CN1293649C - Preparation method of large surface area carbon nano pipe film for field emitting display cathode - Google Patents
Preparation method of large surface area carbon nano pipe film for field emitting display cathode Download PDFInfo
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- CN1293649C CN1293649C CNB2004100258128A CN200410025812A CN1293649C CN 1293649 C CN1293649 C CN 1293649C CN B2004100258128 A CNB2004100258128 A CN B2004100258128A CN 200410025812 A CN200410025812 A CN 200410025812A CN 1293649 C CN1293649 C CN 1293649C
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Abstract
The present invention discloses a preparation method of large surface area carbon nano pipe film cathodes for field emitting displays, which comprises substrate and carbon nano pipe pretreatment, cathode conductive pattern formation, adhesive coating, carbon nano pipe gasoloid (or other forms of disperse phases) formation, formation deposition on a substrate, carbon nano pipe film dring and sintering, etc. The deposition density of a carbon nano pipe film can be changed through adjusting the content and the deposition time of the carbon nano pipe in a disperse phase. The deposition shape of the carbon nano pipe film can be changed by changing the distribution of an electrostatic field. A cathode of super large screen carbon nano pipe field emitting flat plate display can be manufactured by adopting a movable nozzle system or multiple nozzle system. The manufacturing method provided the present invention has the advantages of simple operation and low cost and can be manufactured under an open environment. The manufactured carbon nano pipe film has the advantages of uniform large area, good arrangement and simple localization and has superior characteristic of field emission.
Description
Technical field
The invention belongs to the crossing domain of vacuum microelectronics technique and nanometer technology, be specifically related to utilize electrostatic field and charged carbon nano-tube self CHARGE DISTRIBUTION with the carbon nano-tube oriented substrate surface that is implanted in, form the preparation method of the field-transmitting cathode that has a potential-jump barrier or surface potential barrier at least, particularly a kind of large tracts of land carbon nano-tube film preparation method who is used for cathode of field emission display.
Background technology
Carbon nano-tube field emission display negative electrode technology of preparing mainly contains screen printing technique and direct growth technology two big groups at present.Silk screen print method has advantage simple to operate, but is being restricted aspect the manufacturing high-resolution display panel.This method is normally mixed carbon nano-tube with pulping material, make the slurry of available silk screen process, is printed on the substrate then.Most of pulping material is removed in annealed roasting, thereby makes the carbon nanotube cathod film.The carbon nano-tube thin film cathode of this method gained owing to have only the fraction carbon nano-tube to expose its tip from backing material and remaining pulping material, is difficult to obtain big field emission.Owing to be subjected to the restriction of silk screen printing precision, these class methods are difficult to realize high-precision cathode pattern, therefore are being restricted aspect the manufacturing high-resolution display panel.It also is difficult to make the carbon nano-tube vertical forming in substrate surface in addition; Each launch point is difficult to keep uniformity and bigger current density preferably.And the direct growth method can obtain the selective growth of carbon nano-tube at an easy rate by graphical distribution metallic catalyst, and emission characteristics also is better than the cathode thin film of silk screen print method preparation.But it also has following problem: because growth temperature is higher, make that suitable backing material is limited, and be difficult to keep on large tracts of land evenly; When the growing large-area cathode thin film, the input of equipment and cost of goods manufactured will significantly rise.
Summary of the invention
Defective or deficiency at above-mentioned prior art exists the objective of the invention is to, and the advantage of integrated prior art provides that a kind of technology is simple, cost is low, is fit to make the large tracts of land carbon nano-tube film preparation method of cathode of field emission display.
