CN107799199A - A kind of low cost low temperature sintering piezoresistor silver paste and preparation method thereof - Google Patents

A kind of low cost low temperature sintering piezoresistor silver paste and preparation method thereof Download PDF

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Publication number
CN107799199A
CN107799199A CN201711003354.1A CN201711003354A CN107799199A CN 107799199 A CN107799199 A CN 107799199A CN 201711003354 A CN201711003354 A CN 201711003354A CN 107799199 A CN107799199 A CN 107799199A
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gap
silver powder
low temperature
micro
rolling
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CN107799199B (en
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樊钊锋
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Rainbow group new energy Limited by Share Ltd
Shaanxi rainbow new material Co., Ltd.
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Rainbow Group New Energy Ltd By Share Ltd
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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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
    • H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors

Abstract

A kind of low cost low temperature sintering piezoresistor silver paste and preparation method thereof, by mass fraction：Micro silver powder A 30~70, micro silver powder B 20~30, micro silver powder C 5~20, glass dust 2~6, titanium valve 1~3, additive 1~3, organic diluent 1~15, the various materials of the precise of organic bond 1~15, and be stirred for uniformly；Then rolling is carried out, there is the performance for improving slurry, greatly the characteristics of reduction device production cost.

Description

A kind of low cost low temperature sintering piezoresistor silver paste and preparation method thereof
Technical field
The present invention relates to piezoresistor silver paste technical field, more particularly to a kind of low cost low temperature sintering piezo-resistance Device silver paste and preparation method thereof.
Background technology
Piezoresistor is widely used, and from hand-held electronic product to industrial equipment, its specification and size are varied. With widely using for hand-held electronic product, especially mobile phone, laptop computer, PDA, digital camera, Medical Instruments etc., its electricity The rate request of road system is higher, and requires that operating voltage is lower, and this is just proposed to piezoresistor, and volume is smaller, performance Higher requirement.Existing slurry sintering temperature is high, noble silver dosage is big.
The content of the invention
The invention provides a kind of low cost low temperature sintering piezoresistor silver paste and preparation method thereof, solves sintering The problem of temperature is high, noble silver dosage is larger, there is the performance for improving slurry, greatly reduce device production cost Feature.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of low cost low temperature sinters piezoresistor silver paste, in terms of mass fraction, including：Micro silver powder A 30~70, Micro silver powder B 20~30, micro silver powder C 5~20, glass dust 2~6, titanium valve 1~3, nickel powder 1~3, organic diluent 1~15, have Machine adhesive 1~15.
Described micro silver powder A particle diameter is 0.5~2.5 μm, and micro silver powder B particle diameter is 1.0~4.8 μm, micro silver powder C grain Footpath is 0.5~2.0 μm.
Described glass dust is by Bi2O3、CaO、SrO、ZnO、B2O3、SnO、P2O5、V2O5、K2O presses 40~65wt%, 6- 10wt%, 6~10wt%, 4~10wt%, 5~17wt%, 4-7wt%, 1~5wt%, 1~5wt%, 1~3wt% ratio Sintered after mixing at 1100~1400 DEG C, water quenching, crushing, ball milling obtain.
Described organic bond is in terms of mass fraction, 10~35 parts of small molecule celluloses, 2~5 parts of saturated fatty acids, 1- 5 parts of organically-modified additives, 60~90 parts of organic solvent compositions.
Described organic diluent is diethylene glycol ether, butyl glycol ether, butyl carbitol, n-butanol, cyclohexanol, second Ether, petroleum ether, butyl acetate, terebinthine several mixed liquors.
A kind of low cost low temperature sinters piezoresistor silver paste preparation method for material, including,
Step 1：The preparation of glass dust：
Powder configures and sintering：Bi2O3、CaO、SrO、ZnO、B2O3、SnO、P2O5、V2O5、K2O presses 40~65wt%, 6- 10wt%, 6~10wt%, 4~10wt%, 5~17wt%, 4-7wt%, 1~5wt%, 1~5wt%, 1~3wt% ratio After mixing 25min is sintered at 1100~1400 DEG C；
