CN102044396B - Barrier size used for plasma display and barrier made of same - Google Patents
Barrier size used for plasma display and barrier made of same Download PDFInfo
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- CN102044396B CN102044396B CN2010105712042A CN201010571204A CN102044396B CN 102044396 B CN102044396 B CN 102044396B CN 2010105712042 A CN2010105712042 A CN 2010105712042A CN 201010571204 A CN201010571204 A CN 201010571204A CN 102044396 B CN102044396 B CN 102044396B
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Abstract
The invention relates to barrier size used for a plasma display. The barrier size comprises low melting point glass powder, inorganic filler powder, an organic solvent and an organic resin, wherein the inorganic filler powder accounts for 10-30% by weight of the mixture of the low smelting point glass powder and the inorganic filler powder and has D50 value of 6-12mu m and maximum grain size of 9-30mu m. The invention also provides a barrier made of the size. The barrier has coarse surface, thus improving the adhesion amount of fluorescent powder.
Description
Technical field
The present invention relates to field of display, be specifically related to be used for the slurry of plasma display barrier and by its barrier that makes.
Background technology
Plasma panel be a kind of self-luminous, in light weight, the visual angle is wide, thin thickness, total digitalization, the dynamic good novel flat-plate display device of display effect.
Plasma panel mainly is made up of several parts such as front glass substrate, back glass substrate, barrier, address electrode, show electrode, back medium, preceding medium, diaphragm, fluorescent material.
Forward and backward glass substrate subtend is provided with, and address electrode and show electrode spatial vertical.The barrier effect is to cut apart discharge cell and support forward and backward glass substrate, and its requirements of making is higher, and the barrier surface state directly influences the distribution of fluorescent material.Before in order to improve the attachment state of fluorescent material in the barrier side; A kind of is to make phosphor surface form convex-concave with drying, the sintering character of improving fluorescent material to improve the distribution situation of fluorescent material in the barrier side; Its shortcoming is that the organic resin composition in the fluorescent material is difficult to the tight burning removal, influences luminous efficiency.Another kind is at barrier or the back dielectric surface makes projection or thereby depression has increased coating area of fluorescent powder; But on very meticulous discharge cell, make meticulousr projection or depression; Its difficulty is well imagined, in addition, also easily barrier is caused damage.
Summary of the invention
The purpose of this invention is to provide a kind of new barrier size prescription, to improve the barrier appearance, to improve the extension powder amount of fluorescent material in the barrier side.
Barrier size of the present invention comprises low-melting glass powder, inorganic filler powder, organic solvent and organic resin; Wherein, In the mixed-powder of glass powder with low melting point and inorganic filler powder constituent; The inorganic filler powder accounts for 10%～30% in mass, and its D50 value is 6～12 μ m, and maximum particle diameter is 9～30 μ m.
In a kind of optimal way, above-mentioned inorganic filler powder is an aluminium oxide.
In a kind of exemplary embodiment of the present invention, in above-mentioned mixed-powder, further comprise 25～35% PbO, 10～15% B
2O
3, 15～25% SiO
2, and 10～18% Li
2O and Na
2O, K
2The mixture of O, wherein Li
2O is 5～10%, Na
2O is 2～5%, K
2O is 1～4%.
In another kind of exemplary embodiment of the present invention, in above-mentioned mixed-powder, further comprise 18～35% BaO, 20～35% ZnO, 12～25% B
2O
3, and 7～12% SiO
2
Another object of the present invention is to provide a kind of barrier that is used for plasma panel, be prepared from above-mentioned barrier size.
The barrier surface roughness that this barrier size that employing obtains according to the present invention is made is higher, helps the side of fluorescent material attached to barrier, improves the extension powder amount of fluorescent material in the barrier side, the brightness that finally improves display.
Embodiment
Barrier size main component of the present invention has low-melting glass powder, inorganic filler powder, organic solvent and organic resin, explains respectively in the face of each composition down.
The low-melting glass powder
The low-melting glass powder that the present invention uses preferably uses PbO-B
2O
3-SiO
2-RO system, BaO-ZnO-B
2O
3-SiO
2The glass of system.
At PbO-B
2O
3-SiO
2-RO is in the glass, and RO is an alkali metal oxide, chooses Li
2O, Na
2O, K
2O mixes use for three kinds.In the mixed-powder by low-melting glass powder and inorganic filler powder constituent, the content of PbO is 20～40%, B
2O
3Content be 10～20%, SiO
2Content be 15～30%, Li
2O+Na
2O+K
2The content of O is 10～20%.
The effect of PbO main landing low softening point in glass dust, also the adjustable heat coefficient of expansion.Content is less than 20% glass softening point and obviously rises, and surpasses 600 ℃ like softening point, and bubble is difficult to separate out in the glass.Content was more than 40% o'clock, and it is big that thermal coefficient of expansion becomes, and is unfavorable for the coupling with other devices.Content is preferably in 25～35%.
