CN113823458A - Low-resistance silver paste and preparation method and application thereof - Google Patents
Low-resistance silver paste and preparation method and application thereof Download PDFInfo
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- CN113823458A CN113823458A CN202110947916.8A CN202110947916A CN113823458A CN 113823458 A CN113823458 A CN 113823458A CN 202110947916 A CN202110947916 A CN 202110947916A CN 113823458 A CN113823458 A CN 113823458A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 26
- 239000004332 silver Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 239000013034 phenoxy resin Substances 0.000 claims description 18
- 229920006287 phenoxy resin Polymers 0.000 claims description 18
- 229920001225 polyester resin Polymers 0.000 claims description 18
- 239000004645 polyester resin Substances 0.000 claims description 18
- 229920006395 saturated elastomer Polymers 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 15
- 239000012948 isocyanate Substances 0.000 claims description 13
- 150000002513 isocyanates Chemical class 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 11
- 238000007639 printing Methods 0.000 claims description 11
- 239000002518 antifoaming agent Substances 0.000 claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 7
- 239000003759 ester based solvent Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 2
- 230000001413 cellular effect Effects 0.000 claims 2
- 229920005989 resin Polymers 0.000 description 25
- 239000011347 resin Substances 0.000 description 25
- 239000001993 wax Substances 0.000 description 21
- 239000007788 liquid Substances 0.000 description 15
- 238000003756 stirring Methods 0.000 description 15
- 238000001914 filtration Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 239000012535 impurity Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 description 9
- KUBDPQJOLOUJRM-UHFFFAOYSA-N 2-(chloromethyl)oxirane;4-[2-(4-hydroxyphenyl)propan-2-yl]phenol Chemical compound ClCC1CO1.C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 KUBDPQJOLOUJRM-UHFFFAOYSA-N 0.000 description 9
- 238000001723 curing Methods 0.000 description 7
- 238000000227 grinding Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 238000010008 shearing Methods 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- 238000010023 transfer printing Methods 0.000 description 5
- 238000003828 vacuum filtration Methods 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- -1 ether ester Chemical class 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000013035 low temperature curing Methods 0.000 description 3
- 238000007649 pad printing Methods 0.000 description 3
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 2
- 241001089723 Metaphycus omega Species 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- JDSQBDGCMUXRBM-UHFFFAOYSA-N 2-[2-(2-butoxypropoxy)propoxy]propan-1-ol Chemical compound CCCCOC(C)COC(C)COC(C)CO JDSQBDGCMUXRBM-UHFFFAOYSA-N 0.000 description 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- SVONRAPFKPVNKG-UHFFFAOYSA-N 2-ethoxyethyl acetate Chemical compound CCOCCOC(C)=O SVONRAPFKPVNKG-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004210 ether based solvent Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
- C09D11/104—Polyesters
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/108—Hydrocarbon resins
-
- 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
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Conductive Materials (AREA)
Abstract
The invention provides a low-resistance silver paste and a preparation method and application thereof.
Description
Technical Field
The embodiment of the invention relates to the field of but not limited to conductive materials, and particularly relates to low-resistance silver paste and a preparation method and application thereof.
Background
In the 5G era, the number of smart phone terminal antennas is continuously overlapped, and the smart phone terminal antennas are developed towards the direction of high integration and complexity. For this reason, the internal antenna is becoming the mainstream of antenna design instead of the external antenna.
The existing mobile phone built-in antenna is mainly prepared by double-color injection molding, print forming (PDS), a Flexible Printed Circuit (FPC), Laser (LDS) and the like. The PDS process gradually becomes a preferred antenna scheme of Sub-6 frequency band in the 5G era due to the advantages of stable process, controllable size, high precision, simple and efficient process and the like.
The PDS process is to directly print silver paste on the inner shell of the mobile phone, and the inner shell of the mobile phone is mostly of an arc-shaped structure and is mainly realized by a transfer printing mode. The existing process has the problem of poor consistency of mass production, mainly because the resistance value of PDS silver paste is difficult to reduce to a lower level, the resistance value fluctuation is large in the process of mass printing, and the stability is poor.