Subsequent treatment：Above-mentioned mixing object is cooled to 680 DEG C of progress water quenchings, the Primary product after water quenching is carried out Sub-sieve, 15-25 μm of little particle is crushed to pulverizer, then according to real needs ball mill in aqueous medium existence condition The lower processing for carrying out thinner grade, 3 μm of particle diameter ＜；
Transition temperature is produced at 345~380 DEG C by above-mentioned step, and softening point is 400~485 DEG C of the pressure-sensitive slurry of low temperature Material glass dust；
Step 2：The preparation of organic bond：
10~35 parts of small molecule celluloses, 2~5 parts of saturated fatty acids, 60~90 parts of organic solvent compositions；It is first anti-to glass Answer in kettle and give certain mixing speed at 75~95 DEG C added with solvent, temperature control, be then slowly added into cellulose and satisfy And aliphatic acid, it is fully dissolved, dissolution time is 12~22h；
Step 3, the preparation scheme of slurry：
By mass fraction：Micro silver powder A 30~70, micro silver powder B 20~30, micro silver powder C 5~20, glass dust 2~6, titanium Powder 1~3, additive 1~3, organic diluent 1~15, the various materials of the precise of organic bond 1~15, and be stirred for Uniformly；
Step 4：
By material mixed in step 3, rolling, slitting part carry out rolling on three-roller so that mixture is in uniform cream Shape thing, obtains silver paste.
The condition of rolling is respectively on described three-roller, and condition one is 1. three-roller Stress control is in 20bar, gap 1:15,2. gap is 1:30,3. gap is 1:10,4. gap is 1:15, well mixed material is added on three-roller and premixed, Time is 10min or so；
Then three-roller Stress control is descended in this gap in 10bar, rolling 2 times；
1. condition two is 0 in 20bar, gap for three-roller Stress control:55,2. gap is 1:15,3. gap is 0:55, 4. gap is 0:30, rolling 2 times；
1. condition three is 0 in 20bar, gap for three-roller Stress control:35,2. gap is 0:30,3. gap is 0:25, 4. gap is 0:20；
The slurry form that rolling finishes is in light grey body of paste, has preferable mobility, fineness≤10 μm, viscosity 95 ±5kcps。
The particle diameter of the micro silver powder A is 0.8~2.5 μm, and micro silver powder B granularity is 1.5~4.0 μm of micro silver powder C granularity For 0.2~1.2 μm.
Further, micro silver powder A particle diameter is 1 μm, and micro silver powder B granularity is 2 μm, and micro silver powder C granularity is 1 μm.
Micro silver powder C and titanium valve addition manner are slowly added to during being in the roll milling process.
Beneficial effects of the present invention：
The glass dust of preparation has low softening point and transition temperature, it is had stronger adhesiveness at a lower temperature；
The silver paste has a preferable levelability, good printing net performance, color is shallower, and silver-colored face is than one after making electrode As slurry metallic luster it is more prominent；
This slurry changes the mismatch problem of shrinkage factor on the pressure-sensitive slurry of low temperature；By the addition of special additive, Solves the big problem of voltage drop that electrode is made；
It is low that electrode shows pressure sensitive voltage, the big advantage of capacity.
Embodiment
The present invention is elaborated with reference to embodiment.
Embodiment 1
The various raw material of balance precise for being 0.01g with accuracy：
Step 1：
Glass dust 30g is weighed, titanium valve 10g (being surface-treated before using) is stirred for uniformly；
Step 2：
Weigh 300g micro silver powder A and 200g micro silver powder B, 50g micro silver powder C and pour into three kinds of silver powder in agitator and halve It is even；
Step 3：
Organic bond 350g, diluent 50g, additive 10g is weighed to add jointly in agitator with obtaining in step 2 Silver powder mix 30min again；
Step 4：
Three-roll grinder is started, rolling is carried out as follows：
1) three-roller Stress control is carried out as follows in 20bar, gap condition, and well mixed material is added on three-roller Premix, time 15min；
Gap is 1. Gap is 2. Gap is 3. Gap is 4.
1:15 1:30 1:10 1:15
2) for three-roller Stress control in 10bar, gap condition is carried out as follows rolling, rolling 2 times；
