CN104992801B - A kind of resistance slurry and preparation method thereof - Google Patents
A kind of resistance slurry and preparation method thereof Download PDFInfo
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- CN104992801B CN104992801B CN201510385624.4A CN201510385624A CN104992801B CN 104992801 B CN104992801 B CN 104992801B CN 201510385624 A CN201510385624 A CN 201510385624A CN 104992801 B CN104992801 B CN 104992801B
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Abstract
The present invention provides a kind of resistance slurry and preparation method thereof, and the resistance slurry includes following component：Talcum powder；Organic siliconresin；Quartz；Levelling agent；Thixotropic agent；Graphite；Ultra-fine lowpriced metal alloy powder conductive filler；Calcium oxide；Barium monoxide；Antimony oxide；Adhesive；Ruthenium dioxide pyrochlore.Preparation method：By talcum powder, graphite, calcium oxide, barium monoxide, antimony oxide and ruthenium dioxide pyrochlore high melt, water quenching, grating；Organic siliconresin, levelling agent, thixotropic agent and adhesive are mixed in a water bath；Solid mixture and solution are mixed, ultra-fine lowpriced metal alloy powder conductive filler is added, rolls, produce through three-high mill.The resistance slurry of the present invention and the adhesive force of base material are strong, ageing-resistant, and the resistance as made from the resistance slurry passes through test analysis, and display resistive performance is good, and this method technological requirement is simple, and manufacturing cost is low.
Description
Technical field
The present invention relates to field of electronic materials, and in particular to a kind of resistance slurry and preparation method thereof.
Background technology
Resistance is a kind of conventional electrical equipment, and application field is extensive, and example is as used in integrated circuit, chip, still
With developing rapidly for integrated circuit and chip, current resistance can not meet integrated need there is shortcomings
Will, resistance slurry is into a direction to solve this problem.Therefore, a kind of resistance slurry that can eliminate disadvantages mentioned above is found
The problem of as urgent need to resolve.
Electric slurry is the basic material for manufacturing thick film element, is that one kind passes through three rollings by solid powder and organic solvent
The well mixed paste of system.Existing resistance slurry is often difficult to take into account resistive performance and mechanical performance.Therefore, development of new
Resistance slurry turns into study hotspot.
The content of the invention
Goal of the invention：It is an object of the invention to provide resistance slurry both with a kind of electric conductivity and mechanical performance and its
Preparation method.
Technical scheme：
A kind of resistance slurry, by weight, including following component：Talcum powder 7-10 parts；Organic siliconresin 1.2-2 parts；
0.3 ~ 0.7 part of quartz；Levelling agent 0.5-1 parts；Thixotropic agent 0.5-1 parts；Graphite 8-12 parts；Ultra-fine lowpriced metal alloy powder conduction is filled out
Expect 6-8 parts；Calcium oxide 1-3 parts；Barium monoxide 1-3 parts；Antimony oxide 1-3 parts；Adhesive 10-12 parts；Ruthenium dioxide pyrochlore
2-3 parts.
Including following component preferably, by weight,：Talcum powder 8-9 parts；Organic siliconresin 1.5-1.7 parts；Quartz
0.4 ~ 0.6 part；Levelling agent 0.7-0.8 parts；Thixotropic agent 0.6-0.8 parts；Graphite 9-11 parts；Ultra-fine lowpriced metal alloy powder conduction is filled out
Expect 6-7 parts；Calcium oxide 2-3 parts；Barium monoxide 2-3 parts；Antimony oxide 1-2 parts；Adhesive 10-11 parts；Ruthenium dioxide pyrochlore
3 parts.
It is highly preferred that by weight, by weight, including following component：8 parts of talcum powder；Organic siliconresin 1.6
Part；0.5 part of quartz；0.7 part of levelling agent；0.7 part of thixotropic agent；10 parts of graphite；Ultra-fine 6 parts of lowpriced metal alloy powder conductive filler；
2 parts of calcium oxide；3 parts of barium monoxide；2 parts of antimony oxide；10 parts of adhesive；3 parts of ruthenium dioxide pyrochlore.
The levelling agent is 504 levelling agents or 505 levelling agents.
The thixotropic agent is rilanit special or polyamide wax.
Described adhesive is any one in polyvinyl acetate, polyurethane, butadiene-styrene rubber, nitrocellulose.
