CN1329926C - Electrode thick liquid without lead and silver and mfg. method thereof - Google Patents
Electrode thick liquid without lead and silver and mfg. method thereof Download PDFInfo
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- CN1329926C CN1329926C CNB2005100186995A CN200510018699A CN1329926C CN 1329926 C CN1329926 C CN 1329926C CN B2005100186995 A CNB2005100186995 A CN B2005100186995A CN 200510018699 A CN200510018699 A CN 200510018699A CN 1329926 C CN1329926 C CN 1329926C
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Abstract
The present invention relates to an electrode slurry without lead and silver, which is used for an electrode of an electronic ceramic element, and a manufacturing method thereof. The electrode slurry without lead and silver is composed of the components of the following proportion by weight: 55 to 80 wt% of conductive powder, 2 to 10 wt% of glass binding agent without lead, 2 to 15 wt% of organic resin, 2 to 10 wt% of additive agent and 10 to 25 wt% of solvent. The manufacturing method of the electrode slurry without lead and silver comprises the preparation of the glass binding agent without lead, the preparation of an organic carrier, the prescription of the electrode slurry without lead and silver, the processing technology of the slurry, etc. The slurry manufactured by the present invention is the electrode slurry without lead and silver, wherein the lead content of the electrode slurry without lead and silver is smaller than 100 ppm; the slurry can be sintered at lower temperature of below 500 DEG C when the slurry is applied to the electrode of the electronic ceramic element, and silver electrode slurry sintered within 450 DEG C to 850 DEG C can be obtained by the prescription of the glass binding agent without lead. The electrode has the advantages of strong adhesive force, good solderability, high conductivity, stable and reliable electrical performance, etc.
Description
Technical field
This invention relate to a kind of can be under the lower temperature below 550 ℃ the electrode thick liquid without lead and silver of sintering, this slurry is as the printing burning infiltration electrode of electronic ceramic element.By silk screen printing, make slurry equably attached to the surface of ceramic component, by technologies such as oven dry, sintering, form good silver conductive layer on the surface of ceramic component, make ceramic component show good electric property.
Background technology
The porcelain body of electronic ceramic is semiconductor or dielectric material, make ceramic material show certain electric property, must make the good electrode of conductivity on ceramic material.The electrode material that electronic ceramic is commonly used has the metallic nickel electrode, metal aluminium electrode, argent electrode and silver-colored palladium electrode etc.And the technology of making electrode mainly contains magnetron sputtering, vacuum coating, chemical nickel plating and burning infiltration electrode etc.The apparatus expensive of technologies such as magnetron sputtering, vacuum coating and chemical nickel plating, shortcoming such as cost is higher and production efficiency is lower, therefore, the burning infiltration electrode process is most widely used in actual production.
Electrode slurry is by metal conductive powder, glass binder, and raw material formulated such as organic carrier and additive form.Metal conductive powder plays electric action in electrode, metal powder commonly used has copper powder, aluminium powder, zinc powder and silver powder, owing to the excellent conductivity of silver powder, be difficult for oxidation in air, is a kind of most widely used metal electrode.Inorganic binder melts when sintering processes, with the surface of metal conductive powder attached to ceramic body, forms the uniform conductive film, and the thickness of conducting film is 10-25um.Organic carrier plays peptizaiton, makes slurry be a kind of more stable suspended substance, can place the long period and does not produce precipitation.Additive mainly is a processing performance of improving slurry, makes slurry have certain flowability, thixotropy etc.
At present used glass binder is a kind of boron-silicon-lead glass material, and advantages such as this frit has that fusing point is lower, good fluidity during high temperature melting, good and electrode performance is reliable and stable with the wettability of many ceramic bodies have obtained extensive use always.But this material contains the lead of significant proportion, and lead content has all surpassed more than 50% in glass ingredient usually.Therefore, the use of this slurry has caused bigger pollution to environment.At present, the whole world all replaces boron-silicon-lead glass at a kind of new frit of searching, and the fusing point of lead-less glasses material is generally higher, if fusing point is reduced, instability appears again in its chemical property.In addition, the general wettability with pottery of lead-less glasses material is bad, makes the adhesive force of electrode very little; The lead-less glasses material also variation of electric property that makes ceramic component simultaneously.Therefore, the unleaded electrode slurry that find out a kind of sintering at a lower temperature is a very difficult problem.
