CN111393893A - Nano silver solution for spraying 5G dielectric ceramic filter, preparation method and spraying method thereof - Google Patents
Nano silver solution for spraying 5G dielectric ceramic filter, preparation method and spraying method thereof Download PDFInfo
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- CN111393893A CN111393893A CN202010158256.0A CN202010158256A CN111393893A CN 111393893 A CN111393893 A CN 111393893A CN 202010158256 A CN202010158256 A CN 202010158256A CN 111393893 A CN111393893 A CN 111393893A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P1/00—Auxiliary devices
- H01P1/20—Frequency-selective devices, e.g. filters
- H01P1/2002—Dielectric waveguide filters
Abstract
The invention relates to a nano silver solution for spraying a 5G dielectric ceramic filter and a preparation method and a spraying method thereof; wherein, the nano silver solution for spraying the 5G dielectric ceramic filter is characterized in that: according to the weight portion, the silver salt is 10-60 portions, the solvent is 20-80 portions, the borate is 1-5 portions, the metal oxide is 1-3 portions, the regulator is 5-10 portions, the drier is 7-10 portions, the resin material is 1-5 portions, and the thinner is 10-20 portions. The nano silver solution is adopted for spraying, so that the surface of a 5G dielectric ceramic filter product can be uniformly metallized, the silver consumption is low, the cost is low, the electrical property and the application performance are excellent, and the conductivity is stable.
Description
Technical Field
The invention relates to a raw material for manufacturing a silver conductive coating, in particular to a nano silver solution for spraying a 5G dielectric ceramic filter, and a preparation method and a spraying method thereof.
Background
At present, silver conductive coatings are manufactured on 5G dielectric ceramic filters by using methods such as silver paste soaking coating or spraying blade coating, the silver quantity required by the manufacturing methods is large, the silver content of the silver paste in the manufacturing methods is high (reaching 80% -90% of the silver content), the silver paste consumption is large, but the silver quantity actually coated on a workpiece is not large and is a majority of waste, the overall cost of the 5G dielectric ceramic filter is increased, and the cost of the silver accounts for 30% of the total cost. The existing manufacturing method of the silver conductive coating is not scientific for the concepts of environmental protection and non-renewable resource consumption.
Therefore, further improvements are needed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a nano silver solution for spraying a 5G dielectric ceramic filter and a preparation method and a spraying method thereof; the nano silver solution is adopted for spraying, so that the surface of a product can be uniformly metalized, the silver consumption is low, the cost is low, the electrical property and the application performance are excellent, and the conductivity is stable.
The purpose of the invention is realized as follows:
a nano silver solution for spraying a 5G dielectric ceramic filter is characterized in that: according to the weight portion, the silver salt is 10-60 portions, the solvent is 20-80 portions, the borate is 1-5 portions, the organic metal complex is 1-3 portions, the regulator is 5-10 portions, the drier is 7-10 portions, the resin material is 1-5 portions, and the thinner is 10-20 portions.
The silver salt is one or more of silver nitrate, silver oxalate, silver sulfate and the like.
The solvent is one or more of deionized water, pure water, distilled water and the like.
The borate is one or more of boric acid, sodium borate, potassium borate and the like.
The organic metal complex is one or more of organic bismuth, organic tin, organic silicon and the like.
The regulator is one or more of ascorbic acid, hydrazine hydrate, formaldehyde, malic acid and the like.
The drier is one or more of neodecanoic acid, isooctanoic acid, naphthenic acid and the like.
The resin material is one or more of PVP polyvidone K30, water-based CAB, water-based acrylic acid and the like.
The diluent is one or more of ethylene glycol butyl ether, ethylene glycol hexyl ether, ethylene glycol methyl ether and the like.
The preparation method of the nano silver solution for spraying the 5G dielectric ceramic filter is characterized by comprising the following steps of: comprises the following steps
Step 1, adding silver salt into a part of solvent, mixing and dissolving the silver salt into a transparent solution, heating the solution to 80 ℃, adding a drier while stirring the solution, continuing heating the solution to 120-150 ℃, stopping stirring the solution, and adding a part of diluent to prepare a silver nanoparticle stock solution for later use;
step 2, adding borate into the other part of solvent, mixing and dissolving to obtain a transparent solution, adding an organic metal complex, stirring, and adding a regulator during stirring to obtain a viscous liquid; then adding the rest diluent to prepare an inorganic binder solution after high-temperature sintering;
step 3, dissolving the resin material by using another part of solvent to prepare an organic temporary low-temperature bonding phase solution;
and 4, mixing and stirring the silver nanoparticle stock solution prepared in the step 1 and the inorganic binder liquid prepared in the step 2 to prepare a nano silver nanoparticle suspension, adding the organic temporary low-temperature binder phase solution prepared in the step 3 to obtain a mixed solution, and adding the rest solvent into the mixed solution under stirring to dilute the mixed solution to prepare a nano silver solution.
