CN1740109A - Lead-free black ceramic composition for filter and filter formed using the same - Google Patents

Lead-free black ceramic composition for filter and filter formed using the same Download PDF

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Publication number
CN1740109A
CN1740109A CNA2005100896180A CN200510089618A CN1740109A CN 1740109 A CN1740109 A CN 1740109A CN A2005100896180 A CNA2005100896180 A CN A2005100896180A CN 200510089618 A CN200510089618 A CN 200510089618A CN 1740109 A CN1740109 A CN 1740109A
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amount
scope
composition
unleaded
weight portion
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车准圭
文东建
沈勉基
林翼喆
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Samsung SDI Co Ltd
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Samsung SDI Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J11/00—Gas-filled discharge tubes with alternating current induction of the discharge, e.g. alternating current plasma display panels [AC-PDP]; Gas-filled discharge tubes without any main electrode inside the vessel; Gas-filled discharge tubes with at least one main electrode outside the vessel
    • H01J11/20—Constructional details
    • H01J11/34—Vessels, containers or parts thereof, e.g. substrates
    • H01J11/44—Optical arrangements or shielding arrangements, e.g. filters, black matrices, light reflecting means or electromagnetic shielding means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00—Pigment pastes, e.g. for mixing in paints
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
    • C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
    • C03C2217/475—Inorganic materials
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
    • C03C2217/48—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase having a specific function
    • C03C2217/485—Pigments

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electromagnetism (AREA)
  • Plasma & Fusion (AREA)
  • Ceramic Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Glass Compositions (AREA)

Abstract

Provided are an essentially lead-free black ceramic composition for a filter, a filter formed using the same, and a flat display device including the filter. The lead-free black ceramic composition may include at least one compound selected from the group consisting of B2O3, BaO, and ZnO; and at least one black pigment selected from the group consisting of TiO, CuO, NiO, MnO2, Cr2O3 and Fe2O3. Alternatively, the lead-free black ceramic composition may include Bi2O3; at least one compound selected from the group consisting of B2O3, SiO2, P2O5, Na2O3, Al2O3, BaO, ZnO and TiO2; and at least one black pigment selected from the group consisting of TiO, CuO, NiO, MnO2, Cr2O3 and Fe2O3. The lead-free black ceramic composition for a filter essentially does not contain PbO, which harms human beings and the environment. As a result, the use of the composition is not affected by regulations preventing the use of Pb. In addition, the composition can be calcined at a relatively low temperature and consume a small amount of energy.

Description

Be used for the unleaded black ceramic composition of spectral filter and with the spectral filter of its preparation
CROSS-REFERENCE TO RELATED PATENT
The application requires the right of priority of the korean patent application No.10-2004-0047620 that submits to Korea S Department of Intellectual Property in the korean patent application No.10-2004-0049723 that submitted to Korea S Department of Intellectual Property on June 29th, 2004 and on June 24th, 2004, and its disclosed content quotes in full for reference in this article.
Technical field
The present invention relates to a kind of unleaded black ceramic composition that is used for the spectral filter of plane demonstration, relate in particular to a kind of unleaded black ceramic composition that improves luminous efficiency and contrast gradient that has.
Background technology
Plasma display panel (PDP) because have that the visual angle is wide, colored, response speed is fast, size is big and the advantage of thin thickness can be used as family expenses wall type TV flat-panel screens, be used for the large screen display of office meeting and public arena etc.According to the structure and the driving voltage of discharge cell, PDP can be divided into direct current (DC) PDP and exchange (AC) PDP.
PDP has filter to prevent because external action causes the expansion of plate and shields the near infrared ray that is produced by inert gas plasma by shielding invalid screen on whole surface.
In the spectral filter of PDP, glass substrate is surrounded with preset width with the black ceramic material, so that the invalid screen of shielding PDP plate, the luminous intensity of so obvious raising screen.Therefore, as long as black ceramic is black more, just can obtain better luminous efficiency.
Typically, black matrix is made of the black ceramic composition that contains PbO.Because the glass transformation temperature of this composition is 500 ℃ or lower, can use little heat energy effectively to obtain the effect of blackening.Yet the shortcoming of this composition is to have Pb, and this is unwelcome to environment protection.
The glass transformation temperature that does not contain the black ceramic composition of PbO is higher than 550 ℃, and therefore needs calcining at high temperature.
Summary of the invention
The invention provides electronic application equipment environment amenable, that utilize no PbO black ceramic composition to make.
The present invention also provides a kind of unleaded black ceramic composition of the spectral filter that is used for flat display board as described below.This unleaded black ceramic composition has low glass transformation temperature, obtains effectively black effect with minimum heat energy like this.The filter that forms with unleaded black ceramic composition also is provided, forms the method for filter and uses the flat-panel screens of this filter.
