CN106205777A - Anti-stick formula of piezo silver slurry burnt in a heap and preparation method thereof - Google Patents
Anti-stick formula of piezo silver slurry burnt in a heap and preparation method thereof Download PDFInfo
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- CN106205777A CN106205777A CN201610673826.3A CN201610673826A CN106205777A CN 106205777 A CN106205777 A CN 106205777A CN 201610673826 A CN201610673826 A CN 201610673826A CN 106205777 A CN106205777 A CN 106205777A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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Abstract
The invention discloses a kind of anti-stick formula of piezo silver slurry burnt in a heap and preparation method thereof, mainly it is made up of argentum powder, glass dust, antiplastering aid and organic carrier, the mass fraction of argentum powder is 35%～60%, the mass fraction of organic carrier is 40%～65%, the mass fraction of glass dust is 1%～2%, and antiplastering aid mass fraction is 1%～2%.Organic carrier is made up of ethyl cellulose, polyvinyl butyral resin, acrylic resin and organic solvent four part, and argentum powder uses the high-specific surface area argentum powder of polymolecularity；By three-roll grinder, argentum powder is fully ground mixing with organic carrier disperse i.e. to obtain piezo silver slurry；After the silver slurry that the inventive method provides has sintering, silver layer densification is full, Non-sticking burnt in a heap, good electrical property, the advantages such as adhesion is high, resistance to soldering heat function admirable.
Description
Technical field
The invention belongs to microelectronics electrode material field, particularly relate to a kind of anti-stick piezo silver slurry burnt in a heap
Formula and preparation method thereof.
Background technology
Piezo silver slurry makes piezoelectric ceramics piezo surface and the back side through the one of row metal as a kind of high temperature sintering
Planting electrode slurry, compared with common piezoelectric ceramics silver slurry, this slurry has high density, and (the nickel chromium triangle screen frame of 20cm × 20cm is placed
5000 φ 10, thickness is the piezo ceramic substrate of 100 μm) sintering Non-sticking burnt in a heap, high-volume can be met and quickly produce
Requirement, therefore can be widely used in various pottery electrode process burnt in a heap.
Piezo organic amine is typically made up of, as piezo argentum powder, glass powder, antiplastering aid, organic carrier etc.
Good electrical property and extraordinary bond strength is needed during the electrode tip of face；Piezo silver is starched in sintering process at present, greatly
Most producers all likes high density burnt in a heap to improve production efficiency, reduces cost of labor, so piezo silver slurry is burnt in a heap anti-
Viscous is an important need；The most domestic silver slurry predominantly uses the argentum powder of high-specific surface area and uses antiplastering aid such as metal oxygen
Compound and nikel powder.
Summary of the invention
Goal of the invention: the present invention provides a kind of anti-stick formula of piezo silver slurry burnt in a heap and preparation method thereof, utilizes
This formula and preparation method advantages of simple, after prepared piezo silver slurry has sintering, silver layer densification is full, Non-sticking burnt in a heap,
Good electrical property, adhesion is high, the advantage of resistance to soldering heat function admirable.
Technical scheme:
Beneficial effect: compared with prior art, it is an advantage of the current invention that: the present invention uses and meets sintering furnace oven temperature profile
Gradient burning resin system, sintering process, stop the possibility of bonding die from silver slurry, add use high-specific surface area argentum powder, and
Antiplastering aid nikel powder, significantly reduces the probability of piezo bonding die burnt in a heap, improves piezo production efficiency；And use gradient combustion
Burn the severe degree of reaction when resin system reduces silver layer sintering and effectively raise the consistency of silver layer, and improve table
The electrical property of piezo after the metallization of face；Using the full densification of silver layer after this preparation method sintering, silver layer is bright as silver metallic luster,
The piezo electrical property of each model is good, silver layer horizontal pull ＞ 20N, longitudinal pulling force ＞ 2N, high density rear Non-sticking burnt in a heap.
Detailed description of the invention
Below in conjunction with detailed description of the invention, it is further elucidated with the present invention.
A kind of anti-stick formula of piezo silver slurry burnt in a heap and preparation method thereof, the component of its silver slurry and mass fraction
For: the mass fraction of argentum powder is 35%～60%, and the mass fraction of organic carrier is 40%～65%, the mass fraction of glass dust
Being 1%～2%, antiplastering aid mass fraction is 1%～2%；
The particle diameter of described argentum powder is that particle diameter is distributed as D10 ＜ 100nm, D50 ＜ 500nm, D90 ＜ 1 μm 0, specific surface area
＞ 7m2/ g, argentum powder is a kind of high dispersive, nano level high surface argentum powder；
The component of described organic carrier and the mass fraction that mass fraction is ethyl cellulose are 3%～5%, polyethylene
The mass fraction of butyral is 2%～5%, and the mass fraction of acrylic resin is 1%～3%, the mass fraction of terpineol
Being 20%～40%, the mass fraction of butyl carbitol is 40%～60%, the mass fraction of tributyl citrate be 5%～
10%；The component of described glass powder and mass fraction are silicon dioxide 3%～10%, zinc oxide 3%～10%, lead oxide
25%～40%, bismuth oxide 40%～60%, diboron trioxide 10%～20%, glass dust is can be with 800 DEG C of sintering
Lead bearing glass powder body；Described antiplastering aid is nikel powder, nickel oxide powder, among boron oxide, boric acid or several combination, mass fraction
It is 1%～2%；Antiplastering aid be particle size range be the nikel powder of 0.5～2 μm, nickel oxide powder, boron oxide, boric acid.
