CN1448960A - Starched agent and glass powder for forming dielectric for plasma display board - Google Patents

Starched agent and glass powder for forming dielectric for plasma display board Download PDF

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Publication number
CN1448960A
CN1448960A CN03108404A CN03108404A CN1448960A CN 1448960 A CN1448960 A CN 1448960A CN 03108404 A CN03108404 A CN 03108404A CN 03108404 A CN03108404 A CN 03108404A CN 1448960 A CN1448960 A CN 1448960A
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China
Prior art keywords
glass powder
particle diameter
dielectric
paste
plasma display
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Granted
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CN03108404A
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Chinese (zh)
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CN1277274C (en
Inventor
西川佳范
新宅彻
大下浩之
波多野和夫
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Nippon Electric Glass Co Ltd
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Nippon Electric Glass Co Ltd
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Publication of CN1448960A publication Critical patent/CN1448960A/en
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Anticipated expiration legal-status Critical
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/10—Frit compositions, i.e. in a powdered or comminuted form containing lead
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
    • H01B3/08—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances quartz; glass; glass wool; slag wool; vitreous enamels
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip

Abstract

A dielectric substance-forming paste containing a dielectric substance-forming glass powder, thermoplastic resin and solvent for plasma display panel are provided. The glass powder has a size distribution of a maximum diameter (Dmax) of 15 micrometers or less, a 90% diameter (D90) of 7 micrometer or less, a 75% diameter (D75) of 4 micrometers or less, a 50% diameter of (D50) of 3 micrometers or less, and a 25% diameter (D25) of 2 micrometers or less, and a specific surface area of 1.0-4.0 m<2>/g.

