CN102097268A - 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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- CN102097268A CN102097268A CN2011100096759A CN201110009675A CN102097268A CN 102097268 A CN102097268 A CN 102097268A CN 2011100096759 A CN2011100096759 A CN 2011100096759A CN 201110009675 A CN201110009675 A CN 201110009675A CN 102097268 A CN102097268 A CN 102097268A
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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 is a kind of preparation method who is used for the carbon nano-tube supplementary structure of plasma scope.
Background technology
Plasma scope (PDP) was born in the U.S. early than 1964, had experienced semicentennial development after this, no matter was at device material or aspect the technology, had all obtained very fast progress.The material aspect, dielectric layer, fluorescent material, specific substrate glass, mgo protection layer, novel barrier material etc. have obtained effective developmental research; The technology aspect, manually addressing, automatic addressing, novel Driving technique, new barrier structure or the like all progressively are developed research; In above these technology and the continuous development of material, the pixel of PDP is promoted rapidly.Exactly because the emerging in an endless stream of this continuous innovation, new material and technology, the development of key technology etc. has been impelled the burst of large size plasma TV development for a period of time at present.Though research and finished productization to PDP have all experienced ripe developing stage, it remains more weak point so far.Wherein light efficiency is low, energy consumption is high, the production cost height is its topmost shortcoming.But meanwhile, PDP and its current main market competition adversary CRT (rear-projection TV), LCD (LCD) and OLED (organic electroluminescent LED display) etc. compare the advantage that can't neglect: there is not focus issues in screen, ultra-thin and ultra-light; Wide visual angle broad view, color reducibility is good, colour gamut is wide, color is more bright-coloured, the large scale advantage, the corresponding time is fast, dynamic image is clear.These advantages all are that other Display Techniques are too far behind to catch up.Following development of television trend will be high definition, large-screen and 3D, and plasma display exactly takes advantage in these areas.If so can improve or overcome the defective of PDP, the continuation of PDP technology is researched and developed to be had very big necessity and is worth the place.
For household electrical appliance, the power consumption principal element that to be the consumer consider when selecting TV is a urgent task so reduce the PDP energy consumption.The power consumption of plasm TV belongs to dynamic power consumption, the power that is different picture brightness consumption also is different, with the bright dark dynamic change of picture, and the difference of picture light and shade relies on the control ignition frequency to realize, if, just can realize that the power consumption of light and shade picture all is reduced so can reduce the driving voltage of each discharge.
The reduction of driving voltage can realize by the improvement to PDP structure, material, discharge gas.In general, electrode spacing is more little, discharge space is more little, driving voltage is more little, but this can cause the reduction of light efficiency, brightness etc. simultaneously, so need take all factors into consideration, so the structure of present plasma display has been close to optimization, the space that reduces driving by the change structure is very little; Use the higher material of secondary electron reflectivity to replace magnesium oxide, can reduce driving voltage undoubtedly, but this new material seek and research aspect also have very long road to go away; Change for discharge gas component or pressure equally also is double-edged sword, and light efficiency is reduced.
Find through retrieval prior art, Won Tae LEE etc. are at Jpn.J.Appl.Phys.Vol.41 (2002) pp.6550-6552, Part 1, No.11A, in the article that November 2002 delivers " MgO/Carbon Nanotubes Protective Layerin AC-Plasma Display Panels ", carbon nano-tube has been incorporated in the middle of the PDP device.Manufacture method is that carbon nano-tube is mixed and add other auxiliary agents as the carbon nano-tube slurry with glass dust, with the method for silk screen printing carbon nano-tube is printed on the dielectric layer of PDP front panel, heat-treats then; Its another method is with chemical vapour deposition (CVD) the carbon nano-tube of preparing directly to be deposited on sputter in advance to have on the PDP dielectric layer of nickel.This method mainly contains two weak points, and one is that carbon nano-tube is incorporated into the light transmittance that whole front panel can greatly influence PDP undoubtedly; Owing to the restriction of manufacture method, carbon nano-tube can lie low on matrix, thereby causes field emission performance relatively poor in addition.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of preparation method who is used for the carbon nano-tube supplementary structure of plasma scope is provided, make the cold cathode emission can produce more startup electronics, to reduce driving voltage.More substantial electronics is arranged in discharge process in addition, can increase the apportionment ratio that discharge energy is given 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 may further comprise the steps:
The first step, the preliminary treatment of PDP front panel, sputter Cr-Cu Seed Layer on dielectric layer.
Described PDP front panel is meant conventional surface discharge type AC plasma display (AC-PDP) front panel, comprises address electrode, glass dust dielectric layer that front panel glass basis, transparency electrode and bus electrode are formed.
