CN111627590A - Conductive silver paste for chip inductor and preparation method thereof - Google Patents
Conductive silver paste for chip inductor and preparation method thereof Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000011521 glass Substances 0.000 claims abstract description 66
- 239000000843 powder Substances 0.000 claims abstract description 39
- 229910052709 silver Inorganic materials 0.000 claims abstract description 32
- 239000004332 silver Substances 0.000 claims abstract description 30
- 239000003960 organic solvent Substances 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000002952 polymeric resin Substances 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 229920003002 synthetic resin Polymers 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000005303 weighing Methods 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000004744 fabric Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 20
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 claims description 10
- 229910052681 coesite Inorganic materials 0.000 claims description 10
- 229910052906 cristobalite Inorganic materials 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052682 stishovite Inorganic materials 0.000 claims description 10
- 229910052905 tridymite Inorganic materials 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 229910052593 corundum Inorganic materials 0.000 claims description 9
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000004014 plasticizer Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 5
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 5
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 5
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 5
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 5
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 claims description 5
- 229960001826 dimethylphthalate Drugs 0.000 claims description 5
- 229920000570 polyether Polymers 0.000 claims description 5
- 229940116411 terpineol Drugs 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000020 Nitrocellulose Substances 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- 229920001220 nitrocellulos Polymers 0.000 claims description 4
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 claims description 4
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000001856 Ethyl cellulose Substances 0.000 claims description 3
- 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 claims description 3
- 229920001249 ethyl cellulose Polymers 0.000 claims description 3
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 2
- 241000779819 Syncarpia glomulifera Species 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 239000001739 pinus spp. Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 2
- 229940036248 turpentine Drugs 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims 1
- 125000005375 organosiloxane group Chemical group 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 6
- 239000001913 cellulose Substances 0.000 description 6
- 238000011056 performance test Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000013538 functional additive Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- -1 silver ions Chemical class 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001629 suppression Effects 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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/28—Coils; Windings; Conductive connections
- H01F27/29—Terminals; Tapping arrangements for signal inductances
Abstract
The invention relates to a conductive silver paste for a chip inductor and a preparation method thereof, wherein the conductive silver paste comprises the following components in parts by weight: 75-85 parts of metal silver powder; 3-8 parts of glass powder; 15-31 parts of organic carrier; 1-20 parts of organic solvent. Weighing the polymer resin and the organic solvent, heating the polymer resin and the organic solvent to 80 ℃, keeping the temperature constant until the polymer resin is completely dissolved, and filtering and removing impurities on a 300-400-mesh screen cloth when the polymer resin is cooled to below 25 ℃ to obtain an organic carrier; weighing metal silver powder and glass powder, fully mixing the metal silver powder and the glass powder with an organic solvent and an organic carrier in a mixer, and then dispersing at a high speed by using a high-speed dispersion machine to obtain uniform slurry; and grinding the slurry in a three-roll mill, and finely adjusting by using a roller to control the fineness of the silver paste to be below 8 mu m and the viscosity to be 35-45 Pa.S, thus preparing the conductive silver paste for the chip inductor. The product prepared by the invention has small resistance, good adhesion with a base material after sintering, good platability and good weldability.
Description
Technical Field
The invention belongs to the technical field of conductive silver paste, and particularly relates to conductive silver paste for a chip inductor and a preparation method thereof.
Background
As one of the three passive electronic components, the inductor accounts for about 10-15% of the matching amount of the whole electronic component. The inductors can be classified into two types, namely plug-in inductors and chip inductors, and the chip inductors can be classified into two types, namely winding type inductors and laminated type inductors. The laminated chip inductor (MLCI) breaks through the limitation of the traditional winding process and realizes the miniaturization and large-scale production of products; the high-power chip inductor has the advantages of small volume, low production cost, high reliability, excellent EMI resistance and the like, and becomes the main force of a new generation chip inductor. The inductor has the main functions of signal screening, noise filtering, current stabilizing, electromagnetic interference suppression and the like, and is widely applied to the fields of communication, computers, peripheral products, consumer electronics, office automation, automobile electronics and the like.
Laminated Chip Inductors (MLCI) are generally composed of a substrate, a metal film electrode and an external electrode, wherein conventional external electrode pastes are mostly thick film pastes composed of a lead-containing glass frit mixed with a metal or alloy such as Ag or Ag/Pd. Chinese patent CN105761775B discloses a conductive silver paste for external electrodes of a chip inductor and a preparation method thereof, wherein the conductive silver paste comprises the following raw materials in parts by weight: 65-85 parts of metal silver powder; 3-8 parts of glass powder; 15-31 parts of organic carrier; 1-20 parts of organic solvent. Weighing the polymer resin and the organic solvent, heating the polymer resin and the organic solvent to 80 ℃, keeping the temperature constant until the polymer resin is completely dissolved, and filtering and removing impurities on a 300-400-mesh screen cloth when the polymer resin is cooled to below 40 ℃ to obtain an organic carrier; weighing metal silver powder and glass powder, fully mixing the metal silver powder and the glass powder with an organic solvent and an organic carrier in a mixer, and then dispersing at a high speed by using a high-speed dispersion machine to obtain uniform slurry; and grinding the slurry in a three-high mill, and finely adjusting by using a roller to control the fineness of the silver paste to be less than 10 mu m and the viscosity to be 25-35 Pa.S, thus preparing the conductive silver paste for the external electrode of the chip inductor. The product has a resistivity of 4.68 x 10 silver wires-6Omega cm, good adhesion with base material after sintering, good platability and weldability, but high molding temperature.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the conductive silver paste for the chip inductor and the preparation method thereof.
