CN102097268B - Method for preparing carbon nanotube secondary structure of PDP (Plasma Display Panel) - Google Patents
Method for preparing carbon nanotube secondary structure of PDP (Plasma Display Panel) Download PDFInfo
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- CN102097268B CN102097268B CN201110009675.9A CN201110009675A CN102097268B CN 102097268 B CN102097268 B CN 102097268B CN 201110009675 A CN201110009675 A CN 201110009675A CN 102097268 B CN102097268 B CN 102097268B
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- carbon nanotube
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Abstract
The invention relates to a carbon nanotube secondary structure for a PDP (Plasma Display Panel) and a preparation method of the carbon nanotube secondary structure, belonging to the technical field of PDPs. The method comprises the following steps of: sputtering a seed layer on a medium layer by the pretreatment of a PDP front plate; sequentially carrying out photoresist spin-coating, photoresist baking, exposure and development on the seed layer, and reserving an appointed area to which a structure of the carbon nanotube is added; carrying out mask composite electric plating, composite chemical plating or electrophoresis on the appointed area, and growing a composite carbon nanotube structure, namely pre-treating the carbon nanotube and adding the pre-dispersed carbon nanotube to electric plating, chemical plating or electrophoresis basic liquid to grow the composite carbon nanotube structure; respectively dipping and etching by acetone or alcohol, removing the photoresist, washing the photoresist, and removing the seed layer by an alkalic Cu etching liquid and Cr etching liquid to obtain the carbon nanotube secondary structure. The method disclosed by the invention can generate more starting electrons; in addition, the distribution rate of electrons from the discharging energy can be increased due to a great number of electrons in the discharging process, thereby improving the luminous efficiency.
Description
Technical field
What the present invention relates to is a kind of method of plasma scope technical field, specifically a kind of preparation method of the carbon nano-tube supplementary structure for plasma scope.
Background technology
Plasma scope (PDP) was born in the U.S. early than 1964, had experienced after this semicentennial development, no matter was at device material or aspect technology, had all obtained very fast progress.Material aspect, dielectric layer, fluorescent material, specific substrate glass, mgo protection layer, novel barrier material etc. have obtained effective developmental research; Technology aspect, manually addressing, automatic addressing, novel Driving technique, new barrier structure etc. are all progressively developed research; In above these technology and material development, the pixel of PDP is promoted rapidly.Exactly because the emerging in an endless stream of this continuous innovation, new material and technology, development to key technology etc. have impelled at present the explosive development of large size plasma TV for a period of time.Although the research to PDP and finished productization have all experienced ripe developing stage, it remains more weak point so far.Wherein light efficiency is low, energy consumption is high, production cost height is its topmost shortcoming.But meanwhile, PDP compares with OLED (organic electroluminescent LED display) etc. the advantage can't neglect with its current main market competition opponent CRT (rear-projection TV), LCD (liquid crystal display): screen does not exist focus issues, ultra-thin and ultra-light; Wide visual angle broad view, color reducibility is good, colour gamut is wide, color is more bright-coloured, large scale advantage, the corresponding time is fast, dynamic image is clear.These advantages are all that other Display Techniques are too far behind to catch up.The development trend of following TV will be high definition, large-screen and 3D, and plasma display exactly takes advantage in these areas.If so can improve or overcome the defect of PDP, the continuation research and development of PDP technology are had very large necessity and are worth place.
For household electrical appliance, the power consumption principal element that to be consumer consider in the time selecting TV, is a urgent task so reduce PDP energy consumption.The power consumption of plasm TV belongs to dynamic power consumption, the power that is different picture brightness consumption is also different, with the bright dark dynamic change of picture, and the difference of picture brightness relies on control spark rate to realize, if so can reduce the driving voltage of each electric discharge, the power consumption that just can realize light and shade picture is all reduced.
The reduction of driving voltage can be by realizing the improvement of PDP structure, material, discharge gas.In general, electrode spacing is less, discharge space is less, driving voltage is less, but this can cause the reduction of light efficiency, brightness etc. simultaneously, so need to consider, therefore the structure of present plasma display has been close to optimization, the space that reduces driving by change structure is very little; The material higher with secondary electron reflectivity replaces magnesium oxide, can reduce undoubtedly driving voltage, but this new material seek and research aspect also have Hen Chang road to go away; Be equally also double-edged sword for the change of discharge gas component or pressure, when reducing driving voltage, also can make light efficiency reduce.