Disclosure of Invention
The following is a summary of the subject matter described in detail herein. This summary is not intended to limit the scope of the claims.
The embodiment of the invention provides a low-resistance silver paste which has the characteristics of low resistance value, good adhesive force and certain wear resistance and can be used for preparing a printed antenna of a mobile phone.
In a first aspect, an embodiment of the present invention provides a low resistance silver paste, including the following raw materials in parts by weight:
2-15 parts of saturated polyester resin, 2-10 parts of phenoxy resin, 60-80 parts of silver powder, 8-30 parts of ester solvent, 1-5 parts of closed isocyanate and 1-5 parts of PP wax powder.
The saturated polyester resin and the phenoxy resin are matched, so that the viscosity and the fluidity of the slurry can be adjusted, the stability of the resistance value in the batch printing process is ensured, the phenomena of wire breakage, air holes and the like are reduced in the continuous printing process, and the preparation method is suitable for preparing the printed mobile phone antenna.
The hydroxyl value of the saturated polyester resin and the phenoxy resin may be 10mgKOH/g or less, including 10 mgKOH/g.
The closed isocyanate is used as a curing agent and reacts with hydroxyl in the saturated polyester resin and the phenoxy resin, so that the adhesive force, the mechanical property and the drying property of the silver paste are improved. When the addition amount of the blocked isocyanate is excessive relative to the addition amount of the blocked isocyanate and the resin component, hydroxyl groups in the resin can participate in reaction, and when the surface of the coated substrate has hydroxyl groups, redundant curing agents can also react with the hydroxyl groups on the surface of the substrate, so that the adhesion is further improved.
The silver powder can improve the storage stability of the paste besides providing conductivity. It was found experimentally that in the case where the silver powder content is significantly less than 60 parts, for example, 30 parts or less, the storage stability of the paste is lowered.
Compared with common ketone or ether solvents, the ester solvent can realize lower resistance value and more excellent adhesive force.
The PP wax powder can improve the wear resistance and simultaneously can not improve the resistance value of the silver paste.
Through raw material matching, the silver paste provided by the embodiment of the invention can realize excellent conductivity and adhesion, can realize that the sheet resistance is below 8m omega/□ @1mil even for a low-temperature curing system, for example, blocked isocyanate with the deblocking temperature of below 90 ℃, has the adhesion of 5B (Baige test) on a PC substrate, has certain wear resistance, is opaque after being ground by 300 rings of RCA 175g, has good printability and dryness, is suitable for printing mobile phone antennas in a pad printing mode, and is used for parts which are not easily worn.
According to some embodiments of the invention, the raw material of the low resistance silver paste further comprises an auxiliary agent. The auxiliary agent can be a dispersing agent and a defoaming agent.
The dispersant may be used in an amount of 1 to 5 parts by weight.
The defoaming agent may be used in an amount of 1 to 5 parts by weight.
According to some embodiments of the invention, the ester solvent is at least one of DBE, ether ester type solvent. As an example, the ether ester-based solvent may be a common propylene glycol ether ester-based solvent, a glycol ether ester-based solvent, for example, ethylene glycol ethyl ether acetate, propylene glycol methyl ether acetate, diethylene glycol ethyl ether acetate, or the like.
When the silver paste is used for printing the mobile phone antenna, the curing system is generally required to be cured at a low temperature, for example, the curing temperature is below 100 ℃, and the drying property and the low resistance property are more difficult to be simultaneously achieved in the low-temperature curing process than in the medium-high temperature curing system. The ester solvent is selected, so that the release performance of the resin to the solvent can be regulated and controlled, and the excellent low-resistance characteristic is obtained while the drying rate is ensured.
According to some embodiments of the invention, the blocked isocyanate has a deblocking temperature of less than or equal to 90 ℃ to meet the low temperature cure requirements.
In a second aspect, an embodiment of the present invention further provides a method for preparing the low resistance silver paste, which is characterized by including:
dissolving the saturated polyester resin and the phenoxy resin in the ester solvent according to the proportion, adding the rest raw materials, and uniformly mixing.