The solution that the present invention adopts is that the self-orientating carbon nano-tube film that utilizes electrostatic field and charged carbon nano-tube self CHARGE DISTRIBUTION transplants that (said localization is transplanted and is meant that carbon nano-tube deposits by predetermined figure, the non-localized transplanting then is the non-pattern sedimentation at whole cathode zone), may further comprise the steps:
(1) cleaning of backing material
For the surface backing material of conductive layer is arranged, the ultrasonic cleaning that substrate carries out standard is got final product with absolute alcohol or acetone or organic solvent or their mixture; There is not the backing material of conductive layer for the surface, also need be after above-mentioned cleaning at the surface preparation conductive layer; Conductive layer adopts deposition, plating or method of printing preparation;
(2) purifying of carbon nano-tube and dispersion
The catalyst that exists in the preparation process carbon nano-tube with the molten carbon elimination nanotube of red fuming nitric acid (RFNA); And be washed with distilled water to neutral back intensive drying, and fully grind under dry environment with ball mill then, reduce bigger agglomerated particle;
(3) formation of negative electrode conductive pattern
The negative electrode conductive pattern mainly is meant and meets conductive layer certain design, that have definite shape.Adopt common photoetching process, conductive layer is carried out processing such as photoetching and corrosion, can obtain required cathode pattern.Do not have the backing material of conductive layer for the surface, can obtain required figure by plate-making and method of printing.
(4) coating binding agent
Binding agent can be coated on the method for silk screen printing or electrostatic spray on the negative electrode conductive pattern.The domain of the half tone that silk screen printing is used is consistent with the negative electrode conductive pattern.
(5) formation and the injection of carbon nano-tube aerosol (or other forms of decentralized photo)
Impact methods such as pretreated carbon nano-tube of process or employing mechanical oscillation with high velocity air and all can form the carbon nano-tube aerosol.
Also even carbon nanotube can be dispersed in and make the carbon nano-tube slurry in certain binding agent, directly carry out electrostatic spraying on conductive pattern, can save technical process (3) this moment.
The injection of carbon nano-tube aerosol or carbon nano-tube slurry can adopt common electrostatic spraying device to be achieved.Carbon nano-tube aerosol or carbon nano-tube slurry are transported to the nozzle place of spray gun under the conveying of carrier gas, near nozzle, obtain by discharge tip by electric charge that corona discharge produced, and form charged carbon nanotube powder, then form charged drop for the carbon nano-tube slurry, enter then in the highfield that between discharge tip and conductive pattern, forms;
(6) carbon nano-tube is in the deposition of substrate
Charged powder or charged drop itself charged electrically opposite with the polarity of conductive pattern, stick on the conductive pattern so can under the acting in conjunction of electric field force and strength conveying, fly under conductive pattern and the effect at binding agent.Because the electric field of substrate one end mainly concentrates on the zone at conductive pattern place,, and form the carbon nano-tube film that figure conforms to it so charged powder or charged drop will only be deposited on the zone at conductive pattern place.
(7) drying of carbon nano-tube film and sintering
Carbon nano-tube is after deposition on the substrate, prepared film can be dried in drying equipment, carry out sintering processes then, when sintering temperature is higher, can carry out sintering under inert gas shielding, its sintering temperature is changed to: be raised to 200 ℃ by room temperature in (1) 20 minute; (2) constant temperature is 10 minutes; Be raised to 400 ℃ by 200 ℃ in (3) 20 minutes; (4) constant temperature is 15 minutes; Drop to 200 ℃ by 400 ℃ in (5) 20 minutes; (6) outage cools to room temperature with the furnace.
When using method of the present invention to prepare carbon nano-tube thin film cathode, regulate content and the sedimentation time settled density that can change carbon nano-tube film of carbon nano-tube in decentralized photo, the distribution pattern that changes electrostatic field can change the depositing of thin film shape; Be coated with binding agent on the substrate or in precursor, adding binding agent and all can improve the adhesive force of film on substrate.Adopt method of the present invention can make the negative electrode of jumbotron carbon nanotube field emission plane display, has advantage simple to operate, with low cost, that can under open environment, make, prepared carbon nano-tube film have large tracts of land evenly, arrange good, the simple advantage of localization, have excellent field emission characteristic.
Description of drawings
Fig. 1 is the preparation facilities schematic diagram of carbon nano-tube thin film cathode;
Fig. 2 is aerocolloidal formation of carbon nano-tube and conveying device schematic diagram;
Fig. 3 is a schematic diagram of making the overlarge area film cathode with the movable spray system, and moving nozzle or mobile substrate all can reach the effect of even injection.
Fig. 4 is a schematic diagram of making the overlarge area film cathode with the multiinjector system, and wherein, the multiinjector system can be a nozzle array, also can be listed as mobile multiinjector system by the row or that a plurality of nozzles are formed.