Description

Form paste and the glass powder of plasma display panel with dielectric
Technical field
The present invention relates to form the employed dielectric formation of the dielectric layer material of plasma display panel.
Background technology
Plasma display panel has front glass plate and is formed at the scan electrode that the plasma discharge on this front glass plate is used.On scan electrode, be formed with the dielectric layer that thickness is 30～40 μ m.Require the transparency of this dielectric layer good and have a characteristic of high proof voltage.These characteristics be subjected to a great extent dielectric layer grade, be the domination of bubble state in surface smoothing and the layer.
As the method that forms this dielectric layer, well-known method of past, the pasty state dielectric that powder composition such as glass powder and matchmaker's liquid (thermoplastic resin etc. is dissolved in solvent and form) mixing is made forms material (in the following description it being called " paste that forms dielectric ") and carries out screen printing, burns till again.
But, the paste of existing formation dielectric exist be difficult to form level and smooth and have homogeneous film thickness overlay, residual shortcomings such as a lot of bubbles and residual bubble diameter are big are arranged, so have the problem that is difficult to form transparency height, dielectric layer that withstand voltage properties is high.Therefore, though attempt the quality that viscosity by adjusting matchmaker's liquid and mixed proportion thereof improve dielectric layer, poor with this method reproducibility, can not fundamentally address the above problem.
Summary of the invention
The object of the present invention is to provide a kind of paste that forms dielectric, this paste can form the dielectric layer that transparency is good and withstand voltage properties is high.
Another object of the present invention is to provide a kind of paste that forms dielectric, this paste is suitable for forming the plasma display panel dielectric.
Another purpose of the present invention is to provide a kind of glass powder, and this glass powder is suitable for the formation of the paste of above-mentioned formation dielectric.
Present inventors have carried out various experiments, found that, the particle size distribution that forms the glass powder that is contained in the paste of dielectric by control can achieve the above object, so put forward as the present invention.
According to a kind of form of the present invention, can obtain forming the paste of plasma display panel with dielectric, this paste is characterised in that with in the paste of dielectric, above-mentioned glass powder has maximum particle diameter D at the formation plasma display panel that contains glass powder MAXBe that 15 μ m are following, 90% particle diameter D 90Be that 7 μ m are following, 75% particle diameter D 75Be that 4 μ m are following, 50% particle diameter D 50Be that 3 μ m are following, 25% particle diameter D 25Be the following particle size distribution of 2 μ m, the specific area of above-mentioned glass powder is 1.0～4.0m 2/ g.
According to another kind of form of the present invention, can obtain forming the glass powder of plasma display panel and dielectric, this glass powder is characterised in that to have maximum particle diameter D MAXBe that 15 μ m are following, 90% particle diameter D 90Be that 7 μ m are following, 75% particle diameter D 75Be that 4 μ m are following, 50% particle diameter D 50Be that 3 μ m are following, 25% particle diameter D 25Be the following particle size distribution of 2 μ m, specific area is 1.0～4.0m 2/ g.
Embodiment
Below, the paste of the formation dielectric of the invention process form is illustrated.
The paste that this forms dielectric is suitable for forming the dielectric layer of thickness 30～40 μ m on scan electrode being formed at plasma discharge on the front glass plate of plasma display panel, and main component contains glass powder.The maximum particle diameter D of this glass powder MAXBe that 15 μ m are following, 90% particle diameter D 90Be that 7 μ m are following, 75% particle diameter D 75Be that 4 μ m are following, 50% particle diameter D 50Be that 3 μ m are following, 25% particle diameter D 25Be below the 2 μ m, specific area is 1.0～4.0m 2/ g.When limiting the particle size distribution of glass powder like this, the gap between the glass powder particle is very little, so the bubble that is contained in the dielectric layer after burning till is few, residual bubble is also minimum, and light transmittance is more than 76%.And the surface smoothing raising of dielectric layer is with being called the occasion of the method coating paste of coating in batches, this particular significant effect.
Maximum particle diameter D with glass powder MAXBe chosen to be below the 15 μ m, be preferably 8～10 μ m.Maximum particle diameter D MAXWhen surpassing 15 μ m, the interval between the particle is excessive, residual a lot of bubbles, and this bubble diameter also increases, so can not guarantee enough transparencys.And, the surface smoothing reduction of dielectric layer, proof voltage variation.The maximum particle diameter D of glass powder MAXDuring less than 8 μ m, the recovery rate of glass powder reduces, and the production efficiency variation is so have problems in actual production.