According to some embodiments of the present invention, the saturated polyester resin and the phenoxy resin are dissolved in the ester solvent, wherein heating may be performed during the dissolution process to complete the rapid dissolution of the resin.
According to some embodiments of the invention, before the adding the remaining raw materials, further comprising: and filtering the mixed solution of the saturated polyester resin, the phenoxy resin and the ester solvent for the first time. Wherein, the mesh number of the first filtration can be 500-1000 meshes.
According to some embodiments of the present invention, after adding the rest of the raw materials and mixing, grinding and filtering the obtained mixture for the second time are further included. Wherein, the mesh number of the second filtration can be not lower than the first filtration, for example, in the case that the mesh number of the first filtration is 500-1000 meshes, the mesh number of the second filtration can be 1000 meshes.
In a third aspect, the embodiment of the invention further provides an application of the low-resistance silver paste in printing and forming.
The print forming may be pad printing or screen printing.
In a fourth aspect, an embodiment of the present invention further provides a printed circuit, which is prepared by printing, curing and molding the low resistance silver paste.
The printed wiring may be a printed antenna. When the printed antenna is printed on the mobile phone cover plate, the printing may be pad printing.
In a fifth aspect, an embodiment of the present invention further provides a mobile phone cover plate, where the printed circuit is disposed on the mobile phone cover plate.
In a sixth aspect, an embodiment of the present invention further provides a mobile phone, where the mobile phone includes the above mobile phone cover plate.
The terms:
"silver powder" refers to conductive silver powder known in the art, and may be surface-modified silver powder, which may be spherical or spheroidal in shape and may have a particle size of micron or submicron order, in order to improve dispersibility of the silver powder.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
1) Weighing 60 parts by mass of diethylene glycol ethyl ether acetate, pouring the diethylene glycol ethyl ether acetate into a reaction kettle, starting stirring and heating to 40 ℃, then weighing 27 parts by mass of Degussa L206 saturated polyester resin and 13 parts by mass of Lincarbon PKHH phenoxy resin, slowly adding the Degussa L206 saturated polyester resin and the Lincarbon PKHH phenoxy resin into the reaction kettle, heating while stirring until the resin is completely dissolved at the temperature of 80 ℃, then cooling to normal temperature, and filtering impurities by using a 800-mesh filter bag to obtain a clear and transparent liquid resin carrier;
2) taking 28 parts by mass of the liquid resin carrier obtained in the step 1), adding the liquid resin carrier into a new reaction kettle, sequentially adding 60 parts by mass of submicron conductive silver powder, 5 parts by mass of Asahi-converted MF-K60X-enclosed isocyanate, 1 part by mass of Tianshi PPW-0901 wax powder, 1 part by mass of Luobo-Runji dispersant 24000 and 5 parts by mass of De-Cui 6800 defoaming agent, and uniformly stirring by using a disc type dispersing machine;
3) shearing, grinding and dispersing the uniform material prepared in the step 2) at a high speed by using a three-roller machine to obtain a fine product with the fineness of less than 5 mu m;
4) and (3) carrying out suction filtration on the fine product prepared in the step 3) by using a vacuum filtration device through a 1000-mesh gauze, and removing impurities.
The viscosity was measured by a lyre VT-06 viscometer to be 200dpa.s, the fineness was measured by a blade fineness meter to be 3 μm, a conductive line was transfer-printed on a PC material by a transfer printer to have a print thickness of 8-10 μm, the cured product was baked at 80 ℃ for 1 hour, the pencil hardness was measured to be 3H, the RCA 175g was measured to be 300 cycles without abrasion, the line resistance was 1.1. omega., the square resistance was 6.6 m. omega./□ @1mil, and the adhesion was 5B.