Summary of the invention
The present invention will realize a kind of electrode thick liquid without lead and silver exactly, this slurry can be under the lower temperature below 500 ℃ sintering, and have good adhesive and good electric property.This unleaded electrode slurry also can be regulated by the prescription of frit, obtains the electrode slurry of sintering in 450 ℃ of-850 ℃ of scopes.The technical scheme that the present invention is led to is: a kind of unleaded electrode slurry, and this slurry component is respectively by weight:
Silver conducting powder 55-80%
Crown glass binding agent 2-10%
Organic resin 2-15%
Additive 2-10%
Solvent 10-25%
Used silver powder is that flake powder adds spherical powder, and its ratio is: flake powder 20-80%, the particle diameter of powder are less than the 10um spherical powder, and spherical powder 80-20%, the particle diameter of powder are less than 2um.
The crown glass binding agent is unleaded bismuth Bi-boron-silicon Si frit, and the component of this frit is:
Bi
2O
3 50-80％
B
2O
3 8-15％
SiO
2 1-10％
Al
2O
3 1-8％
ZnO 1-8％
MgO 0-5％
CaO 0-5％
Na
2O 0-5％
Li
2O 0-5％
NiO 0-5％
MnO
2 0-5％
TiO
2 0-5％
Added alkali metal oxide Na in the crown glass binding agent
2O, Li
2Among the O one or more, the total content of alkali metal oxide are 1-5%.Added alkaline earth oxide MgO, one or more among the CaO, the total content of alkaline earth oxide are 1-5%.Added transition metal oxide NiO, MnO
2, TiO
2In one or more, the total content of transition metal oxide is 1-8%.ZnO and Al have been added
2O
3, its content is 1-8%.
Organic resin is one or more in rosin and ethyl cellulose, celluloid, polyvinyl alcohol butyral, the acrylic acid, and its consumption is 2-15%.
Additive comprises thixotropic agent, levelling agent, surfactant and defoamer etc.Thixotropic agent is selected natural gum and starch for use.Surfactant adopts one or more of cyclohexanone, lecithin, zinc naphthenate, and its consumption is the 2-10% of total amount.
Solvent is selected one or more in turpentine oil, terpinol, cyclohexanone, castor oil, turpentine oil, dibutyl phthalate etc., the ethers for use, and consumption is 10-25%.
Electrode thick liquid without lead and silver manufacture method and technology are as follows:
A. the preparation of crown glass binding agent
The component and the content of crown glass binding agent are as follows:
Bi
2O
3 50-80％
B
2O
3 8-15％
SiO
2 1-10％
Al
2O
3 1-8％
ZnO 1-8％
MgO 0-5％
CaO 0-5％
Na
2O 0-5％
Li
2O 0-5％
NiO 0-5％
MnO
2 0-5％
TiO
2 0-5％
Above-mentioned raw materials by weight weighing, is put in the high alumina crucible heat treated in electric furnace after mixing, maximum temperature scope: 1100-1300 ℃, temperature retention time: 10-30min obtains glass particle with the glass Quenching Treatment of fusing, to the glass particle ball mill grinding and reach particle diameter＜10um.
B. the preparation of organic carrier
Organic polymer resin is pressed the 2-15% of raw material weight, solvent carries out weighing by the 5-20% of raw material weight, then macromolecule resin is heated to 80 ℃-100 ℃, up to resin dissolves, with resin filtering and impurity removing on 500-800 purpose screen cloth, obtain organic carrier.
C. the preparation of organic additive
2-10% weighing with thixotropic agent, levelling agent, surfactant and defoamer are pressed raw material weight with 5% weighing that solvent is pressed raw material weight, should mix organic system and stir.
D. the preparation of slurry
By silver-colored conducting powder 55-80%, crown glass binding agent 2-10%, the organic additive for preparing, the organic carrier for preparing weighing in proportion, and dispersed with stirring is carried out three rollers after evenly and is ground in container, and the viscosity of control slurry is 20-150Pa.s, and the granularity of slurry is＜10um.
Owing to adopted above technical scheme, the advantage of manufacture method of the present invention is:
A kind of bismuth-boron that the present invention designs-silicon system lead-free glass material, can replace fully traditional lead glass material that has, this new glass material can melt and have good mobility under lower temperature, and can also with fine wetting, stable performance of ceramic body and good electric property.The present invention has produced the unleaded electrode slurry of a kind of function admirable, good manufacturability also by certain manufacturing process and prescription design.Concrete advantage is as follows:
1. select for use bismuth-boron-silicon frit as the crown glass binding agent, realized the unleaded of electrode slurry.
