CN103508756A - Aqueous alumina medium printing slurry used for ceramic base plate and preparation method thereof - Google Patents

Aqueous alumina medium printing slurry used for ceramic base plate and preparation method thereof Download PDF

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CN103508756A
CN103508756A CN201310298473.XA CN201310298473A CN103508756A CN 103508756 A CN103508756 A CN 103508756A CN 201310298473 A CN201310298473 A CN 201310298473A CN 103508756 A CN103508756 A CN 103508756A
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slurry
printing
parts
polyvinyl alcohol
weight part
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CN103508756B (en
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周正有
邓晓华
罗广圣
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Nanchang University
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Nanchang University
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Abstract

The invention relates to a medium slurry and especially an aqueous medium printing slurry used for a ceramic base plate. The aqueous alumina medium printing slurry comprises the following substances by weight: 60-70 parts of water, 320-380 parts of an alumina powder, 3.2-3.8 parts of a SiO2-MgO glass phase, 30-40 parts of diethylene glycol, and 6.5-7 parts of modified polyvinyl alcohol. The aqueous printing slurry provided by the invention has the advantages of no pollution, little smell and low cost, and shows wide prospects in application.

Description

Water-based alumina medium printing for ceramic substrate is starched and preparation method thereof
Technical field
The present invention relates to a kind of dielectric printing slurry, relate in particular to a kind of slurry of the aqueous medium printing for ceramic substrate.
Technical background
Along with the develop rapidly of information technology, developing rapidly of panel computer and mobile communication technology especially, growing to chip components and parts demand, performance is had higher requirement.In chip components and parts preparation, need to adopt electrode and medium layer in silk-screen printing technique printing, to realize performance, increase substantially and dwindle components and parts size, realize electronic product compact in size, the slimming needs such as flat panel TV, panel computer, mobile phone.
In ceramic substrate, need to be in the inner silk screen printing of ceramic substrate electrode, the insulation between interior electrode and layer insulation all will adopt dielectric paste.In addition alumina medium printing slurry, also can be used as silk screen printing white characters.
Printing slurry is divided into electrocondution slurry and dielectric paste.Electrocondution slurry is now widely used conductive silver slurry and a silver alloys electrocondution slurry, in electronic devices and components, liquid-crystal display, photovoltaic solar cell, the field such as emitting led, is widely used.Dielectric printing slurry is mainly used in the fields such as integrated circuit (IC)-components, sensitive components.It is good that alumina-ceramic has thermal diffusivity, and thermal conductivity is good, high temperature resistant and be used widely.At devices such as oxygen sensors, by printing alumina medium layer, the insulating material being applied to after sintering, can prevent interior electric pole short circuit or breakdown.In addition aluminum oxide printing slurry is widely used in pcb board, for printing white characters etc.
As printing slurry, require slurry to there is good mobility, be difficult for dry, the performance such as sticky net, not network blocking not.The printing slurry of the use of industrialization is at present organic system printing slurry, adopts the difficult volatilization of the high boiling points such as Terpineol 350 as solvent, after interpolation dispersion agent, binding agent, by three roller bundle machines, is prepared into the slurry with certain fluidity and viscosity.Organic solvent must be the solvent of difficult volatilization, can keep the moistening of slurry like this when printing, conventionally adopts Terpineol 350.One ethyl cellulose or polyvinyl butyral acetals of adopting of binding agent more.This organic solvent printing slurry have equipment not easy cleaning, scent of, cost is higher, environmental pollution is serious, the person of production line is injured to the shortcomings such as large.
Adopt aqueous systems printing slurry to there is pollution-free, low smell, low cost and other advantages.But countries in the world also do not have the report of water-based printing slurry at present.
Summary of the invention
In order to address the deficiencies of the prior art, the object of the invention is to provide a kind of pollution-free, low smell, slurry of the aqueous medium printing for ceramic substrate that cost is low and preparation method thereof.
Inventor herein finds through great many of experiments:
Aqueous binders mainly contains polyvinyl alcohol, water-borne acrylic resin, aqueous epoxy resins, aqueous polyurethane, and wherein water-borne acrylic resin, aqueous polyurethane, aqueous epoxy resins viscosity ratio are lower, is difficult to reach the requirement of printing slurry.Adopt polyvinyl alcohol adhesive to realize viscosity adjustable.But, polyvinyl alcohol one will be by heating for dissolving in water, this brings great difficulty to industrialization.This patent first disperses by modified polyvinyl alcohol in organic solvent, and then is dissolved in room temperature water.Adopt polyvinyl alcohol as binding agent, the slurry of preparation is easily dry, and then occurs the problems such as network blocking.As printing slurry, slurry must volatilize slowly, could when silk screen printing, keep moistening.Must add the high boiling organic solvent of difficult volatilization.
