CN101728156B - Electrode slurry for plasma display and application thereof - Google Patents
Electrode slurry for plasma display and application thereof Download PDFInfo
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- CN101728156B CN101728156B CN2009100810385A CN200910081038A CN101728156B CN 101728156 B CN101728156 B CN 101728156B CN 2009100810385 A CN2009100810385 A CN 2009100810385A CN 200910081038 A CN200910081038 A CN 200910081038A CN 101728156 B CN101728156 B CN 101728156B
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Abstract
The invention provides electrode slurry for a plasma display. The electrode slurry comprises an organic matter component, silver powder and low melting-point glass powder, wherein the organic matter component comprises a copolymer skeleton of methyl methacrylate and methacrylic acid; part of carboxyl of the copolymer skeleton have a structure of unsaturated double bond by introducing propylen acyloxy; and all the rest of carboxyl of the copolymer skeleton is neutralized by aqua ammonia. The invention also provides application of the electrode slurry in manufacturing the plasma display. The electrode slurry formed by the invention can be stably stored for a long time and can develop by using pure water.
Description
Technical field
The present invention relates to a kind of electrode slurry that is used for plasma display and this electrode slurry in the application of making plasma display.The formed electrode slurry of the present invention can steady in a long-termly be preserved, and uses pure water to develop.
Background technology
In recent years, flat panel display reached its maturity.Large scale, high definition and low-power consumption are the developing direction of flat-panel monitor.Particularly plasma flat-panel display is owing to have high brightness, high-contrast and low cost, and the characteristics that are easy to large scaleization, and becomes the trend of large scale flat-panel monitor gradually.Plasma display mainly is made up of two glass substrates, and the centre is filled with penning gas, and the red, green, blue three-color phosphor is arranged in the display unit of each pattern.Transparent ITO electrode is arranged on the prebasal plate, on the ITO electrode, be useful on the silver-colored bus electrode that increases conductivity.When display was worked, the addressing electrode on the metacoxal plate was confirmed luminescence unit, ITO electrode discharge ionized gas, thus excite the light-emitting phosphor in the diploe wall of back.
For the quantity that can make pixel on the power, ignition voltage and the raising glass substrate that reduce plasma display, the bus electrode on the prebasal plate and the quality of the addressing electrode on the metacoxal plate are very important.Requiring in definition is not in the extra high plasma flat-panel display, and silk screen printing method for producing confluxes and the process quilt of addressing electrode extensively adopts.The characteristics of this method are that manufacturing process is easier, can save raw material, thereby have obtained using widely.But the weak point of this technology is to form high-precision electrode pattern, and along with the increase of print pass, silk screen is easy to generate inelastic deformation, makes electrode pattern not reach required precision.Patent CN1424738A has introduced with the technology of silk screen printing method for producing silver electrode (referring to Fig. 1).
Because the condition restriction of print process itself is made very difficulty of meticulousr electrode.So someone has proposed to adopt photosensitive paste to make the new method of electrode pattern.This technology is silver coated slurry on whole glass substrate, hides with mask plate then, is ultraviolet ray exposure and the formation sub-image down of 365nm at wavelength.Develop with dilute alkaline soln at last, remove the part that does not have exposure.Fig. 2-4 shows the step that adopts this method to make electrode respectively.
Method through using photosensitive pulp coating exposure is made silver electrode, and its advantage is to form high-precision figure.But this just requires employed photosensitive silver slurry to have good photosensitivity, adhesiveness and resolution.In existing document, mentioned a kind of by methyl methacrylate and the resulting resin of methacrylic acid copolymerization as adhesive, its weight average molecular weight is about 10000.This copolymer has good light transmission, in the main chain of this high polymer, introduces the structure that contains carboxyl simultaneously, gives whole slurry good alkali solubility.But also there is shortcoming in this prepolymer structure and since molecular structure in lack two keys that polymerization can take place, thereby the photocuring ability a little less than.A kind of prepolymer that utilizes the sterically hindered effect protection of side chain carboxyl in the high polymer has been proposed in another piece patent CN1360685A.Functional group-the carboxyl structure that wherein is used for the alkali lye development is positioned at the high polymer side chain, under sterically hindered effect, and basic anhydride that exist in the slurry such as PbO, SiO
2Deng not reaching carboxyl, thereby overcome in the past owing to basic anhydride contact the gelling that produces with carboxyl.But this molecule side chain is complicated, synthetic difficulty, and cost of manufacture is higher.
Summary of the invention
To existing problem in the prior art, the present invention aims to provide a kind of electrode slurry of can steady in a long-term the preservation and not going bad, and this electrode slurry needn't use dilute alkaline soln simultaneously, only needs to use pure water to develop.
