CN1236470C - Fluorescent powder paste composition for plasma display device and method of preparing fluorescent powder film - Google Patents
Fluorescent powder paste composition for plasma display device and method of preparing fluorescent powder film Download PDFInfo
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- CN1236470C CN1236470C CN 03134366 CN03134366A CN1236470C CN 1236470 C CN1236470 C CN 1236470C CN 03134366 CN03134366 CN 03134366 CN 03134366 A CN03134366 A CN 03134366A CN 1236470 C CN1236470 C CN 1236470C
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Abstract
The present invention discloses a composition of fluorescent powder pulp material used for a plasma display and a preparation method for manufacturing a carrier. The preparation method is characterized in that in an organic carrier, more than three types of organic solvents with different distributions of boiling points to achieve the goal that organic substances can not be decomposed in a concentration mode and gradually volatilized as the temperature rises in the process in which the fluorescent powder pulp material is sintered; in this way, the preparation method is favorable to avoiding generated film cavities because of the high-speed volatilization and the high-speed decomposition of the organic substances, and simultaneously, the more than three types of solvents enable solid fluorescent powder particles to be well dispersed in an organic carrier. After the fluorescent powder pulp material manufactured by the present invention is adopted, dried and sintered, uniform and compact fluorescent powder coatings can be formed.
Description
One, technical field
The invention belongs to the Display Technique field, be specifically related to the manufacturing technology of colour plasma display with phosphor slurry feed composition and preparation fluorescent powder membrane method.
Two, background technology
Chromatic alternating-current plasma display (AC-PDP) thus be that the ultraviolet ray excited light-emitting phosphor that is coated in the display unit that utilizes gas discharge to produce is realized coloredly showing that structural representation as shown in Figure 1.Discharge cell is formed by the barrier 5 that is produced on the lower plate 1, and R, G, B three-color phosphor slurry order respectively are coated in the barrier ditch, and fluorescent material not only will cover the barrier bottom of trench, also will be attached to the barrier both sides, and fluorescent coating requires even compact.R, G, B phosphor powder layer are respectively 4 among Fig. 1,6,14.
Present fluorescent powder paste material is solid fluorescence powder particulate is dispersed in the organic carrier and makes.Carrier mainly is made up of organic solvent and organic resin.Choice of Solvent has following requirement in the organic carrier: 1. can dissolve the organic resin as binding agent, as ethyl cellulose, acrylic resin etc.; 2. similar to organic resin polarity; 3. can dissolve each other with multiple solvent; 4. organic solvent can decompose fully, volatilize behind the oven dry of fluorescent powder paste material process, the sintering.At present, organic solvent commonly used has terpinol (219 ℃ of boiling points), acetic acid butyl carbitol (B.C.A) (246.8 ℃ of boiling points), butyl carbitol (230.4 ℃ of boiling points) etc. in the fluorescent powder paste material.
The shortcoming of existing method is that solvent is generally only selected 2 kinds for use, for example acetic acid butyl carbitol (B.C.A) and butyl carbitol, like this when carrying out the fluorescent material sintering, organic substance will volatilize in a large number simultaneously when temperature is 230～250 ℃, cause phosphor powder layer bubble, the cavity that forms owing to giving vent to anger in a large number to occur easily, it is uneven that phosphor surface is occurred, to such an extent as to influence the discharge space uniformity, reduces discharge nargin.
Three, summary of the invention
Defective or deficiency at above-mentioned existing method exists the purpose of this invention is to provide a kind of fluorescent powder slurry materialfor plasma display composition.
Another object of the present invention provides a kind of fluorescent powder slurry materialfor plasma display preparation of compositions fluorescent powder membrane method.
