CN111842927A - Preparation method of silver powder for conductive silver paste of 5G dielectric filter and silver powder - Google Patents
Preparation method of silver powder for conductive silver paste of 5G dielectric filter and silver powder Download PDFInfo
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- CN111842927A CN111842927A CN202010729022.7A CN202010729022A CN111842927A CN 111842927 A CN111842927 A CN 111842927A CN 202010729022 A CN202010729022 A CN 202010729022A CN 111842927 A CN111842927 A CN 111842927A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 250
- 238000002360 preparation method Methods 0.000 title claims abstract description 69
- 239000004332 silver Substances 0.000 claims abstract description 125
- 229910052709 silver Inorganic materials 0.000 claims abstract description 125
- 239000002270 dispersing agent Substances 0.000 claims abstract description 82
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 80
- 238000004519 manufacturing process Methods 0.000 claims abstract description 25
- 238000006722 reduction reaction Methods 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims description 208
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 46
- 239000007800 oxidant agent Substances 0.000 claims description 44
- 239000011259 mixed solution Substances 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 32
- 238000001914 filtration Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 21
- 239000002245 particle Substances 0.000 abstract description 17
- 239000000919 ceramic Substances 0.000 abstract description 7
- 238000004891 communication Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 48
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 31
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 31
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 31
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 30
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 28
- 235000010323 ascorbic acid Nutrition 0.000 description 23
- 239000011668 ascorbic acid Substances 0.000 description 23
- 229960005070 ascorbic acid Drugs 0.000 description 21
- 239000000463 material Substances 0.000 description 16
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- 229910052939 potassium sulfate Inorganic materials 0.000 description 14
- 235000011151 potassium sulphates Nutrition 0.000 description 14
- 229910001961 silver nitrate Inorganic materials 0.000 description 14
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- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 2
- SBJKKFFYIZUCET-JLAZNSOCSA-N Dehydro-L-ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(=O)C1=O SBJKKFFYIZUCET-JLAZNSOCSA-N 0.000 description 2
- SBJKKFFYIZUCET-UHFFFAOYSA-N Dehydroascorbic acid Natural products OCC(O)C1OC(=O)C(=O)C1=O SBJKKFFYIZUCET-UHFFFAOYSA-N 0.000 description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229930003268 Vitamin C Natural products 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 229940072107 ascorbate Drugs 0.000 description 2
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- 230000000694 effects Effects 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 229920001592 potato starch Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- 235000019154 vitamin C Nutrition 0.000 description 2
- 239000011718 vitamin C Substances 0.000 description 2
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 1
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 description 1
- GJQWCDSAOUMKSE-STHAYSLISA-N 2,3-diketogulonic acid Chemical compound OC[C@H](O)[C@@H](O)C(=O)C(=O)C(O)=O GJQWCDSAOUMKSE-STHAYSLISA-N 0.000 description 1
- 125000001731 2-cyanoethyl group Chemical group [H]C([H])(*)C([H])([H])C#N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
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- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920002845 Poly(methacrylic acid) Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
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- 125000002091 cationic group Chemical group 0.000 description 1
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- 238000005354 coacervation Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
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- 238000011156 evaluation Methods 0.000 description 1
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- 230000006870 function Effects 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
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- 238000010899 nucleation Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 description 1
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 description 1
- 235000019252 potassium sulphite Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 description 1
- 229910001958 silver carbonate Inorganic materials 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 235000011008 sodium phosphates Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 229940100445 wheat starch Drugs 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
-
- B22F1/0003—
-
- 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
Abstract
The invention relates to the technical field of 5G communication, in particular to a preparation method of silver powder for conductive silver paste of a ceramic filter and silver powder. The invention provides a method for preparing silver powder, which comprises the steps of adding raw materials in a certain order, carrying out reduction reaction on a reducing agent and a silver source under the conditions of certain concentration, a dispersing agent and the like, thus preparing the silver powder with uniform particle size, flat and smooth particle morphology and moderate specific surface area, wherein the tap density of the obtained silver powder is more than 4.5g/cm3Specific surface area less than 0.9m2The conductive silver paste/G can be used for preparing conductive silver paste of a 5G dielectric filter, and has high compactness, so that the production efficiency of the filter is improved.