One aspect of the present invention provides a kind of electrode slurry that is used for plasma display, and it comprises organic components, silver powder and glass powder with low melting point.In this electrode slurry; Organic components comprises the copolymer skeleton of methyl methacrylate and methacrylic acid; The part carboxyl of this copolymer skeleton has the unsaturated double-bond structure through introducing acryloxy, and the remaining whole carboxyls of this copolymer skeleton neutralize with ammoniacal liquor.
According to electrode slurry of the present invention; Wherein, the copolymer skeleton of methyl methacrylate and methacrylic acid be selected from (methyl) acrylic acid glycidol ether, allyl glycidyl ether, (methyl) acrylic acid Alpha-Methyl epoxy propyl ester, the group that (methyl) acrylic acid α-ethyl epoxy propyl ester is constituted one or more and react and introduce acryloxy.
According to electrode slurry of the present invention; Wherein, Organic components also comprises ultraviolet initiator; This ultraviolet initiator is for being selected from by benzophenone, alpha, alpha-dimethyl oxygen base-α-phenyl acetophenone, α; In α-diethoxy acetophenone, 2-hydroxy-2-methyl-1-phenylacetone, 2-phenyl-2-dimethylamino-1-(4-morpholinyl phenyl)-butanone, 1-hydroxyl-cyclohexyl benzophenone, α-amine alkyl phenones, two benzoyl phenyl phosphine oxide, the group that tetramethyl Michler's keton, 4,4 '-two phenoxy group benzophenone are constituted one or more.
According to electrode slurry of the present invention; Wherein, Organic components also comprises reactive diluent; This reactive diluent is for being selected from by styrene, butyl acrylate, vinylacetate, 1, and 6-hexylene glycol double methacrylate, two contracts/tripropylene glycol double methacrylate, two contracts/in the group that triethylene Glycol double methacrylate, ethoxyquin bisphenol-A double methacrylate, polyethylene glycol double methacrylate are constituted one or more.
According to electrode slurry of the present invention, wherein, the average particle size distribution of silver powder is 1-8 μ m, and average specific surface area is 0.01-2.0m
2/ g.
According to electrode slurry of the present invention, wherein, the average particle size distribution of glass powder with low melting point is 1-8 μ m, and glass transition temperature is 300-500 ℃, and softening point is 400-600 ℃.
According to electrode slurry of the present invention, wherein, organic components content is 10-50%, and silver powder content is 40-80%, and the low-melting glass powder content is 5-20%.
According to electrode slurry of the present invention, wherein also can contain the composition of control slurry pH value.
According to electrode slurry of the present invention, wherein also can contain antifoaming agent and surfactant.
Another aspect of the present invention provides the application of above-mentioned electrode slurry in making plasma display.
New solution proposed by the invention; Utilize the esterification by ring opening effect of epoxide group; In with the copolymerized macromolecule of methyl methacrylate and methacrylic acid, introduce the unsaturated double-bond that the ultraviolet optical cement joins can take place; Use the ammoniacal liquor modification then, in main chain in carboxyl structure, make whole high polymer be neutral.This design is prone to produce the shortcoming of gel precipitation in the time of both can having solved the coexistence of carboxyl and oxide, give whole slurry water dissolubility simultaneously.So when developing, need not to use dilute alkaline soln, and only get final product with an amount of pure water rinsing.
Description of drawings
Fig. 1 is for making the sketch map of upper substrate silver electrode through print process, wherein show glass substrate 1, the silver electrode of confluxing 2, ITO (indium tin oxide) electrode 3;
Fig. 2-4 makes the sketch map of electrode process for adopting the photonasty electrode slurry, and wherein, Fig. 1 is the step of printed silver slurry, and Fig. 2 is the step of ultraviolet photoetching, and Fig. 3 forms the step of electrode for developing.
Embodiment
To at length introduce the embodiment of electrode slurry of the present invention and application thereof below, said details is not used in restriction scope of the present invention.Those skilled in the art should understand, and following specific descriptions are for the ease of understanding the present invention, not being used for limiting protection scope of the present invention.
The invention provides a kind of PDP (plasma panel) and use electrode slurry.This electrode slurry comprises organic components, silver powder and glass powder with low melting point.The present invention introduces acryloxy as ultraviolet curing group in the copolymer macromolecule of methyl methacrylate and methacrylic acid, use the ammoniacal liquor modification simultaneously, makes it have the ability of water development.This scheme both can solve the photoelectric sensitivity conductive silver paste and store unsettled shortcoming, can optimize developing process again simultaneously, used pure water to develop, and had improved production efficiency greatly.
