CN104575887B - A kind of patch type varistor low temperature diffusion slurry and preparation method thereof - Google Patents
A kind of patch type varistor low temperature diffusion slurry and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of patch type varistor low temperature diffusion slurry and its application.The slurry is mainly made of 70% ~ 80% composite nano-powder of percentage by weight and 20% ~ 30% organic carrier；The composite nano-powder is to be made by two water zinc acetates, boric acid, nine water aluminum nitrates, yttrium nitrate hexahydrate, tetra-n-butyl titanate, ethanol, acetic acid raw material by wet chemistry method.The diffusion slurry is by silk-screen printing in the multi-terminal patch type varistor medium membrance electrode periphery for having printed interior electrode, then by the drying of medium diaphragm, lamination, dry bar, the coating of constant temperature isostatic pressing, dumping, sintering, termination electrode, again drying, multi-terminal patch type varistor is made after silver ink firing, it can effectively solve the problems, such as to disturb between terminal and terminal, shorten interelectrode spacing distance in different port, so as to further reduce small product size.
Description
Technical field
The present invention relates to a kind of patch type varistor low temperature diffusion slurry and its preparation side, belong to electronics member device
Part slurry preparation field.
Background technology
Patch type Zinc-oxide piezoresistor is widely used on the power circuit of ultralight, ultra-thin complete machine,
Protected for surge, electrostatic, electromagnetic interference etc..Patch type varistor is compared with traditional wafer-type varistor at present, tool
Have the advantages of small, voltage is low, be widely used in portable set, but patch type Zinc-oxide piezoresistor discharge capacity and
Energy tolerance is also there are a certain distance compared with traditional wafer-type varistor, and in recent years, scientific research personnel is also constantly
Exploitation and improvement material prescription and technique, such as multilayer chip varistors and its manufacture method, Patent No.
200610062048.0 a kind of laminated voltage-sensitive resistor array, Patent No. 201110006114.3, a kind of lamination sheet type are pressure-sensitive
Resistor network and preparation method thereof, Patent No. 200910109186.3, a kind of stacking slice type piezoresistor and its manufacturer
Method, Patent No. 200710075892.1, a kind of low-temperature sintering chip Zinc-oxide piezoresistor and preparation method thereof, Patent No.
201310732238.9 a kind of multilayer chip varistor porcelain and resulting product, Patent No. 200910213815.7,
Method for preparing sheet type multilayer zinc oxide pressure-sensitive electric resistance ceramic powder, Patent No. 200710077136.2, the performance of product obtain
It is significantly increased, but in SMD multi-terminal patch type varistor module internals, a certain terminal occurs overvoltage surge and shows
As producing interference to terminals of adjacent sometimes, therefore also need to the prior art and technique is constantly improved.
The content of the invention
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, there is provided a kind of patch type varistor low temperature
Slurry is spread, diffusion slurry is screen printed onto outside the multi-terminal patch type varistor medium membrance electrode for having printed interior electrode
Part is enclosed, can effectively shield the interference phenomenon between terminals of adjacent, shortens interelectrode spacing distance in different port, from
And further reduce small product size.
To achieve these goals, this invention takes following technical solution：A kind of patch type varistor is expanded with low temperature
Slurry is dissipated, is mainly made of the raw material of following weight percentage：Composite nano-powder：Organic carrier is equal to 70% ~ 80%：20%~
30%；The composite nano-powder is prepared by the analysis pure raw material of following weight percent purity >=99%：Two water second
Sour zinc：Boric acid：Nine water aluminum nitrates：Yttrium nitrate hexahydrate：Tetra-n-butyl titanate：Ethanol：Acetic acid is equal to 5% ~ 12%：2%~5% ：20%~
25% ：30%~38% ：25%~35% ：1%~5% ：2%~8%；The organic carrier is by following mass percent purity >=98%
Analysis pure raw material be prepared：Ethyl cellulose：Dibutyl phthalate：Terpinol：Diethylene glycol monobutyl ether is equal to 10%
~15%：5%~10%：20%~30%：50% ~ 60%,.