Through the retrieval of prior art is found, Won Tae LEE etc. are at Jpn.J.Appl.Phys.Vol.41 (2002) pp.6550-6552, Part 1, No.11A, in the article " MgO/Carbon Nanotubes Protective Layerin AC-Plasma Display Panels " that November 2002 delivers, carbon nano-tube is incorporated in the middle of PDP device.Manufacture method is carbon nano-tube is mixed with glass dust and add other auxiliary agents as carbon nano tube paste, carbon nano-tube is printed on the dielectric layer of PDP front panel by the method for silk screen printing, then heat-treats; Its another method is with chemical vapour deposition (CVD), the carbon nano-tube Direct precipitation of preparing to be had on the PDP dielectric layer of nickel in sputter in advance.The method mainly contains two weak points, and one is carbon nano-tube to be incorporated into whole front panel can greatly affect undoubtedly the light transmittance of PDP; Due to the restriction of manufacture method, carbon nano-tube can lie low on matrix in addition, thereby causes field emission performance poor.
Summary of the invention
The present invention is directed to prior art above shortcomings, a kind of preparation method of the carbon nano-tube supplementary structure for plasma scope is provided, make cold cathode transmitting can produce more startup electronics, to reduce driving voltage.In discharge process, there is in addition more substantial electronics, can increase the apportionment ratio of discharge energy to electronics, improve luminous efficiency.
The present invention is achieved by the following technical solutions:
The preparation method of a kind of carbon nano-tube supplementary structure of the present invention, comprises the following steps:
The first step, the preliminary treatment of PDP front panel, sputter Cr-Cu Seed Layer on dielectric layer.
Described PDP front panel refers to conventional surface discharge type AC plasma display (AC-PDP) front panel, comprises address electrode, the glass dust dielectric layer of front panel glass basis, transparency electrode and bus electrode composition.
Described preliminary treatment refers to carries out physics scouring with nano-calcium carbonate furnishing pasty state, to produce cleaning and to have the surface of suitable crude rugosity, then cleans and dries; The thickness of described Cr-Cu Seed Layer is 100-1000nm.
The thickness of described Cr-Cu Seed Layer is 100-1000nm.
Second step, in Seed Layer, carry out successively spin coating photoresist, drying glue, exposure, development, reserve the appointed area that will add carbon nano tube structure.
Described photoresist thickness is 2-10 μ m.
Described spin coating, big vast glue, exposure, development refer to be undertaken photoresist graphically by UV photoetching technique.
Part that photoresist is developed, that need growing mixed structure that described appointed area refers to, determines graphics shape according to actual requirement.
The 3rd step, the plating of mask composite plating, composite chemical or electrophoresis are carried out in the region of specifying, grow composite carbon nanometer tube structure: carbon nano-tube is carried out pre-treatment and the carbon nano-tube after pre-dispersed carried out under the mode of magnetic agitation, air stirring or ultrasonic agitation to Composite Coatings or electrophoresis with the ratio of 2-10g/L.
Described pre-treatment refers to: carbon nano-tube carried out after ball milling dispersion, and with reflow treatment 1-3h at contain sulfuric acid and nitric acid mixed sour 60-70 DEG C, cooling repeatedly clean to neutrality with deionized water afterwards, last filtering drying.
Described pre-dispersed referring to: adopt ultrasonic dispersion and add dispersant or carry out high-speed homogenization processing, then carbon nano-tube adds in the basic plating solution of plating.
Described Composite Coatings, also needs to control basic plating solution composition (conventional electroplate liquid, chemical plating fluid), current density (0.5-6A/dm in its preparation process
2), the parameter such as plating solution pH value (2-7), temperature (20-70 DEG C), by regulating and appropriately combined these technological parameters, can control laminated film quality and the carbon nano-tube compound quantity in laminated film.
Described electrophoresis, in its preparation process, also need to control the selection (water, ethanol, isopropyl alcohol) of electrophoresis basal liquid, the parameter such as selection and concentration (magnesium nitrate or cationic surfactant 1-20g/L), electrophoretic voltage (3-20V) and temperature (5-40 DEG C) of additive, thereby control dispersiveness and the compactness of final carbon nano tube structure.
The 4th step, respectively sample is soaked to etching with acetone or alcohol, remove photoresist, finally use washed with de-ionized water; Finally remove Cr-Cu Seed Layer completely with alkaline Cu etching liquid and Cr etching liquid respectively, obtain carbon nano-tube supplementary structure.
The present invention relates to the carbon nano-tube supplementary structure that said method prepares, comprise: glass substrate, glass dust dielectric layer, ito transparent electrode, bus electrode, assisted recombination structure, MgO protective layer, barrier and addressing electrode, wherein: assisted recombination structure, MgO protective layer and barrier lay respectively at, under between two glass dust dielectric layers being oppositely arranged, upper glass powder dielectric layer, bus electrode and ito transparent electrode from top to bottom arrange successively, lower-glass powder dielectric layer is placed on addressing electrode, two glass substrates are arranged at respectively, the outside of lower-glass powder dielectric layer.
