CN110120275A - A kind of Metal slurry and preparation method thereof of power battery hermetically sealed connector - Google Patents
A kind of Metal slurry and preparation method thereof of power battery hermetically sealed connector Download PDFInfo
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- CN110120275A CN110120275A CN201810928063.1A CN201810928063A CN110120275A CN 110120275 A CN110120275 A CN 110120275A CN 201810928063 A CN201810928063 A CN 201810928063A CN 110120275 A CN110120275 A CN 110120275A
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- raw material
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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 Metal slurries and preparation method thereof of power battery hermetically sealed connector, the Metal slurry includes metallization raw material and organic adhesive, the mass ratio of the metallization raw material and organic adhesive are as follows: 8-9:1-2, the metallization raw material includes metal oxide active agent, the component and its mass percent of the metal oxide active agent are alumina powder 10~15%, silica 8~15%, titanium dioxide 1%~2%, tantalum pentoxide 1%~2%；The organic binder includes ethyl cellulose, terpineol, organic silicon defoamer, organosilicon levelling agent, and the ethyl cellulose, terpineol, organic silicon defoamer, organosilicon levelling agent mass ratio are 10-15:1000-1199:3:5.The metalized surface roughness of the cell sealing connector obtained after sintering is down to≤1.0um, and the sealing strength of metallization is improved to >=120Mpa.
Description
Technical field
The invention belongs to electric automobile power battery technical fields, and in particular to a kind of gold of power battery hermetically sealed connector
Belong to slurrying material and preparation method thereof.
Background technique
Ceramics are due to intensity is high, dielectric constant is small, volume resistivity is high, dielectric loss is small and heat shock resistance intensity is big
Etc. performance characteristics, ceramic component itself be excellent insulating materials, itself do not have solderability, solder cannot generally also soak it
Profit, metallization are to realize an effective way of ceramic and metal jointing.
Raw material used in ceramic metallization and its formula are the key that metallization.In actual production, different producer
There is different special raw material formulas.The paste or slurry being made of special formulation raw material can effectively realize ceramic particular portion
The purpose of metallization is realized in the coating of position by drying, sintering process.The coating of paste or slurry can pass through manual pen
Apply, it is mechanical apply, the modes such as spray gun spraying and silk-screen printing are completed.
Metallization process is varied, can substantially be divided into thick-film technique and thin-film technique.With thin-film technique (with vapor deposition,
Sputtering, ion plating are main method) it compares, thick-film technique exists significant excellent in terms of the metallization for realizing ceramic component part
Gesture, thus generallyd use in large-scale industrial production.Research thinks that the refractory metal powders such as W, Mo and aluminium oxide are made pottery
It is related that similar thermal expansion coefficient, the sintering character of porcelain are similar and the two matching is good etc..
Thick film ink used in existing ceramic metalizing process is the outstanding paste formed using bonding agent or single solvent
Shape liquid is mixed with metal powder.Interface that carrier in existing thick film ink is in contact with solid powder/particle, tension and
Wellability consistency is poor, influences the stability and air-tightness of metallization process.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of New-energy electric vehicle power battery hermetically sealed connector metal
Slurrying material and preparation method thereof, using Metal slurry provided by the invention to the adhesiveness of cell sealing connector ceramic surface
Enhancing, extends the drying time of slurry, and the metalized surface roughness of the cell sealing connector obtained after sintering is down to≤
1.0um, the sealing strength of metallization are improved to >=120Mpa.
To achieve the above object, the invention provides the following technical scheme:
A kind of New-energy electric vehicle power battery hermetically sealed connector Metal slurry, including metallization raw material and organic bonding
Agent, the mass ratio of the metallization raw material and organic adhesive are as follows: 8-9:1-2, the metallization raw material includes metal oxide
Activating agent, the component and its mass percent of the metal oxide active agent are alumina powder 10~15%, silica 8~
15%, titanium dioxide 1%~2%, tantalum pentoxide 1%~2%；The organic binder includes ethyl cellulose, terpineol, organic
Silicon defoaming agent, organosilicon levelling agent, the ethyl cellulose, terpineol, organic silicon defoamer, organosilicon levelling agent mass ratio are
10 -15:1000-1199 :3 :5。
Further, the organic silicon defoamer is modified silicone and silica mixture, the organosilicon levelling agent
For hydroxy polyethers modified dimethyl polysiloxane.