For achieving the above object, the technical scheme that the present invention solves is: composition comprises fluorescent material, its outstanding progress is also to comprise organic resin in the composition and contains three classes at least or the organic solvent making organic carrier of the above different boiling distribution of three classes, the solvent that described making organic carrier uses is selected from least three classes in following five kind solvents: the first kind is alcohols solvent, is selected from terpinol, ethylene glycol, propylene glycol, glycerol, diethylene glycol (DEG); Second class is the polyfunctional group solvent, is selected from acetic acid butyl carbitol, butyl carbitol, diethanol amine, triethanolamine, carbitol acetic acid esters; The 3rd class is a ketones solvent, is selected from cyclohexanone, acetophenone; The 4th class is an esters solvent, is selected from isoamyl propionate, tributyl citrate, diethyl phthalate, dibutyl phthalate, repefral, glycerol triacetate, butyl borate; The 5th class is the nitrogen-containing compound solvent, is selected from formamide, acetamide; Above-mentioned said organic resin and primary solvent are by weight containing 5～15 parts of organic resins, 50～85 parts of terpinols, 50～85 parts of acetic acid butyl carbitol, 8～30 parts of butyl carbitol, 5～10 parts of cyclohexanone, 3～10 parts of acetamides, 5～15 portions of diethylene glycol (DEG)s, 2～10 parts of glycerol, 2～10 parts of triethanolamines, 5～30 parts of diethyl phthalates, 2～10 parts of dibutyl phthalates respectively.
Can contain in the composition and make the organic carrier that the green emitting phosphor slurry uses, contain the organic resin and the solvent of following weight ratio in the carrier:
4～8 parts of organic resin+55～65 part terpinol+20～23 parts of butyl carbitol+6～10 part triethanolamine+3～7 parts of cyclohexanone;
After carrier prepared, in wherein making the formation slurry, wet end furnish was as follows green solid fluorescent material microparticulate: 35～45 parts of fluorescent material+55～65 part organic carriers.
Can contain in the composition and make the organic carrier that the blue colour fluorescent powder slurry uses, contain the organic resin and the solvent of following weight ratio in the carrier:
4～6 parts of organic resin+58～68 part acetic acid butyl carbitol+8～11 part acetamide+9～12 parts of glycerol+3～6 part triethanolamine+3～6 parts of cyclohexanone;
After carrier prepared, in wherein making the formation slurry, wet end furnish was as follows blue solid fluorescent material microparticulate: 35～45 parts of fluorescent material+55～65 part organic carriers.
The boiling spread of the solvent of selecting for use is 155 ℃～360 ℃.
The method for preparing fluorescent powder film layer, adopt silk screen print method that the fluorescent powder paste material of making is printed on the glass breadboard of carrying out barrier, being placed on microscopically after printing observes, fluorescent powder paste material in the barrier ditch does not have bubble, breadboard is placed in the drying oven dries, bake out temperature is 130 ℃～150 ℃, be 10～15 minutes drying time, be placed on microscopically after the oven dry and observe the fluorescent powder film layer situation, the sidewall of its barrier and bottom of trench all evenly adhere to fluorescent powder film layer, no bulky grain or powder ball do not have the cavity; This breadboard is put into sintering furnace carry out sintering, sintering temperature is 450 ℃～500 ℃, and the time is 28～35 minutes, after sintering finishes, is placed on microscopically and observes, and phosphor powder layer is pure white, fine and smooth, does not have big powder ball, the cavity that stays after the no bubble volatilization.
The present invention compared with prior art, the fluorescent powder film layer that adopts the present invention program to make has good uniformity, the rete brightness that the original technology of brightness makes improves 10～15%.
Four, description of drawings
Accompanying drawing is an AC-PDP device discharging structure schematic diagram.
Five, embodiment
The inventor has provided following embodiment, but the invention is not restricted to these embodiment.
Below in conjunction with embodiment content of the present invention is described further:
With reference to accompanying drawing, following glass sheet 1, lower plate medium 2, addressing electrode 3, green emitting phosphor 4, barrier 5, red fluorescence powder 6, MgO medium protection film 7, upper plate transparent medium 8, last glass sheet 9, metal electrode 10, nesa coating 11, visible light 12, gas discharge 13, blue colour fluorescent powder 14.