Described preliminary treatment is meant that carrying out physics with nano-calcium carbonate furnishing pasty state cleans, and with the surface that produces cleaning and have the suitable crude rugosity, cleans oven dry then; The thickness of described Cr-Cu Seed Layer is 100-1000nm.
The thickness of described Cr-Cu Seed Layer is 100-1000nm.
Second the step, on Seed Layer, carry out spin coating photoresist, drying glue, exposure, development successively, 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 are meant with the UV photoetching technique to be carried out photoresist graphically.
That described appointed area is meant is that photoresist is developed, need the part of growing mixed structure, requires the decision graphics shape according to reality.
The 3rd step, plating of mask composite plating, composite chemical or electrophoresis are carried out in the zone of appointment, grow the composite carbon nanometer tube structure: carbon nano-tube is carried out pre-treatment and with the ratio of 2-10g/L the carbon nano-tube after pre-dispersed carried out compound plating or electrophoresis under the mode of magnetic agitation, air stirring or ultrasonic agitation.
Described pre-treatment is meant: after carbon nano-tube was carried out Ball milling, with the mixed sour 60-70 ℃ of following reflow treatment 1-3h that contains sulfuric acid and nitric acid, the cooling back was cleaned to neutrality repeatedly with deionized water, last filtering drying.
Described pre-dispersed being meant: adopt ultrasonic dispersion and add dispersant or carry out high-speed homogenization and handle, carbon nano-tube adds and electroplates in the basic plating bath then.
Described compound plating also needs to control basic plating bath and forms (conventional electroplate liquid, chemical plating fluid), current density (0.5-6A/dm in its preparation process
2), plating bath pH value (2-7), temperature parameters such as (20-70 ℃), by regulating and these technological parameters of appropriate combination, can control laminated film quality and the carbon nano-tube compound quantity in laminated film.
Described electrophoresis, also need to control the selection (water, ethanol, isopropyl alcohol) of electrophoresis basal liquid, selection and concentration (magnesium nitrate or cationic surfactant 1-20g/L), electrophoretic voltage (3-20V) and the temperature parameters such as (5-40 ℃) of additive in its preparation process, thereby control the dispersiveness and the compactness of final carbon nano tube structure.
The 4th step, respectively sample is soaked etching, remove photoresist, use washed with de-ionized water at last with acetone or alcohol; Remove the Cr-Cu Seed Layer fully with alkaline Cu etching liquid and Cr etching liquid respectively at last, obtain the carbon nano-tube supplementary structure.
The present invention relates to the carbon nano-tube supplementary structure that method for preparing obtains; comprise: glass substrate; the glass dust dielectric layer; ito transparent electrode; bus electrode; the assisted recombination structure; the magnesium oxide diaphragm; barrier and addressing electrode; wherein: the assisted recombination structure; magnesium oxide diaphragm and barrier lay respectively at; between two glass dust dielectric layers that are oppositely arranged down; upper glass powder dielectric layer; bus electrode and ito transparent electrode from top to bottom are provided with successively; lower-glass powder dielectric layer places on the addressing electrode, and two glass substrates are arranged at respectively; the outside of lower-glass powder dielectric layer.
Described barrier is connected perpendicular to glass substrate and in the gap between magnesium oxide diaphragm and the lower-glass powder dielectric layer and with lower-glass powder dielectric layer.
The invention has the advantages that:
Light efficiency can get a promotion when (1) introducing of carbon nano-tube supplementary structure made the reduction of PDP driving voltage; (2) in manufacturing process, the position of supplementary structure is made in position, has same shape, thereby avoided it, and do not add comparing of supplementary structure, can not influence the aperture opening ratio of PDP panel additionally the stopping of visible light with bus electrode over against bus electrode; (3) adopt the manufacture craft of composite plating, guaranteed the field emission performance preferably of carbon nano-tube supplementary structure.
Description of 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 of Fig. 3 supplementary structure individual drive;
Fig. 4 supplementary structure does not add the PDP front-panel structure figure of driving;
Among the figure: 1 glass substrate, 2 glass dust dielectric layers, 3ITO transparency electrode, 4 bus electrodes, 5 assisted recombination structures, 6 magnesium oxide diaphragms, 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, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, 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 the PDP front panel, neither gather into water droplet until the water attached to the surface and also do not become under the plume, ultrasonic then washing back is dried by the fire 30-60min down at 60-80 ℃.
(2) sputter 500nm thickness C r-Cu Seed Layer.
(3) on Seed Layer, carry out spin coating 5 μ m photoresists successively, drying glue successively then, do mask with the mask plate of the figure that drives altogether and carry out the UV exposure, develop.