A kind of preparation method of New-energy electric vehicle power battery hermetically sealed connector Metal slurry: including following step
It is rapid: (1) to prepare metal oxide active agent: taking constituent mass score alumina powder, silica, titanium dioxide, five oxidations two
Tantalum, mixing and ball milling add the carboxylic acid acid rouge block polymer of 0.3%-1% during mixing and ball milling, Control granularity≤2.0 μm, then
Drying and processing is carried out, 80 DEG C of drying temperature, the time 4 hours, obtains metal oxide active agent powder；(2) preparation metallization is former
Material: take the molybdenum powder of mass fraction 30 ~ 50% and 10 ~ 20% manganese powder, with step 1) preparation metal oxide active agent powder into
Row mixing and ball milling obtains the metallization raw material of granularity≤2.0 μm after ball milling, then carries out drying and processing, and drying temperature is 80 DEG C, when
Between be 4 hours, obtain metallization raw material；(3) organic binder is prepared: by ethyl cellulose: terpineol: organic silicon defoamer:
Organosilicon levelling agent is added in vial according to mass ratio, carries out heating and dissolves, until mixing completely, heating temperature is 80 DEG C,
Obtain organic adhesive；(4) it prepares Metal slurry: having what the metallization raw material of step 2 preparation and step 3) were prepared
Machine bonding agent carries out mix grinding, needs to heat in intergrinding process, and heating temperature is 60 ~ 70 DEG C, and the mix grinding time is 24 ~ 48 hours, mix grinding
Slurry obtains New-energy electric vehicle power battery hermetically sealed connector Metal slurry through 300 mesh screen filtrations afterwards.
Further, for the grinding stone that ball milling uses in step (1) and (2) for agate ball, ball milling material ball ratio is 1:2, when ball milling
Between be 72 hours.
Further, drying equipment uses constant temperature baking box in step (1) and (2).
Further, the heating equipment that organic adhesive is prepared in step (3) is infrared oven.
Further, mix grinding uses frequency control jar mill in step (4), and revolving speed is 80 revs/min.
The utility model has the advantages that
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention adds carboxylic acid acid rouge block polymer in metal oxide active agent, can effectively break up raw material processed
The aggregate formed in journey enables raw material to be sufficiently mixed and be crushed, and reaches granularity≤2.0um requirement, to make ceramet
Change layer surface roughness and is down to≤1.0um from≤1.6um；The sealing strength of ceramic metallization, from >=70MPa improve to >=
120MPa。
3, organic silicon defoamer and organosilicon levelling agent are added in slurry of the present invention, is acted synergistically by each component, guarantees
Slurry will not generate blistering in processing and use process, while organic adhesive and metallization raw material are in mix grinding contact process
It does not chemically react, forms solid-liquid mixed slurry, be printed on slurry on ceramic workpiece with certain viscosity and preferable
Mobility.
4, the tension of slurry of the present invention and wettability increase, and slurry can be adhered firmly on ceramic surface after printing, be prolonged
The drying time of long slurry avoids cracking before drying and sintering, improves the qualification rate of product.
5, the dispersing uniformity of solid particle is improved in slurry of the present invention, and sinking speed reduces, and surface covered improves,
The planarization that slurry is coated in workpiece surface can be improved, guarantees its consistency of thickness.
6, simple process provided by the invention, it is easy to operate, the complexity of preparation link is reduced, there is good repetition
Property, it is suitble to industrial production.