A kind of preparation method of resistance slurry, comprises the following steps：
（1）Talcum powder, graphite, calcium oxide, barium monoxide, antimony oxide and ruthenium dioxide pyrochlore are weighed by weight, are fallen
Entering in batch mixer, high-temperature electric resistance furnace melting is put into after being well mixed, smelting temperature is controlled at 1000-1300 DEG C, is incubated 1-6 hours,
Water quenching, grating in two pairs of rollers roller mill is placed in, until grain diameter stops rolling between 2-2.5 microns；
（2）Organic siliconresin, levelling agent, thixotropic agent and adhesive are weighed by weight, are mixed in 80-100 DEG C of water-bath
Close；
（3）By step（1）Obtained solid mixture and step（2）Solution mixing, add ultra-fine lowpriced metal alloy powder
Conductive filler, after stirring, rolled through three-high mill, produce resistance slurry.
Beneficial effect：
The resistance slurry of the present invention and the adhesive force of base material are strong, ageing-resistant, and the resistance as made from the resistance slurry is by surveying
Examination analysis, display resistive performance is good, and this method technological requirement is simple, and manufacturing cost is low.
Embodiment
The present invention is described in further detail below by embodiment.But those skilled in the art will manage
Solution, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Unreceipted specific skill in embodiment
Art or condition person, carried out according to the technology described by document in the art or condition or according to product description.Examination used
Agent or the unreceipted production firm person of instrument, being can be by the conventional products of acquisition purchased in market.
Scope is used as using what the value of range format expression should be interpreted as not only including clearly including in a flexible way
The numerical value of limit value, but also including covering all single numbers or subinterval within the range, just as each numerical value and sub-district
Between be expressly recited out.For example, " about 0.1% to about 5% " concentration range should be understood to not only include what is clearly included
The concentration of about 0.1% to about 5%, in addition to the single concentration in the range of alluding to（Such as, 1%, 2%, 3% and 4%）And subinterval（Example
Such as, 0.1% to 0.5%, 1% to 2.2%, 3.3% to 4.4%）.
Embodiment 1
A kind of resistance slurry, by weight, including following component：7 parts of talcum powder；1.2 parts of organic siliconresin；Quartz
0.3 part；504 0.5 part of levelling agents；0.5 part of rilanit special；8 parts of graphite；Ultra-fine 6 parts of lowpriced metal alloy powder conductive filler；
1 part of calcium oxide；1 part of barium monoxide；1 part of antimony oxide；10 parts of polyvinyl acetate；2 parts of ruthenium dioxide pyrochlore.
Preparation method：
（1）Talcum powder, graphite, calcium oxide, barium monoxide, antimony oxide and ruthenium dioxide pyrochlore are weighed by weight, are fallen
Entering in batch mixer, high-temperature electric resistance furnace melting is put into after being well mixed, smelting temperature is controlled at 1000-1300 DEG C, is incubated 1-6 hours,
Water quenching, grating in two pairs of rollers roller mill is placed in, until grain diameter stops rolling between 2-2.5 microns；
（2）Organic siliconresin, 504 levelling agents, rilanit special and polyvinyl acetate are weighed by weight, at 80-100 DEG C
Water-bath in mix；
（3）By step（1）Obtained solid mixture and step（2）Solution mixing, add ultra-fine lowpriced metal alloy powder
Conductive filler, after stirring, rolled through three-high mill, produce resistance slurry.
Embodiment 2
A kind of resistance slurry, by weight, including following component：8 parts of talcum powder；1.5 parts of organic siliconresin；Quartz
0.4 part；505 0.7 part of levelling agents；0.6 part of polyamide wax；9 parts of graphite；Ultra-fine 6 parts of lowpriced metal alloy powder conductive filler；Oxygen
Change 2 parts of calcium；2 parts of barium monoxide；1 part of antimony oxide；10 parts of polyurethane；3 parts of ruthenium dioxide pyrochlore.
Preparation method：
（1）Talcum powder, graphite, calcium oxide, barium monoxide, antimony oxide and ruthenium dioxide pyrochlore are weighed by weight, are fallen
Entering in batch mixer, high-temperature electric resistance furnace melting is put into after being well mixed, smelting temperature is controlled at 1000-1300 DEG C, is incubated 1-6 hours,
Water quenching, grating in two pairs of rollers roller mill is placed in, until grain diameter stops rolling between 2-2.5 microns；
（2）Organic siliconresin, 505 levelling agents, polyamide wax and polyurethane are weighed by weight, in 80-100 DEG C of water-bath
Middle mixing；
（3）By step（1）Obtained solid mixture and step（2）Solution mixing, add ultra-fine lowpriced metal alloy powder
Conductive filler, after stirring, rolled through three-high mill, produce resistance slurry.
