CN104308183A - Preparation method for flake silver powder for electronic paste - Google Patents
Preparation method for flake silver powder for electronic paste Download PDFInfo
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- CN104308183A CN104308183A CN201410577409.XA CN201410577409A CN104308183A CN 104308183 A CN104308183 A CN 104308183A CN 201410577409 A CN201410577409 A CN 201410577409A CN 104308183 A CN104308183 A CN 104308183A
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Abstract
The invention relates to a preparation method for flake silver powder for electronic paste, and belongs to the field of preparation of metal powder materials. The method comprises the following steps of (a) preparation of silver powder, (b) ball-milling, (c) primary surface modification and (d) secondary surface modification. The preparation method has the advantages that the flake silver powder is low in apparent density, large in specific surface area, high in dispersibility, large in coating area and low in filling amount; and the cost is greatly saved.
Description
Technical field
The invention belongs to the preparation field of metal powder material, be specifically related to a kind of preparation method of electric slurry flake silver powder.
Background technology
Flake silver powder is widely used in the fields such as electronic devices and components, integrated circuit, touch-screen, solar cell, display device, RF identification, electronic tag, it is the best conductive filler making the electronic products such as cryotronics slurry, electrically conductive ink, electrically-conducting paint, electromagnetic screen coating, conductive rubber, conductive plastics, apply in the electronics industry, microelectronics (small-power, low-voltage) and electric (high power, high voltage) two aspects can be divided into.Along with the development trend that civil electrical is light, little, thin, the use in microelectronics will become topmost in.And the application form of silver in microelectronics industry is thin layer, come from the requirement of light, little, the thin and cost of e-machine, realize thin layer technology main at present and comprise the technology of thick film ink technology, electroplating technology and other physics aspect (such as, gas deposition, sputtering etc.), wherein thick film ink technology due to small investment, quantize to produce easily, be applicable to various base material, membrance casting condition is simple, becomes the main mode realizing conductive film layer.And the core of thick-film technique is exactly silver conductive paste.Silver powder purity in electrocondution slurry is wanted high (more than 99.95%), should have enough large specific area and easily disperse, preferably laminated structure, because flake powder is got horizontally in the coating, have larger area coverage.
A kind of fabulous dispersibility can be formed and can not form silver powder of the paste of suspension and preparation method thereof owing to being separated of having is provided in CN101386070B, this technique adopts ammoniacal liquor to make complexing agent, is prepared by the mode of adding reducing agent formalin (formaldehyde).In this kind of method preparation process, there are the following problems in meeting: be that complexing agent is more unstable with ammoniacal liquor, needs frequent adjust ph, and next is reducing agent with formalin, and its reaction speed is very fast, and the particle obtained is uneven.The silver powder granularity obtained is uneven, color is gloomy, poorly conductive.
A kind of novel silver powder and preparation method thereof is proposed in CN102133635B, adopt the preparation of liquid-phase reduction silver powder, the silver powder average grain diameter using this technique to prepare is at 0.5 ~ 4.0 micron, there is good crystal plane, dispersed, particle shape almost spherical, forms the conductive filler of required electrocondution slurry, has good filling characteristic and electric property than conventional silver powder for crystal silicon solar batteries front silver electrode.But silver powder tap density prepared by this technique is comparatively large, specific area is less, and sphericity is bad, and granularity is uneven.
Summary of the invention
The object of this invention is to provide a kind of preparation method of electric slurry flake silver powder, the flake silver powder apparent density of gained is little, and specific area is large.
The technical solution used in the present invention is a kind of preparation method of electric slurry flake silver powder, comprises the following steps:
The preparation of a, silver powder: get liquor argenti nitratis ophthalmicus, adds ascorbic acid solution and reacts, and filters, obtains even-grained ball shape silver powder; The weight ratio of described liquor argenti nitratis ophthalmicus and ascorbic acid solution is 1:1 ~ 1.5;
B, ball milling: described ball shape silver powder is placed in ball mill, add ball-milling medium, ball-milling additive and lubricant and carry out ball milling, filters, obtain the silver powder after ball milling;
C, one-time surface modification: the silver powder after described ball milling is added surface modifier I react >=20 minutes, filter, dry, obtain first time surface modification silver powder;
D, secondary surface modification: described first time surface modification silver powder is placed in ball mill, adds surface modifier II co-ground, get product.
Preferably, in described step a when adding ascorbic acid solution, slowly add while stirring, and add time≤15 minutes.