Described barrier is perpendicular to glass substrate and the gap between MgO protective layer and lower-glass powder dielectric layer and be connected with lower-glass powder dielectric layer.
The invention has the advantages that:
(1) when the introducing of carbon nano-tube supplementary structure makes the reduction of PDP driving voltage, light efficiency can get a promotion; (2) position of supplementary structure is made in to the just position to bus electrode in manufacturing process, there is same shape with bus electrode, thereby avoided it to additionally the stopping of visible ray, with do not add supplementary structure compared with, can not affect the aperture opening ratio of PDP panel; (3) adopt the manufacture craft of composite plating, ensured the good field emission performance of carbon nano-tube supplementary structure.
Brief description of the drawings
Fig. 1 adds the PDP global sections figure of supplementary structure;
The PDP front-panel structure figure that Fig. 2 supplementary structure and address electrode drive altogether;
The PDP front-panel structure figure that Fig. 3 supplementary structure drives separately;
Fig. 4 supplementary structure does not add the PDP front-panel structure figure of driving;
In figure: 1 glass substrate, 2 glass dust dielectric layers, 3ITO transparency electrode, 4 bus electrodes, 5 assisted recombination structures, 6 MgO protective layers, 7 barriers, 8 addressing electrodes, 9 address electrodes add drive end, 10 supplementary structures add drive end.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented under taking technical solution of the present invention as prerequisite, provided detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Preparation Ni base carbon nanotube supplementary structure
(1) carry out physics with nano-calcium carbonate furnishing pasty state and clean PDP front panel, be neither polymerized to water droplet and also do not become under plume until be attached to surperficial water, then after ultrasonic washing, at 60-80 DEG C, dry 30-60min.
(2) sputter 500nm thickness C r-Cu Seed Layer.
(3) in Seed Layer, carry out successively spin coating 5 μ m photoresists, the mask plate of the figure that then drying glue successively, use drive altogether does mask and carries out UV exposure, development.
(4) take Single Walled Carbon Nanotube 10g, carry out 4h under ball milling 500rpm, then use sulfuric acid: nitric acid=3: reflow treatment 2h at 60 DEG C of 1 nitration mixture, cleans to neutrality last vacuum drying repeatedly with deionized water.
(5) preparation electronickelling solution, (as watt plating solution: nickelous sulfate 250g/L, nickel chloride 45g/L, boric acid 30g/L), carrying out successively charcoal treatment, filtering, add additive and dispersant, light current solution, adjust pH value is 4.0.
(6) carbon nano-tube accurately taking after a certain amount of pre-treatment joins in above-mentioned nickel-plating liquid, makes the concentration of carbon nano-tube be controlled at 2～10g/L.
(7) under air stirring and ultrasonic auxiliary stirring, carry out composite plating, grow Ni base carbon nanotube composite construction.Bath temperature is controlled at 20～50 DEG C, current density 1～5A/dm
2.
(8) control electroplating time, making electroplating thickness is 3 μ m, takes out washing and dries up.
(9) acetone 5min, ethanol 5min, washing, removes photoresist; Remove Cr-Cu Seed Layer completely with alkaline Cu etching liquid and Cr etching liquid respectively.
Preparation Cu base carbon nanotube supplementary structure
(1) carry out physics with nano-calcium carbonate furnishing pasty state and clean PDP front panel, be neither polymerized to water droplet and also do not become under plume until be attached to surperficial water, then after ultrasonic washing, at 60-80 DEG C, dry 30-60min.
(2) sputter 200nm thickness C r-Cu Seed Layer.
(3) in Seed Layer, carry out successively spin coating 8 μ m photoresists, the mask plate of the figure that then drying glue successively, use drive separately does mask and carries out UV exposure, development.
(4) take multi-walled carbon nano-tubes 10g, carry out 4h under ball milling 500rpm, first carbon nano-tube is carried out to ball milling dispersion treatment, then use sulfuric acid: nitric acid=3: reflow treatment 2h at 60 DEG C of 1 nitration mixture, cooling repeatedly clean to neutrality with deionized water afterwards, last filtering drying.
(5) preparation copper electroplating solution, (as CuSO
45H
2o 60～100g/L, H
2sO
4180～220g/L, Cl
-30～80mg/L), carrying out successively charcoal treatment, filtering, add additive and dispersant, light current solution, adjust pH value is 4.0.
(6) carbon nano-tube accurately taking after a certain amount of pre-treatment joins in above-mentioned plating solution, makes the concentration of carbon nano-tube be controlled at 2～7g/L.