According to an aspect of the present invention, provide a kind of unleaded black ceramic composition for filter, said composition comprises: at least a B that is selected from 2O 3, the compound among BaO and the ZnO; With at least a TiO, CuO, NiO, the MnO of being selected from 2, Cr 2O 3And Fe 2O 3In mineral black, wherein said composition is unleaded.
According to another aspect of the present invention, provide a kind of unleaded black ceramic composition for filter, said composition comprises: Bi 2O 3, at least a B that is selected from 2O 3, SiO 2, P 2O 5, Na 2O 3, Al 2O 3, BaO, ZnO and TiO 2In compound; With at least a TiO, CuO, NiO, the MnO of being selected from 2, Cr 2O 3And Fe 2O 3In mineral black, wherein said composition is unleaded.
According to a further aspect in the invention, provide a kind of filter that forms by printing and this unleaded black ceramic composition of heat treatment.
In accordance with a further aspect of the present invention, provide a kind of method that forms filter, this method comprises: (a) with at least a B of being selected from 2O 3, compound and dissolving among BaO and the ZnO, wherein this compound is unleaded; (b) product that dissolves is cooled off at short notice, then the product that cools off is ground into glass powder; (c) with glass powder and at least a TiO, CuO, NiO, the MnO of being selected from 2, Cr 2O 3And Fe 2O 3In mineral black mix; (d) product that mixes is mixed the formation composition with the organic carrier that forms by interpolation adhesive and plasticizer in solvent; (e) said composition is printed on the glass substrate; The glass substrate heat treatment that (f) will print.
According to an aspect of the present invention, provide a kind of flat-panel screens that comprises filter, this filter is to utilize to contain at least a B of being selected from 2O 3, the compound among BaO and the ZnO, wherein unleaded and at least a TiO, CuO, NiO, the MnO of being selected from of this compound 2, Cr 2O 3And Fe 2O 3In the unleaded black ceramic composition of mineral black form.
Description of drawings
By the embodiment of detailed description exemplary with reference to the accompanying drawings, above-mentioned and other characteristics of the present invention and advantage will be clearer, wherein:
Fig. 1 is the sectional view of spectral filter of the plasma display panel of embodiment of the present invention;
Fig. 2 is the orthographic plan of spectral filter shown in Figure 1; With
Fig. 3 is the decomposing schematic representation that contains the plasma display panel of spectral filter shown in Figure 1.
Embodiment
Now, with reference to the accompanying drawings the present invention is described more fully.
The unleaded black ceramic composition that is used for according to embodiments of the present invention filter can comprise at least a B of being selected from 2O 3, the compound among BaO and the ZnO, wherein this compound is unleaded; With at least a TiO, CuO, NiO, the MnO of being selected from 2, Cr 2O 3And Fe 2O 3In mineral black.
In forming glass, use B 2O 3, improved dielectric constant and the linear expansion coefficient of glass.
BaO reduces glass transformation temperature and improves the specific inductivity and the coefficient of linear expansion of glass.The amount of BaO is based on the B of 100 weight portions 2O 3Meter arrives in the scope of about 100 weight portions about 33.3.When the amount of BaO surpasses about 100 weight parts, the obvious deterioration of the performance of glass composition, this is undesirable.When the amount of BaO is less than about 33.3 weight parts, do not tell on.
ZnO improves the acid resistance and the chemical resistance of glass.The amount of ZnO is preferably based on the B of 100 weight portions 2O 3Meter arrives in the scope of about 114 weight portions about 16.6.When the amount of ZnO was less than about 16.6 weight portion, the acid resistance of glass descended.When the amount of ZnO surpassed about 114 weight parts, flowability undesirably reduced.
This unleaded black composition contains at least a TiO of being selected from, CuO, NiO, MnO 2, Cr 2O 3And Fe 2O 3In mineral black.TiO, CuO, NiO, MnO 2, Cr 2O 3And Fe 2O 3It is the metal oxide that makes the composition blackening.Just, the mineral black that contains in the composition makes whole composition blackening.
The amount of at least a mineral black is based on the B of 100 weight portions 2O 3Meter arrives in the scope of about 28.5 weight portions about 0.16.When the amount of this at least a mineral black was less than about 0.16 weight part, composition may be deceived inadequately.When the amount of this at least a mineral black surpassed 28.5 weight portion, the performance of this glass composition was degenerated along with the increase of pigment component, and this is undesirable.
In one embodiment of the invention, TiO, CuO, NiO, MnO 2, Cr 2O 3And Fe 2O 3Amount based on the B of 100 weight portions 2O 3Meter arrives in the scope of about 28.5 weight portions about 0.16.
The glass transformation temperature of said composition is about 450 between about 550 ℃, and preferably, between about 480 to about 530 ℃.Because this low glass transformation temperature, can be in low temperature lower calcination said composition, and therefore have low energy consumption.In addition, said composition is harmless, and is considered to environmental protection.