B
2O
3Be a kind of composition that enlarges the vitrifying scope, be of value to the raising sintering character, it has certain influence again to deaeration property simultaneously.Do not contain B
2O
3Or content more after a little while, forms vitrifying difficulty, agglutinating property decline.Content was more than 20% o'clock, and glass is prone to phase-splitting and thermal coefficient of expansion increases.Content is preferably in 10～15%.
SiO
2Be the framework ingredient that forms glass, content is less than at 15% o'clock, the vitrifying difficulty, and glass is also unstable, and the chemical resistance of glass descends.Content was more than 30% o'clock, and glass softening point raises, and glass adhesion variation simultaneously is slack-off, is difficult to discharge bubble.Content is preferably in 15～25%.
Alkali metal oxide Li
2O+Na
2O+K
2O is in order to improve sintering character, to reduce softening point and adjust the high temperature viscosity change simultaneously.Total body burden is less than at 10% o'clock, and agglutinating property descends.Content is higher than at 20% o'clock, and agglutinating property descends, and the high temperature viscosity change slowly is unfavorable for the bubble discharge, and softening point rises.Content is preferably in 10～18%.Wherein each composition mass percent of accounting for alkali metal oxide content is preferably Li
2O is 5～10%, Na
2O is 2～5%, K
2O is 1～4%.
For BaO-ZnO-B
2O
3-SiO
2Be the situation of glass, in the mixed-powder by glass powder with low melting point and inorganic filler powder constituent, the content of BaO is 15～45%, and the content of ZnO is 20～35%, B
2O
3Content be 10～30%, SiO
2Content be 5～15%.
BaO has and reduces softening point, adjustment dielectric constant and high temperature viscosity, increases thermal coefficient of expansion, and has the effect that suppresses the glass phase-splitting, content to be less than at 15% o'clock to be difficult for reaching above-mentioned effect, and content is higher than 45% o'clock thermal coefficient of expansion and obviously increases and be prone to foaming.Content is preferably in 18～35%.
ZnO has the characteristic that reduces thermal coefficient of expansion and softening point, and content is less than 20%, is unsuitable for to reach the effect that reduces the coefficient of expansion and softening point.Content is more than 35%, and the glass uniformity can variation.Content is preferably in 20～35%.
B
2O
3Be a kind of composition that enlarges the vitrifying scope, be of value to the raising sintering character, it has certain influence again to deaeration property simultaneously.Content is less than at 10% o'clock, forms vitrifying difficulty, agglutinating property decline.Content was more than 30% o'clock, and glass is prone to phase-splitting and thermal coefficient of expansion increases.Content is preferably in 12～25%.
SiO
2Be the framework ingredient that forms glass, content is less than 5%, the vitrifying difficulty, and glass is also unstable, and the chemical resistance of glass descends.Content raises more than 15% glass softening point, and glass adhesion variation simultaneously is slack-off, is difficult to discharge bubble.Content is preferably in 7～12%.
The refractive index of above-mentioned glass powder is 1.45～1.85, and thermal coefficient of expansion is 65～85 * 10-7/ ℃, and the thermal softening temperature is 450～630 ℃.The particle size distribution of above-mentioned glass powder is: 50% averaged particles particle diameter (D50) is 0.3～5 μ m, and maximum particle diameter (Dmax) is 5～20 μ m, and specific area is 1.2～2.5m2/g, more preferably 1.0～2.0m2/g.Adopt the glass powder sintering of above-mentioned particle size distribution can make the shape maintains of barrier good, agglutinating property is high, obtain the high barrier of intensity easily.
The inorganic filler powder
In the present invention, in order to obtain coarse barrier surface, in barrier size, introduce the inorganic filler powder of specified particle diameter, the average grain diameter D50 value of this powder is 6～12 μ m, and maximum particle diameter (Dmax) is 9～30 μ m.This powder should have enough mechanical strengths, so that this powder particle can not occur subsiding in being pressed into the process of barrier layer or the size degradation.Operable inorganic filler powder comprises aluminium oxide, zirconia, titanium dioxide, quartz glass etc., also can be their mixture.Preferred what use is alumina powder, and this is because the mechanical strength of aluminium oxide is higher, and its graininess is irregular spheroid, obtains rough surface and the barrier of sufficient mechanical strength is arranged easily in addition.
In the powder of being made up of above-mentioned glass powder with low melting point and inorganic filler, this inorganic filler accounts for 10%～30% in mass, preferably 15～25% ratio.
Organic solvent
The solvent that the present invention uses is used by one or more mixing in terpinol, BC acetate, BC, the diethylene glycol monobutyl ether acetate, and shared stock quality percentage is 15%～40%.