Symbolic representation among above-mentioned each figure divides other to be: 1 is substrate, 2 is conductive pattern, 3 is carbon nano-tube, and 4 is nozzle, and 5 is high voltage source, 6 for being in the charged carbon nanotube powder in the electrostatic field, 7 for producing the aerocolloidal container of carbon nano-tube, and 8 is screen cloth, and 9 is inlet for pressurised gas, 10 is carrier gas inlet, and 11 is carbon nano-tube aerosol delivery outlet.
Embodiment
The useful technique effect that is produced with the present invention for a more clear understanding of the present invention, the present invention is described in more detail below in conjunction with embodiment that accompanying drawing and inventor provide, but the invention is not restricted to these embodiment.
According to technique scheme, the present invention includes following steps:
(1) cleaning of backing material
For the surface backing material of conductive layer is arranged, the ultrasonic cleaning that substrate carries out standard is got final product with absolute alcohol or acetone or organic solvent or their mixture; There is not the backing material of conductive layer for the surface, also need be after above-mentioned cleaning at the surface preparation conductive layer; Conductive layer adopts deposition, plating or method of printing preparation;
(2) purifying of carbon nano-tube and dispersion
Because the catalyst that uses in the preparation process of carbon nano-tube can exist in carbon nano-tube, so it should be removed during use.Detailed process is the catalyst that exists in the preparation process carbon nano-tube with the molten carbon elimination nanotube of red fuming nitric acid (RFNA); And be washed with distilled water to neutral back intensive drying, and fully grind under dry environment with ball mill then, reduce bigger agglomerated particle;
(3) formation of negative electrode conductive pattern
Adopt common photoetching process, conductive layer is carried out processing such as photoetching and corrosion, can obtain required cathode pattern.Do not have the backing material of conductive layer for the surface, can obtain required figure by plate-making and method of printing.
(3) coating binding agent
Binding agent can be coated on the method for silk screen printing or electrostatic spray on the negative electrode conductive pattern.The domain of the half tone that silk screen printing is used is consistent with the negative electrode conductive pattern.
(4) formation and the injection of carbon nano-tube aerosol (or other forms of decentralized photo)
Impact methods such as pretreated carbon nano-tube of process or employing mechanical oscillation with high velocity air and all can form the carbon nano-tube aerosol.Also even carbon nanotube can be dispersed in and make the carbon nano-tube slurry in certain binding agent, directly carry out electrostatic spraying on conductive pattern, can save technical process (3) this moment.
The injection of carbon nano-tube aerosol or carbon nano-tube slurry can adopt common electrostatic spraying device to be achieved.
(5) carbon nano-tube is in the deposition of substrate
Carbon nano-tube aerosol or carbon nano-tube slurry obtain near nozzle by discharge tip by electric charge that corona discharge produced, and form charged carbon nanotube powder or the formed charged drop of carbon nano-tube slurry, enter then in the highfield that between discharge tip and conductive pattern, forms.Because charged powder or charged drop itself institute is charged electrical opposite with the polarity of conductive pattern, stick on the conductive pattern so can under the acting in conjunction of electric field force and strength conveying, fly under conductive pattern and the effect at binding agent.
(6) drying of carbon nano-tube film and sintering
Carbon nano-tube is after deposition on the substrate, prepared film can be dried in drying equipment, carry out sintering processes then, when sintering temperature is higher, can carry out sintering under inert gas shielding, its sintering temperature is changed to: be raised to 200 ℃ by room temperature in (1) 20 minute; (2) constant temperature is 10 minutes; Be raised to 400 ℃ by 200 ℃ in (3) 20 minutes; (4) constant temperature is 15 minutes; Drop to 200 ℃ by 400 ℃ in (5) 20 minutes; (6) outage cools to room temperature with the furnace.
The item that adopts method of the present invention should be noted that:
A) change aerocolloidal concentration of carbon nano-tube or sedimentation time, can change the density of the carbon nano-tube that deposits on the patterned conductive layer;
B) also can adopt the method for heated substrate to carry out synchronous drying while depositing;
C) nozzle depends on factors such as voltage height, air velocity and expection spray area to the distance of substrate;
D) adopt moving nozzle system or multiinjector system, can make the negative electrode of jumbotron carbon nanotube field emission plane display.When using the moving nozzle system, both can moving nozzle, also can mobile substrate, promptly relatively move as long as produce between nozzle and the substrate.When using the multiinjector system, the single-row multiinjector system that can be listed as, the also nozzle array that can form by a plurality of nozzles by the independent row or that a plurality of nozzles are formed.When making more large-area cathode thin film, also can adopt moving nozzle row system.