Description
Technical Field
The invention relates to the technical field of 5G communication, in particular to a preparation method of silver powder for conductive silver paste of a ceramic filter and silver powder.
Background
5g of silver powder for conductive silver paste of the ceramic dielectric filter. The conductive filler is filling type conductive slurry of silver powder, and is a key material of the dielectric filter. The type and proportion of the conductive silver paste, particularly the type and dosage of the additive, can affect parameters such as surface adhesion, sintering temperature, surface roughness and the like of the product. The silver has the advantages of strong conductive capability, thermal expansion coefficient close to that of a porcelain blank, good thermal stability, capability of directly welding metal on a silver layer and the like, and is considered as the optimal selection of the electrode material of the ceramic dielectric filter. The conductivity of the conductive silver paste and the compactness of a conductive layer formed by the conductive silver paste have important influence on the performance of the filter, and the silver powder is used as a functional material of the conductive silver paste, plays a role in conductivity and is an important component of the conductive silver paste, so that the preparation of the silver powder is also the key point in the production of the ceramic filter at present.
The silver powder selection difference easily causes unsmooth and low effective conductivity of a silver layer sintered on the surface of the ceramic, and influences parameters such as a Q value, a silver layer tension, surface roughness and the like of a product. Therefore, a silver conductive layer with high compactness, high adhesive force, high conductivity and good weldability is formed on the surface of the 5G ceramic medium filter, and the conductive slurry silver powder is particularly critical. The particle size, the particle morphology, the specific surface area and the like of the silver powder can influence the compactness of the silver paste. The larger the specific surface area is, the more likely the agglomeration is formed, and the compactness of the silver paste is influenced. Therefore, the quality of the silver powder, the slurry matching property and other parameters are very important to form the silver conductive layer with good consistency, high compactness, high adhesive force, good conductivity and good weldability.
The silver powder produced at present often has the problems of uneven size, large specific surface area, small tap density and the like, which all affect the production efficiency of the 5G dielectric filter.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides a method for preparing a silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B;
c, preparation of a solution: adding a silver source into water to obtain a solution C;
reduction reaction: adding the solution B into the solution A at the temperature of 30-35 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 50-70 mL/min, and stirring to obtain silver paste;
and (3) post-treatment: and adjusting the pH value of the silver paste to 6.5-7.5, cleaning, filtering and drying to obtain the silver powder.
As a preferable technical scheme, the weight ratio of the dispersing agent to the inorganic salt is (10-15): 1.
according to a preferable technical scheme of the invention, in the solution A, the weight of the dispersing agent accounts for 2-5 wt% of the total weight of the solution A.
As a preferable technical solution of the present invention, the weight ratio of the reducing agent to the oxidizing agent is 1: (0.02-0.07).
According to a preferable technical scheme of the invention, in the B solution, the weight of the reducing agent accounts for 15-25 wt% of the total weight of the B solution.
According to a preferable technical scheme of the invention, in the C solution, the weight of the silver source accounts for 10-18 wt% of the total weight of the C solution.
As a preferable technical scheme of the invention, the weight ratio of the dispersing agent to the silver source is (0.1-0.3): 1.
as a preferable technical scheme of the invention, the weight ratio of the reducing agent to the silver source is (0.45-0.6): 1.
the second aspect of the present invention provides a silver powder prepared according to the method for preparing silver powder as described above.
The third aspect of the invention provides an application of the silver powder in preparation of 5G dielectric filter conductive silver paste.
Compared with the prior art, the invention has the following beneficial effects: the invention provides a method for preparing silver powder, which comprises the steps of adding raw materials in a certain order, carrying out reduction reaction on a reducing agent and a silver source under the conditions of certain concentration, a dispersing agent and the like, thus preparing the silver powder with uniform particle size, flat and smooth particle morphology and moderate specific surface area, wherein the tap density of the obtained silver powder is more than 4.5g/cm3Specific surface area less than 0.9m2The conductive silver paste/G can be used for preparing conductive silver paste of a 5G dielectric filter, and has high compactness, so that the production efficiency of the filter is improved.
Drawings
FIG. 1 is a scanning electron microscope image of silver powder prepared by the method provided in example 1.
Fig. 2 is a scanning electron microscope image of the silver powder prepared by the method provided in example 2.