The patch type varistor is with the preparation process of low temperature diffusion slurry：
（1）Boric acid is accurately weighed first to insert in beaker, is added deionized water, under 80 DEG C ~ 95 DEG C water-baths, is used glass bar
It is sufficiently stirred, is allowed to be completely dissolved, then sequentially add two water zinc acetates, nine water aluminum nitrates, yttrium nitrate hexahydrate, continuation does not stop to fill
Divide stirring, until being completely dissolved, form solution, be cooled to room temperature, then add tetra-n-butyl titanate, ethanol and second in the solution
Acid, continues to be sufficiently stirred 30 minutes ~ 60 minutes, forms Sol A；Wherein, two water zinc acetates, boric acid, nine water aluminum nitrates, six water nitre
Sour yttrium, tetra-n-butyl titanate, ethanol, acetic acid percentage by weight are 5% ~ 12%：2%~5% ：20%~25% ：30%~38% ：25%~
35% ：1%~5% ：2% ~ 8%, and deionized water, the weight ratio of boric acid are 20 ~ 50：1；
（2）Sol A is stirred continuously, and ammonium hydroxide is added dropwise dropwise so that and pH value reaches 7.5 ~ 8.5, is allowed to form gel B,
Rapid draing in 85 DEG C ~ 120 DEG C vacuum drying ovens, until drying completely, forms xerogel C；
（3）Then xerogel C is put into alumina crucible, alumina crucible is put into Muffle furnace, at 450 DEG C ~ 550 DEG C
Lower roasting, heats up 5 ~ 8 DEG C/min, when insulation 1 ~ 2 is small, with stove Temperature fall, that is, obtains composite granule D；
（4）Composite granule D is inserted in agate jar, adds zirconium ball, ethanol, when planetary type ball-milling 4 ~ 8 is small, rotating speed
100 ~ 150 revs/min, the then rapid draing in 120 DEG C ~ 140 DEG C baking ovens, until drying completely, obtains composite granule E；Its
In, zirconium ball, ethanol, composite granule weight ratio are 4 ~ 5：2~3：1；
（5）The composite granule E dried in step 4 is pulverized, is inserted in beaker, adds deionized water, stirs 10 ~ 20 points
Clock, forms suspension F, and then ultrasonic wave that the beaker equipped with suspension F is put into 600 ~ 1200W of frequency 20 ~ 25kHz power is thin
Disperseed on born of the same parents' pulverizer, jitter time 3 ~ 5 minutes, 1 ~ 2 second off time；
（6）After scattered, 3 ~ 8 minutes are stood, upper suspension G and lower sediment thing L is obtained, then takes upper suspension
G, is inserted in tophan box, is centrifuged 4 ~ 5 minutes on centrifuge, 4000 ~ 6000 revs/min of centrifugal speed, is taken out, by upper strata
Clear liquid H is collected, spare, the then drying in 65 DEG C ~ 85 DEG C vacuum drying ovens by the powder J of lower floor's sedimentation, until drying completely, so
Pulverized afterwards in agate mortar, you can obtain composite nano-powder K；
（7）By step（6）Middle lower sediment thing L adds step（6）The supernatant liquor H of middle collection, then proceed to stirring 10 ~
20 minutes, suspension M is formed, the ultrasonic wave that the beaker equipped with suspension M is put into 600 ~ 1200W of frequency 20 ~ 25kHz power is thin
Disperseed on born of the same parents' pulverizer, jitter time 3 ~ 5 minutes, 1 ~ 2 second off time, repeat step（6）, continue collection and obtain nanometer
Composite granule K；
（8）Repeat step again（7）3 ~ 5 times, until the composite nano-powder K being collected into is seldom, then will be remaining under
Layer sediment drying, as composite granule D, repeat step（4）~ step（8）, constantly collect composite nano-powder K；
（9）Pure raw material ethyl cellulose, dibutyl phthalate, terpinol, diethylene glycol monobutyl ether will be analyzed by weight
Measure percentage ethyl cellulose：Dibutyl phthalate：Terpinol：Diethylene glycol monobutyl ether is equal to 10% ~ 15%：5%~10%：
20%~30%：Ethyl cellulose room temperature, is first dissolved in diethylene glycol monobutyl ether by 50% ~ 60% precise, add terpinol and
Dibutyl phthalate, be thoroughly mixed 3 ~ 4 it is small when, that is, be made organic carrier；
（10）By step（6）~ step（8）Obtained composite nano-powder K and step（9）Obtained organic carrier presses quality
Percentage：Composite nano-powder：Organic carrier is equal to 70% ~ 80%：20% ~ 30%, precise, is inserted in agate jar, is added
Enter zirconium ball, when planetary type ball-milling 4 ~ 8 is small, 100 ~ 150 revs/min of rotating speed, then takes out, mixed slurry is put into three-roll grinder
Be fully ground rolling 3 ~ 4 it is small when, that is, obtain a kind of patch type varistor low temperature diffusion slurry；Wherein, zirconium ball, slurry feedstock
Weight ratio is 4 ~ 6：1.