Influence for avoiding may causing uniformity owing to edge effect can make projected area greater than graphics area during spraying; Can make (containing moving nozzle row system) the initial coverage of injection and stop all places of certain distance outside the distance substrate of coverage for the moving nozzle system.
Below be the embodiment that the inventor provides.
Embodiment 1: the parallel strip negative electrode of making the small field emission flat panel display with X-Y addressing
Its manufacture process is as follows:
1. the selection of substrate and preliminary treatment
Present embodiment adopts and has the glass (following abbreviation ito glass) of ITO conductive layer as substrate.Selected glass is put into by absolute alcohol and acetone by the cleaning fluid that 1: 1 volume ratio mixes, carried out 15 minutes ultrasonic cleaning, used the deionized water ultrasonic cleaning then 15 minutes, under clean environment, dry standby.
2. the preliminary treatment of carbon nano-tube
The carbon nano-tube that present embodiment adopts is by the multi-walled carbon nano-tubes of CVD method preparation, wherein contains the more impurity based on catalyst granules (mainly being iron and oxide thereof).Its preliminary treatment mainly is these impurity that remove wherein, makes the carbon nanotube dust that does not have agglomerated particle (or agglomerated particle is the least possible) then.Detailed process is: with the molten catalyst that goes of red fuming nitric acid (RFNA), and be washed with distilled water to neutral back intensive drying, fully grind to reduce agglomerated particle under dry environment with ball mill then.(chemistry cuts off)
3. the formation of negative electrode conductive pattern
The negative electrode conductive pattern that present embodiment relates to is one group of strip shaped electric poles parallel to each other.Detailed process is: the mask that (1) preparation photolithographic exposure is used; (2) on the ITO layer, apply photoresists; (3) give baking (4) exposure; (5) develop; (6) post bake; (7) corrosion; (8) remove photoresist.
4. adhesive stripe-coating
Binding agent can be coated on the method for silk screen printing on the negative electrode conductive pattern.The domain of the half tone that silk screen printing is used is consistent with the negative electrode conductive pattern.
5. aerocolloidal formation of carbon nano-tube and injection
Impact through pretreated carbon nanotube dust with high velocity air (as compressed air), can form the carbon nano-tube aerosol.The effect of screen cloth is the bigger agglomerated particle of filtering among Fig. 2.Carrier gas air inlet among this figure shouldn't, be carrier gas directly promptly with compressed air.The carbon nano-tube aerosol spraying can adopt common electrostatic spraying device to be achieved.
6. carbon nano-tube is in the deposition (deposit) of substrate
Near carbon nano-tube aerosol discharge tip place nozzle is charged, and forms charged carbon nanotube powder, enters then in the highfield that forms between discharge tip and conductive pattern.Charged powder flies under conductive pattern and the effect at binding agent under the acting in conjunction of electric field force and strength conveying and sticks on the conductive pattern.For guaranteeing the uniformity on whole area of prepared negative electrode, need to adjust the distance of nozzle to substrate, make projected area greater than Substrate Area.
7. the drying of carbon nano-tube film and sintering
Carbon nano-tube can be dried prepared film after deposition on the substrate in the drying equipment of uniform temperature, carry out sintering processes then.Sintering temperature curve is: be raised to 200 ℃ by room temperature in (1) 20 minute; (2) constant temperature is 10 minutes; Be raised to 400 ℃ by 200 ℃ in (3) 20 minutes; (4) constant temperature is 15 minutes; Drop to 200 ℃ by 400 ℃ in (5) 20 minutes; (6) outage cools to room temperature with the furnace.Take out sample, preparation work is finished.
Embodiment 2: the parallel strip negative electrode of making the long strip type Field Emission Display with X-Y addressing
The manufacture process of present embodiment is identical with embodiment 1, and difference is to have adopted the moving nozzle system in step 5, certainly, adopts nozzle rows to spray also and can finish preparation.