Embodiment 3
A kind of resistance slurry, by weight, including following component：8 parts of talcum powder；1.6 parts of organic siliconresin；Quartz
0.5 part；504 0.7 part of levelling agents；0.7 part of rilanit special；10 parts of graphite；Ultra-fine 6 parts of lowpriced metal alloy powder conductive filler；
2 parts of calcium oxide；3 parts of barium monoxide；2 parts of antimony oxide；10 parts of butadiene-styrene rubber；3 parts of ruthenium dioxide pyrochlore.
Preparation method：
（1）Talcum powder, graphite, calcium oxide, barium monoxide, antimony oxide and ruthenium dioxide pyrochlore are weighed by weight, are fallen
Entering in batch mixer, high-temperature electric resistance furnace melting is put into after being well mixed, smelting temperature is controlled at 1000-1300 DEG C, is incubated 1-6 hours,
Water quenching, grating in two pairs of rollers roller mill is placed in, until grain diameter stops rolling between 2-2.5 microns；
（2）Organic siliconresin, 504 levelling agents, rilanit special and butadiene-styrene rubber are weighed by weight, in 80-100 DEG C of water
Mixed in bath；
（3）By step（1）Obtained solid mixture and step（2）Solution mixing, add ultra-fine lowpriced metal alloy powder
Conductive filler, after stirring, rolled through three-high mill, produce resistance slurry.
Embodiment 4
A kind of resistance slurry, by weight, including following component：9 parts of talcum powder；1.7 parts of organic siliconresin；Quartz
0.6 part；505 0.8 part of levelling agents；0.8 part of polyamide wax；11 parts of graphite；Ultra-fine 7 parts of lowpriced metal alloy powder conductive filler；Oxygen
Change 3 parts of calcium；3 parts of barium monoxide；2 parts of antimony oxide；11 parts of nitrocellulose；3 parts of ruthenium dioxide pyrochlore.
Preparation method：
（1）Talcum powder, graphite, calcium oxide, barium monoxide, antimony oxide and ruthenium dioxide pyrochlore are weighed by weight, are fallen
Entering in batch mixer, high-temperature electric resistance furnace melting is put into after being well mixed, smelting temperature is controlled at 1000-1300 DEG C, is incubated 1-6 hours,
Water quenching, grating in two pairs of rollers roller mill is placed in, until grain diameter stops rolling between 2-2.5 microns；
（2）Organic siliconresin, 505 levelling agents, polyamide wax and nitrocellulose are weighed by weight, at 80-100 DEG C
Mixed in water-bath；
（3）By step（1）Obtained solid mixture and step（2）Solution mixing, add ultra-fine lowpriced metal alloy powder
Conductive filler, after stirring, rolled through three-high mill, produce resistance slurry.
Embodiment 5
A kind of resistance slurry, by weight, including following component：10 parts of talcum powder；2 parts of organic siliconresin；Quartz 0.7
Part；504 1 part of levelling agents；1 part of rilanit special；12 parts of graphite；Ultra-fine 8 parts of lowpriced metal alloy powder conductive filler；Calcium oxide
3 parts；3 parts of barium monoxide；3 parts of antimony oxide；12 parts of nitrocellulose；3 parts of ruthenium dioxide pyrochlore.
Preparation method：
（1）Talcum powder, graphite, calcium oxide, barium monoxide, antimony oxide and ruthenium dioxide pyrochlore are weighed by weight, are fallen
Entering in batch mixer, high-temperature electric resistance furnace melting is put into after being well mixed, smelting temperature is controlled at 1000-1300 DEG C, is incubated 1-6 hours,
Water quenching, grating in two pairs of rollers roller mill is placed in, until grain diameter stops rolling between 2-2.5 microns；
（2）Organic siliconresin, 504 levelling agents, rilanit special and nitrocellulose are weighed by weight, at 80-100 DEG C
Water-bath in mix；
（3）By step（1）Obtained solid mixture and step（2）Solution mixing, add ultra-fine lowpriced metal alloy powder
Conductive filler, after stirring, rolled through three-high mill, produce resistance slurry.
Performance test：
Resistance slurry made from embodiment 1 ~ 5 is applied on ceramic substrate, dried at 250 ~ 280 DEG C, 800 DEG C of burnings
Knot, then soldering lead, adhesive force is tested with puller system, the results are shown in Table 1.For silver electronic paste, its on a ceramic substrate attached
Put forth effort that the 15N required by Technical specifications should be not less than.