In electrode slurry of the present invention, the high molecular skeleton structure of prepolymer is used methyl methacrylate and methacrylic acid copolymer.The high molecular skeleton structure of this copolymer has excellent ultraviolet light permeability, when printing, has good film forming, when 500-600 ℃ of sintering, can fully volatilize, and is residual few.Thereby photoelectric sensitivity conductive silver paste of the present invention can burn till below 600 ℃ through the electrode pattern that forms after the exposure imaging, forms the electrode pattern of high conductivity.High polymer weight average molecular weight of the present invention is preferably 10000-50000, and acid number is preferably 50-200.The high molecular skeleton structure of this prepolymer is by following chemical formulation:
In embodiment of the present invention; Part carboxyl in this prepolymer macromolecule be selected from the group that constitutes by (methyl) acrylic acid glycidol ether, allyl glycidyl ether, (methyl) acrylic acid Alpha-Methyl epoxy propyl ester, (methyl) acrylic acid α-ethyl epoxy propyl ester one or more and react; Double bond structure is introduced in the macromolecule; The unsaturated double-bond structure can issue at UV-irradiation and give birth to the effect of intermolecular glue couplet, generates water-fast high polymer.Remaining whole carboxyl structure makes it to obtain the ability of water development with in the ammoniacal liquor and modification.This prepolymer macromolecule content accounts for the 30-60% (weight ratio) of organic components in the slurry.
In embodiment of the present invention, the ultraviolet initiator in the electrode slurry organic components can cause Raolical polymerizable, generate high polymer, and the characteristic of the high polymer that generates is water insoluble.This ultraviolet initiator is for being selected from by benzophenone, alpha, alpha-dimethyl oxygen base-α-phenyl acetophenone, α; In α-diethoxy acetophenone, 2-hydroxy-2-methyl-1-phenylacetone, 2-phenyl-2-dimethylamino-1-(4-morpholinyl phenyl)-butanone, 1-hydroxyl-cyclohexyl benzophenone, α-amine alkyl phenones, two benzoyl phenyl phosphine oxide, the group that tetramethyl Michler's keton, 4,4 '-two phenoxy group benzophenone are constituted one or more.Preferred 2-phenyl-2-dimethylamino-1-(4-morpholinyl phenyl)-butanone and the composite initiator that contains it are as ultraviolet initiator.The content of ultraviolet initiator is preferably 2-10% (weight ratio).
In embodiment of the present invention, the reactive diluent characteristic in the electrode slurry organic components is that viscosity is little, can curing cross-linked under UV-irradiation, and the overall viscosity that can regulate conductive silver paste, make it to be applicable to the printing coating.This reactive diluent is for being selected from by styrene, butyl acrylate, vinylacetate, 1, and 6-hexylene glycol double methacrylate, two contracts/tripropylene glycol double methacrylate, two contracts/in the group that triethylene Glycol double methacrylate, ethoxyquin bisphenol-A double methacrylate, polyethylene glycol double methacrylate are constituted one or more.Reactive diluent can use separately, also can several kinds of mixing use.Its content is preferably 20-60% (weight ratio).
In embodiment of the present invention, the material that conductivity is provided behind the sintering is a silver powder particles, and the weight content of silver powder particles in electrode slurry is preferably 40-80%.Can select average particle size distribution for use is 1-8 μ m, and average specific surface area is 0.01-2.0m
2The silver powder of/g.
In embodiment of the present invention, because in sintering process, the silver and the tack between the glass substrate of fusing are bad, so must in slurry, add a certain amount of glass powder with low melting point.This glass powder with low melting point can be low-melting PbO-SiO
2Being glass, also can be unleaded Bi
2O
3-ZnO is a glass powder with low melting point.Can select average particle size distribution for use is 1-8 μ m, and glass transition temperature is 300-500 ℃, and softening point is 400-600 ℃ a glass powder with low melting point.
In addition, in order to make electrode slurry of the present invention the time have good levelability and tack can add certain antifoaming agent and surfactant in printing; In order to have excellent storage stability and homogeneity, obtain good coating performance, available acidity or alkaline ester class are regulated the pH value of slurry.These auxiliary agents are absolutely necessary in the manufacturing process of slurry, and in press major part commercialization, thereby this paper does not do too much elaboration.
Embodiment
The preparation of electrode slurry
Methyl methacrylate is mixed the formation copolymer with methacrylic acid with 4: 1 weight ratio, with this copolymer and the mixed formation prepolymer of (methyl) acrylic acid glycidol ether with 4: 1.According to prepolymer 30%, two propiophenones 4%, butyl acrylate 20%, average particle size distribution is that 1-8 μ m and average specific surface area are 0.01-2.0m
2The silver powder 40% of/g, Bi
2O
3-ZnO is the weight ratio of glass powder with low melting point 5%, butanols 1%, with above material mixing and stirring, is adjusted to PH=7 with ammoniacal liquor, forms the photonasty electrode slurry.
