CN101859609B - Lead-free silver electrode slurry and preparation and using method thereof - Google Patents
Lead-free silver electrode slurry and preparation and using method thereof Download PDFInfo
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- CN101859609B CN101859609B CN2010101555998A CN201010155599A CN101859609B CN 101859609 B CN101859609 B CN 101859609B CN 2010101555998 A CN2010101555998 A CN 2010101555998A CN 201010155599 A CN201010155599 A CN 201010155599A CN 101859609 B CN101859609 B CN 101859609B
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- lead
- electrode slurry
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Abstract
The invention belongs to the field of electronic components manufacturing and relates to a preparation and using method for lead-free silver electrode slurry. The slurry comprises the following components in percentage by weight: 2 to 8 percent of lead-free glass adhesive, 60 to 80 percent of conductive silver powder, 15 to 25 percent of organic carrier and 2 to 10 percent of organic additive. The method comprises the following steps of: mixing 2 to 8 percent of the lead-free glass adhesive, 60 to 80 percent of the conductive silver powder, 15 to 25 percent of the organic carrier and 2 to 10 percent of the organic additive together; and performing ball-milling on a mixture by using a planetary ball mill for 2 to 10 hours to obtain the lead-free silver electrode slurry. A Bi2O3-ZnO-B2O3-SiO2 glass adhesive used in the method contains no harmful substance such as lead or the like; production, processing and using processes of the silver electrode slurry have no harmfulness but environmental friendliness; a processing method is simple; and after fritting, the silver electrode slurry prepared by using a lead-free glass material has high bonding strength with ceramic bodies of the electronic components, and has high conductivity and high weldability.
Description
Technical field
The invention belongs to field of electronic components manufacturing, relate to a kind of preparation and using method of lead-free silver electrode slurry.Developed a kind of novel lead-free environmental protection silver electrode paste.
Background technology
Metal electrode sizing is widely used in preparing the electrode of electronic devices and components, generally is to be formed by raw material formulated such as conductive metal powder, glass bond, organic carrier and additives.
The Pb glass that contains higher proportion in traditional electrode slurry, reliable and stable because Pb glass helps to improve electrode with the tack and the electrode performance of pottery, so once be widely used.But owing to contain a high proportion of lead, the production of leaded auxiliary agent and the use of electrode slurry cause bigger pollution to environment, the leaded electronic product of production and selling is forbidden by legislation in many in recent years countries and regions, to reduce environment and the human contamination hazard that causes.
Yet, some problem has appearred in the development of present lead-free silver electrode slurry, as the electrode that burns till and electronic devices and components bulk junction poor with joint efforts, obscission, electronic devices and components unstable properties etc. are arranged.
Summary of the invention
The object of the invention provides a kind of lead-free silver electrode slurry and preparation and using method, solve electrode that existing lead-free silver electrode slurry burns till and electronic devices and components bulk junction poor with joint efforts, problems such as obscission, electronic devices and components unstable properties are arranged.
A kind of lead-free silver electrode slurry is characterized in that each composition weight proportioning is:
Crown glass bonding agent 2～8%
Silver conducting powder 60～80%
Organic carrier 15～25%
Organic additive 2～10%.
Wherein each composition weight proportioning of crown glass bonding agent is:
45％＜Bi
2O
3＜70％
25％＜ZnO＜45％
2％＜B
2O
3＜15％
3％＜SiO
2＜10％。
Above-mentioned ZnO content is preferably 25-35%.
The preferred course of processing of each raw material is:
A. silver-colored conducting powder is preferably mixed less than the particle diameter of the flake powder of 20 μ m and 10～40% spherical powder less than 2 μ m by the particle diameter of weight ratio 60～90%.
B. organic carrier is heated to 90～120 ℃ after 1: 6～1: 10 ethyl cellulose of weight ratio and terpinol are mixed, and all dissolves up to ethyl cellulose.
C. organic additive mixes 1: 2～1: 5 cyclohexanone of weight ratio and terpinol and stirs, and obtains organic additive..
A kind of preparation method of lead-free silver electrode slurry is as follows as mentioned above:
Crown glass bonding agent with 2～8%, 60～80% silver-colored conducting powder, 15～25% organic carriers and 2～10% organic additives mix, and use planetary ball mill ball milling 2～10 hours, obtain lead-free silver electrode slurry.