The present invention of above-mentioned measure is taken to has the following advantages：
（1）The present invention takes nano-powder technology of preparing to prepare composite nano-powder, will as the main body of diffusion slurry
Diffusion slurry is screen printed onto the multi-terminal patch type varistor medium membrance electrode periphery for having printed interior electrode, and with
Medium diaphragm realizes≤900 DEG C low temperature co-fired, realizes effective diffusion of composite nano-powder, can effectively solve terminal and end
The problem of being disturbed between son, shortens interelectrode spacing distance in different port, so as to further reduce small product size.
（2）Preparation method technique of the present invention is simple.
Embodiment
Embodiment 1
A kind of patch type varistor follows these steps to carry out with low temperature diffusion slurry preparation method：
1. accurately weighing 2.3193 grams of boric acid first, insert in 250 milliliters of beakers, add 100 ml deionized waters,
Under 95 DEG C of water-baths, be sufficiently stirred with glass bar, be allowed to be completely dissolved, then sequentially add 8.2343 gram of two water zinc acetate,
21.1065 gram of nine water aluminum nitrate, 32.3399 grams of yttrium nitrate hexahydrates, continuation does not stop to be sufficiently stirred, until being completely dissolved, is formed molten
Liquid, is cooled to room temperature, and then adds 31 grams of tetra-n-butyl titanates, 2 grams of ethanol and 3 grams of acetic acid in the solution, continues to be sufficiently stirred
30 minutes, form Sol A；
2. being stirred continuously, and ammonium hydroxide is added dropwise dropwise so that pH value reaches 7.5 ~ 8.5, is allowed to form gel B, true at 85 DEG C
Rapid draing in empty baking oven, until drying completely, forms xerogel C；
3. then xerogel C is put into alumina crucible, alumina crucible is then put into Muffle furnace, at 450 DEG C
Roasting, heats up 5 DEG C/min, when insulation 1 is small, with stove Temperature fall, that is, obtains composite granule D；
4. composite granule D is inserted in agate jar, 200 grams of zirconium balls, 90 grams of ethanol are added, planetary type ball-milling 8 is small
When, 150 revs/min of rotating speed, the then rapid draing in 120 DEG C of baking ovens, until drying completely, obtains composite granule E；
5. the composite granule E dried in step 4 is pulverized, insert in beaker, add deionized water, stir 10 minutes, shape
Into suspension F, then the beaker equipped with suspension F is put into the ultrasonic cell disruptor of 20 ~ 25kHz of frequency, power 800W
On disperseed, 3 minutes ultrasonic disperse time, 1 second off time；
6. after scattered, 6 minutes are stood, upper suspension G and lower sediment thing L is obtained, then takes upper suspension G,
Insert in tophan box, centrifuged 4 minutes on centrifuge, 4000 revs/min of centrifugal speed, take out, supernatant liquor H is received
Collection, spare, the then drying in 85 DEG C of vacuum drying ovens by the powder J of lower floor's sedimentation, until drying completely, then in agate mortar
In pulverize, you can obtain composite nano-powder K；
7. lower sediment thing L in step 6 to be added in step 6 to the supernatant liquor H collected, stirring 10 minutes is then proceeded to,
Suspension M is formed, the beaker equipped with suspension M is then put into 20 ~ 25kHz of frequency, the supersonic cell of power 800W crushes
Disperseed on machine, jitter time 3 minutes, 1 second off time, repeat step 6, continues collection and obtain composite nano-powder K；
8. again repeat step 7 three times, until the composite nano-powder K being collected into is seldom, then by remaining lower floor
Sediment is dried, and as composite granule D, 4 ~ step 8 of repeat step, constantly collects composite nano-powder K；
9. accurate weigh 12 grams of analysis pure raw material ethyl cellulose, 8 grams of dibutyl phthalate, 25 grams of terpinol, two
Ethyl cellulose room temperature, is first dissolved in diethylene glycol monobutyl ether by 55 grams of ethylene glycol monobutyl ether, adds terpinol and adjacent benzene two
Formic acid dibutyl ester, be thoroughly mixed 4 it is small when, that is, be made organic carrier；
10. it is accurate weigh have made from composite nano-powder K made from 30 grams of step 6 ~ steps 8 and 12 grams of steps 9 it is airborne