The unleaded black ceramic composition that is used for filter of another one embodiment of the present invention also contains Bi in addition 2O 3In preferred embodiments, the composition of the present embodiment comprises Bi 2O 3At least a B that is selected from 2O 3, SiO 2, P 2O 5, Na 2O 3, Al 2O 3, BaO, ZnO and TiO 2In compound, wherein this compound is unleaded; With at least a TiO, CuO, NiO, the MnO of being selected from 2, Cr 2O 3And Fe 2O 3In mineral black.
Use Bi 2O 3To obtain low glass transformation temperature.
At least a B that is selected from 2O 3, SiO 2, P 2O 5, Na 2O 3, Al 2O 3, BaO, ZnO and TiO 2In the amount of compound based on 100 weight portion Bi 2O 3Meter preferably about 25 and the scope of about 100 weight portions in.
Particularly, based on 100 weight portion Bi 2O 3Meter, B 2O 3Amount about 1.25 in the scope of about 40 weight portions, SiO 2Amount about 1.25 in the scope of about 20 weight portions, P 2O 5Amount about 1.25 in the scope of about 40 weight portions, Na 2O 3Amount about 1.25 in the scope of about 40 weight portions, Al 2O 3Amount about 1.25 in the scope of about 10 weight portions, the amount of BaO is about 1.25 in the scope of about 10 weight portions, the amount of ZnO is about 1.25 in the scope of about 20 weight portions, and TiO 2Amount about 0.125 in the scope of about 10 weight portions.
Add B 2O 3Improve the glass transformation temperature of composition by improving eutectic point, still, as the B that adds appropriate amount 2O 3The time, thermal coefficient of expansion descends.In preferred embodiments, B 2O 3Amount based on 100 weight portion Bi 2O 3Meter arrives in the scope of about 40 weight portions about 1.25.Work as B 2O 3Amount when being less than 1.25 weight portion, the fall of composition thermal coefficient of expansion is little.Work as B 2O 3Amount during greater than 40 weight portion, glass transformation temperature improves, this is undesirable.
Add SiO 2Improve the mechanical strength of composition and reduce the thermal coefficient of expansion of composition.SiO 2Amount based on 100 weight portion Bi 2O 3Meter arrives in the scope of about 20 weight portions about 1.25.
Work as SiO 2Amount based on 100 weight portion Bi 2O 3When meter surpassed 20 weight portion, glass transformation temperature undesirably improved.Work as SiO 2Amount when being less than 1.25 weight parts, do not tell on.
Add P 2O 5Can reduce the glass transformation temperature of composition.In one embodiment of the invention, P 2O 5Amount based on 100 weight portion Bi 2O 3Count about 1.25 in the scope of about 40 weight portions.Work as P 2O 5Amount based on 100 weight portion Bi 2O 3When meter surpassed about 40 weight portion, the durability of glass descended.Work as P 2O 5Amount based on 100 weight portion Bi 2O 3When meter surpasses 1.25 weight portion, do not tell on.
Add Na 2O 3Improve the mechanical strength of glass.In some embodiments, said composition comprises Na 2O 3, Na 2O 3Amount based on 100 weight portion Bi 2O 3Meter arrives in the scope of about 40 weight portions about 1.25.Work as Na 2O 3Amount when surpassing about 40 weight portion, glass transformation temperature improves.Work as Na 2O 3Amount when being less than 1.25 weight portion, do not tell on.
Add Al 2O 3Reduce the thermal coefficient of expansion of glass and improve the acid resistance of glass.Al 2O 3Amount based on 100 weight portion Bi 2O 3Meter arrives in the scope of about 20 weight portions about 1.25, and preferred in the scope of 1.25 to 10 weight portions.Work as Al 2O 3Amount when surpassing 20 weight portion, the viscosity of glass obviously improves.Work as Al 2O 3Amount when being less than 1.25 weight portion, do not tell on.
Add the glass transformation temperature that BaO reduces composition.The amount of BaO is based on 100 weight portion Bi 2O 3Meter arrives in the scope of about 10 weight portions about 1.25.When the amount of BaO surpassed 10 weight portion, the durability of glass descended.
Said composition can contain based on 100 weight portion Bi 2O 3Meter is at about 1.25 ZnO that arrive between about 20 weight portions.When the amount of ZnO less than 1.25 the time, the acid resistance of glass descends.When the amount of ZnO surpassed 20 weight portion, the flowability of said composition descended.
Add TiO 2Reduce the thermal coefficient of expansion of glass.In one embodiment, TiO 2Amount based on 100 weight portion Bi 2O 3Meter arrives in the scope of about 10 weight portions about 0.125.Work as TiO 2Amount surpass 10 weight parts, the transmittance of glass descends.