Embodiment 3: the parallel strip negative electrode of making the large-scale Field Emission Display with X-Y addressing
The manufacture process of present embodiment is identical with embodiment 1, and difference is 1) photoetching ITO changes printed silver slurry bar into; 2) in step 5, adopted moving nozzle row spraying system, certainly, adopted nozzle rows to spray also and can finish preparation.
Claims (7)
1. a large tracts of land carbon nano-tube film preparation method who is used for cathode of field emission display is characterized in that, utilizes the self-orientating carbon nano-tube film localization of electrostatic field and charged carbon nano-tube self CHARGE DISTRIBUTION and non-localized to transplant; May further comprise the steps:
(1) cleaning of backing material
For the surface backing material of conductive layer is arranged, the ultrasonic cleaning that substrate carries out standard is got final product with absolute alcohol or acetone or organic solvent or their mixture; There is not the backing material of conductive layer for the surface, also need be after above-mentioned cleaning at the surface preparation conductive layer; Conductive layer adopts deposition, plating or method of printing preparation;
(2) purifying of carbon nano-tube and dispersion
The catalyst that exists in the preparation process carbon nano-tube with the molten carbon elimination nanotube of red fuming nitric acid (RFNA); And be washed with distilled water to neutral back intensive drying, and fully grind under dry environment with ball mill then, reduce bigger agglomerated particle;
(3) formation of negative electrode conductive pattern
Adopt common photoetching process, conductive layer is carried out processing such as photoetching and corrosion, obtain required meeting design and have the cathode pattern of given shape; Do not have the backing material of conductive layer for the surface, obtain required figure by plate-making and method of printing;
(4) coating binding agent
Binding agent can be coated on the negative electrode conductive pattern with the method for silk screen printing or electrostatic spray; The domain of the half tone that silk screen printing is used is consistent with the negative electrode conductive pattern;
(5) aerocolloidal formation of carbon nano-tube and injection
Impact through pretreated carbon nano-tube or adopt mechanical vibration method all can form the carbon nano-tube aerosol or even carbon nanotube is dispersed in and make the carbon nano-tube slurry in certain binding agent with high velocity air, directly on conductive pattern, carry out electrostatic spraying;
Common electrostatic spraying device is adopted in the injection of carbon nano-tube aerosol or carbon nano-tube slurry; Carbon nano-tube aerosol or carbon nano-tube slurry are transported to the nozzle place of spray gun under the conveying of carrier gas, near nozzle, obtain by discharge tip by electric charge that corona discharge produced, and form charged carbon nanotube powder, then form charged drop for the carbon nano-tube slurry, enter then in the highfield that between discharge tip and conductive pattern, forms;
(6) carbon nano-tube is in the deposition of substrate
Charged powder or charged drop enter behind the highfield that forms between discharge tip and the conductive pattern, because institute itself is charged electrical opposite with the polarity of conductive pattern, under the acting in conjunction of electric field force and strength conveying, on conductive pattern, move, stick on the conductive pattern until arriving under conductive pattern and the effect at binding agent;
(7) drying of carbon nano-tube film and sintering
Carbon nano-tube is after deposition on the substrate, prepared film can be dried in drying equipment, carry out sintering processes then, when sintering temperature is higher, carry out sintering under inert gas shielding, its sintering temperature is changed to: 1. be raised to 200 ℃ by room temperature in 20 minutes; 2. constant temperature is 10 minutes; 3. be raised to 400 ℃ by 200 ℃ in 20 minutes; 4. constant temperature is 15 minutes; 5. drop to 200 ℃ by 400 ℃ in 20 minutes; 6. outage cools to room temperature with the furnace.
2. the large tracts of land carbon nano-tube film preparation method who is used for cathode of field emission display as claimed in claim 1, it is characterized in that, employing is dispersed in even carbon nanotube and makes the carbon nano-tube slurry in certain binding agent in step (5), when directly on conductive pattern, carrying out electrostatic spraying, technical process (4) can be saved.