Body, is inserted in agate jar, adds 250 grams of zirconium balls, and when planetary type ball-milling 8 is small, 100 revs/min of rotating speed, then takes out, will
Mixed slurry be put into three-roll grinder be fully ground rolling 3 it is small when, you can obtain a kind of patch type varistor low temperature diffusion
Slurry.
Embodiment 2
A kind of patch type varistor follows these steps to carry out with low temperature diffusion slurry preparation method：
1. accurately weighing 3.4526 grams of boric acid first, insert in 250 milliliters of beakers, add 100 ml deionized waters,
Under 80 DEG C of water-baths, be sufficiently stirred with glass bar, be allowed to be completely dissolved, then sequentially add 5.8596 gram of two water zinc acetate,
23.6378 gram of nine water aluminum nitrate, 31.05 grams of yttrium nitrate hexahydrates, continuation does not stop to be sufficiently stirred, until being completely dissolved, forms solution,
It is cooled to room temperature, then adds 27 grams of tetra-n-butyl titanates, 5 grams of ethanol and 4 grams of acetic acid in the solution, continue to be sufficiently stirred 30 points
Clock, forms Sol A；
2. being stirred continuously, and ammonium hydroxide is added dropwise dropwise so that pH value reaches 7.5 ~ 8.5, is allowed to form gel B, at 120 DEG C
Rapid draing in vacuum drying oven, until drying completely, forms xerogel C；
3. then xerogel C is put into alumina crucible, alumina crucible is then put into Muffle furnace, at 450 DEG C
Roasting, heats up 8 DEG C/min, when insulation 2 is small, with stove Temperature fall, that is, obtains composite granule D；
4. composite granule D is inserted in agate jar, 200 grams of zirconium balls, 90 grams of ethanol are added, planetary type ball-milling 8 is small
When, 100 revs/min of rotating speed, the then rapid draing in 140 DEG C of baking ovens, until drying completely, obtains composite granule E；
5. the composite granule E dried in step 4 is pulverized, insert in beaker, add deionized water, stir 20 minutes, shape
Into suspension F, then the beaker equipped with suspension F is put into the ultrasonic cell disruptor of 20 ~ 25kHz of frequency, power 800W
On disperseed, 3 minutes ultrasonic disperse time, 1 second off time；
6. after scattered, 6 minutes are stood, upper suspension G and lower sediment thing L is obtained, then takes upper suspension G,
Insert in tophan box, centrifuged 5 minutes on centrifuge, 6000 revs/min of centrifugal speed, take out, supernatant liquor H is received
Collection, spare, the then drying in 65 DEG C of vacuum drying ovens by the powder J of lower floor's sedimentation, until drying completely, then in agate mortar
In pulverize, you can obtain composite nano-powder K；
7. lower sediment thing L in step 6 to be added in step 6 to the supernatant liquor H collected, stirring 20 minutes is then proceeded to,
Suspension M is formed, the beaker equipped with suspension M is then put into 20 ~ 25kHz of frequency, the supersonic cell of power 800W crushes
Disperseed on machine, jitter time 3 minutes, 1 second off time, repeat step 6, continues collection and obtain composite nano-powder K；
8. repeat step 7 five times again, until the composite nano-powder K being collected into is seldom, then by remaining lower floor
Sediment is dried, and as composite granule D, 4 ~ step 8 of repeat step, constantly collects composite nano-powder K；
9. accurate weigh 15 grams of analysis pure raw material ethyl cellulose, 5 grams of dibutyl phthalate, 30 grams of terpinol, two
Ethyl cellulose room temperature, is first dissolved in diethylene glycol monobutyl ether by 60 grams of ethylene glycol monobutyl ether, adds terpinol and adjacent benzene two
Formic acid dibutyl ester, be thoroughly mixed 3 it is small when, that is, be made organic carrier；
10. it is accurate weigh have made from composite nano-powder K made from 30 grams of step 6 ~ steps 8 and 12 grams of steps 9 it is airborne
Body, is inserted in agate jar, adds 250 grams of zirconium balls, and when planetary type ball-milling 4 is small, 150 revs/min of rotating speed, then takes out, will
Mixed slurry be put into three-roll grinder be fully ground rolling 3 it is small when, you can obtain a kind of patch type varistor low temperature diffusion
Slurry.