This composition also comprises at least a mineral black.The amount of this at least a mineral black is based on 100 weight portion Bi 2O 3Meter arrives in about 28.5 weight portion scopes about 0.16.
Particularly, TiO, CuO, NiO, MnO 2, Cr 2O 3And Fe 2O 3In a kind of amount based on 100 weight portion Bi 2O 3Meter about 0.16 and about 28.5 weight portions between.
TiO, CuO, NiO, MnO 2, Cr 2O 3And Fe 2O 3In each make the composition blackening so that can absorb outside light.The amount of this at least a mineral black arrives in the scope of about 28.5 weight portions about 0.16.
When the amount of at least a mineral black was less than 0.16 weight part, the effect of blackening did not take place.When the amount of at least a mineral black surpassed 28.5 weight portion, this pigment component had adverse influence to the performance of whole glass composition.
The filter of an embodiment forms by printing and the unleaded black ceramic composition of heat treatment.This spectral filter can further comprise at least a film that is selected from anti-reflective film (AR film), near infrared ray screened film and the electromagnetic shielding film.
Fig. 1 is the sectional view of spectral filter 100 of the plasma display panel of embodiment of the present invention.With reference to figure 1, this filter can comprise transparent glass substrate 103; With the anti-reflective film 101 that forms on transparent glass substrate 103 surfaces, near-infrared (NIR) screened film 102 and 590nm screened film (Ne film) etc.; The black ceramic 104 that forms with another one surface at transparent glass substrate 103, electromagnetic shielding film 105 etc.The film that consists of filter 100 can be connected on the filter support of conduction, or combines with front panel, so that they are fixed on the front surface or rear surface of prebasal plate.
Black ceramic 104 can improve the contrast of image and therefore improve luminous efficiency by nullified screen blackening.Black ceramic 104 can be printed as width along the edge of panel is about 2 to about 4 centimetres.Electromagnetic wave shielding 105 can be metal nethike embrane, electro-conductive material, metallic black additive films or the Cu film with oxidized surface.A purposes of near infrared screened film 102 is to prevent to break down when the user uses a teleswitch.A purposes of Ne film is the orange color state of compensation, and can pass through Pigments in polymeric binder and solvent, and applies the product formation Ne film that disperses.
As described in Figure 1, can form anti-reflective film, near infrared screened film etc. in transparency carrier one side away from panel; And the black ceramic composition can be printed on the transparency carrier relative one side with plate.Yet the position of these films in this article without limits.
Fig. 2 is the orthographic plan of spectral filter 100 shown in Figure 1.Comprise with the right centre portions 110 of front cabinet glassy phase and surround peripheral part 120 of centre portions 110 with the spectral filter 100 of the composition printing of embodiment of the present invention.Be formed for preventing at centre portions 110 external light reflection anti-reflective film, near infrared screened film, shielding 590nm visible light the Ne film, be used for the electromagnetic wave shielding of shielding electromagnetic wave etc.
The method that forms the filter of one embodiment of the invention comprises: (a) with at least a B of being selected from 2O 3, compound and dissolving among BaO and the ZnO, wherein this compound is unleaded; (b) product that dissolves is cooled off at short notice, then the product that cools off is ground into glass powder; (c) with this glass powder and at least a TiO, CuO, NiO, the MnO of being selected from 2, Cr 2O 3And Fe 2O 3In mineral black mix; (d) product that mixes is mixed the formation composition with the organic carrier that forms by interpolation adhesive and plasticizer in solvent; (e) said composition is printed on the glass substrate; (f) glass substrate of printing is somebody's turn to do in heat treatment.
In operating procedure (a), based on 100 weight portion B 2O 3Meter, about 33.3 to about 100 weight portion BaO and about 16.6 to about 114 weight portion ZnO about 1,000 and about 1,100 ℃ between temperature under mix and dissolving.
In operating procedure (c), TiO, CuO, NiO, MnO 2, Cr 2O 3And Fe 2O 3In one of amount about 16 in the scope of about 28.5 weight portions.
In operation steps (d), mixed glass powder and organic carrier with 7: 3 form paste composition like this.This organic carrier can be made up of solvent, adhesive and plasticizer.Can form solvent by mixing butyl carbitol acetate and butylcarbitol.Tackiness agent can be an ethyl cellulose for example, and softening agent can be a dibutyl phthalate etc.Organic carrier can form by mixed solvent, adhesive and plasticizer under the temperature between about 70 to about 90 ℃.
In operating procedure (e), on glass substrate, it is about 5 to about 30 microns that the composition serigraphy is become thickness.
In operation steps (f), can be with printed glass substrate thermal treatment under the temperature between about 500 to 550 ℃, to prevent the glass substrate distortion.When thermal treatment temp during less than 500 ℃, the black effect of composition is little, and when thermal treatment temp during greater than 550 ℃, is difficult to keep the size of film, and this is undesirable.