3. the large tracts of land carbon nano-tube film preparation method who is used for cathode of field emission display as claimed in claim 1, it is characterized in that, by patterned electrode electrostatic field is distributed by predetermined pattern, thereby realize that carbon nano-tube film carries out localization and aligns by predetermined cathode pattern on substrate; The distribution that changes electrostatic field makes carbon nano-tube by new figure deposition.
4. as claim 1 or the 3 described large tracts of land carbon nano-tube film preparation methods that are used for cathode of field emission display, it is characterized in that described electrostatic spray adopts movable spray system or multiinjector system to guarantee the uniformity of prepared film in the overlarge area scope.
5. the large tracts of land carbon nano-tube film preparation method who is used for cathode of field emission display as claimed in claim 4 is characterized in that, described movable spray system comprises single injector movable spray system or multiinjector movable spray system.
6. the large tracts of land carbon nano-tube film preparation method who is used for cathode of field emission display as claimed in claim 5 is characterized in that, described multiinjector system is a row or a row nozzle, or nozzle array.
7. as claimed in claim 5ly be used for the big of cathode of field emission display and carbon distribution nano-tube film preparation method is characterized in that, when adopting the moving nozzle system, moving nozzle, or mobile substrate promptly relatively move as long as produce between nozzle and the substrate.
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| CN1669668B (en) * | 2005-04-08 | 2011-05-04 | 华南理工大学 | Synchronous load quick film-forming method for nano functional film |
| CN1315147C (en) * | 2005-05-24 | 2007-05-09 | 中原工学院 | Panel display of high integration grid structure and manufacturing technology thereof |
| CN100395171C (en) * | 2005-07-07 | 2008-06-18 | 上海交通大学 | Method for preparing nano carbon tube micro structure |
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| CN100371060C (en) * | 2005-09-30 | 2008-02-27 | 清华大学 | Method for assisting dispersal of carbonate nano tube in liquid medium by electric field |
| CN1959896B (en) * | 2005-11-04 | 2011-03-30 | 鸿富锦精密工业（深圳）有限公司 | Field emission of Nano carbon tube, and preparation method |
| CN101192492B (en) * | 2006-11-22 | 2010-09-29 | 清华大学 | Transparent conductive film preparation method |
| CN101192493B (en) * | 2006-11-22 | 2011-02-02 | 鸿富锦精密工业（深圳）有限公司 | Anode device and its producing method |
| CN101458599B (en) * | 2007-12-14 | 2011-06-08 | 清华大学 | Touch screen, method for producing the touch screen, and display device using the touch screen |
| CN101339872B (en) * | 2008-08-15 | 2011-04-06 | 西安交通大学 | Double layer mixing structure carbon nano tube membrane field emission cathode and preparation thereof |
| CN101943850B (en) * | 2009-07-03 | 2013-04-24 | 清华大学 | Sound-producing screen and projection system using same |
| CN102725127B (en) * | 2009-11-24 | 2015-06-10 | 克劳斯·卡尔瓦尔 | Method for surface treating a substrate and device for carrying out the method |
| CN104724670A (en) * | 2014-09-03 | 2015-06-24 | 青岛科技大学 | Manufacturing method of composite material of doped aligned carbon nanotubes |
| CN105016627A (en) * | 2015-06-10 | 2015-11-04 | 青岛科技大学 | Carbon nano-tube conductive glass preparation method |
| CA2899255A1 (en) * | 2015-07-31 | 2017-01-31 | National Research Council Of Canada | Apparatus and method for aerosol deposition of nanoparticles on a substrate |
| CN113088086B (en) * | 2021-04-07 | 2022-08-30 | 青岛科技大学 | Filling method of directionally reinforced organic silicone grease based on carbon nano tube/nano silicon carbide gas-phase dispersed mist |
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| US20030151352A1 (en) * | 2002-01-15 | 2003-08-14 | Kabushiki Kaisha Y.Y.L. | Field emitting apparatus and method |
| KR20030097165A (en) * | 2002-06-19 | 2003-12-31 | (주)서브나노 | field emitter of field emission display device and the manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20030151352A1 (en) * | 2002-01-15 | 2003-08-14 | Kabushiki Kaisha Y.Y.L. | Field emitting apparatus and method |
| KR20030097165A (en) * | 2002-06-19 | 2003-12-31 | (주)서브나노 | field emitter of field emission display device and the manufacturing method thereof |
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