FIG. 3 is a scanning electron microscope image of the silver powder prepared by the method provided in example 3.
FIG. 4 is a scanning electron microscope image of the silver powder prepared by the method provided in example 4.
FIG. 5 is a scanning electron microscope image of the silver powder prepared by the method provided in example 5.
FIG. 6 is a scanning electron microscope image of the silver powder prepared by the method provided in example 6.
FIG. 7 is a scanning electron microscope image of the silver powder prepared by the method provided in example 7.
FIG. 8 is a scanning electron microscope image of the silver powder prepared by the method provided in example 8.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
The present invention is illustrated by the following specific embodiments, but is not limited to the specific examples given below.
The first aspect of the present invention provides a method for preparing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B;
c, preparation of a solution: adding a silver source into water to obtain a solution C;
reduction reaction: adding the solution B into the solution A at the temperature of 30-35 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 50-70 mL/min, and stirring to obtain silver paste;
and (3) post-treatment: and adjusting the pH value of the silver paste to 6.5-7.5, cleaning, filtering and drying to obtain the silver powder.
In a preferred embodiment, the method of the present invention comprises the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B;
c, preparation of a solution: adding a silver source into water to obtain a solution C;
reduction reaction: adding the solution B into the solution A at the temperature of 30-35 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: and adjusting the pH value of the silver paste to 7, cleaning, filtering and drying to obtain the silver powder.
Preparation of solution A
In one embodiment, the weight ratio of the dispersant to the inorganic salt is (10-15): 1; further, the weight ratio of the dispersant to the inorganic salt is 13.3: 1.
preferably, in the solution A, the weight of the dispersant accounts for 2-5 wt% of the total weight of the solution A; further, in the solution A of the present invention, the weight of the dispersant accounts for 3.8 wt% of the total weight of the solution A.
More preferably, the dispersant of the present invention is selected from one or more of polyvinyl acid, polyvinylpyrrolidone, polyethylene glycol, polyacrylic acid, polymethacrylic acid, methyl cellulose, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, carboxymethyl hydroxyethyl cellulose, carboxymethyl starch, carboxyethyl starch, cyanoethyl starch, acetate starch, phosphate starch, cationic starch, polymeric starch, wheat starch, potato starch, and sweet potato starch.
Further preferably, the dispersant of the present invention is polyvinylpyrrolidone.
Polyvinylpyrrolidone is a water-soluble linear polymer compound and is formed by homopolymerization of monomer N-vinyl pyrrolidone (NVP). Has film forming property, cohesiveness, hygroscopicity, solubilization or coacervation effect, complexing ability with certain compounds, etc. The polyvinylpyrrolidone has both hydrophilic group and lipophilic group in its molecule, so that it can be dissolved in water and most organic solvents (such as alcohol, carboxylic acid, amine, halogenated hydrocarbon, etc.), and has low toxicity and good physiological compatibility. The solubility of polyvinylpyrrolidone in water is limited only by its own viscosity. As examples of the polyvinyl pyrrolidone, there are included, but not limited to, PVPK12, PVPK15, PVPK17 (weight average molecular weight 10100), PVPK25 (weight average molecular weight 32000), PVPK30 (weight average molecular weight 37900), PVPK45 (weight average molecular weight 152000), PVPK60, PVPK70, PVPK80, PVPK85 of bubingchu new materials science and technology (shanghai).
More preferably, the weight average molecular weight of the polyvinylpyrrolidone provided by the invention is 30000-400000.
The molecular weight is the weight average molecular weight, statistically averaged over the molecular weight. Usually expressed as Mw, which is equal to the sum of the molecular weight of each molecule multiplied by its weight fraction.
In a preferred embodiment, the inorganic salt according to the invention is selected from the group consisting of sodium sulfate, potassium sulfate, sodium sulfite, potassium sulfite, sodium carbonate, potassium carbonate, sodium phosphate, potassium phosphate, sodium sulfide, potassium sulfide; further, the inorganic salt is potassium sulfate.
Preparation of solution B
In one embodiment, the weight ratio of reducing agent to oxidizing agent of the present invention is 1: (0.02-0.07); further, the weight ratio of the reducing agent to the oxidizing agent is 1: 0.05.
preferably, in the solution B, the weight of the reducing agent accounts for 15-25 wt% of the total weight of the solution B; further, in the solution B of the present invention, the weight of the reducing agent is 18.9 wt% of the total weight of the solution B.