The method that forms filter according to another embodiment of the invention comprises: (a) with about 100 weight portion Bi 2O 3With the about 25 at least a B that are selected to about 100 weight portions 2O 3, SiO 2, P 2O 5, Na 2O 3, Al 2O 3, BaO, ZnO and TiO 2In compound and the dissolving, wherein this compound is unleaded; (b) with the product cooling of dissolving, then the product that cools off is ground into glass powder; (c) this glass powder and about 0.16 is selected from TiO, CuO, NiO, MnO to about 28.5 weight portions 2, Cr 2O 3And Fe 2O 3In a kind of mineral black mix; (d) by being mixed with the organic carrier that forms by interpolation adhesive and plasticizer in solvent, glass powder forms composition: (e) said composition is printed on the glass substrate; (f) glass substrate of heat treatment printing.
In operating procedure (a), at least about 100 weight portion Bi 2O 3, about 1.25 to about 40 weight portion B 2O 3, about 1.25 to about 20 weight portion SiO 2, about 1.25 to about 40 weight portion P 2O 5, about 1.25 to the Na of about 40 weight portions 2O 3, about 1.25 to about 10 weight portion Al 2O 3, about 1.25 to the BaO of about 10 weight portions, about 1.25 to about 20 weight portion ZnO or about 0.125 to about 10 weight portion TiO 2About 1000 and about 1100 ℃ between temperature under mix.
In operating procedure (b), the product cooling of dissolving is pulverized then, thereby form glass powder.
In operating procedure (c), glass powder with based on 100 weight portion Bi 2O 3Meter arrives about 28.5 weight portion MnO at least about 0.16 to about 28.5 weight portion TiO, about 0.16 to about 28.5 weight portion CuO, about 0.16 to about 28.5 weight portion NiO, about 0.16 2, about 0.16 to about 28.5 weight portion Cr 2O 3Or about 0.16 to about 28.5 weight portion Fe 2O 3Mix.
Operation steps (e) and (f) as described in the previous embodiment.
The flat-panel screens of one embodiment of the invention comprises the filter that utilizes unleaded black ceramic composition to form, and this unleaded black ceramic composition contains at least a B of being selected from 2O 3, the compound among BaO and the ZnO, wherein this compound is unleaded; With at least a TiO, CuO, NiO, the MnO of being selected from 2, Cr 2O 3And Fe 2O 3In mineral black.
Flat-panel screens can comprise liquid-crystal display (LCD), field launcher (FED), plasma display panel (PDP) etc.For convenience, PDP will be described in detail in the back as an embodiment.Yet be construed as: the explanation of relevant herein PDP is not intended to describe in the mode of any restriction or constraint, only is because be used for detailed description taken in conjunction with some specific embodiments of the present invention.LCD, FED etc. can replace following PDP.
PDP comprises: transparent front substrate; The metacoxa that is arranged in parallel with prebasal plate; By being fixed in the spectral filter that the unleaded black ceramic composition of printing forms on the transparency carrier of prebasal plate; The partition wall of between prebasal plate and metacoxa, arranging, partition wall is separated emission phototube; Address electrode, it is arranged in a row extension along emission phototube, and is covered by the back dielectric layer; Be arranged in the fluorescent layer in the emission phototube; The a pair of electrode (sustain electrode) of keeping, it extends perpendicular to address electrode, and is covered by preceding dielectric layer; With the discharge gas in emission phototube.
PDP can further comprise at least a film that is selected from anti-reflective film, near infrared shielding film and the electromagnetic shielding film.
Fig. 3 illustrates spectral filter 200, header board 70 and the back plate 60 of PDP.In spectral filter 200, on transparency carrier 203 the black ceramic composition being printed as thickness is 2 to 4 centimetres; Side at transparency carrier 203 is arranged anti-reflective film or near-infrared shielding 206 etc.; And the opposite side at transparency carrier 203 is arranged metal stratum reticulare 205 etc.Header board 70 comprise prebasal plate 51, a pair of be included in the Y that forms on the rear surface of prebasal plate 51 and X electrode keep electrode, cover the preceding dielectric layer 55a that keeps electrode and cover before the protective layer 56 of dielectric layer 55a.Y and X electrode comprise the transparency electrode 53a that is made of for example ITO and 53b and the bus electrode 54 that is made of conducting metal respectively.Back plate 60 comprises metacoxa 52, on the whole surface of metacoxa 52 perpendicular to the back dielectric layer 56b of the address electrode 53c that keeps arrangement of electrodes, overlay address electrode 53c, separate reflected light fulgurite and the partition wall 57 that on the dielectric layer 56b of back, forms and be arranged in fluorescent layer 58 in the emission phototube.