Preferably, the temperature of reacting in described step a is 15 DEG C ~ 25 DEG C, and the time of reaction is 10 ~ 20 minutes.
Preferably, in described step b during ball milling, be the ratio ball milling 2 ~ 8 hours of 10 ~ 50:1 in the weight ratio of ball and ball shape silver powder; Ball adopts single diameter to be that the ball of 4 ~ 20mm carries out; The speed of ball milling is 200 ~ 1000 revs/min.
Preferably, in described step b during ball milling, by the amount of per kilogram ball shape silver powder, add the lubricant of the ball-milling medium of 0.5 ~ 2L, the ball-milling additive of 5 ~ 30g and 4 ~ 40mL respectively.
Preferably, described ball-milling medium comprises absolute ethyl alcohol; Described ball-milling additive is selected from the one in zinc stearate, stearic acid, aluminum stearate, silica, dodecoic acid, hexadecanol or octadecyl alcolol, or their arbitrary proportion mixture; Described lubricant is selected from the one in glycerine, polyethylene glycol, terpinol or triethanolamine, or their arbitrary proportion mixture.
Preferably, in described step c, the addition of surface modifier I adds 0.5 ~ 3L by the silver powder weight after ball milling described in per kilogram; The temperature of drying is 50 DEG C ~ 70 DEG C.
Preferably, described surface modifier I is by the one in polyvinyl alcohol, polyvinylpyrrolidone, titanate coupling agent or silane coupler, or the water-soluble solution of their mixture, is mixed with the surface modifier I that concentration is 10 ~ 30g/L.
Preferably, when grinding in described steps d, in sphere diameter be 2 ~ 6mm ball with first time surface modification silver powder weight ratio be that the ratio of 1 ~ 10:1 grinds 2 ~ 10 hours, the rotating speed of grinding is 20 ~ 50 revs/min; The addition of surface modifier II by described in per kilogram first time surface modification silver powder weight add 2 ~ 10g; Described surface modifier II is selected from the one in OP-10, phenylpropyl alcohol triazole, modified silicone, neopelex or modified waxes powder, or their mixture.
The present invention also provides a kind of described preparation method the flake silver powder obtained.
Beneficial effect of the present invention is:
(1) present invention optimizes ball-milling technology, select high energy wet ball grinding to replace traditional dry method cylinder grinding, make the apparent density of the flake silver powder obtained less, and Ball-milling Time is only 1/5th of traditional Ball-milling Time.
(2) by carrying out twice modification to silver powder surface, improve dispersiveness and the floatability of silver powder, the flake silver powder finally obtained has that apparent density is little, specific area is large, good dispersion, the advantage that surface covered is large, amount of filling is few, has saved cost widely.
Detailed description of the invention
For making those skilled in the art understand production technology of the present invention and technique effect in detail, introduce application of the present invention and technique effect further with concrete production instance below.
Embodiment 1:
The preparation of a, silver powder: get the liquor argenti nitratis ophthalmicus that mass percent concentration is 25%, add mass percent concentration be 15% ascorbic acid solution react, when adding ascorbic acid solution, slowly add while stirring, and the time added is 15 minutes, react 15 minutes under the condition of 20 DEG C after having added, then filter, obtain even-grained ball shape silver powder; The weight ratio of described liquor argenti nitratis ophthalmicus and ascorbic acid solution is 1:1.25;
B, ball milling: be the ratio of 30:1 in the weight ratio of ball and ball shape silver powder, be placed in ball mill by described ball shape silver powder, and ball adopts single diameter to be that the ball of 10mm carries out; Press the amount of per kilogram ball shape silver powder again, the lubricant adding the ball-milling medium of 1L, 20g ball-milling additive and 20mL respectively carries out ball milling, and the time of ball milling is 6 hours, and the speed of ball milling is 600 revs/min, then filters, and obtains the silver powder after ball milling;
Wherein, ball-milling medium is absolute ethyl alcohol; Ball-milling additive is zinc stearate; Lubricant is glycerine.
C, one-time surface modification: add 2L surface modifier I by the weight of the silver powder after ball milling described in per kilogram, react 30 minutes, filters, then dry under the condition of 60 DEG C, obtains first time surface modification silver powder;
Wherein, surface modifier I is by polyvinyl alcohol deionized water dissolving, is mixed with the surface modifier that concentration is 20g/L.
D, secondary surface modification: in ball with first time surface modification silver powder weight ratio be the ratio of 5:1, described first time surface modification silver powder is placed in ball mill, wherein, the agate ball of ball to be diameter be 4mm.Add the amount of 8g surface modifier II again by per kilogram first time surface modification silver powder weight, add surface modifier II co-ground 8 hours, the rotating speed of grinding is 30 revs/min, gets product.Wherein, surface modifier II is OP-10.