The spraying method of the nano silver solution for spraying the 5G dielectric ceramic filter is characterized by comprising the following steps of: the method comprises the following steps:
step a, taking a proper amount of nano silver solution, stirring and transferring the nano silver solution to a pumping hydraulic container on spraying equipment, and adjusting the spraying caliber size and flow rate to perform spraying;
step b, spraying to prepare a uniform silver conductive coating, and then drying in a drying furnace at the low temperature of 100 ℃ and 200 ℃;
and c, sintering at the temperature of 500-600 ℃ for 10min to obtain the compact silver conductive coating.
The invention has the following beneficial effects:
the nano silver solution in the state of aqueous solution can be used for spraying or dip plating, a very compact silver conductive coating can be formed by using extremely low silver content, the thickness is only 1-3 micrometers, the resistivity of the prepared silver conductive coating can be as low as 2m omega (the resistivity of the silver conductive coating prepared by the prior art is 4-6m omega), the directions of electromagnetic waves and guided electromagnetic waves can be well shielded completely, the using amount of silver is only 10-20% of that of the conventional silver paste, the manufacturing cost is greatly reduced, and high economic benefit is brought directly (preliminary statistics can reduce the total cost by 20%). Meanwhile, the nano silver solution has extremely low viscosity and excellent spraying performance, and can be sprayed by using a precision spray gun (or spraying equipment) with the caliber of 0.1-0.3mm, so that the spraying effect of the silver conductive coating is more uniform and delicate, the drying and sintering processes can be processed at low temperature, and the effects of saving heat source energy and saving time are achieved.
Detailed Description
The present invention will be further described with reference to the following examples.
The nano silver solution for spraying the 5G dielectric ceramic filter comprises, by weight, 10-60 parts of silver salt, 20-80 parts of solvent, 1-5 parts of borate, 1-3 parts of organic metal complex, 5-10 parts of regulator, 7-10 parts of drier, 1-5 parts of resin material and 10-20 parts of diluent.
Further, the silver salt is one or more of silver nitrate, silver oxalate, silver sulfate and the like. Specifically, the silver salt is preferably 35 parts silver nitrate (followed by 35 parts silver sulfate, followed by 35 parts silver oxalate).
Further, the solvent is one or more of deionized water, pure water, distilled water and the like. Specifically, the solvent is preferably 60 parts of deionized water (next 60 parts of pure water, next 60 parts of distilled water); it should be noted that, in the process of preparing the nano silver solution, the solvent is used in batches (i.e. added in steps and mixed with different materials).
Further, the borate is one or more of boric acid, sodium borate, potassium borate and the like. Specifically, the borate is preferably 3 parts of boric acid (next 3 parts of sodium borate, next 3 parts of potassium borate).
Furthermore, the organic metal complex is one or more of organic bismuth, organic tin, organic silicon and the like. Specifically, the organometallic complex is preferably 2 parts of organobismuth (next 2 parts of organotin, again 2 parts of organosilicon).
Furthermore, the regulator is one or more of ascorbic acid, hydrazine hydrate, formaldehyde, malic acid and the like. Specifically, the regulator is preferably 10 parts of ascorbic acid (next 10 parts of hydrazine hydrate, next 10 parts of formaldehyde, and finally 10 parts of malic acid).
Furthermore, the drier is one or more of neodecanoic acid, isooctanoic acid, naphthenic acid and the like. Specifically, the drier is preferably 7 parts of neodecanoic acid (next 7 parts of isooctanoic acid, next 7 parts of naphthenic acid).
Further, the resin material is one or more of PVP polyvidone K30, water-based CAB, water-based acrylic acid and the like. Specifically, the resin material is preferably 3 parts PVP povidone K30 (next 3 parts aqueous CAB, again 3 parts aqueous acrylic acid).
Furthermore, the diluent is one or more of ethylene glycol butyl ether, ethylene glycol hexyl ether, ethylene glycol methyl ether and the like which are mixed. Specifically, the diluent is preferably 10 parts ethylene glycol butyl ether (next 10 parts ethylene glycol hexyl ether, next 10 parts ethylene glycol methyl ether).
