WO2005118500A1 - Verre sans plomb en présentant un point de fusion bas - Google Patents

Verre sans plomb en présentant un point de fusion bas Download PDF

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Publication number
WO2005118500A1
WO2005118500A1 PCT/JP2005/009356 JP2005009356W WO2005118500A1 WO 2005118500 A1 WO2005118500 A1 WO 2005118500A1 JP 2005009356 W JP2005009356 W JP 2005009356W WO 2005118500 A1 WO2005118500 A1 WO 2005118500A1
Authority
WO
WIPO (PCT)
Prior art keywords
glass
lead
melting glass
low
zno
Prior art date
Application number
PCT/JP2005/009356
Other languages
English (en)
Japanese (ja)
Inventor
Taishin Shimooka
Naoya Hayakawa
Original Assignee
Central Glass Company, Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from JP2004164321A external-priority patent/JP4765269B2/ja
Priority claimed from JP2004326809A external-priority patent/JP2006111512A/ja
Application filed by Central Glass Company, Limited filed Critical Central Glass Company, Limited
Publication of WO2005118500A1 publication Critical patent/WO2005118500A1/fr

Links

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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J5/00—Details relating to vessels or to leading-in conductors common to two or more basic types of discharge tubes or lamps
    • H01J5/02—Vessels; Containers; Shields associated therewith; Vacuum locks
    • H01J5/04—Vessels or containers characterised by the material thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2217/00—Gas-filled discharge tubes
    • H01J2217/38—Cold-cathode tubes
    • H01J2217/49—Display panels, e.g. not making use of alternating current
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2217/00—Gas-filled discharge tubes
    • H01J2217/38—Cold-cathode tubes
    • H01J2217/49—Display panels, e.g. not making use of alternating current
    • H01J2217/492—Details
    • H01J2217/49264—Vessels