The particle size distribution of glass powder is: 90% particle diameter D 90Being that 7 μ m are following (is preferably 3≤D 90＜7 μ m), 75% particle diameter D 75Being that 4 μ m are following (is preferably 2≤D 75＜4 μ m), 50% particle diameter D 50Being that 3 μ m are following (is preferably 1≤D 50＜3 μ m), 25% particle diameter D 25Being that 2 μ m are following (is preferably 0.5≤D 25＜2 μ m).In the occasion greater than various particle diameters, the interval between the particle increases, and number of bubbles increases, and bubble diameter increases, transparent variation.And, make the surface smoothing reduction of dielectric layer easily.
In addition, as glass powder, containing PbO in Quality Percentage is 50～75% (being preferably 60～72%), B 2O 3Be 2～30% (being preferably 2～20%), SiO 2Be that 2～35% (being preferably 5～30%), ZnO+CaO are the glass of 0～20% (being preferably 0～10%), or to contain PbO in Quality Percentage be 30～55% (being preferably 40～50%), B 2O 3Be 10～40% (being preferably 15～35%), SiO 2Be that 1～15% (being preferably 2～10%), ZnO are 0～30% (being preferably 10～30%), BaO+CaO+Bi 2O 3Be the glass of 0～30% (being preferably 3～20%), or to contain ZnO in Quality Percentage be 40～70% (being preferably 40～60%), B 2O 3Be 20～40% (being preferably 20～35%), SiO 2Be 5～20% (being preferably 5～15%), Na 2O+K 2O+Li 2O is the glass of 2～30% (being preferably 2～20%), or to contain ZnO in Quality Percentage be 25～45% (being preferably 30～40%), Bi 2O 3Be 15～40% (being preferably 20～35%), B 2O 3Be 10～30% (being preferably 15～25%), BiO 2Be that 0.5～8% (being preferably 1～6%), CaO+SrO+BaO are the glass of 8～24% (being preferably 10～20%), under 500～600 ℃ of temperature, burn till, express good flowability, in addition, the transparency and excellent in insulation characteristic and stable are so be very suitable.
Above-mentioned glass powder is very suitable as forming plasma display panel with the material of dielectric.As hereinafter described, use after the formation paste.In addition, not only form paste, also can make living thin slice and use.
Also contain thermoplastic resin, plasticizer and solvent etc. with above-mentioned glass powder as paste main component, that form dielectric.In this paste, glass powder is the composition that has the dielectric layer of high proof voltage for formation, and its content is 30～90 quality %, and is particularly more satisfactory in 50～70 quality % scopes.
Thermoplastic resin is to improve the dried film strength of dielectric layer and give the composition of flexibility, and its content is 0～30 quality %, and is more satisfactory in particular for 0.1～30 quality %, and is better in 1～20 quality % scope.As thermoplastic resin, can use polybutyl methacrylate, polyvinyl butyral resin, polymethyl methacrylate, polyethyl acrylate, ethyl cellulose etc., use these resins separately or these mixed with resin get up are used.
Plasticizer is to control the rate of drying of dielectric layer and give the composition of desciccator diaphragm flexibility, and its content is preferably 0～50 quality %, and it is then better to be in particular 5～30 quality % scopes.As plasticizer, can use BBP(Butyl Benzyl Phthalate, dioctyl phthalate, diisooctyl phthalate ester, two ethyl butyrates, Dibutyl phthalate etc., use these plasticizers separately or these plasticizers are mixed use.
Solvent is to make material become the composition that paste is used, and its content is at 5～60 quality %, particularly more satisfactory in 20～50 quality % scopes.As solvent, can be used alone or as a mixture for example terpineol, dimethanol (list) methyl ether acetate, 2,2,4-trimethyl-1,3-pentadiene-isobutyrate etc.
In addition, except mentioned component, for example flowability, agglutinating property or the thermal coefficient of expansion in order to adjust paste can add ceramic powders such as aluminium oxide, zirconia and reach 10 quality %.
Below, the method for the paste of making above-mentioned formation dielectric is illustrated.
At first, be ready to glass powder, thermoplastic resin, plasticizer, solvent etc.In addition, glass powder will be pulverized with ball mill and fluid energy grinding mill etc., carries out classification by air current classifying etc. again, and it is important making its particle size distribution with regulation.Then,, obtain the material of pasty state, promptly form the paste of dielectric each composition ratio mixing in accordance with regulations.
Below, the method that the paste with this formation dielectric is formed dielectric layer describes.
At first, prepare plasma display panel by used front glass plate.Form scan electrode on the glass plate in front in advance.Then, with stencil printing or in batches the paste that will form dielectric such as coating above scan electrode, be coated on the front glass plate, form the overlay of thickness 30～100 μ m.Then, make overlay dry under 80～120 ℃ of left and right sides temperature.Overlay under 500～600 ℃ temperature, with 5～15 fen clock time burn till, just can be formed dielectric layer thereafter.
Below, several embodiments of the present invention are described with comparative example.
Table 1 expression embodiments of the invention (test portion NO.1～NO.3) and comparative example (test portion N0.4～N0.7)
Table 1
Test portion N0. Embodiment Comparative example
????1 ????2 ????3 ????4 ????5 ????6 ????7
Glass powder D max(μm) D 90(μm) D 75(μm) D 50(μm) D 25(μ m) specific area (m 2/g) ????9.3 ????3.5 ????3.0 ????2.4 ????1.6 ????2.5 ????11.3 ????4.6 ????3.7 ????2.9 ????1.8 ????2.0 ????9.3 ????3.7 ????2.6 ????1.7 ????1.0 ????3.0 ????13.8 ????6.0 ????4.7 ????3.7 ????2.5 ????1.5 ????25.3 ????7.8 ????4.8 ????2.6 ????1.2 ????1.0 ????15.0 ????6.5 ????5.0 ????2.8 ????2.1 ????1.5 ????19.5 ????7.5 ????6.0 ????2.9 ????2.2 ????1.0
