CN113245555A - Petal-shaped conductive silver powder and preparation method thereof - Google Patents
Petal-shaped conductive silver powder and preparation method thereof Download PDFInfo
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- CN113245555A CN113245555A CN202110491132.9A CN202110491132A CN113245555A CN 113245555 A CN113245555 A CN 113245555A CN 202110491132 A CN202110491132 A CN 202110491132A CN 113245555 A CN113245555 A CN 113245555A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 32
- 238000005507 spraying Methods 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 15
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 125000000914 phenoxymethylpenicillanyl group Chemical group CC1(S[C@H]2N([C@H]1C(=O)*)C([C@H]2NC(COC2=CC=CC=C2)=O)=O)C 0.000 claims description 2
- 229920000136 polysorbate Polymers 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 description 9
- 230000001070 adhesive effect Effects 0.000 description 9
- 239000002245 particle Substances 0.000 description 7
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- RYZCLUQMCYZBJQ-UHFFFAOYSA-H lead(2+);dicarbonate;dihydroxide Chemical compound [OH-].[OH-].[Pb+2].[Pb+2].[Pb+2].[O-]C([O-])=O.[O-]C([O-])=O RYZCLUQMCYZBJQ-UHFFFAOYSA-H 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- -1 particle size Chemical compound 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B22F1/0007—
-
- 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
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
Abstract
The invention discloses petal-shaped conductive silver powder and a preparation method thereof, wherein the method comprises the following steps: dissolving silver nitrate in water, stirring and standing, adding a pH regulator, and controlling the pH value of the solution to be 2.5-4.5 to obtain a mixed solution A; dissolving a reducing agent in water, stirring and standing, adding a dispersing agent, and continuously stirring for 30 minutes to obtain a reducing mixed solution B; and (3) adopting a high-pressure mixing pump to mix the mixed liquor A and the reduced mixed liquor B according to a molar ratio of 1: 0.5-1, spraying the mixed solution AB into a drying oven by using high-temperature spraying equipment, wherein the spraying temperature is 50-100 ℃, the spraying speed is 50-100 m/s, powdery solid is obtained at the bottom of the drying oven, and the temperature of the drying oven is 160-230 ℃; and collecting the powdery solid, washing with deionized water, performing centrifugal separation, and drying with a vacuum drying oven to obtain the petal-shaped conductive silver powder. The method has the advantages of simple process, controllable preparation process and capability of realizing batch production.
Description
Technical Field
The invention belongs to the technical field of material preparation, and relates to a preparation method of petal-shaped conductive silver powder. And more particularly, to a method for preparing silver powder by a chemical reduction and spray coating process.
Background
Although the silver powder is a main material applied to silver paste and conductive adhesive in the field of photovoltaic materials, the using amount of the tile-stacked conductive adhesive is continuously increased along with the application of the tile-stacked assembly technology in photovoltaic, foreign conductive adhesive (such as Helish and Hangao) is monopolized at home at present, along with the improvement of the domestic research and development power, the market occupancy of the domestic tile-stacked conductive adhesive is slowly increased, the demand of the silver powder is continuously increased, and the requirements on the performances of the metal silver powder, such as particle size, distribution, morphology, specific surface area and the like, are also gradually strict.
The existing silver powder has the following defects: in the production process, the dispersing agent is mostly directly added into the silver salt solution, and then the silver salt solution is stirred for a certain time and then the reducing agent is added to reduce the silver salt. The preparation method can not ensure that the added dispersing agent is completely dissolved, so that the produced silver powder has poor granularity stability, is thicker than the target silver powder in granularity and larger in specific surface area, and has dispersed and non-concentrated granularity; at home and abroad, oxidation-reduction reaction is carried out in a reaction kettle at most to generate silver powder and control the shape and size of the silver powder, the method is a single-batch secondary production, and the controllability and parameters of the production process are unstable along with the quantity expansion; in terms of product characteristics, the uniformity and the dispersibility of the particle size are insufficient, the particles are easy to agglomerate, and the conductivity is poor. In addition, a large amount of fixed waste and waste water are generated in the existing silver powder preparation process, so that not only is the resource waste caused, but also the environment is polluted.