Definitions

  • the present invention relates to an electronic material substrate typified by a plasma display panel, a liquid crystal display panel, an electorifice luminescent panel, a fluorescent display panel, an electoral chromic display panel, a light emitting diode display panel, a gas discharge display panel, and the like. And a low-melting glass used as a sealing material.
  • PDPs plasma display panels
  • a PDP has many cells between a front substrate and a rear substrate used as a display surface, and an image is formed by plasma discharge in the cells. This cell is partitioned by partition walls, and an electrode is formed for each pixel in order to control the display state of each pixel forming an image.
  • An electrode for discharging plasma is formed on the front glass plate of the plasma display panel, and thin linear silver is often used as the electrode.
  • a highly transparent insulating material is provided around the electrodes. This insulating material is preferably excellent in plasma durability and transparent. For this reason, dielectric glass is often used as an insulating material.
  • dielectric glass is often used as an insulating material.
  • a low melting point glass is used.
  • the dielectric glass reacts with silver of the bus electrode at 450 to 600 ° C at low temperature firing, so that the dielectric glass is colored yellow ( (Yellowing) occurred, and high transmittance could not be obtained.
  • the same effect can be obtained by limiting and limiting the diffusion of silver by Cu (see, for example, Patent Document 1), and by adding SrO in addition to CuO to obtain the same effect as BaO + SrO + MgO.
  • a material for a plasma display having a limited content for example, see Patent Document 2
  • a material for a plasma display having a limited content of BaO + CaO + BiO for example,
  • Patent Document 3 the contents of SiO, B O, ZnO, Bi O, BaO, and Al O were limited.
  • a material for a plasma display (for example, see Patent Document 4) is disclosed.
  • Patent Document 1 JP 2001-52621 A
  • Patent Document 2 Japanese Patent Application Laid-Open No. 2001-80934
  • Patent Document 3 JP 2001-48577 A
  • Patent Document 4 Japanese Patent Application Laid-Open No. 2003-226549
  • lead-based glass has been adopted as low-melting glass, for example, low-melting glass for coating a substrate.
  • the lead component is an important component in lowering the melting point of glass, the adverse effect on the human body and the environment is significant, and in recent years there has been a trend to avoid its use, so lead-free electronic materials such as PDPs are being considered for lead-free use. Being done.
  • JP-A-2001-52621, JP-A-2001-80934, and JP-A-2001-48577 contain a lead which shows a considerable improvement against yellowing.
  • Japanese Patent Application Laid-Open No. 2003-226549 does not contain lead and has a considerable improvement against yellowing. However, it contains bismuth which tends to be avoided from the environmental point of view like lead. RU
  • an object of the present invention is to provide a high-V, lead-free, low-melting-point glass that suppresses yellowing due to a silver reaction and has high visible light transmittance.
  • the first feature of the present invention has a transparent insulating property, and contains 7 to 20 wt.
  • first glass Provided is a lead-free low melting glass (first glass).
  • substantially not including PbO by substantially not including PbO, it is possible to eliminate the effect on the human body and the environment.
  • “contains substantially no PbO” means an amount of PbO mixed as an impurity in the glass raw material. For example, in the range of 0.3 wt% or less in the low melting glass, there is almost no adverse effect as described above, that is, there is almost no influence on the human body, the environment, the insulating property, and the like, and there is substantially no influence of PbO. Will be.
  • SiO is a glass-forming component and can form stable glass.
  • it is a component that controls fluidity during firing of glass. If it is less than 7% (% by weight, the same applies to the following), the above effect cannot be exerted. If it exceeds 20%, the softening point of the glass increases, and moldability and workability become difficult. More preferably, it is in the range of 9 to 18%.
  • B O is a glass-forming component similar to SiO, facilitates glass melting, and provides thermal expansion of glass.
  • the fluidity of the glass becomes insufficient, and the sinterability is impaired.
  • the stability of the glass decreases. More preferably, it is in the range of 36 to 45%.
  • ZnO lowers the softening point of the glass and adjusts the coefficient of thermal expansion to an appropriate range, and is preferably contained in the glass in the range of 25 to 42%. When it is less than 25%, the above effects are exhibited. On the other hand, if it exceeds 42%, the glass becomes unstable and devitrification tends to occur. More preferably, it is in the range of 28 to 37%.
  • R O Li 0, Na 0, K O
  • the coefficient is adjusted to an appropriate range, and the content is preferably in the range of 7 to 20%. If it is less than 7%, the above effect cannot be exerted, while if it exceeds 20%, the coefficient of thermal expansion is excessively increased. More preferably, it is in the range of 10 to 17%.
  • CuO has an effect of mitigating the silver electrode used as a bus electrode wire reacting with the dielectric layer to diffuse silver into the dielectric layer and to develop silver colloidal color (yellowing). It is preferable to contain it in the range of 1 to 2%. If it is less than 0.1%, the above effect cannot be exerted. On the other hand, if it exceeds 2%, the glass is colored and the transparency is lowered. More preferably in the range of 0.1-1%
  • the oxides of Co and Mn react with a silver electrode used as a bus electrode wire of a PDP panel or the like and a dielectric layer, and silver diffuses into the dielectric layer to form silver colloid (yellowing).
  • This has the effect of alleviating the effect, and is preferably contained in the range of 0 to 2%. If it exceeds 2%, the glass is colored and the transparency is reduced. More preferably, it is in the range of 0 to 1%.
  • RO MgO + CaO + SrO + BaO gives glass an appropriate fluidity and adjusts the thermal expansion coefficient to an appropriate range, and is contained in the range of 0 to 10%. If it exceeds 10%, the coefficient of thermal expansion increases excessively. More preferably, it is in the range of 0 to 7%.
  • the weight ratio of B O ZZnO is preferably 0.85 or more and 2 or less. If it is less than 0.85, yellowing will occur
  • the weight ratio of (B O + R O) / SiO is preferably 2 or more and 7 or less! /. Glass less than 2
  • Viscosity is high and sintering is insufficient. If it exceeds 7, fluidity becomes too high and the fluctuation of transmittance becomes large. More preferably, it is in the range of 4-6.
  • 2 3 2 2 5 2 3 2 2 may be added to a total amount of 0.5% as long as the object of the present invention is not impaired.