Embodiment 3
A kind of patch type varistor follows these steps to carry out with low temperature diffusion slurry preparation method：
1. accurately weighing 3.054 grams of boric acid first, insert in 250 milliliters of beakers, 100 ml deionized waters are added, 90
Under DEG C water-bath, it is sufficiently stirred with glass bar, is allowed to be completely dissolved, then sequentially add 10.45 gram of two water zinc acetate, 24.6543
Gram nine water aluminum nitrates, 19.8417 grams of yttrium nitrate hexahydrates, continuation does not stop to be sufficiently stirred, until being completely dissolved, forms solution, cooling
To room temperature, 34 grams of tetra-n-butyl titanates, 3 grams of ethanol and 5 grams of acetic acid are then added in the solution, continue to be sufficiently stirred 60 minutes,
Form Sol A；
2. being stirred continuously, and ammonium hydroxide is added dropwise dropwise so that pH value reaches 7.5 ~ 8.5, is allowed to form gel B, true at 85 DEG C
Rapid draing in empty baking oven, until drying completely, forms xerogel C；
3. then xerogel C is put into alumina crucible, alumina crucible is then put into Muffle furnace, at 500 DEG C
Roasting, heats up 5 DEG C/min, when insulation 2 is small, with stove Temperature fall, that is, obtains composite granule D；
4. composite granule D is inserted in agate jar, 200 grams of zirconium balls, 90 grams of ethanol are added, planetary type ball-milling 6 is small
When, 150 revs/min of rotating speed, the then rapid draing in 120 DEG C of baking ovens, until drying completely, obtains composite granule E；
5. the composite granule E dried in step 4 is pulverized, insert in beaker, add deionized water, stir 10 minutes, shape
Into suspension F, then the beaker equipped with suspension F is put into the ultrasonic cell disruptor of 20 ~ 25kHz of frequency, power 800W
On disperseed, 4 minutes ultrasonic disperse time, 2 seconds off times；
6. after scattered, 8 minutes are stood, upper suspension G and lower sediment thing L is obtained, then takes upper suspension G,
Insert in tophan box, centrifuged 5 minutes on centrifuge, 4000 revs/min of centrifugal speed, take out, supernatant liquor H is received
Collection, spare, the then drying in 65 DEG C of vacuum drying ovens by the powder J of lower floor's sedimentation, until drying completely, then in agate mortar
In pulverize, you can obtain composite nano-powder K；
7. lower sediment thing L in step 6 to be added in step 6 to the supernatant liquor H collected, stirring 10 minutes is then proceeded to,
Suspension M is formed, the beaker equipped with suspension M is then put into 20 ~ 25kHz of frequency, the supersonic cell of power 800W crushes
Disperseed on machine, jitter time 5 minutes, 2 seconds off times, repeat step 6, continues collection and obtain composite nano-powder K；
, then will be remaining until the composite nano-powder K being collected into is seldom 8. repeat step 7 three to five times again
Lower sediment thing is dried, and as composite granule D, 4 ~ step 8 of repeat step, constantly collects composite nano-powder K；
9. it is accurate weigh 10 grams of analysis pure raw material ethyl cellulose, 10 grams of dibutyl phthalate, 30 grams of terpinol,
Ethyl cellulose room temperature, is first dissolved in diethylene glycol monobutyl ether by 50 grams of diethylene glycol monobutyl ether, adds terpinol and adjacent benzene
Dibutyl carboxylic acid, be thoroughly mixed 3 it is small when, that is, be made organic carrier；
10. it is accurate weigh have made from composite nano-powder K made from 30 grams of step 6 ~ steps 8 and 12 grams of steps 9 it is airborne
Body, is inserted in agate jar, adds 250 grams of zirconium balls, and when planetary type ball-milling 4 is small, 100 revs/min of rotating speed, then takes out, will
Mixed slurry be put into three-roll grinder be fully ground rolling 3 it is small when, you can obtain a kind of patch type varistor low temperature diffusion
Slurry.