In having the PDP of said structure, spectral filter 200 is made by the spectral filter support independently, and is coupled in the front cabinet, so that form predetermined space.Yet the structure of PDP is not subjected to the restriction of this paper.For example, spectral filter 200 can be connected on the prebasal plate 51.
The present invention is described in detail with reference to following examples.The purpose of these embodiment just is used for illustrating, rather than is intended to limit the scope of the invention.
Embodiment
Embodiment 1: contain B 2O 3, BaO and ZnO the preparation of lead-free ceramics paste composition
Weighing 100 weight portion B 2O 3, 85.7 weight portion BaO and 100 weight portion ZnO, and dry more than 24 hours with dry ball, thus generate mixture of powders.This mixture of powders fully dissolved about 2 hours under 1000 to 1100 ℃ temperature in alumina crucible, then at short notice cooling, thus form glass.Utilize ball mill to pulverize glass, so that the acquisition average diameter is 1.5 microns glass powder.Then, will contain 0.66 weight portion Cr 2O 3Add in the glass powder with the mineral black of 0.66 weight portion CuO.
Adding ethyl cellulose to part by weight is 10: 90 BUTYL CARBITOL ACETATE TM(Dow Chemicals, Midland is Michigan) with BUTYL CARBITOL TM(Dow Chemicals, Midland is in solution mixture Michigan).Then, the product that generates is mixed with dibutyl phthalate, and 90 ℃ of lower stirrings with the formation organic carrier.With this glass powder and organic carrier mixed, thereby form unleaded black ceramic paste composition with 7: 3.
On the soda-lime glass substrate of ultrasonic wave cleaning, utilize to have 200 order stainless steels and cover the framed screen printing apparatus unleaded black ceramic paste composition is printed as 10 microns of thickness.Institute's resultant was calcined 10 minutes down at 550 ℃, and measured the degree of black then.L, a and b are respectively 23.8 ,-0.12 and 0.03.Usually, along with L decline and a and b were almost 0 o'clock, black degree improves.
Embodiment 2: contain B 2O 3, BaO and ZnO the preparation of unleaded black ceramic paste composition
Weighing 100 weight portion B 2O 3, 85.7 weight portion BaO and 85.7 weight portion ZnO, then with as the identical method manufacturing glass powder of embodiment 1.Then, 1.53 weight part CuO are added in the glass powder as mineral black, and with forming unleaded black ceramic paste composition as embodiment 1 identical method.Apply said composition with silk screen printing, and calcining, so that thickness is 10 microns.Institute's resultant was calcined 10 minutes down at 550 ℃, and measured the degree of blackening.L, a and b are respectively 23.25 ,-0.05 and 0.02.
Embodiment 3: contain Bi 2O 3, B 2O 3, SiO 2And P 2O 5The preparation of unleaded black ceramic paste composition
Weighing 100 weight portion Bi 2O 3, 20 weight portion B 2O 3, 8 weight portion SiO 2With 4 weight portion P 2O 5And dry more than 24 hours with dry ball, thereby generate mixture of powders.This mixture of powders was fully dissolved about 2 hours under about 1100 ℃ temperature about 1000 in alumina crucible, then at short notice cooling, thus form glass.Utilize ball mill fully to pulverize glass, so that the acquisition average diameter is 1.5 microns glass powder.Then, will contain 0.66 weight portion Cr 2O 3Add in the glass powder with the mineral black of 0.66 weight portion CuO.
Adding ethyl cellulose to ratio is 10: 90 BUTYL CARBITOL ACETATE TM(Dow Chemicals, Midland is Michigan) with BUTYL CARBITOL TM(Dow Chemicals, Midland is in solution mixture Michigan).Then, the product that generates is mixed with dibutyl phthalate, and 90 ℃ of lower stirrings with the formation organic carrier.With this glass powder and organic carrier mixed, thereby form unleaded black ceramic paste composition with 7: 3.
On the soda-lime glass substrate of ultrasonic wave cleaning, utilize to have 200 order stainless steels and cover the framed screen printing apparatus unleaded black ceramic paste composition is printed as 10 microns of thickness.Institute's resultant was calcined 10 minutes down at 550 ℃, measured the degree of blackening then.L, a and b are respectively 23.3 ,-0.05 and 0.07.Usually, along with L decline and a and b were almost 0 o'clock, the blackening degree improves.
Embodiment 4: contain Bi 2O 3, B 2O 3, SiO 2And P 2O 5The preparation of unleaded black ceramic paste composition
Weighing 100 weight portion Bi 2O 3, 30.7 weight portion B 2O 3, 15.3 weight portion SiO 2With 6.15 weight portion P 2O 5, and then with making glass powder such as embodiment 1 identical method.Then, 1.53 weight part CuO are added in the glass powder as black pigment, and with forming unleaded black ceramic paste composition as embodiment 1 identical method.Apply said composition with serigraphy, and calcining, so that the thickness of said composition is 10 microns.Institute's resultant was calcined 10 minutes down at 550 ℃, and measured the degree of blackening.L, a and b are respectively 23.75 ,-0.10 and 0.12.