  • the coefficient of thermal expansion at 30 ° C. to 300 ° C. is (65 to 95) ⁇ 10 ”V ° C., and the softening point is preferably 500 ° C. or more and 600 ° C. or less.
  • X 10—Thick film is formed outside of 7 ° C Occasionally, problems such as peeling of the coating and warping of the substrate occur. Preferably, it is in the range of (75-85) X 10 "V ° C.
  • the softening point exceeds 600 ° C., problems such as soft deformation of the substrate occur.
  • it is 520 ° C or more and 580 ° C or less.
  • SiO is a glass-forming component, and coexists with another glass-forming component, B O.
  • More stable glass can be formed, and the content is 11% (% by weight, the same applies to the following). If it exceeds 20%, the softening point of the glass increases, and formability and workability become difficult. More preferably, it is in the range of 14 to 18%.
  • B O is a glass-forming component similar to SiO, and facilitates glass melting and thermal expansion of glass.
  • the fluidity of the glass becomes insufficient and the sinterability is impaired.
  • the stability of the glass is reduced. More preferably, it is in the range of 48 to 63%.
  • ZnO lowers the softening point of the glass and adjusts the thermal expansion coefficient to an appropriate range, and is preferably contained in the glass in the range of 10 to 20%. If it is less than 10%, the above effect cannot be exerted, while if it exceeds 20%, the glass becomes unstable and devitrification tends to occur. More preferably, it is in the range of 10 to 18%.
  • R O Li 0, Na 0, K O
  • the coefficient is adjusted to an appropriate range, and the content is preferably in the range of 10 to 18%. If it is less than 10%, the above effect cannot be exerted, while if it exceeds 18%, the coefficient of thermal expansion is excessively increased. More preferably, it is in the range of 11 to 17%.
  • CuO has the effect of reducing the reaction between the silver electrode used as the bus electrode wire and the dielectric layer, and the diffusion of silver into the dielectric layer to reduce silver colloidal coloration (yellowing). It is preferable to contain it in the range of 1 to 2%. If the content is less than 0.1%, the above effect cannot be exerted. On the other hand, if it exceeds 2%, the glass is colored and the transparency is reduced. More preferably, it is in the range of 0.1 to 1%. RO (MgO + CaO + SrO + BaO) gives the glass a moderate fluidity, It is adjusted to an appropriate range, and is contained in the range of 0 to 20%. If it exceeds 20%, the coefficient of thermal expansion increases excessively. More preferably, it is in the range of 0 to 10%.
  • the weight ratio of B O ZZnO is 2 or more and 6 or less. Yellow if less than 2
  • MnO reacts with a silver electrode used as a bus electrode line and a dielectric layer to form a dielectric layer.
  • It has an effect of mitigating silver colloidal coloring (yellowing) due to the diffusion of silver therein, and is preferably contained in the range of 0 to 2%. If it exceeds 2%, the glass is colored and the transparency is reduced. More preferably, it is in the range of 0 to 1%.
  • substantially not including PbO By substantially not including PbO, it is possible to eliminate the effect on the human body and the environment.
  • “contains substantially no PbO” means an amount of PbO mixed as an impurity into the glass raw material. For example, within the range of 0.3 wt% or less in the low melting glass, the above-mentioned adverse effects, that is, the effects on the human body, the environment, the insulating properties, and the like are almost nil, and the effects of PbO are substantially unaffected. , It will be.
  • the above-mentioned lead-free low-melting glass having a thermal expansion coefficient of (65 to 95) X 10 "V ° C at 30 ° C to 300 ° C and a softening point of 500 ° C to 630 ° C. . coefficient of thermal expansion (65 ⁇ 95) X 10- 7 Z ° C outside the peeling of the coating when a thick film forming, problems such as warpage of the substrate occurs. preferably, (75 ⁇ 85) X 10- 7 / ° C.
  • the softening point exceeds 630 ° C., problems such as soft deformation of the substrate occur, and the temperature is preferably 500 ° C. or more and 590 ° C. or less.
  • They may be electronic material substrates using the above low melting point glass.
  • a substrate for electronic materials with suppressed yellowing can be obtained.
  • they may be PDP panels using the above-mentioned low melting point glass.
  • the first and second glasses of the present invention are preferred as low-melting-point glasses corresponding to the yellowing phenomenon caused by the reaction with silver! /, But their use is limited to an insulating material around the silver electrode. ! /, Not necessarily.
  • the lead-free low-melting glass (first and second glasses) of the present invention can be used, for example, as a front plate or a back plate of PDP glass. When used as a back plate, it is used as a sealing material and a coating material, and is often used in the form of powder.
  • the powdered glass is mixed with a low-expansion ceramic filler such as mullite or alumina, a heat-resistant pigment, or the like at a ratio of 0.6 ⁇ glass Z (glass + filler) weight ⁇ or more, if necessary. Next, the mixture is generally kneaded with an organic oil and pasted.
  • a transparent glass substrate in particular, a soda-lime-silica-based glass or a glass similar thereto (high-strain-point glass), or a low alkali content! /, (Or almost no! ⁇ ) Alumino-lime borosilicate glass is frequently used.
  • Lithium carbonate as 2 2 3 2 sodium carbonate as Na O source, potassium carbonate as K O source,
  • CuO source as CuO source
  • NiO2 manganese source as MnO source
  • carbonic acid as MgO source
  • thermophysical properties thermophysical properties (thermal expansion coefficient, softening point).
  • the remaining glass was flaked by a quenching twin roll forming machine and sized by a pulverizer into a powder having an average particle size of 1 to 3 ⁇ m and a maximum particle size of less than 10 m.
  • ethyl cellulose as a binder and the above glass powder were mixed with a paste oil consisting of ⁇ -terpineol and butyl carbitol acetate to prepare a paste having a viscosity of about 300 ⁇ 50 poise.
  • the coefficient of thermal expansion was determined from the amount of elongation at 30 to 300 ° C when the temperature was increased by 5 ° CZ using a thermal dilatometer.
  • Tables 1 and 2 show the low melting glass composition and the results of various tests.
  • the coefficient of thermal expansion was determined from the amount of elongation at 30 to 300 ° C when the temperature was increased by 5 ° CZ using a thermal dilatometer.
  • Tables 3 and 4 show the low melting glass composition and the results of various tests.
  • Comparative Examples 1 and 2 in Table 4, which are out of the composition range of the present invention, show yellowing as in the conventional case. Is remarkable, or does not show preferable physical properties, and cannot be applied as a low melting glass for coating a substrate such as PDP.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