Specific embodiment
Embodiment 1
A kind of New-energy electric vehicle power battery hermetically sealed connector Metal slurry, including metallization raw material and organic bonding
The mass ratio of agent, the metallization raw material and organic adhesive is 4:1, and the metallization raw material includes metal powder and metal oxygen
Compound activating agent, the component and its mass percent of the metal powder are as follows: 30% molybdenum powder, 20% manganese powder, the metal oxide
The component and its mass percent of activating agent are alumina powder 10%, silica 8%, titanium dioxide 2%, tantalum pentoxide 2%；Institute
Stating organic binder includes ethyl cellulose, terpineol, organic silicon defoamer, hydroxy polyethers modified dimethyl polysiloxane, institute
Stating ethyl cellulose, terpineol, organic silicon defoamer, hydroxy polyethers modified dimethyl polysiloxane mass ratio is 10:1000:3:
5。
A kind of preparation method of New-energy electric vehicle power battery hermetically sealed connector Metal slurry, including following step
It is rapid: (1) to prepare metal oxide active agent: taking constituent mass score alumina powder, silica, titanium dioxide, five oxidations two
Tantalum adds 0.3% carboxylic acid acid rouge block polymer, carries out ball milling on ball mill in the ball grinder equipped with agate ball, expects: ball
Mass ratio be 1:2, Ball-milling Time be 72 hours, until metal oxide active agent powder size≤2.0 μm, strainer is isolated
Agate ball, and metal oxide active agent is placed in constant temperature baking box and carries out drying and processing, 80 DEG C of drying temperature, the time 4 is small
When, it obtains metal oxide active agent powder and stores；(2) preparation metallization raw material: take mass fraction 30 ~ 50% molybdenum powder and
10 ~ 20% manganese powder carries out ball in the ball grinder equipped with agate ball with the metal oxide active agent powder on ball mill
Mill, material: the mass ratio of ball is 1:2, and Ball-milling Time is 72 hours, until metal oxide active agent powder size≤2.0 μm, filter
Net isolates agate ball, and metal oxide active agent is placed in constant temperature baking box and carries out drying and processing, and 80 DEG C of drying temperature,
Time 4 hours, metallization raw material is made；(3) it prepares organic adhesive: preparing organic binder: by ethyl cellulose, terpin
Alcohol, organic silicon defoamer, hydroxy polyethers modified dimethyl polysiloxane are added in vial according to mass ratio, heat molten
Change, until mixing completely, heating temperature is 80 DEG C, obtains organic adhesive；(4) Metal slurry is prepared: will be by step 2 system
The organic adhesive that standby metallization raw material and step 3) are prepared carries out mix grinding according to the ratio of 4:1, adopts in intergrinding process
It is heated with infrared oven, heating temperature is 60~70 DEG C, and mix grinding uses frequency control jar mill, and revolving speed is 80 revs/min, is mixed
Time consuming is 24~48 hours, and slurry obtains the sealing of New-energy electric vehicle power battery and connect through 300 mesh screen filtrations after mix grinding
Connect device Metal slurry.
Embodiment 2
A kind of New-energy electric vehicle power battery hermetically sealed connector Metal slurry, including metallization raw material and organic bonding
The mass ratio of agent, the metallization raw material and organic adhesive is 9:1, and the metallization raw material includes metal powder and metal oxygen
Compound activating agent, the component and its mass percent of the metal powder are as follows: 50% molybdenum powder, 10% manganese powder, the metal oxide
The component and its mass percent of activating agent are alumina powder 15%, silica 1 5%, titanium dioxide 1%, tantalum pentoxide 1%；
The organic binder includes ethyl cellulose, terpineol, organic silicon defoamer, hydroxy polyethers modified dimethyl polysiloxane,
The ethyl cellulose, terpineol, organic silicon defoamer, hydroxy polyethers modified dimethyl polysiloxane mass ratio are 15:1199:
3:5.
A kind of preparation method of New-energy electric vehicle power battery hermetically sealed connector Metal slurry, including following step
It is rapid: (1) to prepare metal oxide active agent: taking constituent mass score alumina powder, silica, titanium dioxide, five oxidations two
Tantalum adds 1% carboxylic acid acid rouge block polymer, carries out ball milling on ball mill in the ball grinder equipped with agate ball, expects: ball
Mass ratio is 1:2, and Ball-milling Time is 72 hours, and until metal oxide active agent powder size≤2.0 μm, strainer isolates Ma
Nao ball, and metal oxide active agent is placed in constant temperature baking box and carries out drying and processing, 80 DEG C of drying temperature, the time 4 hours,
It obtains metal oxide active agent powder and stores；(2) preparation metallization raw material: take mass fraction 30 ~ 50% molybdenum powder and 10 ~
20% manganese powder carries out ball milling in the ball grinder equipped with agate ball with the metal oxide active agent powder on ball mill,
Material: the mass ratio of ball is 1:2, and Ball-milling Time is 72 hours, until metal oxide active agent powder size≤2.0 μm, strainer
Agate ball is isolated, and metal oxide active agent is placed in constant temperature baking box and carries out drying and processing, 80 DEG C of drying temperature, when
Between 4 hours, be made metallization raw material；(3) prepare organic adhesive: preparing organic binder: by ethyl cellulose, terpineol,
Organic silicon defoamer, hydroxy polyethers modified dimethyl polysiloxane are added in vial according to mass ratio, carry out heating and dissolve, directly
It is mixed to complete, heating temperature is 80 DEG C, obtains organic adhesive；(4) Metal slurry is prepared: the gold that step 2 will be prepared
The organic adhesive that categoryization raw material and step 3) are prepared carries out mix grinding according to the ratio of 4:1, uses in intergrinding process infrared
Line oven heat, heating temperature are 60~70 DEG C, and mix grinding uses frequency control jar mill, and revolving speed is 80 revs/min, the mix grinding time
It is 24~48 hours, slurry obtains New-energy electric vehicle power battery hermetically sealed connector gold through 300 mesh screen filtrations after mix grinding
Belong to slurrying material.