Methyl methacrylate is mixed the formation copolymer with methacrylic acid with 4: 1 weight ratio, with this copolymer and the mixed formation prepolymer of (methyl) acrylic acid glycidol ether with 4: 1.According to prepolymer 30%, two propiophenones 4%, styrene 10%, butyl acrylate 5%, vinylacetate 5%, average particle size distribution is that 1-8 μ m and average specific surface area are 0.01-2.0m
2The silver powder 40% of/g, Bi
2O
3-ZnO is the weight ratio of glass powder with low melting point 5%, butanols 1%, with above material mixing and stirring, is adjusted to PH=7 with ammoniacal liquor, forms the photonasty electrode slurry.
Methyl methacrylate is mixed the formation copolymer with methacrylic acid with 4: 1 weight ratio, with this copolymer and the mixed formation prepolymer of (methyl) acrylic acid glycidol ether with 5: 1.According to prepolymer 32%, two propiophenones 2%, butyl acrylate 20%, average particle size distribution is that 1-8 μ m and average specific surface area are 0.01-2.0m
2The silver powder 40% of/g, Bi
2O
3-ZnO is the weight ratio of glass powder with low melting point 5%, butanols 1%, with above material mixing and stirring, is adjusted to PH=7 with ammoniacal liquor, forms the photonasty electrode slurry.
Comparative example 1
Methyl methacrylate is mixed the formation copolymer with methacrylic acid with 4: 1 weight ratio, with this copolymer and the mixed formation prepolymer of (methyl) acrylic acid glycidol ether with 4: 1.According to prepolymer 30%, two propiophenones 4%, butyl acrylate 20%, average particle size distribution is that 1-8 μ m and average specific surface area are 0.01-2.0m
2The silver powder 40% of/g, Bi
2O
3-ZnO is the weight ratio of glass powder with low melting point 5%, butanols 1%, with above material mixing and stirring, forms the photonasty electrode slurry.
Comparative example 2
Methyl methacrylate is mixed the formation copolymer with methacrylic acid with 4: 1 weight ratio, with this copolymer and the mixed formation prepolymer of (methyl) acrylic acid glycidol ether with 4: 1.According to prepolymer 30%, two propiophenones 4%, styrene 10%, butyl acrylate 5%, vinylacetate 5%, average particle size distribution is that 1-8 μ m and average specific surface area are 0.01-2.0m
2The silver powder 40% of/g, Bi
2O
3-ZnO is the weight ratio of glass powder with low melting point 5%, butanols 1%, with above material mixing and stirring, forms the photonasty electrode slurry.
Comparative example 3
Methyl methacrylate is mixed the formation copolymer with methacrylic acid with 4: 1 weight ratio, with this copolymer and the mixed formation prepolymer of (methyl) acrylic acid glycidol ether with 5: 1.According to prepolymer 32%, two propiophenones 2%, butyl acrylate 20%, average particle size distribution is that 1-8 μ m and average specific surface area are 0.01-2.0m
2The silver powder 40% of/g, Bi
2O
3-ZnO is the weight ratio of glass powder with low melting point 5%, butanols 1%, with above material mixing and stirring, forms the photonasty electrode slurry.
The water development property of electrode slurry
The electrode slurry development property of embodiment 1-3, comparative example 1-3 is compared, and method is to use 3%～6% Na respectively
2CO
3Solution and pure water solution are attempted embodiment 1-3, comparative example 1-3 are developed, and whether realize that figure develops and judge concrete developing performance through observing.Table 1 has been listed the development property mensuration result of the electrode slurry of embodiment 1-3, comparative example 1-3.
The development property mensuration result of table 1 electrode slurry
| | |
| Embodiment | |
| 1 | Use pure water can realize that figure develops |
| |
Use pure water can realize that figure develops |
| |
Use pure water can realize that figure develops |
| Comparative example 1 | Use 3%～6% Na 2CO 3Solution can realize that figure develops, and uses pure water can't realize that figure develops. |
| Comparative example 2 | Use 3%～6% Na 2CO 3Solution can realize that figure develops, and uses pure water can't realize that figure develops. |
| Comparative example 3 | Use 3%～6% Na 2CO 3Solution can realize that figure develops, and uses pure water can't realize that figure develops. |
The electrode slurry storage stability
Known similar electrode slurry shelf life of products of the prior art is generally less than 6 months, and electrode slurry of the present invention can reach 6 months 0～5 ℃ of following shelf-life of condition.
