CN105161221B - Preparation method of copper electronic paste for piezoelectric ceramics - Google Patents
Preparation method of copper electronic paste for piezoelectric ceramics Download PDFInfo
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- CN105161221B CN105161221B CN201510683443.XA CN201510683443A CN105161221B CN 105161221 B CN105161221 B CN 105161221B CN 201510683443 A CN201510683443 A CN 201510683443A CN 105161221 B CN105161221 B CN 105161221B
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Abstract
The invention discloses a preparation method of copper electronic paste for piezoelectric ceramics. The method comprises steps of: preparing an organic carrier by using terpilenol, ethyl cellulose, dibutyl carbitol, ethylene glycol monoethyl ether acetate, polyether antifoaming agent, and silane coupling agent; mixing and dispersing copper powder, glass powder, thixotropic agent, and surfactant with the organic carrier so as to obtain the copper electronic paste for piezoelectric ceramics. The method is easy to operate and may achieve production without complex equipment. The copper powder is low in price so as to greatly reduce the production cost of the electronic paste. The prepared copper electronic paste is used for preparing piezoelectric ceramic material. Compared with a method for preparing a piezoelectric ceramic by using conventional silver paste, aluminum paste or the like, the method solves a problem of metal ionic migration and a defect of low adhesion strength and improves the vibration frequency and the conductive performance of the piezoelectric ceramic. The copper electronic paste can be sintered in the air and stored for a long time, and has excellent high-temperature stability performance and oxidation resistance.
Description
Technical field
The invention belongs to electronic package material field, it is related to a kind of preparation method of piezoelectric ceramics copper electric slurry.
Background technology
Piezoelectric ceramics is one can be by mechanical energy and the ceramic material of the mutual phase transformation of electric energy.It is widely used in ultrasound to change
Can device, underwater acoustic transducer, electroacoustic transducer, ceramic filter/transformer/frequency discriminator, high pressure generator, Infrared Detectors, sound
The technical fields such as surface wave device, electro-optical device, ignition and blasting device and piezolectric gyroscope.
With the development of electrode component manufacturing technology, into the nineties in 20th century, electronic product requirement miniaturization,
Slimming, high efficiency.Single-layer ceramic device is increasingly changed into multilayerceramic device, and the vibration frequency requirement to piezoelectric ceramics is more next
Higher, this requires there is intensity higher between electrode layer and base layer.Current silver electronic paste is commonly used to make pottery with piezoelectricity
Porcelain, but have that adhesive strength is low, Ag+The problems such as migration, cause silver electrode to depart from base layer in use, make electronics unit
Device is impaired or fails.
Cu has the high frequency characteristics and electric conductivity more more excellent than Au, and without Ag+Migration defect.But Cu
Be easy to oxidation in atmosphere, particularly Micron-Sized Copper Powders Coated forms one layer of dielectric oxide film after oxidation on its surface, make copper powder by
Conductor becomes insulator, greatly limit use of the copper powder in electric slurry field.Therefore prepare one kind and can be used for piezoelectric ceramics
Copper electric slurry, to improve the vibration frequency of piezoelectric ceramics, expand the application field of piezoelectric ceramics；Starched instead of noble metal electronics
Material, reduces production cost, has broad application prospects.
The content of the invention
It is an object of the invention to provide a kind of piezoelectric ceramics preparation method of copper electric slurry, it is used to improve existing piezoelectricity
The adhesive strength of the electric conductivity and electrode layer of electrode and base layer in ceramics.
The technical solution adopted in the present invention is, a kind of piezoelectric ceramics preparation method of copper electric slurry, it is specific press with
Lower step is implemented：
Step 1, prepares organic carrier：
By terpinol, ethyl cellulose, dibutyl carbitol (DBC), diethylene glycol ether acetate, polyether antifoam agent and silane
Coupling agent, stirs to raw material in addition agitator tank and is completely dissolved, and then deaeration treatment, obtains organic carrier；
Step 2, prepares copper electric slurry：
Will be during glass dust, thixotropic agent, surfactant and organic carrier obtained in step 1 add agitator tank, stirring is to complete
Full mixing；It is subsequently adding copper powder to continue to stir, is well mixed, obtains copper electric slurry；
Step 3, grinding distribution：
By copper electric slurry grinding distribution obtained in step 2, then deaeration treatment, obtains final product copper electric slurry finished product.