Therefore, how to provide a preparation method of pollution-free and high-conductivity petal-shaped silver powder is an urgent technical problem to be solved in the field.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing petal-shaped silver powder by chemical reduction and spraying, which does not generate fixed waste and waste water and has no pollution.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of petal-shaped conductive silver powder specifically comprises the following steps:
1) dissolving silver nitrate in water, stirring and standing, and adding a pH regulator for mixing to obtain a mixed solution A;
2) dissolving a reducing agent in water, stirring and standing, adding a dispersing agent, stirring and mixing to obtain a reducing mixed solution B;
3) after the mixed solution A and the reduced mixed solution B are mixed, spraying the mixed solution AB into a drying oven by using high-temperature spraying equipment for drying to obtain powdery solid;
4) and collecting the powdery solid, washing with deionized water, performing centrifugal separation, and drying in a vacuum drying oven to finally obtain the petal-shaped conductive silver powder.
Preferably, the pH value of the mixed solution A is 2.5-4.5, and the pH regulator is nitric acid.
Preferably, the reducing agent is at least one of sodium borohydride, sodium citrate, hydrazine, formaldehyde and glucose.
Preferably, the dispersant is at least one of tween, PVA, sodium oleate, glycol, a silane coupling agent and polyurethane.
Preferably, the mixing molar ratio of the mixed liquor A to the reducing mixed liquor B is 1: 0.5-1, and the temperature of the high-temperature spraying equipment is 50-100 ℃, and the spraying speed is 50-100 m/s; the temperature of the drying box is 160-230 ℃.
Preferably, the centrifugal separation speed is 1500-3000 r/min, and the vacuum drying temperature is 120-150 ℃.
The invention also claims the petal-shaped conductive silver powder prepared by the method.
According to the technical scheme, compared with the prior art, the petal-shaped conductive silver powder and the preparation method thereof provided by the invention have the following excellent effects:
the preparation method is simple in preparation process and low in cost, the silver salt and the reducing agent solution are mixed through the mixing pump, then the mixed solution is sprayed into the drying oven through the spraying equipment, and nucleation and growth of crystal grains are controlled through the mixing speed and the spraying speed, so that the size and the shape of silver particles are controlled, the particle size of the silver powder is 0.5-50 microns, the silver powder is petal-shaped, and the conductive adhesive prepared from the silver powder is small in contact resistance and high in conductivity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic view of the structure of the drying box of the present invention.
FIG. 2 is a Scanning Electron Micrograph (SEM) of silver powder of example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a preparation method of petal-shaped silver powder with no pollution and high conductivity.
The present invention will be further specifically illustrated by the following examples for better understanding, but the present invention is not to be construed as being limited thereto, and certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing disclosure are intended to be included within the scope of the invention.
The technical solution of the present invention will be further described with reference to the following specific examples.
Example 1
1) Dissolving 1Kg of silver nitrate in water, stirring and standing, and adding nitric acid to adjust the pH value of the solution to 3.0 to obtain a mixed solution A;
2) dissolving 0.6Kg of sodium borohydride in water, stirring and standing, adding sodium oleate, and continuously stirring for 30 minutes to obtain a reduction mixed solution B;
3) mixing the mixed solution A and the reduced mixed solution B by using a mixing pump, and spraying the mixed solution AB into a drying box by using high-temperature spraying equipment; the temperature of the spraying equipment is 50 ℃, and the spraying speed is 60 m/s; the temperature of the drying box is 180 ℃;
4) and then collecting the powdery solid, washing with deionized water, centrifuging at 1500 rpm, and vacuum drying at 120 ℃ to obtain the petal-shaped conductive silver powder.
Example 2
1) Dissolving 0.8Kg of silver nitrate in water, stirring and standing, and adding nitric acid to adjust the pH value of the solution to 4.0 to obtain a mixed solution A;
2) dissolving 0.5Kg of sodium borohydride in water, stirring and standing, adding PVA, and continuing stirring for 30 minutes to obtain a reduction mixed solution B;
3) mixing the mixed solution A and the reduced mixed solution B by using a mixing pump, and spraying the mixed solution AB into a drying box by using high-temperature spraying equipment; the temperature of the spraying equipment is 60 ℃, and the spraying speed is 100 m/s; the temperature of the drying box is 200 ℃;
4) and then collecting the powdery solid, washing with deionized water, centrifuging at 2000 r/min, and vacuum drying at 100 ℃ to obtain the petal-shaped conductive silver powder.