Comparative Examples 1: the Comparative Examples of using plumbous embodiment 1
(Shinceramic Co., Ltd.: this glass powder contains PbO, SiO except using conventional leaded black ceramic 2, Na 2O 3Deng, and this black pigment contains Cr 2O 3And CuO) in addition, Comparative Examples 1 is carried out with embodiment 1 identical method.L, a and b are respectively 23.41 ,-0.08 and 0.12.
Comparative Examples 2: the Comparative Examples of using the embodiment 2 of conventional unleaded black ceramic paste composition
(Shinceramic Co., Ltd.: this glass powder contains SiO except using conventional unleaded black ceramic 2, Na 2O 3Deng, and this mineral black contains Cr 2O 3And CuO) in addition, Comparative Examples 2 is carried out with the method identical with embodiment 1.L, a and b are respectively 27.22 ,-0.05 and 0.15.
Comparative Examples 3: the Comparative Examples of using the embodiment 3 of conventional unleaded black ceramic paste composition
(Shinceramic Co., Ltd.: this glass powder contains SiO to the unleaded black ceramic that uses in Comparative Examples 2 2, Na 2O 3Deng, and this mineral black contains Cr 2O 3And CuO) carry out serigraphy, and calcining, so that thickness is 10 microns.Institute's resultant was calcined 10 minutes down at 600 ℃, and measured the degree of blackening.L, a and b are respectively 23.64 ,-0.10 and 0.17.
The hue coordinate of table 1 black paste-type
L A b
Embodiment 1 23.8 -0.12 0.03
Embodiment 2 23.25 -0.05 0.02
Embodiment 3 23.3 -0.05 0.07
Embodiment 4 23.75 -0.10 0.12
Comparative Examples 1 23.41 -0.08 0.12
Comparative Examples 2 27.22 -0.05 0.15
Comparative Examples 3 23.64 -0.10 0.17
In Comparative Examples 1, the L of hue coordinate is enough little, so that the black degree of black ceramic is big, therefore can obtain excellent PDP luminous efficiency.Yet, when environmental legislation is strengthened,, will not allow to use said composition owing to wherein have Pb.
In Comparative Examples 2, composition does not contain Pb, therefore is not subjected to the restriction of environmental legislation.Yet said composition is calcined down at 550 ℃, so L is quite big, this means that color is more gloomy than the embodiment of embodiment of the present invention.
In Comparative Examples 3, composition does not contain Pb, and L is an ideal.Yet calcining heat is quite high, and needs higher energy consumption, thereby causes economic loss.
In embodiment 1-4, this glass composition does not contain Pb.In addition, this glass composition has low glass transformation temperature, and therefore needs little heat energy to realize effective luminous efficiency.
According to the present invention, can make and do not contain unleaded black ceramic composition human and the compound Pb O that environment is harmful to.The present composition is harmless and environmental protection to the mankind, and is not therefore banned use of the influence of the rules of Pb.In addition, said composition can be at quite low temperature lower calcination, and consumes a small amount of heat energy.
Though the present invention has been described in detail and describes in conjunction with its exemplary embodiment, it should be understood by one skilled in the art that for: can make various changes in this article in form and details and not deviate from the spirit and scope that the present invention such as claims define.

Claims (22)

1. unleaded black ceramic composition that is used for the flat-panel screens spectral filter, said composition comprises:
At least a B that is selected from 2O 3, the compound among BaO and the ZnO, wherein this compound is unleaded; With at least a TiO, CuO, NiO, the MnO of being selected from 2, Cr 2O 3And Fe 2O 3In mineral black.
2. unleaded black ceramic composition as claimed in claim 1, wherein the amount of BaO is based on 100 weight portion B 2O 3Meter arrives in the scope of about 100 weight portions about 33.3.
3. unleaded black ceramic composition as claimed in claim 1, wherein the amount of ZnO is based on 100 weight portion B 2O 3Meter arrives in the scope of about 114 weight portions about 16.6.
4. unleaded black ceramic composition as claimed in claim 1, wherein this at least a TiO, CuO, NiO, MnO of being selected from 2, Cr 2O 3And Fe 2O 3In the amount of mineral black based on 100 weight portion B 2O 3Meter arrives in the scope of about 28.5 weight portions about 0.16.
5. unleaded black ceramic composition as claimed in claim 1, it has about 450 to about 550 ℃ glass transformation temperature.
6. unleaded black ceramic composition as claimed in claim 6, wherein its glass transformation temperature arrives in about 530 ℃ scope about 480.