Number of bubbles (individual) is greater than below 10 μ m, the 10 μ m ????0 ????0 ????0 ????3 ????0 ????1 ????4 ????2 ????15 ????2 ????7 ????1 ????10 ????2
Surface roughness Ra (μ m) ????0.31 ????0.42 ????0.30 ????0.92 ????2.25 ????1.35 ????1.90
Transmitance (%) ????83 ????81 ????82 ????75 ????72 ????74 ????74
Each test portion of table 1 will form paste in quality % glass powder 65%, ethyl cellulose 5% and terpineol 30% mixing.
Glass powder is produced as follows.At first, will be in quality % PbO 65.0%, B 2O 35.0%, SiO 225.0%, the raw material of CaO 5.0% is in harmonious proportion so that to become softening point be 560 ℃ glass, and the platinum crucible of packing into after evenly mixing forms after dissolving 2 hours under 1300 ℃ of temperature.Then, should pulverize with the fluid energy grinding mill by the shaping thing, carry out air current classifying again, obtain particle size distribution and be: maximum particle diameter D MAXBe 9.3～25.3 μ m, 90% particle diameter D 90Be 3.5～7.8 μ m, 75% particle diameter D 75Be 2.6～6.0 μ m, 50% particle diameter D 50Be 1.7～3.7 μ m, 25% particle diameter D 25Be 1.0～2.5 μ m, have 1.0～3.0m 2The glass powder of the specific area of/g.In addition, maximum particle diameter D MAX, 90% particle diameter D 90, 75% particle diameter D 75, 50% particle diameter D 50And 25% particle diameter D 25Be that laser diffraction formula particle size distribution meter " マ イ Network ロ ト ラ ッ Network SPA " with Nikkiso Company Limited's system is confirmed.
Then, each test portion is carried out screen printing thick on the cum calce soda glass pane surface of 1.7mm, burnt till 10 minutes under 570 ℃ of temperature dry back, just forms the glass-film of the about 30 μ m of film thickness.Then, the surface roughness Ra of resulting glass-film, the state and the transmitance of bubble are estimated.The results are shown in table 1.
As shown in Table 1, embodiments of the invention NO.1～NO.3 test portion, the surface roughness Ra of glass-film is 0.30～0.42 μ m, and in addition, greater than the bubble of 10 μ m, the bubble below the 10 μ m is not less, is 0～3, and transmitance is 81～83%.
And the test portion NO.4～NO.7 of comparative example, surface roughness Ra is higher, is 0.92～2.25 μ m, in addition, has more than 4 greater than the bubble of 10 μ m, and transmitance is lower, is 72～75%.
These evaluation results show, if adopt the NO.1～NO.3 test portion of the embodiment of the invention, can form withstand voltage properties height and the good dielectric layer of the transparency.
In addition, the state of bubble is with the 1cm of stereomicroscope to the test portion after burning till 2Count and estimate greater than 10 μ m bubble numbers and the bubble number below the 10 μ m in the scope.The surface roughness of glass-film is measured with contact pin type surface roughness meter.Transmitance is measured with spectrophotometer.Transmitance has been measured the diffusion transmitance of wavelength 550nm.In addition, used test portion when measuring transmitance uses employed test portion when measuring the bubble number, measures the value that expression enters glass plate with the spectrophotometer UV-3100 of Shimadzu Seisakusho Ltd.'s system.
Table 2 expression other embodiments of the invention.
Table 2
Test portion NO. Embodiment
????8 ????9 ????10 ????11 ????12 ????13
Glass powder is formed PbO B 2O 3SiO 2CaO TiO 2Al 2O 3ZnO BaO ZrO 2Bi 2O 3Li 2O Na 2O ????70 ????3 ????25 ????2 ????64 ????14 ????11 ????2 ????1 ????3 ????2 ????1 ????2 ????46 ????20 ????4 ????1 ????20 ????9 ????18 ????3 ????12 ????35 ????32 ????25 ????7 ????1 ????49 ????12 ????2 ????1 ????3 ????20 ????11 ????3 ????49 ????12 ????5
Softening point (℃) ????545 ????520 ????520 ????555 ????555 ????575
Glass powder granularity D max(μm) D 90(μm) D 75(μm) D 50(μm) D 25(μ m) specific area (m 2/g) ????9.5 ????3.2 ????2.9 ????2.3 ????1.5 ????2.6 ????10.0 ????5.5 ????3.9 ????2.8 ????1.9 ????2.2 ????8.5 ????3.2 ????2.1 ????1.5 ????0.8 ????3.5 ????9.3 ????3.5 ????2.5 ????1.5 ????0.9 ????3.0 ????8.8 ????3.2 ????2.2 ????1.7 ????0.9 ????3.3 ????10.0 ????5.4 ????3.8 ????2.7 ????1.9 ????2.2
Firing temperature (℃) firing time (branch) ????555 ????10 ????540 ????10 ????530 ????10 ????565 ????10 ????565 ????10 ????585 ????10
Number of bubbles (individual) is greater than below 10 μ m, the 10 μ m ????0 ????1 ????0 ????3 ????0 ????1 ????0 ????1 ????0 ????1 ????0 ????3
Surface roughness Ra (μ m) ????0.3 ????0.35 ????0.1 ????0.3 ????0.1 ????0.35
Transmitance (%) ????85 ????86 ????80 ????80 ????79 ????80
Each test portion of table 2, adopt the method identical to be in harmonious proportion, to make with the test portion of table 1 after, use the same method and estimate.In addition, burn till under the conditions shown in Table 2.
Its result, NO.8～NO.13 test portion, the surface light roughness Ra of glass-film is 0.10～0.5 μ m, and greater than the bubble of 10 μ m, the bubble below the 10 μ m is not less, is 1～3, and transmitance is 79～86%.
As mentioned above, after the formed overlay of paste with the formation dielectric of the invention process form burnt till, become have level and smooth and uniformly thickness, almost do not have a glass-film of residual bubble.Therefore, can form transparency height, dielectric layer that withstand voltage properties is high.
The possibility of utilizing on the industry
Formation dielectric paste of the present invention is well suited at the plasma discharge that is formed on the front glass plate of plasma display panel and forms dielectric layer with scan electrode.