More preferably, the reducing agent of the present invention is selected from one of formaldehyde, hydrazine hydrate, ascorbic acid, sodium borohydride and formic acid; further, the reducing agent of the present invention is ascorbic acid.
Ascorbic acid, vitamin C, has a structure similar to glucose, is a polyhydroxy compound, and has acid properties because two adjacent enol-type hydroxyl groups at the 2 nd and 3 rd positions in the molecule are easily dissociated to release H +, which is also called ascorbic acid. Vitamin C has strong reducibility and is easily oxidized into dehydrovitamin C, but the reaction is reversible, and ascorbic acid and dehydroascorbic acid have the same physiological function, but if the dehydroascorbic acid is continuously oxidized to generate diketogulonic acid, the reaction is irreversible and the physiological effect is completely lost.
Further preferably, the oxidant is selected from one of hydrogen peroxide, peroxyacetic acid and ammonium persulfate; further, the oxidant of the present invention is hydrogen peroxide.
Solution C
In one embodiment, in the solution C, the weight of the silver source accounts for 10-18 wt% of the total weight of the solution C; further, in the solution C of the present invention, the weight of the silver source accounts for 14 wt% of the total weight of the solution C.
Preferably, the weight ratio of the dispersing agent and the silver source is (0.1-0.3): 1; further, the weight ratio of the dispersant to the silver source is 0.2: 1.
more preferably, the weight ratio of the reducing agent and the silver source is (0.45-0.6): 1. (ii) a Further, the weight ratio of the reducing agent and the silver source is 0.52: 1.
further preferably, the silver source of the present invention is selected from one of silver nitrate, silver ammonia complex, silver oxide, silver carbonate, silver carboxylate; further, the silver source of the invention is silver nitrate.
Post-treatment
In one embodiment, the pore size of the washing filtration is 0.2 to 1 μm.
In filtration, the pore size is the size of the largest particle that is allowed to pass through.
In order to meet the requirements of the silver paste of the filter, the specific surface area of the silver powder needs to be controlled, and a larger tap density is achieved, the applicant finds that when ascorbic acid is used as a reducing agent, and a small amount of hydrogen peroxide is added as an initiator, the generation and concentration of ascorbate ions in ascorbic acid can be promoted, so that when a silver source is added, the silver ions are surrounded by the ascorbate ions with higher concentration to generate explosive nucleation to form a crystal nucleus with high dispersibility, and due to attack of an electrophilic hydrogen peroxide reagent, oxygen ions formed by ascorbic acid and the like in the initial stage are attached to the surface of the crystal nucleus, and a layer of macromolecular ascorbic acid and a dispersing agent with certain molecular weight are attached to the crystal nucleus to jointly generate a bit group and an electrostatic effect to reduce agglomeration, as the reduction reaction progresses, the surface point position of the silver powder is reduced, the electrostatic repulsion force is reduced, aggregation growth occurs, and uniform spherical secondary particles are, obtaining uniform and smooth silver powder. And the applicant found that when the oxidizing agent is added too much or too little, or the molecular weight of the dispersant is not suitable, the particle size distribution and surface properties of the silver powder are affected, thereby affecting the filter.
The second aspect of the present invention provides a silver powder produced according to the method for producing a silver powder as described above.
The third aspect of the invention provides an application of the silver powder, which is used for preparing the conductive silver paste of the 5G dielectric filter.