Embodiment 3
A kind of New-energy electric vehicle power battery hermetically sealed connector Metal slurry, including metallization raw material and organic bonding
The mass ratio of agent, the metallization raw material and organic adhesive is 4:1, and the metallization raw material includes metal powder and metal oxygen
Compound activating agent, the component and its mass percent of the metal powder are as follows: 35% molybdenum powder, 15% manganese powder, the metal oxide
The component and its mass percent of activating agent are alumina powder 12%, silica 1 2%, titanium dioxide 1%, tantalum pentoxide 2%；
The organic binder includes ethyl cellulose, terpineol, organic silicon defoamer, organosilicon levelling agent, the ethyl cellulose,
Terpineol, organic silicon defoamer, organosilicon levelling agent mass ratio are 12:1100:3:5.
A kind of preparation method of New-energy electric vehicle power battery hermetically sealed connector Metal slurry, including following step
It is rapid: (1) to prepare metal oxide active agent: taking constituent mass score alumina powder, silica, titanium dioxide, five oxidations two
Tantalum adds 0.5% carboxylic acid acid rouge block polymer, carries out ball milling on ball mill in the ball grinder equipped with agate ball, expects: ball
Mass ratio be 1:2, Ball-milling Time be 72 hours, until metal oxide active agent powder size≤2.0 μm, strainer is isolated
Agate ball, and metal oxide active agent is placed in constant temperature baking box and carries out drying and processing, 80 DEG C of drying temperature, the time 4 is small
When, it obtains metal oxide active agent powder and stores；(2) preparation metallization raw material: take mass fraction 30 ~ 50% molybdenum powder and
10 ~ 20% manganese powder carries out ball in the ball grinder equipped with agate ball with the metal oxide active agent powder on ball mill
Mill, material: the mass ratio of ball is 1:2, and Ball-milling Time is 72 hours, until metal oxide active agent powder size≤2.0 μm, filter
Net isolates agate ball, and metal oxide active agent is placed in constant temperature baking box and carries out drying and processing, and 80 DEG C of drying temperature,
Time 4 hours, metallization raw material is made；(3) it prepares organic adhesive: preparing organic binder: by ethyl cellulose: terpin
Alcohol: organic silicon defoamer: organosilicon levelling agent is added in vial according to mass ratio, carries out heating and dissolves, until mix completely,
Heating temperature is 80 DEG C, obtains organic adhesive；(4) prepare Metal slurry: by the metallization raw material for preparing step 2 and
The organic adhesive that step 3) is prepared carries out mix grinding according to the ratio of 4:1, is heated in intergrinding process using infrared oven,
Heating temperature is 60~70 DEG C, and mix grinding uses frequency control jar mill, and revolving speed is 80 revs/min, and the mix grinding time is 24~48 small
When, slurry obtains New-energy electric vehicle power battery hermetically sealed connector Metal slurry through 300 mesh screen filtrations after mix grinding.
The New-energy electric vehicle power battery hermetically sealed connector Metal slurry of preparation, covers painting battery by silk-screen printing
Hermetically sealed connector ceramic material surfaces extend the drying time of slurry, can be avoided and crack before drying and sintering, sintering
The metalized surface roughness of the cell sealing connector obtained afterwards is down to≤1.0um, the sealing strength of metallization from≤1.6um
It improves from >=70MPa to >=120Mpa, the qualification rate of cell sealing connector is also improved.
The preferred embodiment of the patent is described in detail above, but this patent is not limited to above-mentioned embodiment party
Formula within the knowledge of one of ordinary skill in the art can also be under the premise of not departing from this patent objective
It makes a variety of changes.
