off by etching technique;
C) again another protective layer coating is coated on described dielectric layer and the gate layer, promptly finishes described cathode construction and make.
3. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 1, the negative electrode layer that it is characterized in that described cathode construction is connected with the negative electrode of iontophoretic electrode by cathode wire, and the anode of iontophoretic electrode is connected with described metal decking.
4. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 1 is characterized in that described metal decking is platinum or titanium panel.
5. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 1 is characterized in that described electric field strength is 0.5～10V/cm.
6. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 5 is characterized in that described electric field strength is 2V/cm.
7. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 1, it is characterized in that described CNT (carbon nano-tube) is a kind of CNT (carbon nano-tube) made from arc discharge, its be average carbon length of tube below 5 μ m, the CNT (carbon nano-tube) structure of the average a kind of multiple wall of carbon pipe caliber below 100nm.
8. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 1 is characterized in that the solution that is added in the described electrophoresis tank comprises: as ethanol, pure water, CNT (carbon nano-tube) powder, the auxiliary salt inidum chloride of solvent.
9. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 8, the pure water amount that it is characterized in that described interpolation is 1%～10%.
10. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 9, the pure water amount that it is characterized in that described interpolation is 5%.
11. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 8, the weight concentration that it is characterized in that the CNT (carbon nano-tube) powder of described interpolation is 0.1%～0.005%.
12. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 11, the weight concentration that it is characterized in that the CNT (carbon nano-tube) powder of described interpolation is 0.02%.
13. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 8, the weight concentration that it is characterized in that the auxiliary salt inidum chloride of described interpolation is 0.1%～0.005%.
14. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 13, the weight concentration that it is characterized in that the auxiliary salt inidum chloride of described interpolation is 0.01%.
15. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 1 is characterized in that it is simply to bake with 80 ℃ that described low temperature bakes.
16. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 1 is characterized in that described sintering is to carry out sintering process with 400 ℃.
17. the method for improving the CNT (carbon nano-tube) electron emission source performance of Field Emission Display as claimed in claim 1 is characterized in that with the CNT (carbon nano-tube) electrophoresis solution of described auxiliary salt inidum chloride at average unit are 250 μ m
2In, the CNT (carbon nano-tube) nodule of 10 μ m can be controlled at below 5%.
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| CNB2005100538566A CN100437881C (en) | 2005-03-14 | 2005-03-14 | Method of inproving nano-carbon tube electronic emitting performance of field emitting display |
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| CN100437881C true CN100437881C (en) | 2008-11-26 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030102222A1 (en) * | 2001-11-30 | 2003-06-05 | Zhou Otto Z. | Deposition method for nanostructure materials |
| US6616497B1 (en) * | 1999-08-12 | 2003-09-09 | Samsung Sdi Co., Ltd. | Method of manufacturing carbon nanotube field emitter by electrophoretic deposition |
| CN1570220A (en) * | 2004-04-23 | 2005-01-26 | 清华大学 | Process for preparing carbon nano tube film through electrophoresis deposition |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6616497B1 (en) * | 1999-08-12 | 2003-09-09 | Samsung Sdi Co., Ltd. | Method of manufacturing carbon nanotube field emitter by electrophoretic deposition |
| US20030102222A1 (en) * | 2001-11-30 | 2003-06-05 | Zhou Otto Z. | Deposition method for nanostructure materials |
| CN1570220A (en) * | 2004-04-23 | 2005-01-26 | 清华大学 | Process for preparing carbon nano tube film through electrophoresis deposition |
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