CN1634786A - Lead free glass powder for preparing medium pulp and method for making same - Google Patents

Lead free glass powder for preparing medium pulp and method for making same Download PDF

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Publication number
CN1634786A
CN1634786A CN 200310110340 CN200310110340A CN1634786A CN 1634786 A CN1634786 A CN 1634786A CN 200310110340 CN200310110340 CN 200310110340 CN 200310110340 A CN200310110340 A CN 200310110340A CN 1634786 A CN1634786 A CN 1634786A
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CN
China
Prior art keywords
oxide
glass powder
lead
free glass
weight percent
Prior art date
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Pending
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CN 200310110340
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Chinese (zh)
Inventor
王大巍
陈军
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BOE Technology Group Co Ltd
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BOE Technology Group Co Ltd
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Publication date
Application filed by BOE Technology Group Co Ltd filed Critical BOE Technology Group Co Ltd
Priority to CN 200310110340 priority Critical patent/CN1634786A/en
Publication of CN1634786A publication Critical patent/CN1634786A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C12/00Powdered glass; Bead compositions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/062Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/066Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc

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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

Disclosed is a lead free glass powder for preparing medium pulp, which is a granule made from at least BaO, B2O3, ZnO, Na2O and K2O by melting and crashing, and method for making same. The making method includes raw materials weighing according to the component and weight ratio; thorough blending of the raw materials; melting the mixed materials; rolling the mixture to obtain sheet glass with cracks; grinding the sheet glass into powder and sieving. The invention has the advantages of environmental protection, low cost and convenient operation.