Organic solvent has many types according to its chemical constitution and character, can select the organic solvent of different components and ratio according to the size of the chemical analysis of solid fluorescence powder, diameter of particle and surface appearance etc., and these several solvents can dissolve each other.Above-mentioned a few kind solvent has different chemical actions, and the boiling spread of these solvents is 155 ℃～360 ℃.Should select the organic solvent of different components, different proportion, different boiling distribution during the preparation fluorescent powder paste material according to the different performance of different fluorescent material, make the solia particle of fluorescent material have sufficient dispersion stabilization, the fluorescent powder paste material that method the was made into organic substance in oven dry and sintering process that adopts the present invention to introduce simultaneously can not concentrated volatilization, but volatilization gradually under different temperatures, thereby behind sintering, obtain even, flawless fluorescent coating.
In order to more clearly understand inherent mechanism of the present invention, we are system of selection and the principle that example illustrates various organic solvents with a kind of carrier compound of green powder.For example carrier compound is:
6% organic resin+5% cyclohexanone+70% terpinol+14% diethyl phthalate+5% triethanolamine
Above-mentioned formula rate is weight percentage.Wherein organic resin is selected ethyl cellulose for use, and we have selected the different organic solvent of four classes relevant solvent: i.e. ketones solvent cyclohexanone, and its boiling point is 155.65 ℃; Alcohols solvent terpinol, its boiling point are 219 ℃; Esters solvent diethyl phthalate, its boiling point are 295 ℃; Polyfunctional group solvent triethanolamine, its boiling point are 360 ℃.Terpinol is as the basic solvent in the carrier, ethyl cellulose dissolved well, and its content elects 70% as, and terpinol is easy to volatilization, decomposes in the fluorescent powder paste material sintering process; Cyclohexanone can ethyl cellulose dissolved, is again a kind of surfactant, can improve the wettability of the slurry and the surface of solids; Diethyl phthalate and triethanolamine also can both ethyl cellulose dissolved as secondary solvent, and in addition, diethyl phthalate or plasticizer can improve the printing of slurry; Triethanolamine is a good dispersant, and it makes fluorescent powder paste material have good stability.The boiling point of meanwhile back two kinds of solvents is respectively 295 ℃ and 360 ℃, and this just makes fluorescent powder paste material organic solvent in sintering process can progressively volatilize, decompose, and has avoided the concentrated decomposition of organic solvent, thereby has improved the uniformity of phosphor powder layer.
As mentioned above, select the rule of organic solvent to be: basic solvent reply organic resin has good dissolubility, and boiling point is about 210～250 ℃, and percentage by weight is between 50～85%; Secondary solvent requires also can dissolve organic resin, and has other effects concurrently as surfactant, plasticizer and dispersant, and boiling point is about 155～360 ℃.The above solvent weight percent of higher boiling point (300 ℃) generally is lower than 10%, if high boiling solvent content is too much, can make fluorescent powder paste material organic substance in sintering process can not fully volatilize, decompose, to such an extent as to influence the luminescent properties of fluorescent material.
Embodiment 1: make a kind of prescription of red fluorescence powder slurry with carrier:
12 parts of organic resin+55 part acetic acid butyl carbitol+25 part butyl carbitol+8 parts of triethanolamines
After carrier prepares, red solid fluorescent material microparticulate in wherein making the formation slurry.Wet end furnish is as follows:
45 parts of fluorescent material+55 part organic carriers
Adopt silk screen print method that the fluorescent powder paste material of making is printed on the glass breadboard of carrying out barrier, be placed on microscopically after printing and observe, the fluorescent powder paste material in the barrier ditch does not have bubble.Breadboard is placed in the drying oven dries, bake out temperature is 130 ℃～150 ℃, and be 10～15 minutes drying time; be placed on microscopically after the oven dry and observe the fluorescent powder film layer situation; sidewall and the bottom of trench that can see barrier all evenly adhere to fluorescent powder film layer, and no bulky grain or powder ball do not have the cavity.This breadboard is put into sintering furnace carry out sintering, sintering temperature is 480 ℃, 30 minutes.After sintering finishes, be placed on microscopically and observe, can see that phosphor powder layer is pure white, fine and smooth, do not have big powder ball, the cavity that stays after the no bubble volatilization.