(4) take by weighing Single Walled Carbon Nanotube 10g, carry out 4h under the ball milling 500rpm, use sulfuric acid then: 60 ℃ of following reflow treatment 2h of nitration mixture of nitric acid=3: 1, clean to neutrality last vacuum drying repeatedly with deionized water.
(5) preparation electronickelling solution, (as the watt plating bath: nickelous sulfate 250g/L, nickel chloride 45g/L, boric acid 30g/L), carrying out charcoal treatment, filtration, adding additive and dispersant, light current successively, to separate, adjust the pH value be 4.0.
(6) carbon nano-tube that accurately takes by weighing after a certain amount of pre-treatment joins in the above-mentioned nickel-plating liquid, makes the concentration of carbon nano-tube be controlled at 2～10g/L.
(7) carry out composite plating under air stirring and the ultrasonic auxiliary stirring, grow Ni base carbon nanotube composite construction.Bath temperature is controlled at 20～50 ℃, current density 1～5A/dm
2
(8) the control electroplating time makes that electroplating thickness is 3 μ m, takes out washing and dries up.
(9) photoresist is removed in acetone 5min, ethanol 5min, washing; Remove the Cr-Cu Seed Layer fully 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 the PDP front panel, neither gather into water droplet until the water attached to the surface and also do not become under the plume, ultrasonic then washing back is dried by the fire 30-60min down at 60-80 ℃.
(2) sputter 200nm thickness C r-Cu Seed Layer.
(3) on Seed Layer, carry out spin coating 8 μ m photoresists successively, drying glue successively then, do mask with the mask plate of the figure of individual drive and carry out the UV exposure, develop.
(4) take by weighing multi-walled carbon nano-tubes 10g, carry out 4h under the ball milling 500rpm, at first carbon nano-tube is carried out Ball milling and handle, use sulfuric acid then: 60 ℃ of following reflow treatment 2h of nitration mixture of nitric acid=3: 1, the cooling back is cleaned to neutrality repeatedly with deionized water, last filtering drying.
(5) preparation copper electroplating solution is (as CuSO
45H
2O 60～100g/L, H
2SO
4180～220g/L, Cl
-30～80mg/L), carrying out charcoal treatment, filtration, adding additive and dispersant, light current successively, to separate, adjust the pH value be 4.0.
(6) carbon nano-tube that accurately takes by weighing after a certain amount of pre-treatment joins in the above-mentioned plating bath, makes the concentration of carbon nano-tube be controlled at 2～7g/L.
(7) carry out composite plating under the ultrasonic agitation, grow Cu base carbon nanotube composite construction.Bath temperature is controlled at 20～30 ℃, current density 1～3A/dm
2
(8) the control electroplating time makes that electroplating thickness is 6 μ m, takes out washing and dries up.
(9) photoresist is removed in acetone 5min, ethanol 5min, washing; Remove the Cr-Cu Seed Layer fully 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 the PDP front panel, neither gather into water droplet until the water attached to the surface and also do not become under the plume, ultrasonic then washing back is dried by the fire 30-60min down at 60-80 ℃.
(2) sputter 500nm thickness C r-Cu Seed Layer.
(3) on Seed Layer, carry out spin coating 5 μ m photoresists successively, drying glue successively then, do mask with the mask plate that does not add drive pattern and carry out the UV exposure, develop.
(4) take by weighing multi-walled carbon nano-tubes 10g, carry out 4h under the ball milling 500rpm, use sulfuric acid then: 70 ℃ of following reflow treatment 2h of nitration mixture of nitric acid=3: 1, the cooling back is cleaned to neutrality repeatedly with deionized water.
(5) get above-mentioned carbon nano-tube aqueous solutions, centrifugal 10min gets upper solution under the 5000rmp, adds magnesium nitrate 2-10g/L, and ultrasonic dispersion 1h.
(6) the PDP panel is done negative electrode, controls two die opening 3-10cm, is carrying out electrophoresis 2-6min under the 5-15V voltage under room temperature.
(7) use acetone 5min, ethanol 5min, washing then, remove photoresist; Remove the Cr-Cu Seed Layer fully with Cu etching liquid and Cr etching liquid.
Claims (9)
1. a preparation method who is used for the carbon nano-tube supplementary structure of plasma scope is characterized in that, may further comprise the steps:
The first step, the preliminary treatment of PDP front panel, sputter Cr-Cu Seed Layer on dielectric layer;
Second the step, on Seed Layer, carry out spin coating photoresist, drying glue, exposure, development successively, reserve the appointed area that will add carbon nano tube structure;
The 3rd step, plating of mask composite plating, composite chemical or electrophoresis are carried out in the zone of appointment, grow the composite carbon nanometer tube structure: carbon nano-tube is carried out pre-treatment and with the ratio of 2-10g/L the carbon nano-tube after pre-dispersed carried out compound plating or electrophoresis under the mode of magnetic agitation, air stirring or ultrasonic agitation;
The 4th step, respectively sample is soaked etching, remove photoresist with acetone or alcohol; Remove the Cr-Cu Seed Layer fully with alkaline Cu etching liquid and Cr etching liquid respectively at last, obtain the carbon nano-tube supplementary structure.