The features of the present invention is also resided in,
Each raw material is respectively according to mass percent in step 1：Terpinol 50%~80%, ethyl cellulose 3%~
15%, dibutyl carbitol (DBC) 8%~20%, diethylene glycol ether acetate 3%~16%, polyether antifoam agent 1%~6%, silicon
Alkane coupling agent 1%~3%, above constituent mass percentage sum is 100%.
Whipping temp is 60~90 DEG C, and mixing time is 120min.
Agitator tank is vacuum power agitator tank, and speed is improved per hour once in whipping process, and rotating speed is carried by 30~80rpm
It is high to 50~100rpm, dispersion rate brings up to 1000~4000rpm by 500~3000rpm.
Step 2 is specially：
Glass dust, thixotropic agent, surfactant and organic carrier obtained in step 1 are added vacuum power agitator tank by 2.1
In, 10~30min is stirred, control 50~90 DEG C of whipping temp, 40~90rpm of rotating speed, 1000~3000rpm of dispersion rate；
2.2 will copper powder add agitator tank in, stir 10~40min, control 50~90 DEG C of whipping temp, rotating speed 40~
90rpm, 1000~3000rpm of dispersion rate, stirring stand 8~12h after terminating, and obtain copper electric slurry.
Each raw material is respectively according to mass percent in step 2：Copper powder 60%~80%, glass dust 4%~13%, thixotroping
Agent 0.5%~4%, surfactant 0.5%~4%, organic carrier 10%~30% obtained in step 1, above constituent mass
Percentage sum is 100%..
Thixotropic agent by mass percentage by：Polyamide curing agent 35%~70%, polyurethane 20%~45%, dibutyl card
Must alcohol 5%~20%, above constituent mass percentage sum be 100%, mix.
Surfactant is any one or a few mixing in glycerine, RC-101 wetting agents, polyvinyl chloride.
Copper powder size described in step 2 is 1 μm.
Step 3 is specially：Copper electric slurry is rolled into slurry on three a kind of jade machines, until slurry fineness≤8 μm, then -3~
Vacuum defoamation treatment under 1KPa.
The beneficial effects of the invention are as follows,
(1) a kind of piezoelectric ceramics of the invention preparation method of copper electric slurry, the advantage is that it is simple to operate, need not
Complicated equipment can be produced, and copper powder is cheap in addition, so greatly reducing the production cost of electric slurry.
(2) copper electric slurry obtained in the present invention is prepared for piezoceramic material, and using traditional silver paste, aluminium paste etc.
Piezoelectric ceramics is compared obtained in slurry, solves the problems, such as the defect of metal ion transport and low adhesive strength, improves piezoelectricity
The vibration frequency and electric conductivity of ceramics.
(3) the copper electric slurry that the inventive method is prepared can be sintered in atmosphere, can long-term storage, with excellent height
Temperature stability energy and antioxygenic property.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.
The invention provides a kind of piezoelectric ceramics preparation method of copper electric slurry, specifically implement according to the following steps：
Step 1, prepares organic carrier：
Weigh following raw material respectively according to mass percent：Terpinol 50%~80%, ethyl cellulose 3%~15%,
Dibutyl carbitol (DBC) 8%~20%, diethylene glycol ether acetate 3%~16%, polyether antifoam agent 1%~6% is silane coupled
Agent 1%~3%, above constituent mass percentage sum is 100%.The raw material that will be weighed is stirred in adding vacuum power agitator tank
Mix, 60~90 DEG C of whipping temp, stir 120min, be completely dissolved raw material, that is, obtain organic carrier.
Speed is improved per hour once in whipping process, and rotating speed brings up to 50~100rpm, dispersion rate by 30~80rpm
1000~4000rpm is brought up to by 500~3000rpm；Stir the vacuum defoamation under -3~1KPa after terminating.
Polyether antifoam agent used and the commercially available conventional product of silane coupler in the present invention, silane coupler can be KH550,
KH560 etc..
After stirring terminates, such as ethyl cellulose is not completely dissolved, small dispersion machine can be added to continue to stir mixed liquor until
Dissolving.