The preparation method of the nano silver solution for spraying the 5G dielectric ceramic filter comprises the following steps (the preferred materials are taken as examples for explanation)
Step 1, adding 35 parts of silver nitrate into 10 parts of deionized water, mixing and dissolving into a transparent solution, heating, when the transparent solution is heated to 80 ℃, slowly adding 7 parts of neodecanoic acid while stirring, continuously heating to 120 ℃ and 150 ℃, stopping stirring, forming a yellowish viscous liquid, adding 5 parts of ethylene glycol monobutyl ether to prepare a silver nanoparticle stock solution, and after the silver nanoparticle stock solution is cooled, putting the silver nanoparticle stock solution into a plastic tank for later use;
step 2, adding 3 parts of boric acid into 10 parts of deionized water, mixing and dissolving to obtain a transparent solution, adding 2 parts of organic bismuth, stirring, and adding 10 parts of ascorbic acid in the stirring process to obtain a viscous liquid through mixing; then adding the rest 5 parts of ethylene glycol butyl ether to prepare an inorganic binder solution after high-temperature sintering;
step 3, dissolving 3 parts of PVP polyvidone K30 in 10 parts of deionized water to prepare an organic temporary low-temperature binding phase solution;
and 4, mixing and stirring the silver nanoparticle stock solution prepared in the step 1 and the inorganic binder liquid prepared in the step 2 to prepare a yellowish-to-deep-yellowish nano silver nanoparticle suspension, adding the organic temporary low-temperature binder phase solution prepared in the step 3 to obtain a mixed solution, and adding the rest 30 parts of deionized water into the mixed solution under stirring to dilute the mixed solution to prepare a nano silver solution.
Further, silver neodecanoate (silver isooctanoate or silver naphthenate, etc.) is prepared from silver nitrate (silver oxalate or silver sulfate, etc.) and neodecanoic acid (isooctanoate or naphthenic acid, etc.) in a stainless steel reaction kettle heated by high-temperature heat transfer oil.
The spraying method of the nano silver solution for spraying the 5G dielectric ceramic filter comprises the following steps:
step a, taking a proper amount of nano silver solution, stirring and transferring the nano silver solution to a pumping hydraulic container on spraying equipment, and adjusting the spraying caliber size and flow according to actual needs to spray;
step b, spraying to prepare a uniform silver conductive coating, and then drying in a drying furnace at the low temperature of 100 ℃ and 200 ℃;
and c, sintering at the temperature of 500-600 ℃ for 10min to obtain the compact silvery conductive coating.
The nano silver solution is suitable for the spraying process of the silver conductive coating in the 5G dielectric ceramic filter, the 5G dielectric ceramic filter is formed by high-temperature die casting of ceramic powder materials with high electric constants such as zirconium oxide and yttrium oxide, the surface hardness is high, and a glass phase is generated, so when the silver conductive coating on the surface of the 5G dielectric ceramic filter is manufactured, elements such as boron, silicon, tin or bismuth are added into the nano silver solution to serve as a binder for assisting silver materials to be adhered to the 5G dielectric ceramic filter during high-temperature sintering; the nano silver solution adopts organic silicon, organic tin or organic bismuth and the like as metal oxides (the organic metal forms oxides at a certain temperature) to combine into a material similar to glass powder, can form a molten glass phase at the sintering temperature of 300-400 ℃, and is combined with a substrate of a 5G dielectric ceramic filter to firmly adhere silver nano particles; specifically, the characteristics of organic metal capable of being sintered into metal oxide are utilized to be combined with organic silver under the catalysis condition to generate simple substance silver crystals capable of being sintered at low temperature, and the simple substance silver crystals and the metal oxide form a glass phase to be used as an adhesion promoter, so that the silver conductive coating with strong adhesion and good conductivity is manufactured. Silver nanoparticles adopt silver salt which is converted into organic silver, and the organic silver and the organic metal form a silver conductive coating which can be sintered and formed under certain catalytic conditions; the silver nano particles are low in sintering temperature, and combined with metal oxides to form a silver conductive coating with strong adhesive force and good conductivity to cover the surface of the 5G dielectric ceramic filter. By applying the nano silver solution, the prepared product has small insertion loss, good electromagnetic wave shielding efficiency and excellent conductivity; in addition, the nano silver solution is matched with a proper film forming agent, so that the nano silver solution can have good adhesive force on 5G dielectric ceramic filters made of various materials.
The foregoing is a preferred embodiment of the present invention, and the basic principles, principal features and advantages of the invention are shown and described. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are intended to illustrate the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and the invention is intended to be protected by the following claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A nano silver solution for spraying a 5G dielectric ceramic filter is characterized in that: according to the weight portion, the silver salt is 10-60 portions, the solvent is 20-80 portions, the borate is 1-5 portions, the organic metal complex is 1-3 portions, the regulator is 5-10 portions, the drier is 7-10 portions, the resin material is 1-5 portions, and the thinner is 10-20 portions.