Diffusion slurry prepared by embodiment 1 ~ 3 is screen printed onto to the pressure-sensitive electricity of multi-terminal patch type for having printed interior electrode
Hinder medium membrance electrode periphery, then by the drying of medium diaphragm, lamination, baking bar, constant temperature isostatic pressing, dumping ,≤900
DEG C the low temperature co-fired effective diffusion for realizing composite nano-powder fixed position, then termination electrode coating, again after drying, silver ink firing
Multi-terminal patch type varistor is made, can effectively solve the problems, such as to disturb between terminal and terminal, shortens in different port
Interelectrode spacing distance, so as to further reduce small product size.
Claims (2)
1. a kind of patch type varistor low temperature diffusion slurry, it is characterised in that the low temperature diffusion slurry is mainly by following
The raw material composition of percentage by weight：Composite nano-powder K：Organic carrier is equal to 70% ~ 80%：20%~30%；Described is nano combined
Powder K is the analysis pure raw material preparation by following weight percentage, purity >=99%：Two water zinc acetates：Boric acid：Nine water aluminum nitrates：
Yttrium nitrate hexahydrate：Tetra-n-butyl titanate：Ethanol：Acetic acid is equal to 5% ~ 12%：2%~5% ：20%~25% ：30%~38% ：25%~35%
：1%~5% ：2%~8%；The organic carrier is prepared by the analysis pure raw material of following weight percentage, purity >=98%：
Ethyl cellulose：Dibutyl phthalate：Terpinol：Diethylene glycol monobutyl ether is equal to 10% ~ 15%：5%~10%：20%~30%：
50%~60%。
2. a kind of preparation method of patch type varistor low temperature diffusion slurry according to claim 1, its feature exist
In the preparation method comprises the concrete steps that：
（1）Boric acid is accurately weighed first to insert in beaker, adds deionized water, it is abundant with glass bar under 80 DEG C ~ 95 DEG C water-baths
Stirring, is allowed to be completely dissolved, and then sequentially adds two water zinc acetates, nine water aluminum nitrates, yttrium nitrate hexahydrate, and continuation does not stop fully to stir
Mix, until being completely dissolved, form solution, be cooled to room temperature, then add tetra-n-butyl titanate, ethanol and acetic acid in the solution,
Continue to be sufficiently stirred 30 minutes ~ 60 minutes, form Sol A；Wherein, two water zinc acetates, boric acid, nine water aluminum nitrates, six water nitric acid
Yttrium, tetra-n-butyl titanate, ethanol, acetic acid percentage by weight are 5% ~ 12%：2%~5% ：20%~25% ：30%~38% ：25%~35%
：1%~5% ：2% ~ 8%, and deionized water, the weight ratio of boric acid are 20 ~ 50：1；
（2）It is stirred continuously, and ammonium hydroxide is added dropwise dropwise so that pH value reaches 7.5 ~ 8.5, is allowed to form gel B, at 85 DEG C ~ 120 DEG C
Rapid draing in vacuum drying oven, until drying completely, forms xerogel C；
（3）Then xerogel C is put into alumina crucible, alumina crucible is then put into Muffle furnace, at 450 DEG C ~ 550 DEG C
Lower roasting, programming rate during from room temperature to 450 DEG C ~ 550 DEG C is 5 ~ 8 DEG C/min, when insulation 1 ~ 2 is small, with stove Temperature fall,
Obtain composite granule D；
（4）Composite granule D is inserted in agate jar, adds zirconium ball, ethanol, when planetary type ball-milling 4 ~ 8 is small, rotating speed 100 ~