Step 2, prepares copper electric slurry：
2.1 weigh respectively according to mass percent：1 μm of copper powder 60%~80%, glass dust 4%~13%, thixotropic agent
0.5%~4%, surfactant 0.5%~4%, organic carrier 10%~30% obtained in step 1, above constituent mass hundred
It is 100% to divide than sum；
Wherein, thixotropic agent by mass percentage by：Polyamide curing agent 35%~70%, polyurethane 20%~45%, two
Butyl carbitol 5%~20%, above constituent mass percentage sum is 100%, is mixed；Polyamides of the present invention
The commercially available all kinds of model polyamide curing agents of amine hardener can be used, such as ZY-650 polyamide curing agents；
Surfactant is any one or a few mixing in glycerine, RC-101 wetting agents, polyvinyl chloride；
2.2 glass dust that will be weighed, thixotropic agent, surfactant and organic carrier obtained in step 1 add vacuum power
In agitator tank, 10~30min of stirring controls 50~90 DEG C of whipping temp, 40~90rpm of rotating speed, dispersion rate to well mixed
1000~3000rpm；
2.3 copper powders that will weigh are added in agitator tanks, 10~40min of stirring to well mixed, control whipping temp 50~
90 DEG C, 40~90rpm of rotating speed, 1000~3000rpm of dispersion rate, stirring stand 8~12h after terminating, and obtain copper electric slurry.
Step 3, grinding distribution：
Copper electric slurry obtained in step 2 is rolled into slurry 8~12 times on three a kind of jade machines, grinding distribution, until slurry fineness≤8
μm, the then vacuum defoamation under -3~1KPa obtains final product copper electric slurry finished product.
A kind of piezoelectric ceramics of the present invention preparation method of copper electric slurry, simple to operate, need not be complicated equipment is
Can be produced, copper powder is cheap in addition, be greatly reduced the production cost of electric slurry.) copper obtained in the present invention is electric
Sub- slurry is prepared for piezoceramic material, compared with using piezoelectric ceramics obtained in slurry such as traditional silver paste, aluminium pastes, is solved
The defect of the problem of metal ion transport and low adhesive strength, improves the vibration frequency and electric conductivity of piezoelectric ceramics.Additionally,
The copper electric slurry that the inventive method is prepared can be sintered in atmosphere, can long-term storage, with excellent high temperature stability performance
And antioxygenic property.
Embodiment 1
Step 1, prepares organic carrier：
Weigh following raw material respectively according to mass percent：Terpinol 63%, ethyl cellulose 7%, dibutyl carbitol (DBC)
8%, diethylene glycol ether acetate 16%, polyether antifoam agent 4%, silane coupler 2%, above constituent mass percentage sum
It is 100%.The raw material that will be weighed is stirred in adding vacuum power agitator tank, and 70 DEG C of whipping temp stirs 120min, makes raw material complete
CL, speed is improved once in whipping process per hour, and rotating speed brings up to 80rpm by 50rpm, and dispersion rate is by 1000rpm
Bring up to 2000rpm；The vacuum defoamation under -1KPa after terminating is stirred, that is, is completed organic carrier and is prepared.
Step 2, prepares copper electric slurry：
2.1 weigh respectively according to mass percent：1 μm of copper powder 65%, glass dust 13%, thixotropic agent 4%, surfactant
0.5%, organic carrier 17.5% obtained in step 1, above constituent mass percentage sum is 100%；
Wherein thixotropic agent by mass percentage by：Polyamide curing agent 35%, polyurethane 45%, dibutyl carbitol (DBC)
20%, above constituent mass percentage sum is 100%, is mixed；Surfactant is RC-101 wetting agents；
2.2 glass dust that will be weighed, thixotropic agent, surfactant and organic carrier obtained in step 1 add vacuum power
In agitator tank, 20min is stirred, control 70 DEG C of whipping temp, rotating speed 60rpm, dispersion rate 1000rpm；
2.3 copper powders that will be weighed are added in agitator tank, stir 30min, control 70 DEG C of whipping temp, rotating speed 60rpm, dispersion
Speed 1000rpm, stirring stands 10h after terminating, and obtains copper electric slurry.
Step 3, grinding distribution：
Copper electric slurry obtained in step 2 is rolled into slurry 10 times on three a kind of jade machines, grinding distribution, until slurry fineness≤8 μm,
Then the vacuum defoamation under -1KPa, obtains final product copper electric slurry finished product.
Embodiment 2
Step 1, prepares organic carrier：
Weigh following raw material respectively according to mass percent：Terpinol 50%, ethyl cellulose 15%, dibutyl carbitol (DBC)
20%, diethylene glycol ether acetate 6%, polyether antifoam agent 6%, silane coupler 3%, above constituent mass percentage sum
It is 100%.The raw material that will be weighed is stirred in adding vacuum power agitator tank, and 60 DEG C of whipping temp stirs 120min, makes raw material complete
CL, speed is improved once in whipping process per hour, and rotating speed brings up to 50rpm by 30rpm, and dispersion rate is carried by 500rpm
Height arrives 1000rpm；The vacuum defoamation under -3KPa after terminating is stirred, that is, is completed organic carrier and is prepared.