Description

The lead-free glass powder and the manufacture method thereof that are used for the modulated media slurry
Technical field
The present invention relates to a kind of composition and manufacture method of lead-free glass powder, particularly a kind ofly can carry out the composition and the manufacture method of synthetic lead-free glass powder the dielectric paste that is used to make vacuum fluorescent display (VFD), plasma display (PDP) medium layer.
Background technology
In recent years; along with vacuum fluorescent display (VFD), plasma display (PDP) are applied to all kinds of occasions more and more as flat-panel display device; make its market demand increase day by day; simultaneously; because people are to the deep understanding of environment protection and the enhancing day by day of protection consciousness, this series products problem that influences to physical environment in production, recycling process has also caused social extensive concern.
In the inside of vacuum fluorescent display (VFD), a medium layer is arranged between anode wiring layer and the anode.In the inside of plasma display (PDP), be provided with transparent dielectric layer between bus electrode and the discharge space, and, the back glass substrate inner surface also be laid with reflecting medium layer.
Medium layer and transparent dielectric layer, reflecting medium layer all are in manufacturing processed, with the dielectric paste matrix surface that is laid in, make by sintering again.The main component of dielectric paste is a glass powder.
Traditional dielectric paste normally adopts the flint glass powder, and its main component is PbO-SiO 2-B 2O 3Content plumbous in this dielectric paste generally surpasses 50%.Adopt the flint glass powder to make the pollution in the production process bigger, lead also reacts easily in sintering process, and the recovery of waste and old device is also comparatively difficult.The more important thing is, because plumbous pollution to environment makes the method that adopts this material to make dielectric paste can not satisfy people to environment protection institute requirement.
At present, external existing on a small quantity about the open report of lead-free medium slurry, mainly contain ZnO-B 2O 3-SiO 2Series, ZnO-Bi 2O 3-B 2O 3Series, P 2O 5Series and V 2O 5-ZnO-B 2O 3Series.
ZnO-B 2O 3-SiO 2The sintering temperature of series is higher, and contains a large amount of fillers in the composition of slurry, and cost is increased.
ZnO-Bi 2O 3-B 2O 3Contain a large amount of precious metal Bi in the series slurry, so price is more expensive.
P 2O 5Series: as P 2O 5-Al 2O 3-B 2O 3, P 2O 5-ZnO-Na 2O, P 2O 5-ZnO-BaO, the water resisting property of this series slurry is poor.
V 2O 5-ZnO-B 2O 3The color and the consistency of series slurry are relatively poor.
Because the interior continuous increase of world wide to environmental requirement, to vacuum fluorescent display (VFD), the restriction of contained objectionable constituent such as lead also constantly increases in plasma display (PDP) device, for example, the deadline that products containing lead is used in restriction has been announced in Europe, therefore, make not leaded, do not contain noble metal, and has good use properties and cheap glass powder, and, now become vacuum fluorescent display (VFD) with this glass powder manufacturing dielectric paste, one of major issue that the personage needed to be resolved hurrily of plasma display (PDP) manufacturing.
Summary of the invention
Main purpose of the present invention is to provide a kind of lead-free glass powder that is used for the modulated media slurry at the existing deficiency of present employed dielectric paste, does not contain PbO, P in this lead-free glass powder 2O 5Or V 2O 5, in product processing, there is not hazardness, help the recovery of environment protection and waste and old device simultaneously.
Another object of the present invention is to provide the manufacture method of above-mentioned lead-free glass powder, can produce the needed lead-free glass powder of different media slurry that is used for vacuum fluorescent display (VFD), plasma display (PDP) different media layer easily by this method.
The objective of the invention is to be achieved through the following technical solutions:
A kind of lead-free glass powder that is used for the modulated media slurry, it is by barium oxide (BaO), boron oxide (B at least 2O 3), zinc oxide (ZnO), sodium oxide (Na 2O) and potassium oxide (K 2O) granule of making through melting, pulverizing; The weight percent of its each component is respectively that barium oxide (BaO) is 10%-50%, boron oxide (B 2O 3) be that 10%-30%, zinc oxide (ZnO) they are 20%-40%, sodium oxide (Na 2O) be 1%-4%, potassium oxide (K 2O) be 1%-6%.
It also is included in weight percent shared in the described lead-free glass powder and is no more than 3% Lithium Oxide 98min (Li 2O) or weight percent be no more than 12% calcium oxide (CaO) or weight percent and be no more than 10% silicon oxide (SiO 2) or weight percent be no more than 10% aluminum oxide (Al 2O 3) or its arbitrary combination.
Make the method for above-mentioned lead-free glass powder, it may further comprise the steps:
Step 1: take by weighing raw material according to composition and weight proportion;
Step 2: with the raw material thorough mixing that is taken by weighing;
Step 3: with mixed raw material fusing;
Step 4: the sheet glass that the compound rolling of fusing postcooling in the step 3 is become to have crackle;
Step 5: it is powdery that the sheet glass in the step 4 is ground, and sieves.
By technique scheme as can be known, do not contain the material that can pollute and endanger environment in each component of the present invention, also do not contain noble metal, it is with low cost, is convenient to manipulate.
Embodiment
Below, by discussing and in conjunction with specific embodiments the present invention being described in more details.
The present invention is the parent glass powder that is used for VFD and the last dielectric paste of PDP.Because dielectric paste is the insulating property that guarantee between conductive layer and other associated components in function main on VFD and the PDP, therefore it is well opacifying property to require this material to have, for stablizing of guaranteed performance and technology, need consider that also dielectric paste must have the coefficient of expansion that adapts with substrate; Must guarantee repeatedly do not damaging other parts in the sintering; Must have the good insulation performance; Also to guarantee the smooth of its surface at last.
Main component of the present invention is BaO, B 2O 3, ZnO, Na 2O, K 2O.Its function is for guaranteeing the fundamental property of dielectric paste, as thermal expansivity, sintering temperature and insulating property etc.
The introducing of BaO and ZnO is in order to improve the resistivity of glass, to reduce its dielectric loss.B 2O 3Adding be in order to reduce the high temperature viscosity of glass, make glass be easy to form.Na 2O, K 2O, Li 2O is glassy transition point, softening temperature and the sintering temperature that is used for regulating glass powder, can reduce the temperature of fusion of glass simultaneously, and the high temperature that is beneficial to glass forms, but should notice that they can influence the thermal expansivity of glass simultaneously.
Add CaO among the present invention,, make it be easy to fusing and clarification in order to reduce the high temperature viscosity of glass; Add SiO among the present invention 2, Al 2O 3, be used to regulate the thermal expansivity of glass, guarantee the stability of glass in the sintering process.
Following table is the composition and the salient features table of 3 preferred embodiments of lead-free glass powder involved in the present invention, and wherein, what per-cent was represented is weight percentage.
Lead-free glass powder embodiment composition and performance index
Composition or performance Embodiment 1 Embodiment 2 Embodiment 3
????BaO ????40% ????18.5% ????33%
????B 2O 3 ????17% ????28% ????14.7%
????ZnO ????20% ????40% ????25.9%
????CaO ????8% ????4% ????6%
????Na 2O ????1.6% ????2% ????1.2%
????K 2O ????2.1% ????4.6% ????2.4%
????Li 2O ????1% ????1% ????2.1%
????Al 2O 3 ????5% ????- ????6%
????SiO 2 ????5.3% ????1.9% ????8.7%
Density kg/m 3 ????3.61×10 3 ????3.24×10 3 ????3.60×10 3
Thermal expansivity (1/ ℃) ????94.1×10 -7 ????71.7×10 -7 ????86.1×10 -7
Softening temperature (℃) ????566 ????563 ????564
Sintering temperature (℃) ????590 ????585 ????590
Insulation resistance (Ω) ????1×10 12 ????1.2×10 12 ????1.7×10 12
In the various embodiments described above, by adjust each component in lead-free glass powder weight percent and by adding a spot of Li 2O, CaO, SiO 2, Al 2O 3, Bi 2O 3Every fundamental property index of lead-free glass powder is adjusted.
The preparation process of glass powder of the present invention is as follows: at first prepare burden according to glass ingredient, with corresponding mixer batch mixing 90 minutes, the insulation discharging after 60 minutes in 1250 ℃ change material stove in the crucible of packing into then, roll into the sheet glass that has tiny crack through roller mill then, the sheet glass of this moment is water white.With pack in ball grinder ball milling at least 72 hours of gained sheet glass, cross and to get particle diameter behind 200 mesh standard sieves less than 5 microns white glass powder.
It should be noted last that: above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art is to be understood that: still can make amendment or be equal to replacement the present invention, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.