2. the preparation method of carbon nano-tube supplementary structure according to claim 1, it is characterized in that, preliminary treatment described in the first step is meant that carrying out physics with nano-calcium carbonate furnishing pasty state cleans, and with the surface that produces cleaning and have the suitable crude rugosity, cleans oven dry then; The thickness of described Cr-Cu Seed Layer is 100-1000nm.
3. the preparation method of carbon nano-tube supplementary structure according to claim 1 is characterized in that, described photoresist thickness is 2-10 μ m.
4. the preparation method of carbon nano-tube supplementary structure according to claim 1, it is characterized in that, described pre-treatment is meant: after carbon nano-tube is carried out Ball milling, with the mixed sour 60-70 that contains sulfuric acid and nitric acid ℃ following reflow treatment 1-3h, the cooling back is cleaned to neutrality repeatedly with deionized water, last filtering drying.
5. the preparation method of carbon nano-tube supplementary structure according to claim 1 is characterized in that, described pre-dispersed being meant: adopt ultrasonic dispersion and add dispersant and/or carry out high-speed homogenization and handle.
6. the preparation method of carbon nano-tube supplementary structure according to claim 1 is characterized in that, the basic plating bath that described compound plating is adopted 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/dm
2, temperature is 20-70 ℃.
7. the preparation method of carbon nano-tube supplementary structure according to claim 1, it is characterized in that, the electrophoresis basal liquid that described electrophoresis adopted is that water, ethanol or isopropyl alcohol, additive are that the magnesium nitrate of 1-20g/L or cationic surfactant, electrophoretic voltage are 3-20V, and temperature is 5-40 ℃.
8. carbon nano-tube supplementary structure for preparing according to the described method of above-mentioned arbitrary claim; it is characterized in that; comprise: glass substrate; the glass dust dielectric layer; ito transparent electrode; bus electrode; the assisted recombination structure; the magnesium oxide diaphragm; barrier and addressing electrode; wherein: the assisted recombination structure; magnesium oxide diaphragm and barrier lay respectively at; between two glass dust dielectric layers that are oppositely arranged down; upper glass powder dielectric layer; ito transparent electrode and bus electrode from top to bottom are provided with successively; lower-glass powder dielectric layer places on the addressing electrode, and two glass substrates are arranged at respectively; the outside of lower-glass powder dielectric layer.
9. carbon nano-tube supplementary structure according to claim 8 is characterized in that, described barrier is connected perpendicular to glass substrate and in the gap between magnesium oxide diaphragm and the lower-glass powder dielectric layer and with lower-glass powder dielectric layer.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010025962A1 (en) * | 2000-03-31 | 2001-10-04 | Masayuki Nakamoto | Field emmision type cold cathode device, manufacturing method thereof and vacuum micro device |
| WO2005014889A2 (en) * | 2003-07-10 | 2005-02-17 | The University Of North Carolina - Chapel Hill | Deposition method for nanostructure materials |
| US20050212430A1 (en) * | 2003-11-29 | 2005-09-29 | Jeong-Chull Ahn | Plasma display panel |
| WO2006095947A1 (en) * | 2005-03-11 | 2006-09-14 | Seoul National University Industry Foundation | Method of forming electron emitter tips using copper-carbon nanotube composite electroplating |
| CN1975963A (en) * | 2005-10-05 | 2007-06-06 | 乐金电子（南京）等离子有限公司 | Front panel of plasma display board and manufacturing method and plasma display board equipped with the same |
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2011
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010025962A1 (en) * | 2000-03-31 | 2001-10-04 | Masayuki Nakamoto | Field emmision type cold cathode device, manufacturing method thereof and vacuum micro device |
| WO2005014889A2 (en) * | 2003-07-10 | 2005-02-17 | The University Of North Carolina - Chapel Hill | Deposition method for nanostructure materials |
| US20050212430A1 (en) * | 2003-11-29 | 2005-09-29 | Jeong-Chull Ahn | Plasma display panel |
| WO2006095947A1 (en) * | 2005-03-11 | 2006-09-14 | Seoul National University Industry Foundation | Method of forming electron emitter tips using copper-carbon nanotube composite electroplating |
| CN1975963A (en) * | 2005-10-05 | 2007-06-06 | 乐金电子（南京）等离子有限公司 | Front panel of plasma display board and manufacturing method and plasma display board equipped with the same |
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