After stirring terminates, such as ethyl cellulose is not completely dissolved, small dispersion machine can be added to continue to stir mixed liquor until
Dissolving.
Step 2, prepares copper electric slurry：
2.1 weigh respectively according to mass percent：1 μm of copper powder 60%, glass dust 7%, thixotropic agent 0.5%, surface-active
Agent 2.5%, organic carrier 30% obtained in step 1, above constituent mass percentage sum is 100%；
Wherein, thixotropic agent by mass percentage by：Polyamide curing agent 70%, polyurethane 20%, dibutyl carbitol (DBC)
10%, above constituent mass percentage sum is 100%, is mixed；Surfactant is polyvinyl chloride；
2.2 glass dust that will be weighed, thixotropic agent, surfactant and organic carrier obtained in step 1 add vacuum power
In agitator tank, 10min is stirred, control 50 DEG C of whipping temp, rotating speed 40rpm, dispersion rate 2000rpm；
2.3 copper powders that will be weighed are added in agitator tank, stir 10min, control 50 DEG C of whipping temp, rotating speed 40rpm, dispersion
Speed 2000rpm, stirring stands 8h after terminating, and obtains copper electric slurry.
Step 3, grinding distribution：
Copper electric slurry obtained in step 2 is rolled into slurry 8 times on three a kind of jade machines, grinding distribution, until slurry fineness≤8 μm,
Then the vacuum defoamation under -3KPa, obtains final product copper electric slurry finished product.
Embodiment 3
Step 1, prepares organic carrier：
Weigh following raw material respectively according to mass percent：Terpinol 80%, ethyl cellulose 3%, dibutyl carbitol (DBC)
12%, diethylene glycol ether acetate 3%, polyether antifoam agent 1, silane coupler 1%, above constituent mass percentage sum is
100%.The raw material that will be weighed is stirred in adding vacuum power agitator tank, and 90 DEG C of whipping temp stirs 120min, makes raw material complete
Dissolving, speed is improved once in whipping process per hour, and rotating speed brings up to 100rpm by 80rpm, and dispersion rate is carried by 3000rpm
Height arrives 4000rpm；The vacuum defoamation under 1KPa after terminating is stirred, that is, is completed organic carrier and is prepared.
Step 2, prepares copper electric slurry：
2.1 weigh respectively according to mass percent：1 μm of copper powder 80%, glass dust 4%, thixotropic agent 2%, surfactant
4%, organic carrier 10% obtained in step 1, above constituent mass percentage sum is 100%；
Wherein, thixotropic agent by mass percentage by：Polyamide curing agent 60%, polyurethane 35%, dibutyl carbitol (DBC)
5%, above constituent mass percentage sum is 100%, is mixed；Surfactant is the mixed of glycerine and RC-101 wetting agents
Compound；
2.2 glass dust that will be weighed, thixotropic agent, surfactant and organic carrier obtained in step 1 add vacuum power
In agitator tank, 30min is stirred, control 90 DEG C of whipping temp, rotating speed 90rpm, dispersion rate 3000rpm；
2.3 copper powders that will be weighed are added in agitator tank, stir 40min, control 90 DEG C of whipping temp, rotating speed 90rpm, dispersion
Speed 3000rpm, stirring stands 12h after terminating, and obtains copper electric slurry.
Step 3, grinding distribution：
Copper electric slurry obtained in step 2 is rolled into slurry 12 times on three a kind of jade machines, grinding distribution, until slurry fineness≤8 μm,
Then the vacuum defoamation under 1KPa, obtains final product copper electric slurry finished product.