Example 2
1) Weighing 60 parts by mass of DBE, pouring the DBE into a reaction kettle, stirring and heating to 40 ℃, then weighing 20 parts by mass of the delousel 206 saturated polyester resin and 20 parts by mass of the carbon-linked PKHH phenoxy resin, slowly adding the resin into the reaction kettle, stirring and heating until the resin is completely dissolved at the temperature of 80 ℃, then cooling to normal temperature, and filtering impurities by using a 800-mesh filter bag to obtain a clear and transparent liquid resin carrier;
2) taking 28 parts by mass of the liquid resin carrier obtained in the step 1), adding the liquid resin carrier into a new reaction kettle, sequentially adding 60 parts by mass of submicron conductive silver powder, 1 part by mass of Asahi-converted MF-K60X-enclosed isocyanate, 5 parts by mass of Tianshi PPW-0901 wax powder, 5 parts by mass of Luobo-Runji dispersant 24000 and 1 part by mass of De-Cui 6800 defoaming agent, and uniformly stirring by using a disc type dispersing machine;
3) shearing, grinding and dispersing the uniform material prepared in the step 2) at a high speed by using a three-roller machine to obtain a fine product with the fineness of less than 5 mu m.
4) And (3) carrying out suction filtration on the fine product prepared in the step 3) by using a vacuum filtration device through a 1000-mesh gauze, and removing impurities.
The viscosity was measured by a lyre VT-06 viscometer to be 200dpa.s, the fineness was measured by a blade fineness meter to be 3 μm, a conductive line was transfer-printed on a PC material by a transfer printer to have a print thickness of 8-10 μm, the cured product was baked at 80 ℃ for 1 hour, the pencil hardness was measured to be 3H, the RCA 175g was measured to be 300 cycles without abrasion, the line resistance was 1.2. omega., the square resistance was 6.7 m. omega./□ @1mil, and the adhesion was 5B.
Example 3
1) Weighing 30 parts by mass of DBE and 30 parts by mass of diethylene glycol butyl ether acetate, pouring the DBE and the diethylene glycol butyl ether acetate into a reaction kettle, starting stirring and heating to 40 ℃, then weighing 13 parts by mass of degussa L206 saturated polyester resin and 27 parts by mass of carbon-linked PKHH phenoxy resin, slowly adding the polyester resin and the carbon-linked PKHH phenoxy resin into the reaction kettle, stirring and heating until the resin is completely dissolved at the temperature of 80 ℃, then cooling to normal temperature, and filtering impurities by using a 800-mesh filter bag to obtain a clear and transparent liquid resin carrier;
2) taking 16 parts by mass of the liquid resin carrier obtained in the step 1), adding the liquid resin carrier into a new reaction kettle, sequentially adding 80 parts by mass of submicron conductive silver powder, 1 part by mass of Asahi-converted MF-K60X-enclosed isocyanate, 1 part by mass of Tianshi PPW-0901 wax powder, 1 part by mass of Luobo-Rui dispersant 24000 and 1 part by mass of De-Cui 6800 defoaming agent, and uniformly stirring by using a disc type dispersing machine;
3) shearing, grinding and dispersing the uniform material prepared in the step 2) at a high speed by using a three-roller machine to obtain a fine product with the fineness of less than 5 mu m.
4) And (3) carrying out suction filtration on the fine product prepared in the step 3) by using a vacuum filtration device through a 1000-mesh gauze, and removing impurities.
The viscosity measured by a Ribo VT-06 viscometer is 210dpa.s, the fineness measured by a scraper fineness meter is 3 mu m, a transfer printing machine is used for transfer printing a conductive circuit on a PC material, the printing thickness is 8-10 mu m, the conductive circuit is cured after being baked for 1 hour at 80 ℃, the pencil hardness test is 3H, the RCA 175g test is 300 circles and is not worn, the line resistance is 1.1 omega, the square resistance is 6.5m omega/□ @1mil, and the adhesion force is 5B.