Preparation method is as follows:
Step 1, is substantially dissolved in a certain amount of organic molten by ethyl cellulose, polyvinyl butyral resin, acrylic resin
Agent is configured to organic carrier, heats under the conditions of i.e. 60～90 DEG C and unanimously stir, until being clear solution；Described ethyl cellulose
Element, polyethylene acetal butyral and acrylic resin form the gradient burning meeting furnace temperature in proportion according to oven temperature profile；
Step 2, joins according to described glass powder component and mass fraction and takes raw material use high speed powder beater by raw material mixing
Uniformly, being contained in alumina crucible use Muffle furnace heating, smelting temperature is 1200 DEG C～1300 DEG C, and shrend uses wine after drying
Essence, as medium, planetary ball mill 300rmp ball milling 4h～6h, i.e. can obtain meeting the glass powder of size distribution requirements；
Step 3, uses batch mixer to mix by described proportioning described organic carrier, argentum powder, glass powder and antiplastering aid
Closing uniformly, re-use three-high mill grinding distribution 8 times, obtain fineness≤5 μm, viscosity is the finished product piezo use of 25～40Pa.s
Silver slurry.
Embodiment 1
1) by 4% ethyl cellulose, the polyvinyl butyral resin of 4%, the acrylic resin of 1%, the terpineol of 40%,
The butyl carbitol of 45% and the tributyl citrate of 6% use agitator fully to dissolve under conditions of 80 DEG C, and preparation has
Airborne body.
2) use Muffle furnace at 1200 DEG C by silicon dioxide 5%, zinc oxide 5%, lead oxide 30%, bismuth oxide
50%, diboron trioxide 10%.Use planetary ball mill 300rpm ball milling 5h after being smelted into uniform glass phase shrend, prepare glass
Glass powder body
3) the 1st is taken) and 2) step gained organic carrier 42g, glass powder 2g, nikel powder 1g and argentum powder 55g mixing, use stirring
After machine is sufficiently stirred for, after re-using three-roll grinder grinding distribution, i.e. obtain the front silver slurry of piezo 55% silver content.
Embodiment 2
1) by 6% ethyl cellulose, the polyvinyl butyral resin of 6%, the acrylic resin of 3%, the terpineol of 35%,
The butyl carbitol of 45% and the tributyl citrate of 5% use agitator fully to dissolve under conditions of 80 DEG C, and preparation has
Airborne body.
2) the 1st is taken) step gained organic carrier 58g, the glass powder 1g obtained in example 1, nikel powder 1g and argentum powder 40g mix
Close, after using blender to be sufficiently stirred for, after re-using three-roll grinder grinding distribution, i.e. obtain the piezo back of the body of 40% silver content
Face silver slurry.
Claims (6)
1. the formula of an anti-stick piezo silver slurry burnt in a heap, it is characterised in that: the component of silver paste is: argentum powder, organic
Carrier, glass dust and antiplastering aid, wherein, the mass fraction of argentum powder is 35%～60%, and the mass fraction of organic carrier is 40%
～65%, the mass fraction of glass dust is 1%～2%, and antiplastering aid mass fraction is 1%～2%；
The component of described organic carrier is ethyl cellulose, polyvinyl butyral resin, acrylic resin, organic solvent, wherein, second
The mass fraction of base cellulose is 3%～5%, and the mass fraction of polyvinyl butyral resin is 2%～5%, acrylic resin
Mass fraction is 1%～3%, and described organic solvent is the group of one or more in terpineol, butyl carbitol or citric acid
Closing, wherein, the mass fraction of terpineol is 20%～40%, and the mass fraction of butyl carbitol is 40%～60%, citric acid
The mass fraction of tributyl is 5%～10%；
The component of described glass dust is silicon dioxide, zinc oxide, lead oxide, bismuth oxide and diboron trioxide, wherein quality
Mark is respectively as follows: silicon dioxide 3%～10%, zinc oxide 3%～10%, lead oxide 25%～40%, bismuth oxide 40%
～60%, diboron trioxide 10%～20%；
Described antiplastering aid is nikel powder, nickel oxide powder, the one or more combination in boron oxide, boric acid, mass fraction be 1%～
2%.