By adding suitable alkali metal, alkaline earth oxide and transition metal oxide, reduced glass
The fusing point of material has increased the chemical stability of frit and good electrical property has been arranged.
2. select low-melting crown glass binding agent for use, can obtain can be under the lower temperature below 550 ℃ the slurry of sintering.Also can regulate, obtain the electrode slurry of sintering in 500 ℃ of-850 ℃ of scopes by the prescription of crown glass binding agent.Advantage such as this electrode has strong adhesion, solderability is good, conductivity is high and electric performance stablity is reliable.
3. select the use of arranging in pairs or groups by a certain percentage of flake silver powder and spherical powder for use, make slurry have better adhesive force and electric conductivity.
4. select suitable organic carrier and additive, make slurry have good manufacturability, satisfy big fully
The technological requirement of producing.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Electrode thick liquid without lead and silver manufacture method and technology are as follows: a kind of unleaded electrode slurry, and this slurry component is respectively by weight:
Silver conducting powder 55-80%
Crown glass binding agent 2-10%
Organic resin 2-15%
Additive 2-10%
Solvent 10-25%
Used silver powder is that flake powder adds spherical powder, and its ratio is: flake powder 20-80%, the particle diameter of powder are less than the 10um spherical powder, and spherical powder 80-20%, the particle diameter of powder are less than 2um.
The crown glass binding agent is unleaded bismuth Bi-boron-silicon Si frit, and the component of this frit is:
Bi
2O
3 50-80％
B
2O
3 8-15％
SiO
2 1-10％
Al
2O
3 1-8％
ZnO 1-8％
MgO 0-5％
CaO 0-5％
Na
2O 0-5％
Li
2O 0-5％
NiO 0-5％
MnO
2 0-5％
TiO
2 0-5％
Added alkali metal oxide Na in the crown glass binding agent
2O, Li
2Among the O one or more, the total content of alkali metal oxide are 1-5%.
Added alkaline earth oxide MgO in the crown glass binding agent, one or more among the CaO, the total content of alkaline earth oxide are 1-5%.
Added transition metal oxide NiO in the crown glass binding agent, MnO
2, TiO
2In one or more, the total content of transition metal oxide is 1-8%.
ZnO and Al have been added in the crown glass binding agent
2O
3, its content is 1-8%.
Organic resin is one or more in rosin and ethyl cellulose, celluloid, polyvinyl alcohol butyral, the acrylic acid, and its consumption is 2-15%.
Additive comprises thixotropic agent, levelling agent, surfactant and defoamer etc.Thixotropic agent is selected natural gum and starch for use.Surfactant adopts one or more of cyclohexanone, lecithin, zinc naphthenate, and its consumption is the 2-10% of total amount.
Solvent is selected one or more in turpentine oil, terpinol, cyclohexanone, castor oil, turpentine oil, dibutyl phthalate etc., the ethers for use, and consumption is 10-25%.
The slurry manufacturing process comprises following process:
A. the preparation of crown glass binding agent
The component and the content of crown glass binding agent are as follows:
Bi
2O
3 50-80％
B
2O
3 8-15％
SiO
2 1-10％
Al
2O
3 1-8％
ZnO 1-8％
MgO 0-5％
CaO 0-5％
Na
2O 0-5％
Li
2O 0-5％
NiO 0-5％
MnO
2 0-5％
TiO
2 0-5％
Above-mentioned raw materials by weight weighing, is put in the high alumina crucible heat treated in electric furnace after mixing, maximum temperature scope: 1100-1300 ℃, temperature retention time: 10-30min obtains glass particle with the glass Quenching Treatment of fusing, to the glass particle ball mill grinding and reach particle diameter＜10um.
B. the preparation of airborne body
Organic polymer resin is pressed the 2-15% of raw material weight, solvent carries out weighing by the 5-20% of raw material weight, then macromolecule resin is heated to 80 ℃-100 ℃, up to resin dissolves, with resin filtering and impurity removing on 500-800 purpose screen cloth, obtain organic carrier.
C. the preparation of organic additive
2-10% weighing with thixotropic agent, levelling agent, surfactant and defoamer are pressed raw material weight with 5% weighing that solvent is pressed raw material weight, should mix organic system and stir.
D. the preparation of slurry
By silver-colored conducting powder 55-80%, crown glass binding agent 2-10%, the organic additive for preparing, the organic carrier for preparing weighing in proportion, and dispersed with stirring is carried out three rollers after evenly and is ground in container, and the viscosity of control slurry is 20-150Pa.s, and the granularity of slurry is＜10um.