Gap is 1. Gap is 2. Gap is 3. Gap is 4.
1:15 1:30 1:10 1:15
3) for three-roller Stress control in 20bar, gap condition is carried out as follows rolling, rolling 2 times；
Gap is 1. Gap is 2. Gap is 3. Gap is 4.
0:55 1:05 0:55 0:30
4) for three-roller Stress control in 20bar, gap condition is carried out as follows rolling, rolling 1 time；
Gap is 1. Gap is 2. Gap is 3. Gap is 4.
0:35 0:30 0:25 0:20
The slurry form that rolling finishes is in light grey body of paste, has preferable mobility, fineness≤10 μm, and viscosity is 100±5kcps。
Embodiment 2
The various raw material of balance precise for being 0.01g with accuracy：
Step 1：
Glass dust 35g is weighed, titanium valve 30g (being surface-treated before using) is stirred for uniformly；
Step 2：
Weigh 400g micro silver powder A and 200g micro silver powder B, 50g micro silver powder C and pour into three kinds of silver powder in agitator and halve It is even；
Step 3：
Weigh organic bond 300g, diluent 25g, additive 25g add jointly in agitator with silver powder in step 2 30min is mixed again；
Step 4：
Three-roll grinder is started, rolling is carried out as follows：
1) three-roller Stress control is carried out as follows in 20bar, gap condition, and well mixed material is added on three-roller Premix, time are 15min or so.
Gap is 1. Gap is 2. Gap is 3. Gap is 4.
1:15 1:30 1:10 1:15
2) for three-roller Stress control in 10bar, gap condition is carried out as follows rolling, rolling 2 times.
Gap is 1. Gap is 2. Gap is 3. Gap is 4.
1:15 1:30 1:10 1:15
3) for three-roller Stress control in 20bar, gap condition is carried out as follows rolling, rolling 2 times.
Gap is 1. Gap is 2. Gap is 3. Gap is 4.
0:55 1:05 0:55 0:30
4) for three-roller Stress control in 20bar, gap condition is carried out as follows rolling, rolling 1 time.
Gap is 1. Gap is 2. Gap is 3. Gap is 4.
0:35 0:30 0:20 0:25
The slurry form that rolling finishes is in light grey body of paste, has preferable mobility, fineness≤10 μm, and viscosity is 105±5kcps。
Embodiment 3
The various raw material of balance precise for being 0.01g with accuracy：
Step 1：
Glass dust 40g is weighed, titanium valve 15g (being surface-treated before using) is stirred for uniformly；
Step 2：
Weigh 350g micro silver powder A and 200g micro silver powder B, 50g micro silver powder C and pour into three kinds of silver powder in agitator and halve It is even；
Step 3：
Weigh organic bond 300g, diluent 35g, additive 10g add jointly in agitator with silver powder in step 2 30min is mixed again；
Step 4：
Three-roll grinder is started, rolling is carried out as follows：
1) three-roller Stress control is carried out as follows in 20bar, gap condition, and well mixed material is added on three-roller Premix, time are 10min or so.
Gap is 1. Gap is 2. Gap is 3. Gap is 4.
1:15 1:30 1:10 1:15
2) for three-roller Stress control in 10bar, gap condition is carried out as follows rolling, rolling 2 times.
Gap is 1. Gap is 2. Gap is 3. Gap is 4.
1:15 1:30 1:10 1:15
3) for three-roller Stress control in 20bar, gap condition is carried out as follows rolling, rolling 2 times.
Gap is 1. Gap is 2. Gap is 3. Gap is 4.
0:55 1:15 0:55 0:30
4) for three-roller Stress control in 20bar, gap condition is carried out as follows rolling, rolling 1 time.
The slurry form that rolling finishes is in light grey body of paste, has preferable mobility, fineness≤10 μm, viscosity 95 ±5kcps。
After the stable 12h of the slurry prepared, the slurry is obtained after crossing 300 eye mesh screens, is printed simultaneously in pressure sensitive substrate Dry at 120-150 DEG C, sintered under 400-480 DEG C of low temperature, finally carry out performance detection.
Product and test after the glass dust drying ball milling prepared；
Granularity and molten state test：It it is 3 μm with laser particle analyzer test granularity；The powder after ball milling is taken to be put into aluminum oxide The sintering experiment under different temperatures is carried out in crucible, observes its molten state (powder almost all after 480 DEG C of sintering 10min Fusing, shows smooth glass surface after cooling).
A kind of high performance pressure sensitive silver paste is invented, this silver paste sintering temperature is between 400-480 DEG C, and the silver paste can be made Used to substitute high content silver paste, base metal slurry (copper slurry, aluminium paste, nickel slurry etc.) can be coated on the silver paste top layer.