Claims (5)
1. a kind of Metal slurry of power battery hermetically sealed connector, including metallization raw material and organic adhesive, the metal
Change the mass ratio of raw material and organic adhesive are as follows: 8-9:1-2, which is characterized in that the metallization raw material includes metal oxide
Activating agent, the component and its mass percent of the metal oxide active agent are alumina powder 10~15%, silica 8~
15%, titanium dioxide 1%~2%, tantalum pentoxide 1%~2%；The organic binder includes ethyl cellulose, terpineol, organic
Silicon defoaming agent, organosilicon levelling agent, the ethyl cellulose, terpineol, organic silicon defoamer, organosilicon levelling agent mass ratio are
10 -15:1000-1199 :3 :5。
2. power battery hermetically sealed connector Metal slurry according to claim 1, which is characterized in that the organosilicon disappears
Infusion is modified silicone and silica mixture, and the organosilicon levelling agent is hydroxy polyethers modified dimethyl polysiloxane.
3. a kind of preparation method of power battery hermetically sealed connector Metal slurry as described in claim 1, which is characterized in that
The following steps are included: (1) prepares metal oxide active agent: taking constituent mass score alumina powder, silica, titanium dioxide
Titanium, tantalum pentoxide, mixing and ball milling, mixing and ball milling add the carboxylic acid acid rouge block polymer of 0.3%-1%, Control granularity in the process
≤ 2.0 μm, then drying and processing is carried out, 80 DEG C of drying temperature, the time 4 hours, obtain metal oxide active agent powder；(2) it makes
Standby metallization raw material: taking the molybdenum powder of mass fraction 30 ~ 50% and 10 ~ 20% manganese powder, living with the metal oxide of step 1) preparation
Property agent powder carry out mixing and ball milling, obtain the metallization raw material of granularity≤2.0 μm after ball milling, then carry out drying and processing, drying temperature
Degree is 80 DEG C, and the time is 4 hours, obtains metallization raw material；(3) organic binder is prepared: by ethyl cellulose: terpineol: having
Machine silicon defoaming agent: organosilicon levelling agent is added in vial according to mass ratio, carries out heating and dissolves, until mixing completely, heating
Temperature is 80 DEG C, obtains organic adhesive；(4) Metal slurry is prepared: by the metallization raw material and step 3) of step 2 preparation
The organic adhesive that is prepared carries out mix grinding, needs to heat in intergrinding process, and heating temperature is 60 ~ 70 DEG C, and the mix grinding time is 24 ~
48 hours, slurry obtained New-energy electric vehicle power battery hermetically sealed connector metallization paste through 300 mesh screen filtrations after mix grinding
Material.
4. the preparation method of power battery hermetically sealed connector Metal slurry according to claim 3, which is characterized in that step
Suddenly for the grinding stone that ball milling uses in (1) and (2) for agate ball, ball milling material ball ratio is 1:2, and Ball-milling Time is 72 hours.
5. the preparation method of power battery hermetically sealed connector Metal slurry according to claim 3, which is characterized in that step
Suddenly mix grinding uses frequency control jar mill in (4), and revolving speed is 80 revs/min.
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| CN201810928063.1A CN110120275A (en) | 2018-08-15 | 2018-08-15 | A kind of Metal slurry and preparation method thereof of power battery hermetically sealed connector |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114550973A (en) * | 2020-11-24 | 2022-05-27 | 娄底市安地亚斯电子陶瓷有限公司 | Thick film paste for screen printing and preparation method thereof |
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| CN103183978A (en) * | 2011-12-27 | 2013-07-03 | 比亚迪股份有限公司 | Ink composition and application for same, as well as product with selectively-metallized surface and preparation method for same |
| CN105568266A (en) * | 2014-10-10 | 2016-05-11 | 比亚迪股份有限公司 | Plastic product and plastic base surface selective metallization method |
| CN106588123A (en) * | 2016-12-16 | 2017-04-26 | 康文涛 | Activated molybdenum-manganese slurry used in ceramic metallization and preparing method thereof |
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| CN101808677A (en) * | 2007-07-27 | 2010-08-18 | 波士顿科学希姆德公司 | Goods with ceramic coated surfaces |
| CN103183978A (en) * | 2011-12-27 | 2013-07-03 | 比亚迪股份有限公司 | Ink composition and application for same, as well as product with selectively-metallized surface and preparation method for same |
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| CN114550973A (en) * | 2020-11-24 | 2022-05-27 | 娄底市安地亚斯电子陶瓷有限公司 | Thick film paste for screen printing and preparation method thereof |
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