7. unleaded black ceramic composition that is used for spectral filter, said composition comprises:
Bi 2O 3；
At least a B that is selected from 2O 3, SiO 2, P 2O 5, Na 2O 3, Al 2O 3, BaO, ZnO and TiO 2In compound, wherein this compound is unleaded; With
At least a TiO, CuO, NiO, the MnO of being selected from 2, Cr 2O 3And Fe 2O 3In mineral black.
8. unleaded black ceramic composition as claimed in claim 7, wherein this at least a B that is selected from 2O 3, SiO 2, P 2O 5, Na 2O 3, Al 2O 3, BaO, ZnO and TiO 2In the amount of compound based on 100 weight portion Bi 2O 3Meter arrives in the scope of about 100 weight portions about 25.
9. unleaded black ceramic composition as claimed in claim 8 is wherein based on 100 weight portion Bi 2O 3Meter, B 2O 3Amount about 1.25 in the scope of about 40 weight portions, SiO 2Amount about 1.25 in the scope of about 20 weight portions, P 2O 5Amount about 1.25 in the scope of about 40 weight portions, Na 2O 3Amount about 1.25 in the scope of about 40 weight portions, Al 2O 3Amount about 1.25 in the scope of about 10 weight portions, the amount of BaO is about 1.25 in the scope of about 10 weight portions, the amount of ZnO is about 1.25 in the scope of about 20 weight portions, and TiO 2Amount about 0.125 in the scope of about 10 weight portions.
10. unleaded black ceramic composition as claimed in claim 7, wherein the amount of this at least a mineral black is based on 100 weight portion Bi 2O 3Meter arrives in the scope of about 28.5 weight portions about 0.16.
11. unleaded black ceramic composition as claimed in claim 10, wherein TiO, CuO, NiO, MnO 2, Cr 2O 3And Fe 2O 3In each amount based on 100 weight portion Bi 2O 3Arrive in the scope of about 28.5 weight portions about 0.16.
12. filter that forms by any one described unleaded black ceramic composition in printing and the heat treatment claim 1 to 11.
13. spectral filter as claimed in claim 12, it further comprises at least a film that is selected from antireflection (AR) film, near infrared shielding film and the electromagnetic shielding film.
14. a method that forms spectral filter, this method comprises:
(a) with at least a B that is selected from 2O 3, compound and dissolving among BaO and the ZnO, wherein said compound is unleaded;
(b) with the product cooling of dissolving, then the product that cools off is pulverized to form glass powder;
(c) with this glass powder and at least a TiO, CuO, NiO, the MnO of being selected from 2, Cr 2O 3And Fe 2O 3In mineral black mix;
(d) product that mixes is mixed the formation composition with the organic carrier that forms by interpolation adhesive and plasticizer in solvent;
(e) said composition is printed on the glass substrate; With
(f) glass substrate of printing is somebody's turn to do in thermal treatment.
15. method as claimed in claim 14, wherein, in operating procedure (a), based on 100 weight portion B 2O 3Meter, the amount of BaO arrives in about 100 weight portion scopes about 33.3, and the amount of ZnO arrives in about 114 weight portion scopes about 16.6.
16. method as claimed in claim 14, wherein, in operating procedure (c), based on 100 weight portion B 2O 3Meter, TiO, CuO, NiO, MnO 2, Cr 2O 3And Fe 2O 3In one of amount about 16 in the scope of about 28.5 weight portions.
17. method as claimed in claim 14, wherein, in operation steps (d), with 7: 3 mixed glass powder and organic carrier.
18. method as claimed in claim 14, wherein, in operation steps (e), on glass substrate, it is about 5 to about 30 microns that said composition is printed as thickness.
19. method as claimed in claim 14 wherein, in operation steps (f), is heat-treated under about 550 ℃ temperature about 500.
20. flat-panel screens that comprises the spectral filter of claim 12.
21. flat-panel screens as claimed in claim 20, it is a kind of in plasma display panel, liquid-crystal display and the field launcher.
22. as the flat-panel screens of claim 21, wherein said plasma display panel further comprises at least a film that is selected from anti-reflective film, near infrared shielding film and the electromagnetic shielding film.
CNA2005100896180A 2004-06-24 2005-06-24 Lead-free black ceramic composition for filter and filter formed using the same Pending CN1740109A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113651607A (en) * 2021-08-12 2021-11-16 广东宏宇新型材料有限公司 Ceramic tile with night sky and river decoration effect
CN113999044A (en) * 2021-11-12 2022-02-01 郑州磨料磨具磨削研究所有限公司 Porous ceramic plate and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113651607A (en) * 2021-08-12 2021-11-16 广东宏宇新型材料有限公司 Ceramic tile with night sky and river decoration effect
CN113999044A (en) * 2021-11-12 2022-02-01 郑州磨料磨具磨削研究所有限公司 Porous ceramic plate and preparation method thereof

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