2. The nano silver solution for sputtering of 5G dielectric ceramic filter according to claim 1, wherein: the silver salt is one or a mixture of more than two of silver nitrate, silver oxalate and silver sulfate.
3. The nano silver solution for sputtering of 5G dielectric ceramic filter according to claim 3, wherein: the borate is one or a mixture of more than two of boric acid, sodium borate and potassium borate.
4. The nano silver solution for sputtering of 5G dielectric ceramic filter according to claim 1, wherein: the organic metal complex is one or more of organic bismuth, organic tin and organic silicon.
5. The nano silver solution for sputtering of 5G dielectric ceramic filter according to claim 1, wherein: the regulator is one or more of ascorbic acid, hydrazine hydrate, formaldehyde and malic acid.
6. The nano silver solution for sputtering of 5G dielectric ceramic filter according to claim 1, wherein: the drier is one or more of neodecanoic acid, isooctanoic acid and naphthenic acid.
7. The nano silver solution for sputtering of 5G dielectric ceramic filter according to claim 1, wherein: the resin material is one or more of PVP polyvidone K30, water-based CAB and water-based acrylic acid.
8. The nano silver solution for sputtering of 5G dielectric ceramic filter according to claim 1, wherein: the diluent is one or a mixture of more than two of ethylene glycol butyl ether, ethylene glycol hexyl ether and ethylene glycol methyl ether.
9. The method for preparing a nanosilver solution for sputtering a 5G dielectric ceramic filter as claimed in claim 1, wherein: comprises the following steps
Step 1, adding silver salt into a part of solvent, mixing and dissolving the silver salt into a transparent solution, heating the solution to 80 ℃, adding a drier while stirring the solution, continuing heating the solution to 120-150 ℃, stopping stirring the solution, and adding a part of diluent to prepare a silver nanoparticle stock solution for later use;
step 2, adding borate into the other part of solvent, mixing and dissolving to obtain a transparent solution, adding an organic metal complex, stirring, and adding a regulator during stirring to obtain a viscous liquid; then adding the rest diluent to prepare an inorganic binder solution after high-temperature sintering;
step 3, dissolving the resin material by using another part of solvent to prepare an organic temporary low-temperature bonding phase solution;
and 4, mixing and stirring the silver nanoparticle stock solution prepared in the step 1 and the inorganic binder liquid prepared in the step 2 to prepare a nano silver nanoparticle suspension, adding the organic temporary low-temperature binder phase solution prepared in the step 3 to obtain a mixed solution, and adding the rest solvent into the mixed solution under stirring to dilute the mixed solution to prepare a nano silver solution.
10. A sputtering method of a nanosilver solution for sputtering a 5G dielectric ceramic filter according to claim 1, wherein: the method comprises the following steps:
step a, taking a proper amount of nano silver solution, stirring and transferring the nano silver solution to a pumping hydraulic container on spraying equipment, and adjusting the spraying caliber size and flow rate to perform spraying;
step b, spraying to prepare a uniform silver conductive coating, and then drying in a drying furnace at the low temperature of 100 ℃ and 200 ℃;
and c, sintering at the temperature of 500-600 ℃ for 10min to obtain the compact silver conductive coating.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010158256.0A CN111393893A (en) | 2020-03-09 | 2020-03-09 | Nano silver solution for spraying 5G dielectric ceramic filter, preparation method and spraying method thereof |
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| CN202010158256.0A CN111393893A (en) | 2020-03-09 | 2020-03-09 | Nano silver solution for spraying 5G dielectric ceramic filter, preparation method and spraying method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112034147A (en) * | 2020-08-19 | 2020-12-04 | 江苏国瓷泓源光电科技有限公司 | Method for detecting weldability of silver paste of ceramic filter |
| CN112712913A (en) * | 2020-12-15 | 2021-04-27 | 陕西彩虹新材料有限公司 | Silver oxide slurry for electronic component and preparation method thereof |
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| CN112034147A (en) * | 2020-08-19 | 2020-12-04 | 江苏国瓷泓源光电科技有限公司 | Method for detecting weldability of silver paste of ceramic filter |
| CN112034147B (en) * | 2020-08-19 | 2022-08-12 | 江苏国瓷泓源光电科技有限公司 | Method for detecting weldability of silver paste of ceramic filter |
| CN112712913A (en) * | 2020-12-15 | 2021-04-27 | 陕西彩虹新材料有限公司 | Silver oxide slurry for electronic component and preparation method thereof |
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Application publication date: 20200710 |