Example 4
1) Weighing 60 parts by mass of diethylene glycol ethyl ether acetate, pouring the diethylene glycol ethyl ether acetate into a reaction kettle, starting stirring and heating to 40 ℃, then weighing 20 parts by mass of Degussa L206 saturated polyester resin and 20 parts by mass of Lincarbon PKHH phenoxy resin, slowly adding the Degussa L206 saturated polyester resin and the Lincarbon PKHH phenoxy resin into the reaction kettle, heating while stirring until the resin is completely dissolved at the temperature of 80 ℃, then cooling to normal temperature, and filtering impurities by using a 800-mesh filter bag to obtain a clear and transparent liquid resin carrier;
2) taking 20 parts by mass of the liquid resin carrier in the step 1), adding the liquid resin carrier into a new reaction kettle, sequentially adding 75 parts by mass of submicron conductive silver powder, 1.5 parts by mass of Asahi-formed MF-K60X enclosed isocyanate, 1.5 parts by mass of Tianshi PPW-0901 wax powder, 1 part by mass of Luobo-Runji dispersant 24000 and 1 part by mass of De-Cui 6800 defoaming agent, and uniformly stirring by using a disc type dispersing machine;
3) shearing, grinding and dispersing the uniform material prepared in the step 2) at a high speed by using a three-roller machine to obtain a fine product with the fineness of less than 5 mu m.
4) And (3) carrying out suction filtration on the fine product prepared in the step 3) by using a vacuum filtration device by using a 1000-mesh gauze to remove impurities.
The viscosity was measured by a lyre VT-06 viscometer to be 200dpa.s, the fineness was measured by a blade fineness meter to be 3 μm, a conductive line was transfer-printed on a PC material by a transfer printer to have a print thickness of 8-10 μm, the cured product was baked at 80 ℃ for 1 hour, the pencil hardness was measured to be 3H, the RCA 175g was measured to be 300 cycles without abrasion, the line resistance was 1.0 Ω, the sheet resistance was 6.3m Ω/□ @1mil, and the adhesion was 5B.
Example 5
1) Weighing 60 parts by mass of diethylene glycol ethyl ether acetate, pouring the diethylene glycol ethyl ether acetate into a reaction kettle, starting stirring and heating to 40 ℃, then weighing 20 parts by mass of Degussa L206 saturated polyester resin and 20 parts by mass of Lincarbon PKHH phenoxy resin, slowly adding the Degussa L206 saturated polyester resin and the Lincarbon PKHH phenoxy resin into the reaction kettle, heating while stirring until the resin is completely dissolved at the temperature of 80 ℃, then cooling to normal temperature, and filtering impurities by using a 800-mesh filter bag to obtain a clear and transparent liquid resin carrier;
2) taking 17 parts by mass of the liquid resin carrier obtained in the step 1), adding the liquid resin carrier into a new reaction kettle, sequentially adding 78 parts by mass of submicron conductive silver powder, 1.5 parts by mass of Asahi-modified MF-K60X enclosed isocyanate, 1.5 parts by mass of Tianshi PPW-0901 wax powder, 1 part by mass of Luobo-Runji dispersant 24000 and 1 part by mass of De-Cui 6800 defoaming agent, and uniformly stirring by using a disc type dispersing machine;
3) shearing, grinding and dispersing the uniform material prepared in the step 2) at a high speed by using a three-roller machine to obtain a fine product with the fineness of less than 5 mu m.
4) And (3) carrying out suction filtration on the fine product prepared in the step 3) by using a vacuum filtration device by using a 1000-mesh gauze to remove impurities.
The viscosity measured by a lyre VT-06 viscometer is 230dpa.s, the fineness measured by a scraper fineness meter is 3 μm, a transfer printing machine is used for transfer printing a conductive circuit on a PC material, the printing thickness is 8-10 μm, the conductive circuit is cured after being baked for 1 hour at 80 ℃, the pencil hardness test is 3H, the RCA 175g test is 300 circles without abrasion, the line resistance is 1.0 omega, the square resistance is 6.3m omega/□ @1mil, and the adhesion force is 5B.
Example 6
Compared with the example 1, the difference is that the PP wax powder is replaced by Tianshi PPW-0901 wax powder by equal amount of PPW-0931PP wax or PPW-0922PP wax, and the rest is not changed. The measured line resistance is 1.3 omega, and the performances are equivalent except the resistance.