Example 3
1) Dissolving 1.2Kg of silver nitrate in water, stirring and standing, and adding nitric acid to adjust the pH value of the solution to 4.5 to obtain a mixed solution A;
2) dissolving 0.5Kg of sodium borohydride in water, stirring and standing, adding a silane coupling agent, and continuously stirring for 30 minutes to obtain a reduction mixed solution B;
3) mixing the mixed solution A and the reduced mixed solution B by using a mixing pump, and spraying the mixed solution AB into a drying box by using high-temperature spraying equipment; the temperature of the spraying equipment is 80 ℃, and the spraying speed is 80 m/s; the temperature of the drying box is 180 ℃;
4) and then collecting the powdery solid, washing with deionized water, centrifuging at 3000 r/min, and vacuum drying at 150 ℃ to obtain the petal-shaped conductive silver powder.
The petal-shaped silver powder prepared by the invention has simple process and stable batch. It not only has high electric conductivity and oxidation resistance, has still reduced manufacturing cost, as shown in table 1, adopts petaloid silver powder as the conducting particle and compares with japanese imported silver powder, particle diameter: 0.5-50 um; the silver content is 99.99%; color: silver white; resistivity of 0.6X 10-4Omega cm or more.
TABLE 1 comparison of Performance parameters for petaloid silver powders
Compared with the conductive adhesive of a Hangao acrylic acid system, the conductive adhesive prepared by using the petal-shaped silver powder has the advantages that the petal-shaped silver powder enables the organic silica gel to have good conductivity and aging resistance as shown in Table 2. At present, manufacturers for manufacturing the conductive adhesive for the laminated tile component in the market are few, and an acrylic acid system is adopted by Hangao companies, and because the acrylic acid system is poor in aging resistance and large in stress, the battery piece is easy to fragment when in use. And the organic silicon pure silver conductive adhesive prepared from the petal-shaped silver powder can well solve the problems.
TABLE 2 comparison of Performance parameters of conductive pastes prepared with foreign silver powders
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. The preparation method of the petal-shaped conductive silver powder is characterized by comprising the following steps:
1) dissolving silver nitrate in water, stirring and standing, and adding a pH regulator for mixing to obtain a mixed solution A;
2) dissolving a reducing agent in water, stirring and standing, adding a dispersing agent, stirring and mixing to obtain a reducing mixed solution B;
3) after the mixed solution A and the reduced mixed solution B are mixed, spraying the mixed solution AB into a drying oven by using high-temperature spraying equipment for drying to obtain powdery solid;
4) and collecting the powdery solid, washing with deionized water, performing centrifugal separation, and drying in a vacuum drying oven to finally obtain the petal-shaped conductive silver powder.
2. The method for preparing petal-shaped conductive silver powder according to claim 1, wherein the pH of the mixture A is 2.5-4.5, and the pH regulator is nitric acid.
3. The method for preparing petal-shaped conductive silver powder according to claim 1, wherein the reducing agent is at least one of sodium borohydride, sodium citrate, hydrazine, formaldehyde and glucose.
4. The method for preparing petal-shaped conductive silver powder according to claim 1, wherein the dispersant is at least one of tween, PVA, sodium oleate, ethylene glycol, silane coupling agent and polyurethane.
5. The method for preparing the petal-shaped conductive silver powder according to claim 1, wherein the mixing molar ratio of the mixed solution A to the reducing mixed solution B is 1: 0.5-1, and the temperature of the high-temperature spraying equipment is 50-100 ℃, and the spraying speed is 50-100 m/s; the temperature of the drying box is 160-230 ℃.
6. The method for preparing petal-shaped conductive silver powder according to claim 1, wherein the centrifugal separation speed is 1500-3000 r/min, and the vacuum drying temperature is 120-150 ℃.
7. A petaloid conductive silver powder prepared by the method of claim 1.
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| CN202110491132.9A CN113245555A (en) | 2021-05-06 | 2021-05-06 | Petal-shaped conductive silver powder and preparation method thereof |
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