Claims (4)
1. a kind of piezoelectric ceramics preparation method of copper electric slurry, it is characterised in that specifically implement according to the following steps：
Step 1, prepares organic carrier：
By terpinol, ethyl cellulose, dibutyl carbitol (DBC), diethylene glycol ether acetate, polyether antifoam agent and silane coupled
Agent, stirs to raw material in addition agitator tank and is completely dissolved, and then deaeration treatment, obtains organic carrier；
Each raw material is respectively according to mass percent：Terpinol 50%~80%, ethyl cellulose 3%~15%, two fourths
Base carbitol 8%~20%, diethylene glycol ether acetate 3%~16%, polyether antifoam agent 1%~6%, silane coupler
1%~3%, above constituent mass percentage sum is 100%；
Step 2, prepares copper electric slurry：
Will glass dust, thixotropic agent, surfactant and obtained in step 1 organic carrier add agitator tank in, stirring to completely mix
Close；It is subsequently adding copper powder to continue to stir, is well mixed, obtains copper electric slurry；
Each raw material is respectively according to mass percent：Copper powder 60%~80%, glass dust 4%~13%, thixotropic agent 0.5%
~4%, surfactant 0.5%~4%, organic carrier 10%~30% obtained in step 1, above constituent mass percentage it
Be 100%；
The thixotropic agent by mass percentage by：Polyamide curing agent 35%~70%, polyurethane 20%~45%, dibutyl card
Must alcohol 5%~20%, above constituent mass percentage sum be 100%, mix；
The surfactant is any one or a few mixing in glycerine, RC-101 wetting agents, polyvinyl chloride；
Specially：
2.1, by glass dust, thixotropic agent, surfactant and organic carrier addition vacuum power agitator tank obtained in step 1, stir
10~30min is mixed, 50~90 DEG C of whipping temp, 40~90rpm of rotating speed, 1000~3000rpm of dispersion rate is controlled；
2.2, by copper powder addition agitator tank, stir 10~40min, control 50~90 DEG C of whipping temp, 40~90rpm of rotating speed to divide
1000~3000rpm of speed is dissipated, stirring stands 8~12h, obtains copper electric slurry after terminating；
Step 3, grinding distribution：
By copper electric slurry grinding distribution obtained in step 2, then deaeration treatment, obtains final product copper electric slurry finished product.
2. a kind of piezoelectric ceramics according to claim 1 preparation method of copper electric slurry, it is characterised in that described to stir
Temperature is mixed for 60~90 DEG C, mixing time is 120min.
3. a kind of piezoelectric ceramics according to claim 1 preparation method of copper electric slurry, it is characterised in that described to stir
Tank to be mixed for vacuum power agitator tank, speed is improved per hour once in whipping process, rotating speed brings up to 50 by 30~80rpm~
100rpm, dispersion rate brings up to 1000~4000rpm by 500~3000rpm.
4. a kind of piezoelectric ceramics according to claim 1 preparation method of copper electric slurry, it is characterised in that step 2
Described in copper powder size be 1 μm.
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| CN106205771B (en) * | 2016-06-30 | 2018-05-15 | 金陵科技学院 | A kind of preparation method of oxidation resistant copper conductor slurry |
| CN106782885B (en) * | 2016-12-19 | 2018-07-03 | 西安工程大学 | A kind of preparation method of nano silver wire-copper staple fiber-copper composite electron slurry |
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| CN102664057A (en) * | 2012-05-17 | 2012-09-12 | 合肥工业大学 | Conductive copper paste for surface electrodes of chip ceramic capacitor and preparation method thereof |
| CN103555251A (en) * | 2013-10-18 | 2014-02-05 | 中山职业技术学院 | High-heat-conductivity high-reliability ultraviolet-curing LED (light-emitting diode) electrically-conductive silver adhesive and preparation method thereof |
| CN104201325A (en) * | 2014-08-20 | 2014-12-10 | 浙江中科立德新材料有限公司 | Novel lithium ion battery homogenizing and stirring process |
| CN104361950A (en) * | 2014-10-21 | 2015-02-18 | 西安工程大学 | Preparation method of carbon-clad copper electronic paste |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4020764B2 (en) * | 2001-12-21 | 2007-12-12 | Ｊｆｅミネラル株式会社 | Super fine metal slurry with excellent dispersibility |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101339821A (en) * | 2008-08-15 | 2009-01-07 | 深圳市圣龙特电子有限公司 | Copper paste without lead and cadmium and manufacturing method therefor |
| CN102664057A (en) * | 2012-05-17 | 2012-09-12 | 合肥工业大学 | Conductive copper paste for surface electrodes of chip ceramic capacitor and preparation method thereof |
| CN103555251A (en) * | 2013-10-18 | 2014-02-05 | 中山职业技术学院 | High-heat-conductivity high-reliability ultraviolet-curing LED (light-emitting diode) electrically-conductive silver adhesive and preparation method thereof |
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| CN104361950A (en) * | 2014-10-21 | 2015-02-18 | 西安工程大学 | Preparation method of carbon-clad copper electronic paste |
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