It can be seen that the low-resistance silver paste of the embodiment has high curing efficiency at low temperature below 90 ℃, the resistance value of the printed circuit is below 1.5 omega, the sheet resistance can realize below 8m omega/□ @1mil, the low-resistance silver paste has good adhesive force on a PC substrate, and the low-resistance silver paste has certain wear resistance in a Baige test 5B, can meet the performance requirement of a low-resistance mobile phone antenna because the RCA 175g is ground for 300 circles, and has remarkable application value.
In the above examples, some of the test methods are illustrated below:
viscosity: reading by measuring 1Min at 25 ℃ with a Liyin VT-06 viscometer and a 2# rotor;
square resistance: printed wiring (length x width) 100mm x 1mm, cured under baking conditions, measured the resistance of the wiring R (omega) using a direct current resistance meter, measured the thickness d (mum) of the sample using a thickness meter, and then calculated the sheet resistance R according to the following formula□(mΩ/□@1mil)。
Comparative example 1
The difference from example 2 is that the diethylene glycol monoethyl ether acetate was replaced with the same amount of isophorone, which is a ketone solvent with a close boiling point, and the rest was unchanged. The line resistance was measured to be 3 Ω and the adhesion force was found to be 4B.
Comparative example 2
The difference from example 2 is that diethylene glycol ethyl ether acetate was replaced with the same amount of ethylene glycol butyl ether as the high boiling ether solvent, and the rest was unchanged. The line resistance was measured to be 3.5 Ω and the adhesion force was measured to be 4B.
Comparative example 3
The difference compared to example 1 is that the PP wax powder was replaced with the other wax powders of table 1 and part of the test results are shown in table 1.
TABLE 1
Wax powder type and brand | Line resistor | Wear resistance |
PTFE-0103 polytetrafluoroethylene wax powder | 2.3Ω | 300 circles |
PTFE-0104 polytetrafluoroethylene wax powder | 1.8Ω | 280 rings |
NEW-0401C polyamide wax | 2.0Ω | 180 circles |
PEW-0320A polyethylene wax | 1.9Ω | 120 circles |
Example 1: PPW-0901PP wax | 1.1Ω | 300 circles |
From the above results, it is known that the ester solvent has a good drying effect and an optimal resistance value and adhesion. The resistance value of PP waxes is significantly lower than other types of waxes, while the wear resistance is good.
While the preferred embodiments of the present invention have been described in detail, it will be understood by those skilled in the art that the foregoing and various other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention.
Claims (10)
1. The low-resistance silver paste is characterized by comprising the following raw materials in parts by weight:
2-15 parts of saturated polyester resin, 2-10 parts of phenoxy resin, 60-80 parts of silver powder, 8-30 parts of ester solvent, 1-5 parts of closed isocyanate and 1-5 parts of PP wax powder.
2. The low resistance silver paste of claim 1, further comprising: dispersing agents and defoaming agents; and optionally, 1-5 parts of a dispersant; and optionally, the defoaming agent is 1-5 parts.
3. The low-resistance silver paste as recited in claim 1, wherein the ester solvent is at least one of DBE and ether ester solvents.
4. The low resistance silver paste of claim 1, wherein the blocked isocyanate has a deblocking temperature of less than or equal to 90 ℃.
5. The method for preparing the low-resistance silver paste according to any one of claims 1 to 4, wherein the method comprises the following steps:
dissolving the saturated polyester resin and the phenoxy resin in the ester solvent according to the proportion, adding the rest raw materials, and uniformly mixing.
6. Use of the low resistance silver paste according to any one of claims 1 to 4 in print forming.
7. A printed circuit, which is prepared by printing, curing and molding the low-resistance silver paste as claimed in any one of claims 1 to 4.
8. The printed wiring of claim 7 wherein said printed wiring is a printed antenna.
9. A cover plate for a cellular phone, wherein the printed wiring of claim 8 is provided on the cover plate for a cellular phone.
10. A handset comprising the handset cover of claim 9.
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