Embodiment 1
A kind of unleaded electrode slurry (preparation 100g), its production technology is as follows:
1. crown glass binder formula (preparation 100g): Bi
2O
375g, B
2O
310g, SiO
23g, Al
2O
32g, ZnO 3g, Na
2O 3g, TiO
23g, CaO 1g
2. glass smelting and ball-milling technology: 1200 ℃, 30min, the back ball milling that quenches is to less than 10um.
3. conduction silver powder is selected the silver powder of particle diameter less than 10um for use, wherein, and flake powder 60%, spherical powder 40%.
4. organic carrier and organic additive preparation.Organic carrier: terpinol 10g, ethyl cellulose and 80-100 ℃ of heat treated makes it fully dissolve mixing.Organic additive: terpinol 5g, zinc naphthenate 3g.
5. slurry preparation: by silver-colored conducting powder 70g, unorganic glass binding agent 3g, add prepare carrier and organic additive arranged, and dispersed with stirring is carried out three rollers after evenly and is ground in container, the viscosity of control slurry is 20-150Pas, the granularity of slurry is＜10um.
6. size performance:
Granularity:＜10um
Viscosity: 20-150Pas, test condition: 7.5RPM
Adhesive force:＞10N/mm
2
Side's resistance:＜5m Ω/
Lead tolerance:＜100ppm
Sintering temperature: 480 ℃
Embodiment 2
A kind of unleaded electrode slurry (preparation 100g), its production technology is as follows:
1. crown glass binder formula (preparation 100g): Bi
2O
370g, B
2O
38g, SiO
25g, Al
2O
32g, ZnO 3g, Na
2O 3g, MnO
24g, TiO
22g, CaO 3g
2. glass smelting and ball-milling technology: 1200 ℃, 30min, the back ball milling that quenches is to less than 10um.
3. conduction silver powder is selected the silver powder of particle diameter less than 10um for use, wherein, and flake powder 30%, spherical powder 70%.
4. organic carrier and organic additive preparation.Organic carrier: terpinol 10g. ethyl cellulose 7g, and, make it fully dissolve mixing 80-100 ℃ of heat treated.Organic additive: terpinol 5g, zinc naphthenate 3g.
5. slurry preparation: by silver-colored conducting powder 75g, unorganic glass binding agent 5g, add the organic carrier and the organic additive that prepare, and dispersed with stirring is carried out three rollers after evenly and ground in container, the viscosity of control slurry is 20-150Pas, and the granularity of slurry is＜10um.
6. size performance:
Granularity:＜10um
Viscosity: 20-150Pas, test condition: 7.5RPM
Adhesive force:＞10N/mm
2
Side's resistance:＜5m Ω/
Lead tolerance:＜100ppm
Sintering temperature: 510 ℃
Embodiment 3
A kind of unleaded electrode slurry (preparation 100g), its production technology is as follows:
1. crown glass binder formula (preparation 100g): Bi
2O
355g, B
2O
315g, SiO
28g, Al
2O
35g, ZnO 4g, Na
2O 5g, TiO
25g, CaO 3g
2. glass smelting and ball-milling technology: 1300 ℃, 20min, the back ball milling that quenches is to less than 10um.
3. conduction silver powder is selected the silver powder of particle diameter less than 10um for use, wherein, and flake powder 70%, spherical powder 30%.
4. organic carrier and organic additive preparation.Organic carrier: terpinol 15g, ethyl cellulose 7g, and, make it fully dissolve mixing 80-100 ℃ of heat treated.Organic additive: terpinol 5g, zinc naphthenate 3g.
5. slurry preparation: by silver-colored conducting powder 60g, unorganic glass binding agent 10g adds organic carrier and the organic additive prepare, and dispersed with stirring is carried out three rollers after evenly and ground in container, the viscosity of control slurry is 20-150Pas, and the granularity of slurry is＜10um.
6. size performance:
Granularity:＜10um
Viscosity: 20-150Pas, test condition: 7.5RPM
Adhesive force:＞10N/mm
2
Side's resistance:＜10m Ω/
Lead tolerance:＜100ppm
Sintering temperature: 650 ℃
Claims (9)
1 one kinds of electrode thick liquid without lead and silver is characterized in that: this slurry component is respectively by weight:
Silver conducting powder 55-80%
Crown glass binding agent 2-10%
Organic resin 2-15%
Additive 2-10%
Solvent 10-25%
Glass binder is a kind of lead-less glasses material, and this frit is bismuth-boron-silicon based material, and has added Al
2O
3, ZnO, MgO, CaO, Na
2O, Li
2O, NiO, MnO
2, TiO
2, the prescription of crown glass binding agent is by weight ratio:
Bi
2O
3 50-80％
B
2O
3 8-15％
SiO
2 1-10％
Al
2O
3 1-8％
ZnO 1-8％
MgO 0-5％
CaO 0-5％
Na
2O 0-5％
Li
2O 0-5％
NiO 0-5％
MnO
2 0-5％
TiO
2 0-5％。
2. electrode thick liquid without lead and silver according to claim 1 is characterized in that: added alkali metal oxide Na in the crown glass binding agent
2O, Li
2Among the O one or more, the total content of alkali metal oxide are 1-5%.