A kind of using method of lead-free silver electrode slurry is as follows as mentioned above:
Adopt lead-free silver electrode slurry to prepare ceramic electronic component, the lead-free silver electrode slurry for preparing is coated in an end of ceramic electronic component, 150～200 ℃ of oven dry 30～60 minutes, take out then and be cooled to room temperature, again with identical the method coating other end and oven dry.The electronic devices and components that applied electrode are carried out burning infiltration under 450～850 ℃, temperature retention time is 0.5～2 hour, is cooled to room temperature then, promptly obtains ceramic electronic component.
Above-mentioned lead-free silver electrode slurry can be used for preparing the electrode of electronic devices and components, comprises ceramic chip inductor device, ceramic chip capacitor, ceramic plate resistor etc.
The invention has the advantages that: the Bi of use
2O
3-ZnO-B
2O
3-SiO
2Harmful substances such as glass bond is not leaded, there are not harmfulness in the production and processing of silver electrode paste and use yet, environmental friendliness, processing method is simple, with the silver electrode paste of this kind lead-less glasses material preparation after burning infiltration with electronic devices and components ceramic body bond strength height, good conductivity, solderability is good.
Embodiment
Embodiment 1
According to weight ratio 55: 25: 15: 5 weighing Bi
2O
3, ZnO, B
2O
3And SiO
2, be mixed with the crown glass bonding agent.
Weighing 18.2g ethyl cellulose and 181.8g terpinol mix after by 90 ℃ oil bath heating, all dissolve up to ethyl cellulose, obtain organic carrier.
The cyclohexanone of weighing 16.7g and the terpinol of 33.3g mix and stir, and obtain organic additive.
The 20 μ m flake silver powders of 640g and the 2 μ m ball shape silver powders of 160g are mixed, and then an above-mentioned leadless glass powder of organic carrier, additive, silver powder and 50g for preparing mixes, with planetary ball mill ball milling 10 hours, obtain electrode thick liquid without lead and silver.
Preparation negative tempperature coefficient thermistor: the electrode thick liquid without lead and silver for preparing is coated in an end of negative tempperature coefficient thermistor, was positioned over 150 ℃ of drying in oven 1 hour, take out and be cooled to after the room temperature again with the identical method coating other end and dry.
The negative tempperature coefficient thermistor that will apply electrode at last carries out burning infiltration under 850 ℃ in Muffle furnace, temperature retention time is 30 minutes, is cooled to room temperature then.
Embodiment 2
According to weight ratio 55: 30: 5: 10 weighing Bi
2O
3, ZnO, B
2O
3And SiO
2, be mixed with the crown glass bonding agent.
Weighing 13.6g ethyl cellulose and 136.4g terpinol mix after by 100 ℃ oil bath heating, all dissolve up to ethyl cellulose, obtain organic carrier.
The cyclohexanone of weighing 28.6g and the terpinol of 71.4g mix and stir, and obtain organic additive.
The 20 μ m flake silver powders of 420g and the 1 μ m ball shape silver powder of 280g are mixed, and then an above-mentioned lead-free glass powder of organic carrier, additive, silver powder and 20g for preparing mixes, with planetary ball mill ball milling 5 hours, obtain electrode thick liquid without lead and silver.
Preparation ferrite chip inductor: the electrode thick liquid without lead and silver for preparing is coated in an end of ferrite chip inductor, was positioned over 150 ℃ of drying in oven 1 hour, take out and be cooled to after the room temperature again with the identical method coating other end and dry.
The ferrite chip inductor that will apply electrode at last is positioned over and carries out burning infiltration in the Muffle furnace under 450 ℃, and temperature retention time is 2 hours, is cooled to room temperature then.
Embodiment 3
According to weight ratio 80: 10: 5: 5 weighing Bi
2O
3, ZnO, B
2O
3And SiO
2, be mixed with the crown glass bonding agent.
Weighing 35.7g ethyl cellulose and 214.3g terpinol mix after by 120 ℃ oil bath heating, all dissolve up to ethyl cellulose, obtain organic carrier.
The cyclohexanone of weighing 3.3g and the terpinol of 16.7g mix and stir, and obtain organic additive.
The 5 μ m flake silver powders of 540g and the 1 μ m ball shape silver powder of 60g are mixed, and then the above-mentioned lead-free glass powder of organic carrier, additive, silver powder and 70g for preparing is mixed, use planetary ball mill ball milling 2 hours, obtain electrode thick liquid without lead and silver.
Prepare ceramic chip capacitor: the electrode thick liquid without lead and silver for preparing is coated in an end of ceramic chip capacitor, is positioned over and places oven dry in 30 minutes in 200 ℃ of baking ovens, take out and be cooled to after the room temperature again with the identical method coating other end and dry.