Organic resin
The organic resin that the present invention uses is by ethyl cellulose, acrylic resin, and one or more of acrylic acid series condensate, polyvinyl alcohol, polyvinyl butyral resin etc. mix use, and shared stock quality percentage is 1%～5%.Content is lower than at 1% o'clock, is difficult to guarantee dried barrier shape, and content is higher than at 5% o'clock, and the barrier film strength increases, and is unfavorable for the etching processing of follow-up barrier, reduces production efficiency, yields decline.
The object of the invention realizes through following technical scheme:
Process the figure that needs respectively at upper and lower base plate, use the shaggy barrier of fabrication techniques of the present invention then.Said method adopts following steps:
A, make barrier accomplishing addressing electrode, medium, adopt barrier size provided by the invention, the manufacture craft of barrier comprises coatings, drying, pad pasting, development, blasting craft, passes through the sintering process completion at last.
B, when making show electrode, make ITO earlier, make the BUS electrode again;
C, use print process or cladding process are made the about 30 microns transparent dielectric layers of a layer thickness on electrode;
D, vapor deposition layer protecting film;
E, at last with the upper and lower base plate that machines to, sealing-in exhaust finally charges into height and contains xenon-133 gas to obtain high luminous efficiency.
Through above-described coating, drying, pad pasting, development, blasting craft, observe the barrier surface behind sintering, still there is small rough structure, as at microscopically, visible a large amount of small pin holes.These small pin holes just let the surface, particularly barrier head portion of fluorescent material attached to barrier more easily.
The barrier rough surface helps weakening because the stress that sintering process produces prevents that barrier from producing slight crack.
Add certain yittrium oxide and aluminium oxide and not only can increase surface roughness, and increase the rate of finished products that compression strength improves barrier.
Embodiment
Embodiment 1
According to the nominal value in table 1 and the table 2, the PbO with 25%, 16% B
2O
3, 16% SiO
2, 10% Li
2O, 5% Na
2O, 3% K
2The O raw materials mix is even, 1200 ℃ of following fusions, rolls behind the sheet quenching and pulverizes at ball mill, and it is 2 μ m that classification forms 50% averaged particles particle diameter (D50), and maximum particle diameter (Dmax) is the glass powder of 10 μ m.Grinding classification, to form 50% averaged particles particle diameter (D50) be 6 μ m, and maximum particle diameter (Dmax) is 25% the Al of 20 μ m
2O
3Powder.With glass powder and Al
2O
3In punching block, being pressed into diameter after powder evenly mixes is φ 5mm, and length is the exemplar of 60mm, in 50～350 ℃ of scopes, measures the thermal coefficient of expansion of exemplar, and the thermal coefficient of expansion measurement result is 78 * 10
-7, see table 4.
To glass powder and Al
2O
3The terpinol of interpolation 19% and 3% ethyl cellulose in the abundant rolling of three roller mills, mixing, obtain barrier size with this mixture in the mixture of powder.
Above-mentioned barrier size is printed on the surface has on the glass print of transparent ITO electrode, print glass is PD200 plasma panel special glass, and print is of a size of 15mm * 15mm; The barrier film layer thickness that barrier size obtains after repeatedly printing drying is 160 μ m, then with print at 560 ℃ of following sintering, and the insulation 20min; Printing one deck silver is starched on the barrier rete behind the sintering again, dry back sintering print, 560 ℃ of sintering temperatures; Temperature retention time 20min; Use the HEWLETT 4194A of Hewlett-Packard measuring instrument to measure the dielectric constant of print, record dielectric constant values, see table 4.
Above-mentioned barrier size is printed on the PD200 glass print of 300mm * 300mm; After repeatedly printing drying, obtain the thick barrier rete of 160 μ m; On the barrier rete, attach the dry type photoresist, the mask of utilizing pattern line width 50 μ m is to dry type photoresist exposure on the print, and exposure is 400mj/cm2; Produce the dry type photoresist film development of developing machine to print with Korea S SAMILCLEANTEC company, developer solution is 0.3% Na
2CO
3Solution at 80 ℃ down behind the dry 10min, uses Japanese ALPS company sand-blasting machine that print is carried out blasting treatment the print after developing; Sand grains is a stainless steel, and average grain diameter is 10 μ m, produces the stripping machine with Korea S SAMILCLEANTEC company after sandblast is accomplished and peels off remaining dry type photoresist; Stripper solution is 2% KOH solution, and dry 15min under 150 ℃ puts into Japanese COYO sintering furnace sintering, 560 ℃ of sintering temperatures again with the print behind the stripping; Temperature retention time 20min forms the barrier figure.Above-mentioned barrier figure is observed visible a large amount of small pin holes under 40 times of stereoscopes.