Claims (10)

1. a kind of low cost low temperature sinters piezoresistor silver paste, it is characterised in that in terms of mass fraction, including：Micro silver powder A 30~70, micro silver powder B 20~30, micro silver powder C 5~20, glass dust 2~6, titanium valve 1~3, nickel powder 1~3, organic diluent 1 ~15, organic bond 1~15.
2. a kind of low cost low temperature sintering piezoresistor silver paste according to claim 1, it is characterised in that described Micro silver powder A particle diameter is 0.5~2.5 μm, and micro silver powder B granularity is 1.0~4.8 μm, and micro silver powder C granularity is 0.5~2.0 μ m。
3. a kind of low cost low temperature sintering piezoresistor silver paste according to claim 1, it is characterised in that described Micro silver powder A particle diameter is 1 μm, and micro silver powder B granularity is 2 μm, and micro silver powder C granularity is 1 μm.
4. a kind of low cost low temperature sintering piezoresistor silver paste according to claim 1, it is characterised in that described Glass dust is by Bi2O3、CaO、SrO、ZnO、B2O3、SnO、P2O5、V2O5、K2O presses 40~65wt%, 6-10wt%, 6~ 10wt%, 4~10wt%, 5~17wt%, 4-7wt%, 1~5wt%, 1~5wt%, 1~3wt% ratio mixing after Sintered at 1100~1400 DEG C, water quenching, crushing, ball milling obtain.
5. a kind of low cost low temperature sintering piezoresistor silver paste according to claim 1, it is characterised in that described Organic bond is in terms of mass fraction, and 10~35 parts of small molecule celluloses, 2~5 parts of saturated fatty acids, 1-5 parts are organically-modified to be added Add agent, 60~90 parts of organic solvent compositions.
6. a kind of low cost low temperature sintering piezoresistor silver paste according to claim 1, it is characterised in that described Organic diluent is diethylene glycol ether, butyl glycol ether, butyl carbitol, n-butanol, cyclohexanol, ether, petroleum ether, acetic acid Butyl ester, terebinthine several mixed liquors.
7. a kind of low cost low temperature sinters piezoresistor silver paste preparation method for material, it is characterised in that including,
Step 1：The preparation of glass dust：
Powder configures and sintering：Bi2O3、CaO、SrO、ZnO、B2O3、SnO、P2O5、V2O5、K2O presses 40~65wt%, 6- 10wt%, 6~10wt%, 4~10wt%, 5~17wt%, 4-7wt%, 1~5wt%, 1~5wt%, 1~3wt% ratio After mixing 25min is sintered at 1100~1400 DEG C；
Subsequent treatment：Above-mentioned mixing object is cooled to 680 DEG C of progress water quenchings, the Primary product after water quenching is divided Sieve, 15-25 μm of little particle is crushed to pulverizer, then according to real needs ball mill under aqueous medium existence condition Carry out the processing of thinner grade, 3 μm of particle diameter ＜；
Transition temperature is produced at 345~380 DEG C by above-mentioned step, and the pressure-sensitive slurry of low temperature that softening point is 400~485 DEG C is used Glass dust；
Step 2：The preparation of organic bond：
10~35 parts of small molecule celluloses, 2~5 parts of saturated fatty acids, 60~90 parts of organic solvent compositions；First to glass reaction kettle In give certain mixing speed at 75~95 DEG C added with solvent, temperature control, be then slowly added into cellulose and saturated fat Fat acid, makes it fully dissolve, dissolution time is 12~22h；
Step 3, the preparation scheme of slurry：
By mass fraction：Micro silver powder A 30~70, micro silver powder B 20~30, micro silver powder C 5~20, glass dust 2~6, titanium valve 1~ 3rd, additive 1~3, organic diluent 1~15, the various materials of the precise of organic bond 1~15, and be stirred for uniformly；
Step 4：
By material mixed in step 3, rolling, slitting part carry out rolling on three-roller so that and mixture is in uniform paste, Obtain silver paste.
8. a kind of low cost low temperature sintering piezoresistor silver paste preparation method for material according to claim 7, its feature exist In the condition of rolling is respectively on described three-roller, 1. condition one is 1 in 20bar, gap for three-roller Stress control:15, 2. gap is 1:30,3. gap is 1:10,4. gap is 1:15, well mixed material is added on three-roller and premixed, the time For 10min or so；
Then three-roller Stress control is descended in this gap in 10bar, rolling 2 times；
1. condition two is 0 in 20bar, gap for three-roller Stress control:55,2. gap is 1:15,3. gap is 0:55, gap 4. for 0:30, rolling 2 times；
1. condition three is 0 in 20bar, gap for three-roller Stress control:35,2. gap is 0:30,3. gap is 0:25, gap 4. for 0:20；
The slurry form that rolling finishes is in light grey body of paste, has a preferable mobility, fineness≤10 μm, and viscosity is 95 ± 5kcps。
9. a kind of low cost low temperature sintering piezoresistor silver paste preparation method for material according to claim 7, its feature exist In the particle diameter of the micro silver powder A is 0.8~2.5 μm, and the granularity that micro silver powder B granularity is 1.5~4.0 μm of micro silver powder C is 0.2 ~1.2 μm.
10. a kind of low cost low temperature sintering piezoresistor silver paste preparation method for material according to claim 7, the rolling During micro silver powder C and titanium valve addition manner be during be slowly added to.
CN201711003354.1A 2017-10-24 2017-10-24 A kind of low cost low temperature sintering piezoresistor silver paste and preparation method thereof Active CN107799199B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108899108A (en) * 2018-06-06 2018-11-27 彩虹集团新能源股份有限公司 A kind of low temperature touch screen printing silver paste and preparation method thereof
CN109545423A (en) * 2018-11-01 2019-03-29 上海匡宇科技股份有限公司 Electrode of solar battery silver paste composition
CN115910509A (en) * 2022-11-11 2023-04-04 淄博中领电子有限公司 Surface-junction type piezoresistor disc, preparation process thereof and electromagnetic pollution absorption device