Though describe and the present invention be described through specific embodiment, should be appreciated that for a person skilled in the art, under the situation that does not deviate from the spirit and scope of the present invention, can carry out various modifications and be equal to replacement the present invention.Therefore, the invention is not restricted to the specific embodiment described in this article.More properly, protection scope of the present invention is limited by the accompanying claims.
Claims (10)
1. electrode slurry that is used for plasma display; Comprise organic components, silver powder and glass powder with low melting point; Said electrode slurry is characterised in that; Said organic components comprises the copolymer skeleton of methyl methacrylate and methacrylic acid, and the part carboxyl of said copolymer skeleton has the unsaturated double-bond structure through introducing acryloxy, and the remaining whole carboxyls of said copolymer skeleton neutralize with ammoniacal liquor.
2. electrode slurry according to claim 1, said copolymer skeleton react and introduce acryloxy with being selected from by in (methyl) acrylic acid glycidol ether, allyl glycidyl ether, (methyl) acrylic acid Alpha-Methyl epoxy propyl ester, the group that (methyl) acrylic acid α-ethyl epoxy propyl ester is constituted one or more.
3. electrode slurry according to claim 1; Said organic components also comprises ultraviolet initiator; Said ultraviolet initiator is for being selected from by benzophenone, alpha, alpha-dimethyl oxygen base-α-phenyl acetophenone, α; In α-diethoxy acetophenone, 2-hydroxy-2-methyl-1-phenylacetone, 2-phenyl-2-dimethylamino-1-(4-morpholinyl phenyl)-butanone, 1-hydroxyl-cyclohexyl benzophenone, α-amine alkyl phenones, two benzoyl phenyl phosphine oxide, the group that tetramethyl Michler's keton, 4,4 '-two phenoxy group benzophenone are constituted one or more.
4. electrode slurry according to claim 1; Said organic components also comprises reactive diluent; Said reactive diluent is for being selected from by styrene, butyl acrylate, vinylacetate, 1, and 6-hexylene glycol double methacrylate, two contracts/tripropylene glycol double methacrylate, two contracts/in the group that triethylene Glycol double methacrylate, ethoxyquin bisphenol-A double methacrylate, polyethylene glycol double methacrylate are constituted one or more.
5. electrode slurry according to claim 1, the average particle size distribution of said silver powder are 1-8 μ m, and average specific surface area is 0.01-2.0m
2/ g.
6. electrode slurry according to claim 1, the average particle size distribution of said glass powder with low melting point are 1-8 μ m, and glass transition temperature is 300-500 ℃, and softening point is 400-600 ℃.
7. electrode slurry according to claim 1, said organic components content is 10-50%, and said silver powder content is 40-80%, and said low-melting glass powder content is 5-20%.
8. electrode slurry according to claim 1 also contains the composition of controlling the slurry pH value.
9. electrode slurry according to claim 1 also contains antifoaming agent and surfactant.
10. according to the application of each described electrode slurry among the claim 1-9 in making plasma display.
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|---|---|---|---|
| CN2009100810385A CN101728156B (en) | 2009-03-31 | 2009-03-31 | Electrode slurry for plasma display and application thereof |
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|---|---|---|---|
| CN2009100810385A CN101728156B (en) | 2009-03-31 | 2009-03-31 | Electrode slurry for plasma display and application thereof |
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| CN101728156B true CN101728156B (en) | 2012-02-29 |
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| CN102509682A (en) * | 2011-12-31 | 2012-06-20 | 四川虹欧显示器件有限公司 | Electrode slurry used for plasma display screen, preparation method thereof and electrode prepared from electrode slurry |
| CN110335700B (en) * | 2019-06-28 | 2021-11-26 | 乾宇电子材料(苏州)有限公司 | High-temperature sintering type yellow light conductive paste, conductive circuit and preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1585040A (en) * | 2003-08-21 | 2005-02-23 | 太阳油墨制造株式会社 | Photosensitive electric conductive composition and plasma display panel |
| CN1945752A (en) * | 2005-06-29 | 2007-04-11 | E.I.内穆尔杜邦公司 | Method for manufacturing a conductive composition and a rear substrate of a plasma display |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1585040A (en) * | 2003-08-21 | 2005-02-23 | 太阳油墨制造株式会社 | Photosensitive electric conductive composition and plasma display panel |
| CN1945752A (en) * | 2005-06-29 | 2007-04-11 | E.I.内穆尔杜邦公司 | Method for manufacturing a conductive composition and a rear substrate of a plasma display |
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