(7) under ultrasonic agitation, carry out composite plating, grow Cu base carbon nanotube composite construction.Bath temperature is controlled at 20～30 DEG C, current density 1～3A/dm
2.
(8) control electroplating time, making electroplating thickness is 6 μ m, takes out washing and dries up.
(9) acetone 5min, ethanol 5min, washing, removes photoresist; Remove Cr-Cu Seed Layer completely with alkaline Cu etching liquid and Cr etching liquid respectively.
Electrophoresis carbon nano-tube supplementary structure
(1) carry out physics with nano-calcium carbonate furnishing pasty state and clean PDP front panel, be neither polymerized to water droplet and also do not become under plume until be attached to surperficial water, then after ultrasonic washing, at 60-80 DEG C, dry 30-60min.
(2) sputter 500nm thickness C r-Cu Seed Layer.
(3) in Seed Layer, carry out successively spin coating 5 μ m photoresists, then drying glue successively, do mask with the mask plate that does not add drive pattern and carry out UV exposure, development.
(4) take multi-walled carbon nano-tubes 10g, carry out 4h under ball milling 500rpm, then use sulfuric acid: nitric acid=3: reflow treatment 2h at 70 DEG C of 1 nitration mixture, cooling repeatedly clean to neutrality with deionized water afterwards.
(5) get above-mentioned carbon nano-tube aqueous solutions, under 5000rmp, centrifugal 10min, gets upper solution, adds magnesium nitrate 2-10g/L, and ultrasonic dispersion 1h.
(6) PDP panel does negative electrode, controls two die opening 3-10cm, carries out electrophoresis 2-6min under 5-15V voltage under room temperature.
(7) then use acetone 5min, ethanol 5min, washing, remove photoresist; Remove Cr-Cu Seed Layer completely with Cu etching liquid and Cr etching liquid.
Claims (2)
1. for a preparation method for the carbon nano-tube supplementary structure of plasma scope, it is characterized in that, comprise the following steps:
The first step, the preliminary treatment of PDP front panel, sputter Cr-Cu Seed Layer on dielectric layer;
Second step, in Seed Layer, carry out successively spin coating photoresist, drying glue, exposure, development, reserve the appointed area that will add carbon nano tube structure;
The 3rd step, the plating of mask composite plating, composite chemical or electrophoresis are carried out in the region of specifying, grow composite carbon nanometer tube structure: carbon nano-tube is carried out pre-treatment and the carbon nano-tube after pre-dispersed carried out under the mode of magnetic agitation, air stirring or ultrasonic agitation to Composite Coatings or electrophoresis with the ratio of 2-10g/L;
The 4th step, respectively sample is soaked to etching with acetone or alcohol, remove photoresist; Finally remove Cr-Cu Seed Layer completely with alkaline Cu etching liquid and Cr etching liquid respectively, obtain carbon nano-tube supplementary structure;
Preliminary treatment described in the first step refers to carries out physics scouring with nano-calcium carbonate furnishing pasty state, to produce cleaning and to have the surface of suitable crude rugosity, then cleans and dries; The thickness of described Cr-Cu Seed Layer is 100-1000nm;
The basic plating solution that described Composite Coatings adopts is that pH is conventional electroplate liquid or the chemical plating fluid of 2-7, and the current density of setting is 0.5-6A/dm2, and temperature is 20-70 DEG C;
The electrophoresis basal liquid that described electrophoresis adopts is that water, ethanol or isopropyl alcohol, the additive magnesium nitrate that is 1-20g/L or cationic surfactant, electrophoretic voltage are 3-20V, and temperature is 5-40 DEG C;
Described photoresist thickness is 2-10 μ m; Described preliminary treatment refers to: carbon nano-tube carried out after ball milling dispersion, and with reflow treatment 1-3h at contain sulfuric acid and nitric acid mixed sour 60-70 DEG C, cooling repeatedly clean to neutrality with deionized water afterwards, last filtering drying.
2. the preparation method of carbon nano-tube supplementary structure according to claim 1, is characterized in that, described pre-dispersed referring to: adopt ultrasonic dispersion and add dispersant and/or carry out high-speed homogenization processing.
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| US7455757B2 (en) * | 2001-11-30 | 2008-11-25 | The University Of North Carolina At Chapel Hill | Deposition method for nanostructure materials |
| KR100589406B1 (en) * | 2003-11-29 | 2006-06-14 | 삼성에스디아이 주식회사 | Plasma display panel |
| KR100656781B1 (en) * | 2005-03-11 | 2006-12-13 | 재단법인서울대학교산학협력재단 | Method for forming electron emitter tip by copper-carbon nanotube composite electroplating |
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