Claims (7)

1, a kind of lead-free glass powder that is used for the modulated media slurry is characterized in that: it is by barium oxide (BaO), boron oxide (B at least 2O 3), zinc oxide (ZnO), sodium oxide (Na 2O) and potassium oxide (K 2O) granule of making through melting, pulverizing; The weight percent of its each component is respectively that barium oxide (BaO) is 10%-50%, boron oxide (B 2O 3) be that 10%-30%, zinc oxide (ZnO) they are 20%-40%, sodium oxide (Na 2O) be 1%-4%, potassium oxide (K 2O) be 1%-6%.
2, the lead-free glass powder that is used for the modulated media slurry according to claim 1, it is characterized in that: the particle diameter of described granule is less than 5 microns.
3, the lead-free glass powder that is used for the modulated media slurry according to claim 1 and 2 is characterized in that: it also is included in weight percent shared in the described lead-free glass powder and is no more than 3% Lithium Oxide 98min (Li 2O) or weight percent be no more than 12% calcium oxide (CaO) or weight percent and be no more than 10% silicon oxide (SiO 2) or weight percent be no more than 10% aluminum oxide (Al 2O 3) or its arbitrary combination.
4, the lead-free glass powder that is used for the modulated media slurry according to claim 1 and 2 is characterized in that: it comprises that also weight percent is no more than 5% bismuth oxide (Bi 2O 3).
5, a kind of arbitrary described manufacture method that is used for the lead-free glass powder of modulated media slurry of claim 1-4 of making, it is characterized in that: it may further comprise the steps:
Step 1: take by weighing raw material according to composition and weight proportion;
Step 2: with the raw material thorough mixing that is taken by weighing;
Step 3: with mixed raw material fusing;
Step 4: the sheet glass that the compound rolling of fusing postcooling in the step 3 is become to have crackle;
Step 5: it is powdery that the sheet glass in the step 4 is ground, and sieves.
6, manufacture method according to claim 5 is characterized in that: described step 3 is with the mixed raw material crucible of packing into, 1250 ℃ of fusings 60 minutes down.
7, according to claim 5 or 6 described manufacture method, it is characterized in that: described step 5 is that sheet glass is packed in the ball grinder, and ball milling is crossed 200 mesh standard sieves after 72 hours.
CN 200310110340 2003-12-29 2003-12-29 Lead free glass powder for preparing medium pulp and method for making same Pending CN1634786A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200310110340 CN1634786A (en) 2003-12-29 2003-12-29 Lead free glass powder for preparing medium pulp and method for making same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200310110340 CN1634786A (en) 2003-12-29 2003-12-29 Lead free glass powder for preparing medium pulp and method for making same

Publications (1)

Publication Number Publication Date
CN1634786A true CN1634786A (en) 2005-07-06

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101066839B (en) * 2007-06-05 2011-07-27 东华大学 No-lead glass powder for electrode coating and its preparation process
CN102667963A (en) * 2009-12-18 2012-09-12 欧丽安株式会社 Dielectric composition for a plasma display panel
CN111423127A (en) * 2020-04-21 2020-07-17 北京北旭电子材料有限公司 Preparation method of glass powder and glass powder
CN115215553A (en) * 2022-08-02 2022-10-21 上海晶材新材料科技有限公司 Low-temperature co-fired ceramic green tape and substrate easy to match with metal slurry for co-firing and preparation method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101066839B (en) * 2007-06-05 2011-07-27 东华大学 No-lead glass powder for electrode coating and its preparation process
CN102667963A (en) * 2009-12-18 2012-09-12 欧丽安株式会社 Dielectric composition for a plasma display panel
CN111423127A (en) * 2020-04-21 2020-07-17 北京北旭电子材料有限公司 Preparation method of glass powder and glass powder
CN115215553A (en) * 2022-08-02 2022-10-21 上海晶材新材料科技有限公司 Low-temperature co-fired ceramic green tape and substrate easy to match with metal slurry for co-firing and preparation method

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