Examples
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
Example 1
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 2 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 10: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 15 wt% of the total weight of the solution B, and the weight ratio of the reducing agent to the oxidizing agent is 1: 0.02, wherein the reducing agent is ascorbic acid, and the oxidizing agent is hydrogen peroxide;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 10 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.1: 1, the weight ratio of the reducing agent to the silver source is 0.45: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK30, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Example 2
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 2.5 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 10: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 16 wt% of the total weight of the solution B, and the weight ratio of the reducing agent to the oxidizing agent is 1: 0.03, the reducing agent is ascorbic acid and the oxidizing agent is hydrogen peroxide;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 10.5 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.1: 1, the weight ratio of the reducing agent to the silver source is 0.48: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK30, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Example 3
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 3 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 10.5: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 16 wt% of the total weight of the solution B, and the weight ratio of the reducing agent to the oxidizing agent is 1: 0.03, the reducing agent is ascorbic acid and the oxidizing agent is hydrogen peroxide;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 10.5 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.1: 1, the weight ratio of the reducing agent to the silver source is 0.5: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK30, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Example 4
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 3.5 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 11: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 17 wt% of the total weight of the solution B, and the weight ratio of the reducing agent to the oxidizing agent is 1: 0.03, the reducing agent is ascorbic acid and the oxidizing agent is hydrogen peroxide;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 11 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.2: 1, the weight ratio of the reducing agent to the silver source is 0.5: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK25, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Example 5
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 3.8 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 11.5: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 17 wt% of the total weight of the solution B, and the weight ratio of the reducing agent to the oxidizing agent is 1: 0.03, the reducing agent is ascorbic acid and the oxidizing agent is hydrogen peroxide;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 11.5 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.2: 1, the weight ratio of the reducing agent to the silver source is 0.5: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK25, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Example 6
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 3.8 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 12: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 18 wt% of the total weight of the solution B, and the weight ratio of the reducing agent to the oxidizing agent is 1: 0.04, wherein the reducing agent is ascorbic acid, and the oxidizing agent is hydrogen peroxide;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 12 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.1: 1, the weight ratio of the reducing agent to the silver source is 0.5: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK25, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Example 7
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 5 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 15: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 25 wt% of the total weight of the solution B, and the weight ratio of the reducing agent to the oxidizing agent is 1: 0.07, the reducing agent is ascorbic acid and the oxidizing agent is hydrogen peroxide;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 18 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.3: 1, the weight ratio of the reducing agent to the silver source is 0.6: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK25, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Example 8
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 3.8 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 13.3: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 18.9 wt% of the total weight of the B solution, and the weight ratio of the reducing agent to the oxidizing agent is 1: 0.05, the reducing agent is ascorbic acid, and the oxidizing agent is hydrogen peroxide;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 14 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.2: 1, the weight ratio of the reducing agent to the silver source is 0.52: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK25, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Example 9
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 3.8 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 13.3: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 18.9 wt% of the total weight of the B solution, and the weight ratio of the reducing agent to the oxidizing agent is 1: 0.05, the reducing agent is ascorbic acid, and the oxidizing agent is hydrogen peroxide;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 14 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.2: 1, the weight ratio of the reducing agent to the silver source is 0.52: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK17, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Example 10
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 3.8 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 13.3: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 18.9 wt% of the total weight of the B solution, and the weight ratio of the reducing agent to the oxidizing agent is 1: 0.05, the reducing agent is ascorbic acid, and the oxidizing agent is hydrogen peroxide;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 14 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.2: 1, the weight ratio of the reducing agent to the silver source is 0.52: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK45, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Example 11
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 3.8 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 13.3: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: adding a reducing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 18.9 wt% of the total weight of the B solution, and the reducing agent is ascorbic acid;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 14 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.2: 1, the weight ratio of the reducing agent to the silver source is 0.52: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK25, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Example 12
This example provides a method for producing silver powder, comprising the steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A; the weight of the dispersant accounts for 3.8 wt% of the total weight of the solution A, and the weight ratio of the dispersant to the inorganic salt is 13.3: 1, the dispersing agent is polyvinylpyrrolidone, and the inorganic salt is potassium sulfate;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B; the weight of the reducing agent accounts for 18.9 wt% of the total weight of the B solution, and the weight ratio of the reducing agent to the oxidizing agent is 1: 0.5, the reducing agent is ascorbic acid, and the oxidizing agent is hydrogen peroxide;
c, preparation of a solution: adding a silver source into water to obtain a solution C; the weight of the silver source accounts for 14 wt% of the total weight of the C solution, and the weight ratio of the dispersing agent to the silver source is 0.2: 1, the weight ratio of the reducing agent to the silver source is 0.52: 1, the silver source is silver nitrate;
reduction reaction: adding the solution B into the solution A at 32 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 60mL/min, and stirring to obtain silver paste;
and (3) post-treatment: adjusting pH of silver paste to 7, washing with filter plate with aperture of 0.2 μm, filtering, and drying to obtain silver powder.