The ceramic chip capacitor that will apply electrode slurry at last is positioned over and carries out burning infiltration in the Muffle furnace under 850 ℃, and temperature retention time is 1 hour, is cooled to room temperature then.
Claims (4)
1. lead-free silver electrode slurry is characterized in that each composition weight proportioning is:
Crown glass bonding agent 2～8%, silver-colored conducting powder 60～80%, organic carrier 15～25%,
Organic additive 2～10%;
Wherein each composition weight proportioning of crown glass bonding agent is:
45％＜Bi
2O
3＜70％，25％＜ZnO＜45％，2％＜B
2O
3＜15％，3％＜SiO
2＜10％。
2. a kind of according to claim 1 lead-free silver electrode slurry is characterized in that each raw material course of processing is:
A. silver-colored conducting powder: mix less than the particle diameter of the flake powder of 20 μ m and 10～40% spherical powder less than 2 μ m by the particle diameter of weight ratio 60～90%;
B. organic carrier: be heated to 90～120 ℃ after 1: 6～1: 10 ethyl cellulose of weight ratio and terpinol mixed, all dissolve up to ethyl cellulose;
C. organic additive: 1: 2～1: 5 cyclohexanone of weight ratio and terpinol are mixed and stir, obtain organic additive.
3. a kind of as claimed in claim 1 or 2 lead-free silver electrode slurry is characterized in that the preparation method is as follows:
Crown glass bonding agent with 2～8%, 60～80% silver-colored conducting powder, 15～25% organic carriers and 2～10% organic additives mix, and use planetary ball mill ball milling 2～10 hours, obtain lead-free silver electrode slurry.
4. as a kind of lead-free silver electrode slurry as described in the claim 3, it is characterized in that using method is as follows:
Adopt lead-free silver electrode slurry to prepare ceramic electronic component, the lead-free silver electrode slurry for preparing is coated in an end of ceramic electronic component, 150～200 ℃ of oven dry 30～60 minutes, take out then and be cooled to room temperature, again with identical the method coating other end and oven dry; The electronic devices and components that applied electrode are carried out burning infiltration under 450～850 ℃, temperature retention time is 0.5～2 hour, is cooled to room temperature then, promptly obtains ceramic electronic component; Described ceramic electronic component is negative tempperature coefficient thermistor, ferrite chip inductor or ceramic chip capacitor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101555998A CN101859609B (en) | 2010-04-21 | 2010-04-21 | Lead-free silver electrode slurry and preparation and using method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101555998A CN101859609B (en) | 2010-04-21 | 2010-04-21 | Lead-free silver electrode slurry and preparation and using method thereof |
Publications (2)
| Publication Number | Publication Date |
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| CN101859609A CN101859609A (en) | 2010-10-13 |
| CN101859609B true CN101859609B (en) | 2011-09-21 |
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ID=42945440
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| CN2010101555998A Expired - Fee Related CN101859609B (en) | 2010-04-21 | 2010-04-21 | Lead-free silver electrode slurry and preparation and using method thereof |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102324264A (en) * | 2011-07-04 | 2012-01-18 | 江苏瑞德新能源科技有限公司 | Preparation method for silver paste for silicon-based solar cells |
| CN102324263B (en) * | 2011-07-04 | 2013-04-10 | 江苏瑞德新能源科技有限公司 | Silver paste for solar cells and preparation method thereof |
| CN109215837A (en) * | 2018-11-14 | 2019-01-15 | 安徽兆拓新能源科技有限公司 | A kind of conductive silver slurry used for solar batteries and preparation method thereof |
| CN111276410B (en) * | 2018-12-04 | 2022-05-24 | 陈引干 | Preparation method of high-power module |
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| CN1053516C (en) * | 1996-12-24 | 2000-06-14 | 广东肇庆风华电子工程开发有限公司 | Slurry for silver leads of surface installed multi-layer disc ceramic capacitor |
| CN1329926C (en) * | 2005-05-13 | 2007-08-01 | 范琳 | Electrode thick liquid without lead and silver and mfg. method thereof |
| TW200926210A (en) * | 2007-09-27 | 2009-06-16 | Murata Manufacturing Co | Ag electrode paste, solar battery cell, and process for producing the solar battery cell |
| CN101609724A (en) * | 2008-06-20 | 2009-12-23 | 北京有色金属研究总院 | A kind of electrode thick liquid without lead and silver and preparation method thereof |
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Granted publication date: 20110921 Termination date: 20140421 |