In the dispersion of powder: powder does not disperse, between powder granule, easily to reunite, slurry is easily dry.
On sintering: dielectric printing slurry must add glassy phase with substrate in sintering process, to sinter DB into.Glassy phase has reduced sintering temperature, has improved upper and lower medium layer sticking power.Adding glassy phase is mainly to reduce sintering temperature, improves the sticking power of medium layer and substrate, glassy phase one with SiO 2be main, add a small amount of MgO.Amount of glassy phase is 1% left and right, and sintering temperature can be reduced to 1200 ℃.
Through great many of experiments, show that concrete technical scheme is as follows:
For the aqueous medium printing slurry of ceramic substrate, comprise the material of following weight part:
The SiO of alumina powder jointed, the 3.2-3.8 weight part of the water of 60-70 weight part, 320-380 weight part 2the modified polyvinyl alcohol of the Diethylene Glycol of-MgO glassy phase, 30-40 weight part, 6.5-7.0 weight part.
This aqueous medium printing is starched, and preferably includes the material of following weight part:
The SiO of alumina powder jointed, 3.3 weight parts of the water of 60 weight parts, 380 weight parts 2the modified polyvinyl alcohol of the Diethylene Glycol of-MgO glassy phase, 40 weight parts, 6.5 weight parts.
Described modified polyvinyl alcohol is PVAC polyvinylalcohol 1899.
The invention still further relates to the preparation method of the above-mentioned slurry of the aqueous medium printing for ceramic substrate:
In water, add alumina powder jointed and SiO 2-MgO glassy phase; Then use Diethylene Glycol disperse modified polyvinyl alcohol; Mix; Through three-high mill, be milled into mobility slurry.
This water-based printing slurry is compared with traditional organic system slurry, has following beneficial effect:
[1] low-carbon (LC), environmental protection, nontoxic, odorlessness, reduced the infringement of organic solvent volatilization to health aborning;
[2] reduce organic system slurry and when printing, cleaned more difficult shortcoming;
[3] reduced cost.
Embodiment
Figure BDA0000352228510000031
Example one:
In 100g water, put into polyvinyl alcohol adhesive 5.0-6.5g, be heated to 85 ℃ of dissolvings.In order to prevent that polyvinyl alcohol adhesive and alumina powder jointed flocculation phenomenon from occurring, and adds 1g left and right acetone.Then add 230-250g alumina powder jointed (analytical pure, particle diameter is 1 μ m, Tianjin, Tianjin great Mao chemical reagents corporation, lower with).Stir, through three-high mill, be milled into mobility slurry.Slurry is the group of rising easily, and standing easy caking is two days later easily dry.By easy sticky net after silk screen printing.Occur coming off after 1200 ℃ of sintering with substrate.
Example two:
In 100g water, put into polyvinyl alcohol adhesive 5.0-6.5g, be heated to 85 ℃ of dissolvings.In order to prevent that polyvinyl alcohol adhesive and alumina powder jointed flocculation phenomenon from occurring, and adds a small amount of acetone.Then the SiO that adds the alumina powder jointed and 2.3-2.5g of 230-250g 2-MgO glassy phase.Stir, through three-high mill, be milled into mobility slurry.Slurry is the group of rising easily, standing two days later easily caking.By easy sticky net after silk screen printing, easily dry.After 1200 ℃ of sintering, become DB with substrate, the density recording with Archimedes's drainage is 2.6g/cm 3.
Example three:
In order to prevent easily dry and infiltration powder, add Diethylene Glycol solvent.The boiling point of Diethylene Glycol reaches 245 ℃, and dissolves each other with water.In 70g water, add the alumina powder jointed and 3g left and right SiO of 300g 2-MgO glassy phase, then disperses 6.5-7.0g PVAC polyvinylalcohol 1899 with 30g Diethylene Glycol, mixes.Through three-high mill, be milled into mobility slurry, add the printing slurry mobility of Diethylene Glycol very good.Sticky net not during printing, is difficult for dry.After 1200 ℃ of sintering, become DB with substrate, the density recording with Archimedes's drainage is 3.0g/cm 3.
Example four:
Further improve solid content, improve sintered magnet density.In 60g water, add the alumina powder jointed and 3.2g SiO of 320g 2-MgO glassy phase, then disperses 6.5-7.0g PVAC polyvinylalcohol 1899 with 40g Diethylene Glycol, mixes.Through three-high mill, be milled into mobility slurry, add the printing slurry mobility of Diethylene Glycol very good.Sticky net not during printing, is difficult for dry.After 1200 ℃ of sintering, become DB with substrate, the density recording with Archimedes's drainage is 3.2g/cm 3.
Example five: optimize solid content and binder content.In 60g water, add the alumina powder jointed and 3.8g SiO of 380g 2-MgO glassy phase, then disperses 6.5g PVAC polyvinylalcohol 1899 with 40g Diethylene Glycol, mixes.Through three-high mill, be milled into mobility slurry, within standing one month, slurry does not lump.Sticky net not during printing, is difficult for dry.After 1200 ℃ of sintering, become DB with substrate, the density recording with Archimedes's drainage is 3.7g/cm 3, approach alumina-ceramic theoretical density.