Embodiment 2:
The preparation of a, silver powder: get the liquor argenti nitratis ophthalmicus that mass percent concentration is 20%, add mass percent concentration be 20% ascorbic acid solution react, when adding ascorbic acid solution, slowly add while stirring, and the time added is 10 minutes, react 20 minutes under the condition of 25 DEG C after having added, then filter, obtain even-grained ball shape silver powder; The weight ratio of described liquor argenti nitratis ophthalmicus and ascorbic acid solution is 1:1;
B, ball milling: be the ratio of 10:1 in the weight ratio of ball and ball shape silver powder, be placed in ball mill by described ball shape silver powder, and ball adopts single diameter to be that the ball of 20mm carries out; Press the amount of per kilogram ball shape silver powder again, the lubricant adding the ball-milling medium of 0.5L, 30g ball-milling additive and 4mL respectively carries out ball milling, and the time of ball milling is 2 hours, and the speed of ball milling is 1000 revs/min, then filters, and obtains the silver powder after ball milling;
Wherein, ball-milling medium is absolute ethyl alcohol; Ball-milling additive is made up of the component of following weight portion: zinc stearate 1 part, silica 1 part, dodecoic acid 1 part and octadecyl alcolol 1 part; Lubricant is made up of the component of following weight portion: glycerine 1 part, terpinol 1 part.
C, one-time surface modification: add 3L surface modifier I by the weight of the silver powder after ball milling described in per kilogram, react 20 minutes, filters, then dry under the condition of 70 DEG C, obtains first time surface modification silver powder;
Wherein, surface modifier I is by polyvinyl alcohol: the weight ratio of titanate coupling agent is after 1:1 mixing, with deionized water dissolving, is mixed with the surface modifier that concentration is 30g/L.
D, secondary surface modification: in ball with first time surface modification silver powder weight ratio be the ratio of 10:1, described first time surface modification silver powder is placed in ball mill, wherein, the agate ball of ball to be diameter be 2mm.Add the amount of 10g surface modifier II again by per kilogram first time surface modification silver powder weight, add surface modifier II co-ground 2 hours, the rotating speed of grinding is 50 revs/min, gets product.Wherein, surface modifier II is made up of the component of following weight portion: phenylpropyl alcohol triazole 1 part, modified silicone 1 part and 1 part, modified waxes powder.
Embodiment 3:
The preparation of a, silver powder: get the liquor argenti nitratis ophthalmicus that mass percent concentration is 25%, add mass percent concentration be 20% ascorbic acid solution react, when adding ascorbic acid solution, slowly add while stirring, and the time added is 12 minutes, react 10 minutes under the condition of 15 DEG C after having added, then filter, obtain even-grained ball shape silver powder; The weight ratio of described liquor argenti nitratis ophthalmicus and ascorbic acid solution is 1:1.5;
B, ball milling: be the ratio of 50:1 in the weight ratio of ball and ball shape silver powder, be placed in ball mill by described ball shape silver powder, and ball adopts single diameter to be that the ball of 4mm carries out; Press the amount of per kilogram ball shape silver powder again, the lubricant adding the ball-milling medium of 2L, 5g ball-milling additive and 40mL respectively carries out ball milling, and the time of ball milling is 8 hours, and the speed of ball milling is 200 revs/min, then filters, and obtains the silver powder after ball milling;
Wherein, ball-milling medium is absolute ethyl alcohol; Ball-milling additive is made up of the component of following weight portion: stearic acid 1 part, silica 1 part, dodecoic acid 1 part and hexadecanol 1 part; Lubricant is made up of the component of following weight portion: glycerine 1 part, terpinol 1 part and triethanolamine 1 part.
C, one-time surface modification: add 0.5L surface modifier I by the weight of the silver powder after ball milling described in per kilogram, react 35 minutes, filters, then dry under the condition of 50 DEG C, obtains first time surface modification silver powder;
Wherein, surface modifier I is by polyvinylpyrrolidone: the weight ratio of titanate coupling agent is after 1:1 mixing, with deionized water dissolving, is mixed with the surface modifier that concentration is 10g/L.