3 electrode thick liquid without lead and silver according to claim 1 is characterized in that: added alkaline earth oxide MgO in the crown glass binding agent, one or more among the CaO, the total content of alkaline earth oxide are 1-5%.
4 electrode thick liquid without lead and silver according to claim 1 is characterized in that: added transition metal oxide NiO in the crown glass binding agent, MnO
2, TiO
2In one or more, the total content of transition metal oxide is 1-8%.
5 electrode thick liquid without lead and silver according to claim 1, it is characterized in that: silver-colored conducting powder is made up of a certain proportion of spherical powder and flake silver powder, ratio is (percentage by weight): spherical powder: the % of flake powder=(20-80): (80-20) %, the particle diameter of spherical powder is less than 2um, and the particle diameter of flake powder is less than 10um.
6 electrode thick liquid without lead and silver according to claim 1 is characterized in that: the used organic resin of unleaded slurry is selected one or more in rosin and ethyl cellulose, celluloid, polyvinyl alcohol butyral and the acrylic acid for use, and its consumption is 2-15%.
7 electrode thick liquid without lead and silver according to claim 1, it is characterized in that: the used organic additive of unleaded slurry comprises thixotropic agent, levelling agent, surfactant and defoamer, thixotropic agent is selected natural gum and starch for use, surfactant adopts one or more of cyclohexanone, lecithin, zinc naphthenate, and its consumption is:
Thixotropic agent: 0.5-5%
Levelling agent: 0.5-5%
Surfactant: 0.5-5%
Defoamer: 0.5-5%.
8 electrode thick liquid without lead and silver according to claim 1, it is characterized in that: the used organic solvent of unleaded slurry is selected turpentine oil, terpinol, cyclohexanone, castor oil, turpentine oil, dibutyl phthalate for use, and in the ethers one or more, consumption is 10-25%.
The manufacture method of 9 one kinds of unleaded electrode slurrys is characterized in that, the slurry manufacturing process comprises following process:
A. the preparation of crown glass bonding agent
The prescription of the crown glass bonding agent that requires according to right 1 carries out weighing, be put in after mixing in the high alumina crucible, heat treated in electric furnace, maximum temperature scope: 1100-1300 ℃, temperature retention time: 10-30min, the glass Quenching Treatment of fusing is obtained glass particle, to the glass particle ball mill grinding and reach particle diameter＜10um;
B. the preparation of organic carrier
Organic polymer resin is pressed the 2-15% of raw material weight, solvent carries out weighing by the 5-20% of raw material weight, then macromolecule resin is heated to 80 ℃-100 ℃, up to resin dissolves, with resin filtering and impurity removing on 500-800 purpose screen cloth, obtain organic carrier;
C. the preparation of organic additive
2-10% weighing with thixotropic agent, levelling agent, surfactant and defoamer are pressed raw material weight with 5% weighing that solvent is pressed raw material weight, should mix organic system and stir;
D. the preparation of slurry
Silver-colored conducting powder is pressed the 55-80% of raw material weight, the organic carrier that b prepares, the organic additive for preparing among the c, and crown glass binding agent mixing stirring;
E. the manufacturing of unleaded slurry
The mixed material that obtains among the d is ground on three-roll grinder, obtain homodisperse slurry, the granularity＜10um of slurry, viscosity 20-150Pa.s by certain process of lapping.
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|---|---|---|---|
| CNB2005100186995A CN1329926C (en) | 2005-05-13 | 2005-05-13 | Electrode thick liquid without lead and silver and mfg. method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100186995A CN1329926C (en) | 2005-05-13 | 2005-05-13 | Electrode thick liquid without lead and silver and mfg. method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1687992A CN1687992A (en) | 2005-10-26 |
| CN1329926C true CN1329926C (en) | 2007-08-01 |
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| CN1687992A (en) | 2005-10-26 |
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