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Publication number Priority date Publication date Assignee Title
CN102768872A (en) * 2012-06-29 2012-11-07 彩虹集团电子股份有限公司 Lead-free environment friendly silver paste for piezoresistor and preparation method thereof
CN103854718A (en) * 2012-12-03 2014-06-11 西北稀有金属材料研究院 Solar cell front electrode slurry material and preparation method thereof
CN104123977A (en) * 2014-06-30 2014-10-29 彩虹集团电子股份有限公司 Annular piezoresistor silver paste, preparation method and application thereof
CN107258002A (en) * 2015-02-27 2017-10-17 大州电子材料 Silver paste composition, using its formed solar cell preceding electrode and use its solar cell

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102768872A (en) * 2012-06-29 2012-11-07 彩虹集团电子股份有限公司 Lead-free environment friendly silver paste for piezoresistor and preparation method thereof
CN103854718A (en) * 2012-12-03 2014-06-11 西北稀有金属材料研究院 Solar cell front electrode slurry material and preparation method thereof
CN104123977A (en) * 2014-06-30 2014-10-29 彩虹集团电子股份有限公司 Annular piezoresistor silver paste, preparation method and application thereof
CN107258002A (en) * 2015-02-27 2017-10-17 大州电子材料 Silver paste composition, using its formed solar cell preceding electrode and use its solar cell

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108899108A (en) * 2018-06-06 2018-11-27 彩虹集团新能源股份有限公司 A kind of low temperature touch screen printing silver paste and preparation method thereof
CN109545423A (en) * 2018-11-01 2019-03-29 上海匡宇科技股份有限公司 Electrode of solar battery silver paste composition
CN115910509A (en) * 2022-11-11 2023-04-04 淄博中领电子有限公司 Surface-junction type piezoresistor disc, preparation process thereof and electromagnetic pollution absorption device

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