150 revs/min, the then rapid draing in 120 DEG C ~ 140 DEG C baking ovens, until drying completely, obtains composite granule E；Wherein, zirconium
Ball, ethanol, composite granule D weight ratios are 4 ~ 5：2~3：1；
（5）By step（4）The composite granule E of middle drying pulverizes, and inserts in beaker, adds deionized water, stirs 10 ~ 20 minutes,
Suspension F is formed, then the beaker equipped with suspension F is put into the supersonic cell of 20 ~ 25kHz of frequency, 600 ~ 1200W of power
Disperseed on pulverizer, jitter time 3 ~ 5 minutes, 1 ~ 2 second off time；
（6）After scattered, 3 ~ 8 minutes are stood, upper suspension G and lower sediment thing L is obtained, then takes upper suspension G, put
Enter in tophan box, centrifuged 4 ~ 5 minutes on centrifuge, 4000 ~ 6000 revs/min of centrifugal speed, taken out, by supernatant liquor
H is collected, spare, the then drying in 65 DEG C ~ 85 DEG C vacuum drying ovens by the powder J of lower floor's sedimentation, until drying completely, Ran Hou
Pulverized in agate mortar, you can obtain composite nano-powder K；
（7）By step（6）Middle lower sediment thing L adds step（6）The supernatant liquor H of middle collection, then proceedes to 10 ~ 20 points of stirring
Clock, forms suspension M, then the beaker equipped with suspension M is put into the ultrasonic wave of 20 ~ 25kHz of frequency power, 600 ~ 1200W
Disperseed on cell disruptor, jitter time 3 ~ 5 minutes, 1 ~ 2 second off time, repeat step（6）, continue collection and received
Rice composite granule K；
（8）Repeat step again（7）3 ~ 5 times, then remaining lower sediment thing is dried, as composite granule D, repeat step
（4）~ step（8）, collect composite nano-powder K；
（9）Will analysis pure raw material ethyl cellulose, dibutyl phthalate, terpinol, diethylene glycol monobutyl ether by weight hundred
Divide and compare ethyl cellulose：Dibutyl phthalate：Terpinol：Diethylene glycol monobutyl ether is equal to 10% ~ 15%：5%~10%：20%~
30%：Ethyl cellulose room temperature, is first dissolved in diethylene glycol monobutyl ether by 50% ~ 60% precise, adds terpinol and adjacent benzene
Dibutyl carboxylic acid, be thoroughly mixed 3 ~ 4 it is small when, that is, be made organic carrier；
（10）By step（6）~ step（8）Obtained composite nano-powder K and step（9）Obtained organic carrier presses quality percentage
Than：Composite nano-powder K：Organic carrier is equal to 70% ~ 80%：20% ~ 30%, precise, is inserted in agate jar, adds zirconium
Ball, when planetary type ball-milling 4 ~ 8 is small, 100 ~ 150 revs/min of rotating speed then takes out, and it is abundant that mixed slurry is put into three-roll grinder
When grinding rolling 3 ~ 4 is small, you can obtain a kind of patch type varistor low temperature diffusion slurry；Wherein, zirconium ball, slurry feedstock weight
Amount is than being 4 ~ 6：1, the slurry feedstock refers to composite nano-powder K and organic carrier.
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| US6372027B1 (en) * | 1999-05-31 | 2002-04-16 | Alfachimici S.P.A. | Process for promoting adhesion between an inorganic substrate and an organic polymer |
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| 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 |
| CN102208228A (en) * | 2011-01-17 | 2011-10-05 | 深圳市圣龙特电子有限公司 | Nickel-copper conductive paste for electronic component electrode and manufacturing technology thereof |
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