Un verre à base de SiO2-B2O3-ZnO-R2O-CuO sans plomb présentant un point de fusion bas (un premier verre), lequel présente une propriété de transparence et d'isolement et comprend, en % en poids, 7 à 20 % de SiO2, 32 à 50 % de B2O3, 25 à 42 % de ZnO, 7 à 20 % de R2O (Li2O + Na2O + K2O), 0,1 à 2 % de CuO et 0 à 10 % de RO (MgO + CaO + SrO + BaO) ; et un verre à base de SiO2-B2O3-ZnO-R2O-CuO sans plomb présentant un point de fusion bas (un second verre), lequel présente une propriété de transparence et d'isolement, et comprend, en % en poids, 11 à 20 % de SiO2, 45 à 65 % de B2O3, 10 à 20 % de ZnO, 10 à 18 % de R2O (Li2O + Na2O + K2O) et 0,1 à 2 % de CuO.
PCT/JP2005/009356 2004-06-02 2005-05-23 Verre sans plomb en présentant un point de fusion bas WO2005118500A1 (fr)

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
JP2004-164321 2004-06-02
JP2004164321A JP4765269B2 (ja) 2004-06-02 2004-06-02 無鉛低融点ガラス
JP2004266948 2004-09-14
JP2004-266948 2004-09-14
JP2004-326809 2004-11-10
JP2004326809A JP2006111512A (ja) 2004-09-14 2004-11-10 無鉛低融点ガラス

Publications (1)

Publication Number Publication Date
WO2005118500A1 true WO2005118500A1 (fr) 2005-12-15

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Application Number Title Priority Date Filing Date
PCT/JP2005/009356 WO2005118500A1 (fr) 2004-06-02 2005-05-23 Verre sans plomb en présentant un point de fusion bas

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KR (1) KR20070009992A (fr)
TW (1) TW200602281A (fr)
WO (1) WO2005118500A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102187045B1 (ko) * 2014-01-29 2020-12-04 엘지이노텍 주식회사 세라믹 광변환 부재용 유리 조성물 및 이를 이용한 세라믹 광변환 부재
KR101593470B1 (ko) * 2014-04-03 2016-02-12 공주대학교 산학협력단 형광체 담지용 유리 조성물 및 파장 변환기, 그것을 포함하는 발광 장치

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09278482A (ja) * 1996-04-12 1997-10-28 Nippon Electric Glass Co Ltd 低誘電率ガラス組成物
JP2000313635A (ja) * 1999-04-26 2000-11-14 Nippon Electric Glass Co Ltd プラズマディスプレーパネル用材料
JP2001146436A (ja) * 1999-11-16 2001-05-29 Nippon Electric Glass Co Ltd 蛍光表示管用絶縁材料及び隔壁材料
JP2002087843A (ja) * 2000-09-11 2002-03-27 Asahi Glass Co Ltd 低融点ガラス

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09278482A (ja) * 1996-04-12 1997-10-28 Nippon Electric Glass Co Ltd 低誘電率ガラス組成物
JP2000313635A (ja) * 1999-04-26 2000-11-14 Nippon Electric Glass Co Ltd プラズマディスプレーパネル用材料
JP2001146436A (ja) * 1999-11-16 2001-05-29 Nippon Electric Glass Co Ltd 蛍光表示管用絶縁材料及び隔壁材料
JP2002087843A (ja) * 2000-09-11 2002-03-27 Asahi Glass Co Ltd 低融点ガラス

Also Published As

Publication number Publication date
TWI322137B (fr) 2010-03-21
KR20070009992A (ko) 2007-01-19
TW200602281A (en) 2006-01-16

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