D, secondary surface modification: in ball with first time surface modification silver powder weight ratio be the ratio of 1:1, described first time surface modification silver powder is placed in ball mill, wherein, the agate ball of ball to be diameter be 6mm.Add the amount of 2g surface modifier II again by per kilogram first time surface modification silver powder weight, add surface modifier II co-ground 10 hours, the rotating speed of grinding is 20 revs/min, gets product.Wherein, surface modifier II is made up of the component of following weight portion: phenylpropyl alcohol triazole 1 part and neopelex 1 part.
Embodiment 4:
The preparation of a, silver powder: get the liquor argenti nitratis ophthalmicus that mass percent concentration is 25%, add mass percent concentration be 25% ascorbic acid solution react, when adding ascorbic acid solution, slowly add while stirring, and the time added is 8 minutes, react 12 minutes under the condition of 18 DEG C after having added, then filter, obtain even-grained ball shape silver powder; The weight ratio of described liquor argenti nitratis ophthalmicus and ascorbic acid solution is 1:1.3;
B, ball milling: be the ratio of 20:1 in the weight ratio of ball and ball shape silver powder, be placed in ball mill by described ball shape silver powder, and ball adopts single diameter to be that the ball of 12mm carries out; Press the amount of per kilogram ball shape silver powder again, the lubricant adding the ball-milling medium of 1.2L, 16g ball-milling additive and 15mL respectively carries out ball milling, and the time of ball milling is 4 hours, and the speed of ball milling is 400 revs/min, then filters, and obtains the silver powder after ball milling;
Wherein, ball-milling medium is absolute ethyl alcohol; Ball-milling additive is made up of the component of following weight portion: stearic acid 3 parts, silica 2 parts, dodecoic acid 1 part and hexadecanol 1 part; Lubricant is made up of the component of following weight portion: glycerine 2 parts, terpinol 2 parts and triethanolamine 1 part.
C, one-time surface modification: add 2.5L surface modifier I by the weight of the silver powder after ball milling described in per kilogram, react 40 minutes, filters, then dry under the condition of 65 DEG C, obtains first time surface modification silver powder;
Wherein, surface modifier I is by polyvinylpyrrolidone: the weight ratio of silane coupler is after 1:1 mixing, with deionized water dissolving, is mixed with the surface modifier that concentration is 15g/L.
D, secondary surface modification: in ball with first time surface modification silver powder weight ratio be the ratio of 6:1, described first time surface modification silver powder is placed in ball mill, wherein, the agate ball of ball to be diameter be 5mm.Add the amount of 7g surface modifier II again by per kilogram first time surface modification silver powder, add surface modifier II co-ground 4 hours, the rotating speed of grinding is 30 revs/min, gets product.Wherein, surface modifier II is made up of the component of following weight portion: phenylpropyl alcohol triazole 1 part, modified silicone 1 part and neopelex 1 part.
For verifying technique effect of the present invention, spy makes following contrast test, refers to table 1.
The contrast test of table 1 embodiment of the present invention and commercially available prod Japan 301
Finally it should be noted that, above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although with reference to above-described embodiment to invention has been detailed description, those skilled in the art are to be understood that, still can modify to the present invention or equivalent replacement, and not departing from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in right of the present invention.
Claims (10)
1. a preparation method for electric slurry flake silver powder, is characterized in that, comprises the following steps:
The preparation of a, silver powder: get liquor argenti nitratis ophthalmicus, adds ascorbic acid solution and reacts, and filters, obtains even-grained ball shape silver powder; The weight ratio of described liquor argenti nitratis ophthalmicus and ascorbic acid solution is 1:1 ~ 1.5;
B, ball milling: described ball shape silver powder is placed in ball mill, add ball-milling medium, ball-milling additive and lubricant and carry out ball milling, filters, obtain the silver powder after ball milling;
C, one-time surface modification: the silver powder after described ball milling is added surface modifier I react >=20 minutes, filter, dry, obtain first time surface modification silver powder;
D, secondary surface modification: described first time surface modification silver powder is placed in ball mill, adds surface modifier II co-ground, get product.
2. the preparation method of a kind of electric slurry flake silver powder according to claim 1, is characterized in that, in described step a when adding ascorbic acid solution, slowly adding while stirring, and add time≤15 minutes.
3. the preparation method of a kind of electric slurry flake silver powder according to claim 1, is characterized in that, the temperature of reacting in described step a is 15 DEG C ~ 25 DEG C, and the time of reaction is 10 ~ 20 minutes.
4. the preparation method of a kind of electric slurry flake silver powder according to claim 1, is characterized in that, in described step b during ball milling, is the ratio ball milling 2 ~ 8 hours of 10 ~ 50:1 in the weight ratio of ball and ball shape silver powder; Ball adopts single diameter to be that the ball of 4 ~ 20mm carries out; The speed of ball milling is 200 ~ 1000 revs/min.