Embodiment 2: make a kind of prescription of green emitting phosphor slurry with carrier:
6 parts of organic resin+60 part terpinol+21 parts of butyl carbitol+8 part triethanolamine+5 parts of cyclohexanone
After carrier prepares, green solid fluorescent material microparticulate in wherein making the formation slurry.Wet end furnish is as follows:
40 parts of fluorescent material+60 part organic carriers
Adopt silk screen print method that the fluorescent powder paste material of making is printed on the glass breadboard of carrying out barrier then, be placed on microscopically after printing and observe, the fluorescent powder paste material in the barrier ditch does not have bubble.Breadboard is placed in the drying oven dries, bake out temperature is 120 ℃～140 ℃, and be 12～14 minutes drying time.Be placed on microscopically after the oven dry and observe the fluorescent powder film layer situation, can see that the sidewall of barrier and bottom of trench all evenly adhere to fluorescent powder film layer, no bulky grain or powder ball do not have the cavity.This breadboard is put into sintering furnace carry out sintering, sintering temperature is 470 ℃～485 ℃, and the time is 30～32 minutes.After sintering finishes, be placed on microscopically and observe, can see that phosphor powder layer is pure white, fine and smooth, do not have big powder ball, the cavity that stays after the no bubble volatilization.
Embodiment 3: make a kind of prescription of blue colour fluorescent powder slurry with carrier:
5 parts of organic resin+65 part acetic acid butyl carbitol+10 part acetamide+10 parts of glycerol+5 part triethanolamine+5 parts of cyclohexanone
After carrier prepares, blue solid fluorescent material microparticulate in wherein making the formation slurry.Wet end furnish is as follows:
40 parts of fluorescent material+60 part organic carriers
The method for preparing fluorescent powder film layer is with embodiment 1 or 2.
Embodiment 4: make a kind of prescription of green emitting phosphor slurry with carrier:
10 parts of organic resin+67 part terpinol+15 parts of diethyl phthalate+8 part dibutyl phthalates
After carrier prepares, green solid fluorescent material microparticulate in wherein making the formation slurry.Wet end furnish is as follows:
40 parts of fluorescent material+60 part organic carriers
The method for preparing fluorescent powder film layer is with embodiment 1 or 2.
Embodiment 5: make a kind of prescription of blue colour fluorescent powder slurry with carrier:
5 parts of organic resin+62 part terpinol+10 parts of acetamide+15 portion diethylene glycol (DEG)+8 parts of dibutyl phthalates
After carrier prepares, blue solid fluorescent material microparticulate in wherein making the formation slurry.Wet end furnish is as follows:
40 parts of fluorescent material+60 part organic carriers
The method for preparing fluorescent powder film layer is with embodiment 1 or 2.
According to the made fluorescent powder paste material of technical scheme of the present invention, embodiment can enumerate a lot, repeats no more here.Can obtain high-quality fluorescent coating behind the fluorescent powder paste material drying of making according to the present invention, the sintering.
At organic resin content is the organic solvent that uses three classes or the above different boiling of three classes to distribute in the organic carrier of 5～15 parts (weight ratios), make fluorescent material existing dispersed preferably in organic carrier, there is simultaneously different boiling points to distribute again, occurs the venting peak of decomposing and volatilizing and causing when avoiding high temperature sintering.