Claims (6)

1. one kind forms the dielectric paste that plasma display panel is used, it is characterized in that, contain glass powder, form plasma display panel with in the paste of dielectric, above-mentioned glass powder has maximum particle diameter D MAXBe that 15 μ m are following, 90% particle diameter D 90Be that 7 μ m are following, 75% particle diameter D 75Be that 4 μ m are following, 50% particle diameter D 50Be that 3 μ m are following, 25% particle diameter D 25Be the following particle size distribution of 2 μ m, the specific area of above-mentioned glass powder is 1.0～4.0m 2/ g.
2. formation plasma display panel according to claim 1 is characterized in that with the paste of dielectric, and PbO is 50～75% to above-mentioned glass powder, B by containing in Quality Percentage 2O 3Be 2～30%, SiO 2The glass that be 2～35%, ZnO+CaO is D～20% constitutes.
3. formation plasma display panel according to claim 1 is characterized in that with the paste of dielectric, and PbO is 30～55% to above-mentioned glass powder, B by containing in Quality Percentage 2O 3Be 10～40%, SiO 2Be 1～15%, ZnO is 0～30%, BaO+CaO+Bi 2O 3Be that 0～30% glass constitutes.
4. formation plasma display panel according to claim 1 is characterized in that with the paste of dielectric, and ZnO is 40～70% to above-mentioned glass powder, B by containing in Quality Percentage 2O 3Be 20～40%, SiO 2Be 5～20%, Na 2O+K 2O+Li 2O is 2～30% glass formation.
5. formation plasma display panel according to claim 1 is characterized in that with the paste of dielectric, and ZnO is 25～45% to above-mentioned glass powder, Bi by containing in Quality Percentage 2O 3Be 15～40%, B 2O 3Be 10～30%, SiO 2Be 0.5～8%, CaO+SrO+BaO is that 8～24% glass constitutes.
6. a glass powder that forms plasma display panel with dielectric is characterized in that having maximum particle diameter D MAXBe that 15 μ m are following, 90% particle diameter D 90Be that 7 μ m are following, 75% particle diameter D 75Be that 4 μ m are following, 50% particle diameter D 50Be that 3 μ m are following, 25% particle diameter D 25Be the following particle size distribution of 2 μ m, specific area is 1.0～4.0m 2/ g
CNB031084044A 2002-03-28 2003-03-28 Starched agent and glass powder for forming dielectric for plasma display board Expired - Fee Related CN1277274C (en)

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JP2003050725A JP2004006259A (en) 2002-03-28 2003-02-27 Dielectric formation paste for plasma display panel, and glass powder therefor
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7482753B2 (en) 2003-10-30 2009-01-27 Samsung Sdi Co., Ltd. Plasma display panel with angled dielectric film
CN101685735B (en) * 2008-09-28 2011-03-30 四川虹欧显示器件有限公司 Inorganic powder composition for plasma display panel barrier slurry

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060000515A (en) * 2004-06-29 2006-01-06 대주전자재료 주식회사 Pb-free glass composition for barrier ribs of plasma display panel
JP4788391B2 (en) * 2006-02-23 2011-10-05 パナソニック株式会社 Method for manufacturing plasma display panel
GB201812052D0 (en) * 2018-07-24 2018-09-05 Johnson Matthey Plc Particle mixture, kit, ink, methods and article

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7482753B2 (en) 2003-10-30 2009-01-27 Samsung Sdi Co., Ltd. Plasma display panel with angled dielectric film
US8043653B2 (en) 2003-10-30 2011-10-25 Samsung Sdi Co., Ltd. Method of forming a dielectric film and plasma display panel using the dielectric film
CN101685735B (en) * 2008-09-28 2011-03-30 四川虹欧显示器件有限公司 Inorganic powder composition for plasma display panel barrier slurry

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