Table 1
。
As shown in Table 1, after being sintered on resistance slurry ceramic substrate produced by the present invention, its sheet resistance reaches 40 m Ω/
More than, aging intensity reaches 16 N/mm2More than, viscosity is more than 170Pa.s/RPM, and adhesive force reaches more than 20N, property
Can be excellent.
Claims (7)
- A kind of 1. resistance slurry, it is characterised in that by weight, including following component：Talcum powder 7-10 parts；Organic siliconresin 1.2-2 part；0.3~0.7 part of quartz；Levelling agent 0.5-1 parts；Thixotropic agent 0.5-1 parts；Graphite 8-12 parts；Ultra-fine lowpriced metal alloy Powder conductive filler 6-8 parts；Calcium oxide 1-3 parts；Barium monoxide 1-3 parts；Antimony oxide 1-3 parts；Adhesive 10-12 parts；Ruthenium-oxide Pyrochlore 2-3 parts.
- A kind of 2. resistance slurry according to claim 1, it is characterised in that by weight, including following component：Talcum Powder 8-9 parts；Organic siliconresin 1.5-1.7 parts；0.4~0.6 part of quartz；Levelling agent 0.7-0.8 parts；Thixotropic agent 0.6-0.8 parts；Stone Black 9-11 parts；Ultra-fine lowpriced metal alloy powder conductive filler 6-7 parts；Calcium oxide 2-3 parts；Barium monoxide 2-3 parts；Antimony oxide 1-2 Part；Adhesive 10-11 parts；3 parts of ruthenium dioxide pyrochlore.
- 3. a kind of resistance slurry according to claim 1, it is characterised in that by weight including following component：Talcum 8 parts of powder；1.6 parts of organic siliconresin；0.5 part of quartz；0.7 part of levelling agent；0.7 part of thixotropic agent；10 parts of graphite；Ultra-fine base metal closes 6 parts of bronze conductive filler；2 parts of calcium oxide；3 parts of barium monoxide；2 parts of antimony oxide；10 parts of adhesive；3 parts of ruthenium dioxide pyrochlore.
- 4. a kind of resistance slurry according to any one of claims 1 to 3, it is characterised in that the levelling agent is 504 levellings Agent or 505 levelling agents.
- 5. a kind of resistance slurry according to any one of claims 1 to 3, it is characterised in that the thixotropic agent is hydrogenation castor Sesame oil or polyamide wax.
- 6. a kind of resistance slurry according to any one of claims 1 to 3, it is characterised in that described adhesive is poly-vinegar acid Any one in ethene, polyurethane, butadiene-styrene rubber, nitrocellulose.
- 7. any one of claims 1 to 3 a kind of preparation method of resistance slurry, it is characterised in that comprise the following steps：(1) talcum powder, graphite, calcium oxide, barium monoxide, antimony oxide and ruthenium dioxide pyrochlore are weighed by weight, are poured into mixed In material machine, high-temperature electric resistance furnace melting is put into after being well mixed, smelting temperature is controlled at 1000-1300 DEG C, is incubated 1-6 hours, water quenching, Grating in two pairs of rollers roller mill is placed in, until grain diameter stops rolling between 2-2.5 microns；(2) organic siliconresin, levelling agent, thixotropic agent and adhesive are weighed by weight, are mixed in 80-100 DEG C of water-bath；(3) solid mixture obtained step (1) and the solution mixing of step (2), it is conductive to add ultra-fine lowpriced metal alloy powder Filler, after stirring, rolled through three-high mill, produce resistance slurry.
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| CN108550416A (en) * | 2018-05-18 | 2018-09-18 | 苏州天鸿电子有限公司 | A kind of chip resistor resistance slurry |
| WO2020028999A1 (en) * | 2018-08-06 | 2020-02-13 | 苏州速腾电子科技有限公司 | Resistance paste for chip resistor and preparation method therefor |
| CN110590238A (en) * | 2019-07-29 | 2019-12-20 | 常州澳弘电子股份有限公司 | Preparation method of resistor paste for embedding resistor PCB |
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| JPS62119277A (en) * | 1985-11-18 | 1987-05-30 | Copal Co Ltd | Printing paste for thick film |
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| CN101692410A (en) * | 2009-08-21 | 2010-04-07 | 广东风华高新科技股份有限公司 | Silver paste of MLCC terminal electrode |
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