The formula of anti-stick piezo silver slurry burnt in a heap the most according to claim 1, it is characterised in that: the grain of described argentum powder
Footpath is distributed as D10 ＜ 100nm, D50 ＜ 500nm, D90 ＜ 1 μm 0, specific surface area ＞ 7m2/g。
The formula of anti-stick piezo silver slurry burnt in a heap the most according to claim 1, it is characterised in that: described antiplastering aid is
Particle size range is the nikel powder of 0.5～2 μm, nickel oxide powder, boron oxide, boric acid.
The formula of anti-stick piezo silver slurry burnt in a heap the most according to claim 1, it is characterised in that: described argentum powder is one
Plant high dispersive, nano level high surface argentum powder.
The formula of anti-stick piezo silver slurry burnt in a heap the most according to claim 1, it is characterised in that: described glass dust is
Can be with the lead bearing glass powder body of 800 DEG C of sintering.
6. the preparation method of an anti-stick piezo silver slurry burnt in a heap, it is characterised in that comprise the following steps:
Step 1, is substantially dissolved in organic solvent has been configured to ethyl cellulose, polyvinyl butyral resin, acrylic resin
Airborne body, heats under the conditions of i.e. 60～90 DEG C and unanimously stirs, until being clear solution；Described ethyl cellulose, polyethylene contract
Butyral and acrylic resin form the gradient burning meeting furnace temperature in proportion according to oven temperature profile；
Step 2, joins according to described glass powder component and mass fraction and takes raw material by raw material mix homogeneously, be contained in crucible use
Muffle furnace heats, and smelting temperature is 1200 DEG C～1300 DEG C, shrend use after drying ethanol as medium, ball milling, the most available
Meet the glass powder of size distribution requirements；
Step 3, by described organic carrier, argentum powder, glass powder and antiplastering aid by described proportioning mix homogeneously, then grinding point
Dissipating, obtain fineness≤5 μm, viscosity is the silver slurry of 25～40Pa.s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610673826.3A CN106205777A (en) | 2016-08-16 | 2016-08-16 | Anti-stick formula of piezo silver slurry burnt in a heap and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610673826.3A CN106205777A (en) | 2016-08-16 | 2016-08-16 | Anti-stick formula of piezo silver slurry burnt in a heap and preparation method thereof |
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| CN106205777A true CN106205777A (en) | 2016-12-07 |
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| CN201610673826.3A Pending CN106205777A (en) | 2016-08-16 | 2016-08-16 | Anti-stick formula of piezo silver slurry burnt in a heap and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113161037A (en) * | 2021-04-28 | 2021-07-23 | 佛山市顺德区百锐新电子材料有限公司 | Acid-resistant atomizer silver paste and preparation method thereof |
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| CN1548496A (en) * | 2003-05-12 | 2004-11-24 | 贵研铂业股份有限公司 | Antiadhesion agent and method of preventing chip adhesion during sintering high temperature silve paste |
| CN1673139A (en) * | 2004-12-30 | 2005-09-28 | 贵州振华亚太高新电子材料有限公司 | Lead-free electroplated silver slurry for outer electrode of multilayer chip element |
| 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 |
| CN103274700A (en) * | 2013-04-23 | 2013-09-04 | 云南银峰新材料有限公司 | Method for preparing ceramic medium slurry for screen printing |
| CN103390443A (en) * | 2013-06-25 | 2013-11-13 | 彩虹集团电子股份有限公司 | Lead-free electrode silver paste for semiconductive ceramic capacitors and preparation method of lead-free electrode silver paste |
| CN104347151A (en) * | 2013-08-02 | 2015-02-11 | 上海匡宇电子技术有限公司 | Conductive silver paste and preparation method thereof |
-
2016
- 2016-08-16 CN CN201610673826.3A patent/CN106205777A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1548496A (en) * | 2003-05-12 | 2004-11-24 | 贵研铂业股份有限公司 | Antiadhesion agent and method of preventing chip adhesion during sintering high temperature silve paste |
| CN1673139A (en) * | 2004-12-30 | 2005-09-28 | 贵州振华亚太高新电子材料有限公司 | Lead-free electroplated silver slurry for outer electrode of multilayer chip element |
| 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 |
| CN103274700A (en) * | 2013-04-23 | 2013-09-04 | 云南银峰新材料有限公司 | Method for preparing ceramic medium slurry for screen printing |
| CN103390443A (en) * | 2013-06-25 | 2013-11-13 | 彩虹集团电子股份有限公司 | Lead-free electrode silver paste for semiconductive ceramic capacitors and preparation method of lead-free electrode silver paste |
| CN104347151A (en) * | 2013-08-02 | 2015-02-11 | 上海匡宇电子技术有限公司 | Conductive silver paste and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113161037A (en) * | 2021-04-28 | 2021-07-23 | 佛山市顺德区百锐新电子材料有限公司 | Acid-resistant atomizer silver paste and preparation method thereof |
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Application publication date: 20161207 |