The step and the process conditions of embodiment 2 to 6 and comparative example 1,2 are identical with embodiment 1, only carry out according to table 1 and 2 listed actual conditionses, but the D50 value of aluminium oxide are 3 μ m in the comparative example 2.
The low-melting glass powder of table 1 embodiments of the invention and comparative example and inorganic powder filler composition and content
Composition and the content of the alkali metal RO of table 2 embodiments of the invention and comparative example
The performance of table 3 embodiment of the invention and comparative example relatively
| Thermal coefficient of expansion | Dielectric constant (1MHz) | The barrier appearance | |
| Embodiment 1 | 78×10 -7 | 9.27 | Good |
| Embodiment 2 | 74×10 -7 | 9.15 | Good |
| Embodiment 3 | 76×10 -7 | 9.13 | Very |
| Embodiment 4 | 72×10 -7 | 9.50 | Very |
| Embodiment 5 | 74×10 -7 | 9.31 | Good |
| Embodiment 6 | 75×10 -7 | 9.07 | Good |
| Comparative example 1 | 75×10 -7 | 8.62 | Difference |
| Comparative example 2 | 76×10 -7 | 8.58 | Difference |
In table 3, " good " is illustrated under 100 times of stereoscopes, can be observed the uniform pit of a large amount of diameter 2-5um, and " very " expression can be observed pit but distributing homogeneity is inconsistent, and " poor " expression dimple size is undesirable, either large or small.
Can find out that by the data shown in the table 3 thermal coefficient of expansion of barrier size of the present invention is 72 * 10
-7～78 * 10
-7, with PD200 plasma panel special glass thermal coefficient of expansion 83 * 10
-7Coupling is good, and dielectric constant meets the requirement on electric performance of plasma panel between 9.07～9.05, and the barrier of formation is compared the barrier appearance with two comparative examples and is distributed with a large amount of pin holes, helps fluorescent material and adheres to.
The description of above specific embodiments of the invention and embodiment is to be used for explanation and purpose of description, should not regard limitation of the present invention as.They are not detailed or limit the invention to the precise forms that disclosed, and obviously according to above-mentioned instruction, many improvement, embodiment and to change be possible.Therefore, scope of the present invention comprises field as this paper discloses, and by accompanying claims with and equivalence replacement contained.
Claims (4)
1. a barrier size that is used for plasma panel comprises low-melting glass powder, inorganic filler powder, organic solvent and organic resin, wherein; In the mixed-powder of said glass powder with low melting point and inorganic filler powder constituent; The inorganic filler powder accounts for 10%～30% in mass, and its D50 value is 6～12 μ m, and maximum particle diameter is 9～30 μ m; Wherein, said mixed-powder comprises 25～35% PbO, 10～15% B
2O
3, 15～25% SiO
2, and 10～18% Li
2O and Na
2O, K
2The mixture of O, wherein Li
2O is 5～10%, Na
2O is 2～5%, K
2O is 1～4%; Or said mixed-powder comprises 18～35% BaO, 20～35% ZnO, 12～25% B
2O
3, and 7～12% SiO
2
2. barrier size according to claim 1, wherein, the inorganic filler powder accounts for 15～25% in mass in said mixed-powder.
3. barrier size according to claim 1, wherein, said inorganic filler powder is an aluminium oxide.
4. a barrier that is used for plasma panel is characterized in that, each described barrier size is prepared among the said barrier employing claim 1-3.
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|---|---|---|---|
| CN2010105712042A CN102044396B (en) | 2010-09-30 | 2010-12-02 | Barrier size used for plasma display and barrier made of same |
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|---|---|---|---|
| CN201010504146.1 | 2010-09-30 | ||
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| CN102044396B true CN102044396B (en) | 2012-05-30 |
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| CN103050353A (en) * | 2013-01-14 | 2013-04-17 | 安徽鑫昊等离子显示器件有限公司 | Barrier slurry and preparation method thereof |
| CN103606502A (en) * | 2013-11-15 | 2014-02-26 | 四川虹欧显示器件有限公司 | A plasma display barrier repairing slurry and a repairing method thereof |
| CN107359099A (en) * | 2017-07-12 | 2017-11-17 | 合肥轻风飏电气科技有限责任公司 | A kind of electronic display |
| CN113461334B (en) * | 2021-06-11 | 2022-11-18 | 浙江安力能源有限公司 | Glass solder for sealing ceramic diaphragm of sodium-nickel battery and metal-ceramic hot-pressing sealing ceramic end cover, preparation and application thereof |
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| JP2003257322A (en) * | 2002-02-28 | 2003-09-12 | Nippon Electric Glass Co Ltd | Paste for forming partitioning wall |
| US7241712B2 (en) * | 2005-02-28 | 2007-07-10 | National Taiwan University Technology | Low-temperature sintered barium titanate microwave dielectric ceramic material |
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