Claims (3)
1, a kind of fluorescent powder slurry materialfor plasma display composition, composition comprises fluorescent material, it is characterized in that, also comprise organic resin in the composition and contain three classes at least or the organic solvent making organic carrier of the above different boiling distribution of three classes, the boiling spread of the solvent of selecting for use is 155 ℃～360 ℃, wherein, contain in the composition and make the organic carrier that the green emitting phosphor slurry uses, contain the organic resin and the solvent of following weight ratio in the carrier:
4～8 parts of organic resin+55～65 part terpinol+20～23 parts of butyl carbitol+6～10 part triethanolamine+3～7 parts of cyclohexanone;
After carrier prepared, in wherein making the formation slurry, wet end furnish was as follows green solid fluorescent material microparticulate: 35～45 parts of fluorescent material+55～65 part organic carriers.
2, a kind of fluorescent powder slurry materialfor plasma display composition, composition comprises fluorescent material, it is characterized in that, also comprise organic resin in the composition and contain three classes at least or the organic solvent making organic carrier of the above different boiling distribution of three classes, the boiling spread of the solvent of selecting for use is 155 ℃～360 ℃, wherein, contain in the composition and make the organic carrier that the blue colour fluorescent powder slurry uses, contain the organic resin and the solvent of following weight ratio in the carrier:
4～6 parts of organic resin+58～68 part acetic acid butyl carbitol+8～11 part acetamide+9～12 parts of glycerol+3～6 part triethanolamine+3～6 parts of cyclohexanone;
After carrier prepared, in wherein making the formation slurry, wet end furnish was as follows blue solid fluorescent material microparticulate: 35～45 parts of fluorescent material+55～65 part organic carriers.
3, a kind of method for preparing fluorescent powder film layer, its feature comprises: adopt silk screen print method that claim 1 or the 2 described fluorescent powder slurry materialfor plasma display compositions made are printed on the glass breadboard of carrying out barrier, being placed on microscopically after printing observes, fluorescent powder paste material in the barrier ditch does not have bubble, breadboard is placed in the drying oven dries, bake out temperature is 130 ℃～150 ℃, be 10～15 minutes drying time, be placed on microscopically after the oven dry and observe the fluorescent powder film layer situation, the sidewall of its barrier and bottom of trench all evenly adhere to fluorescent powder film layer, no bulky grain or powder ball do not have the cavity; This breadboard is put into sintering furnace carry out sintering, sintering temperature is 450 ℃～500 ℃, and the time is 28～35 minutes, after sintering finishes, is placed on microscopically and observes, and phosphor powder layer is pure white, fine and smooth, does not have big powder ball, the cavity that stays after the no bubble volatilization.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101106048B (en) * | 2006-06-28 | 2011-02-16 | 东丽株式会社 | Fluorophor paste and method for manufacturing display device |
| CN101376804B (en) * | 2008-09-28 | 2011-04-20 | 江苏博睿光电有限公司 | PDP fluorescent powder pulp for spraying and preparation thereof |
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| CN100368505C (en) * | 2005-10-13 | 2008-02-13 | 四川世纪双虹显示器件有限公司 | Fluorescent powder slurry for plasma display |
| JP5088561B2 (en) * | 2007-02-23 | 2012-12-05 | Ｊｓｒ株式会社 | Liquid crystal alignment agent |
| CN101864297A (en) * | 2010-06-29 | 2010-10-20 | 彩虹集团公司 | Sizing agent for long-afterglow luminescent panel and preparation method |
| CN103642498B (en) * | 2013-11-19 | 2015-05-27 | 四川虹欧显示器件有限公司 | Red fluorescent powder slurry used for plasma panels and preparation method and applications thereof |
| CN112133469B (en) * | 2020-09-28 | 2022-03-11 | 长春黄金研究院有限公司 | Mixed organic solvent for preparing high-temperature sintering conductive slurry |
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2003
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101106048B (en) * | 2006-06-28 | 2011-02-16 | 东丽株式会社 | Fluorophor paste and method for manufacturing display device |
| CN101376804B (en) * | 2008-09-28 | 2011-04-20 | 江苏博睿光电有限公司 | PDP fluorescent powder pulp for spraying and preparation thereof |
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