Claims (4)

1. for the aqueous medium printing slurry of ceramic substrate, it is characterized in that comprising the material of following weight part: the SiO of alumina powder jointed, the 3.2-3.8 weight part of the water of 60-70 weight part, 320-380 weight part 2the modified polyvinyl alcohol of the Diethylene Glycol of-MgO glassy phase, 30-40 weight part, 6.5-7.0 weight part.
2. the aqueous medium printing for ceramic substrate as claimed in claim 1 slurry, is characterized in that comprising the material of following weight part: the SiO of alumina powder jointed, 3.8 weight parts of the water of 60 weight parts, 380 weight parts 2the modified polyvinyl alcohol of the Diethylene Glycol of-MgO glassy phase, 40 weight parts, 6.5 weight parts.
3. the slurry of the aqueous medium printing for ceramic substrate as claimed in claim 1, is characterized in that described modified polyvinyl alcohol is PVAC polyvinylalcohol 1899.
4. the preparation method who starches for the aqueous medium printing of ceramic substrate described in claim 1: add alumina powder jointed and SiO at water 2-MgO glassy phase; Then use Diethylene Glycol disperse modified polyvinyl alcohol; Mix; Through three-high mill, be milled into mobility slurry.
CN201310298473.XA 2013-07-17 2013-07-17 Aqueous alumina medium printing slurry used for ceramic base plate and preparation method thereof Expired - Fee Related CN103508756B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0465308A (en) * 1990-07-02 1992-03-02 Sumitomo Chem Co Ltd Production of aluminum nitride powder having good sintering property
CN1635583A (en) * 2003-12-29 2005-07-06 京东方科技集团股份有限公司 Leadless medium slurry and making method
CN101891390A (en) * 2009-12-31 2010-11-24 四川虹欧显示器件有限公司 Lead-free medium slurry and manufacturing method thereof
CN101894762A (en) * 2010-06-12 2010-11-24 深圳大学 Metal heat-conducting substrate and manufacturing method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0465308A (en) * 1990-07-02 1992-03-02 Sumitomo Chem Co Ltd Production of aluminum nitride powder having good sintering property
CN1635583A (en) * 2003-12-29 2005-07-06 京东方科技集团股份有限公司 Leadless medium slurry and making method
CN101891390A (en) * 2009-12-31 2010-11-24 四川虹欧显示器件有限公司 Lead-free medium slurry and manufacturing method thereof
CN101894762A (en) * 2010-06-12 2010-11-24 深圳大学 Metal heat-conducting substrate and manufacturing method thereof

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