The polyvinylpyrrolidone was purchased from PVPK25, new materials science and technology (shanghai) ltd.
This example also provides a silver powder prepared according to the preparation method described above.
Evaluation of Performance
The following experiments were performed as experimental groups provided in the examples.
1. And (4) SEM test: the silver powder prepared by the method provided in examples 8 to 12 was subjected to SEM test, and the size distribution and surface properties of the silver powder were observed and evaluated:
(1) size distribution of silver powder: the 1 grade is that the gaps among the silver powder particles are obvious, aggregation is slightly generated among the particles, the 2 grade is that aggregation is generated among a small amount of the silver powder particles, the 3 grade is that aggregation is generated among part of the particles, and the 4 grade is that aggregation is generated among most of the silver powder particles.
(2) Surface roughness of silver powder: the level 1 is that the surface of the silver powder is smooth and flat, the level 2 is that the surface of the silver powder has a small amount of unevenness, the level 3 is that the surface of the silver powder is uneven and increased, and the level 4 is that the surface of the silver powder is uneven and obvious. The results are provided in the examples and are shown in Table 1.
Table 1 performance characterization test
2. And (3) testing the performance of the silver powder: the silver powders prepared by the methods provided in the examples were subjected to particle size distribution (unit: μm), tap density, specific surface area, water content, heat loss rate and scanning electron microscope test, and the results are shown in table 2.
Table 2 characterization test of properties
Fig. 1 to 8 are respectively electron microscope pictures of the silver powder provided in embodiments 1 to 8, it can be observed that the particle size distribution of the silver powder is relatively uniform, the gaps between particles are obvious, no aggregation occurs, and the surface of the silver powder particles is smooth and flat, which is beneficial to forming conductive silver paste with high compactness and adhesive force, and improves the working efficiency of the filter.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. The preparation method of the silver powder is characterized by comprising the following steps of:
preparation of solution A: adding a dispersing agent and inorganic salt into water, and mixing to obtain a solution A;
b, preparation of a solution: sequentially adding a reducing agent and an oxidizing agent into water, and mixing to obtain a solution B;
c, preparation of a solution: adding a silver source into water to obtain a solution C;
reduction reaction: adding the solution B into the solution A at the temperature of 30-35 ℃ to obtain a mixed solution, then dropwise adding the solution C into the mixed solution at the speed of 50-70 mL/min, and stirring to obtain silver paste;
and (3) post-treatment: and adjusting the pH value of the silver paste to 6.5-7.5, cleaning, filtering and drying to obtain the silver powder.
2. The method for producing silver powder according to claim 1, wherein the weight ratio of the dispersant to the inorganic salt is (10 to 15): 1.
3. the method for producing silver powder according to claim 1, wherein the dispersant is present in the solution A in an amount of 2 to 5 wt% based on the total weight of the solution A.
4. The method for producing silver powder according to claim 1, wherein the weight ratio of the reducing agent to the oxidizing agent is 1: (0.02-0.07).
5. The method for producing silver powder according to claim 1, wherein the reducing agent is contained in the B solution in an amount of 15 to 25 wt% based on the total weight of the B solution.
6. The method for producing silver powder according to any one of claims 1 to 5, wherein the weight of the silver source in the C solution is 10 to 18 wt% based on the total weight of the C solution.
7. The method for producing silver powder according to claim 6, wherein the weight ratio of the dispersant to the silver source is (0.1 to 0.3): 1.
8. the method for producing silver powder according to claim 6, wherein the weight ratio of the reducing agent to the silver source is (0.45 to 0.6): 1.
9. a silver powder produced by the method for producing a silver powder according to any one of claims 1 to 8.
10. The use of the silver powder according to claim 9 for preparing 5G dielectric filter conductive silver paste.
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| CN114939667A (en) * | 2021-06-16 | 2022-08-26 | 河南金渠银通金属材料有限公司 | Preparation method of micron-sized silver powder and application of micron-sized silver powder in filter |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114939667A (en) * | 2021-06-16 | 2022-08-26 | 河南金渠银通金属材料有限公司 | Preparation method of micron-sized silver powder and application of micron-sized silver powder in filter |
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