5. the preparation method of a kind of electric slurry flake silver powder according to claim 1, it is characterized in that, in described step b during ball milling, by the amount of per kilogram ball shape silver powder, add the lubricant of the ball-milling medium of 0.5 ~ 2L, the ball-milling additive of 5 ~ 30g and 4 ~ 40mL respectively.
6. the preparation method of a kind of electric slurry flake silver powder according to claim 5, it is characterized in that, described ball-milling medium comprises absolute ethyl alcohol; Described ball-milling additive is selected from the one in zinc stearate, stearic acid, aluminum stearate, silica, dodecoic acid, hexadecanol or octadecyl alcolol, or their arbitrary proportion mixture; Described lubricant is selected from the one in glycerine, polyethylene glycol, terpinol or triethanolamine, or their arbitrary proportion mixture.
7. the preparation method of a kind of electric slurry flake silver powder according to claim 1, is characterized in that, in described step c, the addition of surface modifier I adds 0.5 ~ 3L by the silver powder weight after ball milling described in per kilogram; The temperature of drying is 50 DEG C ~ 70 DEG C.
8. the preparation method of a kind of electric slurry flake silver powder according to claim 7, it is characterized in that, described surface modifier I is by the one in polyvinyl alcohol, polyvinylpyrrolidone, titanate coupling agent or silane coupler, or the water-soluble solution of their mixture, be mixed with the surface modifier I that concentration is 10 ~ 30g/L.
9. the preparation method of a kind of electric slurry flake silver powder according to claim 1, it is characterized in that, when grinding in described steps d, in sphere diameter be 2 ~ 6mm ball with first time surface modification silver powder weight ratio be that the ratio of 1 ~ 10:1 grinds 2 ~ 10 hours, the rotating speed of grinding is 20 ~ 50 revs/min; The addition of surface modifier II by described in per kilogram first time surface modification silver powder weight add 2 ~ 10g; Described surface modifier II is selected from the one in OP-10, phenylpropyl alcohol triazole, modified silicone, neopelex or modified waxes powder, or their mixture.
10. the flake silver powder obtained based on preparation method according to any one of claim 1-9.
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| CN105108134B (en) * | 2015-08-04 | 2017-03-08 | 成都新柯力化工科技有限公司 | A kind of paste metallic composite for 3D printing and preparation method thereof |
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| CN105345013B (en) * | 2015-11-10 | 2017-07-07 | 南京瑞盈环保科技有限公司 | A kind of preparation method of the narrow flake silver powder of sheet rate particle diameter distribution high |
| CN105618734A (en) * | 2016-01-12 | 2016-06-01 | 昆明理工大学 | Method for surface modification of flaky silver powder |
| CN105880628B (en) * | 2016-05-13 | 2018-02-23 | 江苏理工学院 | A kind of preparation method of Bright Silver Powder for jewellery industry |
| CN105772743A (en) * | 2016-05-13 | 2016-07-20 | 江苏理工学院 | Preparing method for flake silver powder applied to touch screen |
| CN105880628A (en) * | 2016-05-13 | 2016-08-24 | 江苏理工学院 | Preparation method of bright silver powder used in jewelry industry |
| CN107243627A (en) * | 2017-05-22 | 2017-10-13 | 山东大学 | A kind of surface modifying method of solar cell front side silver paste material silver powder |
| CN107876795A (en) * | 2017-12-05 | 2018-04-06 | 深圳市中金岭南科技有限公司 | A kind of preparation method of monocrystalline copper powder |
| CN107876795B (en) * | 2017-12-05 | 2020-06-05 | 深圳市中金岭南科技有限公司 | Preparation method of single crystal copper powder |
| CN110434352A (en) * | 2019-07-30 | 2019-11-12 | 北京氦舶科技有限责任公司 | A kind of low-temperature cured conductive silver paste silver powder and preparation method thereof |
| CN110791224A (en) * | 2019-10-28 | 2020-02-14 | 广东省石油与精细化工研究院 | Modified silver powder and conductive adhesive containing same |
| CN110791224B (en) * | 2019-10-28 | 2021-01-15 | 广东省石油与精细化工研究院 | Modified silver powder and conductive adhesive containing same |
| CN112705726A (en) * | 2020-12-17 | 2021-04-27 | 暨南大学 | Preparation method of shape-controllable nano silver powder |
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Application publication date: 20150128 |