The purpose of the invention can be realized by the following technical scheme: the conductive silver paste for the chip inductor is characterized by comprising the following components in parts by weight: 75-85 parts of metal silver powder; 3-8 parts of glass powder; 15-31 parts of organic carrier; 1-20 parts of organic solvent.
More preferably, the silver powder is a compound formed by mixing spherical silver powder and flake silver powder according to the mass ratio of 5-6: 1, the particle size of the spherical silver powder is 0.3-0.6 mu m, and the tap density is 3.2-4.8 g/ml; the flake silver powder has a particle diameter of 0.5-0.7 μm and a tap density of 1.0-3.0 g/ml.
The dispersibility of the glass powder and the silver powder in the organic carrier determines the welding strength and the electroplability of the silver paste. According to the invention, the spherical silver powder and the flake silver powder are highly combined by selecting and matching the spherical silver powder and the flake silver powder in a special proportion.
More preferably, the glass powder is a mixture formed by mixing glass powder-L and glass powder-H according to the mass ratio of 2:1,
the glass powder-L is lead-free glass powder with the particle size of 0.5-2 mu m and the sintering temperature of 550-650 ℃, and comprises the following components in parts by weight: bi2O320-40、SiO210-20、B2O310-20、ZnO 5-15、TiO21-6、 SrO 1-5、Al2O35-20、CuO 1-5、NiO 1-5、V2O51-5，
The glass powder-H is lead-free glass powder with the particle size of 0.5-2 mu m and the sintering temperature of 650-750 ℃, and comprises the following components in parts by weight: bi2O350-70、B2O310-30、ZnO 5-15、SiO23-10、Sb2O33-10、 Al2O30-3、Na2O 0-3、Cr2O30-2、Fe2O30-1、ZrO20-1、NiO 0-1、Ag2O 0-1。
Three components of lead-free glass powder are adopted for matching, the sheet resistance application range and the sintering range of the silver paste are widened, and Bi is adopted in the glass powder2O3、B2O3、V2O5The three oxides reduce the melting point, other technical elements adjust the thermal expansion coefficient of the glass powder, and meanwhile, the adhesive force of the silver paste to the electrode is improved; the grain diameter of the glass powder is controlled in a very stable range, so that the stability of a slurry viscosity system is ensured, and simultaneously, the stability of the slurry viscosity system is ensuredThe glass powder can stably exert the performance in the slurry.
The glass powder-L and the glass powder-H are mixed according to the mass ratio of 2:1, so that the dispersion of the mixed silver powder can be improved, the combination of the glass powder and the silver powder can reach the single-layer distribution of the ion level, the silver ions and the tin surface of the glass are promoted to generate more sufficient oxidation-reduction reaction, the electric conductivity is improved, the adhesion with a base material is good after sintering, and the electroplatability and the weldability are improved.
Further preferably, the organic carrier comprises the following components in parts by weight: 10-30 parts of high molecular resin and 70-90 parts of organic solvent.
More preferably, the polymer resin is one or more of ethyl cellulose, nitrocellulose and rosin.
Further preferably, the organic solvent is one or a mixture of more of butyl ether, 12-ester alcohol, ethylene glycol ethyl ether, turpentine, cyclohexanone and terpineol mixed in any proportion.
More preferably, the raw materials also comprise 0.2 to 0.3 weight part of leveling agent polyether modified organic siloxane and 0.2 to 0.3 weight part of plasticizer dimethyl phthalate.
A preparation method of conductive silver paste for a chip inductor comprises the following steps:
(1) preparing an organic carrier: weighing the polymer resin and the organic solvent, heating the polymer resin and the organic solvent to 80 ℃, keeping the temperature constant until the polymer resin is completely dissolved, and filtering and removing impurities on a 300-400-mesh screen cloth when the polymer resin is cooled to below 25 ℃ to obtain an organic carrier;
(2) preparing silver paste: weighing metal silver powder and glass powder, fully mixing the organic solvent and the organic carrier in a mixer, and dispersing at high speed by using a high-speed dispersion machine to obtain uniform slurry;
(3) production of silver paste: and grinding the slurry in a three-roll mill, and finely adjusting by using a roller to control the fineness of the silver slurry to be below 8 mu m and the viscosity to be 35-45 Pa.S, thus preparing the conductive silver slurry for the chip inductor.
The dispersing speed of the high-speed dispersing machine in the step (2) is 65-70 r/min.
Compared with the prior art, the invention has the following advantages:
according to the invention, through the selection and matching of the spherical silver powder and the flake silver powder in a special proportion, the combination of the glass powder and the silver powder can achieve single-layer distribution of ion level, so that more sufficient oxidation-reduction reaction of silver ions and a glass tin surface is promoted, and an electrode surface with moderate roughness can be obtained after sintering, thereby improving welding strength and electroplatability. By introducing V into the glass powder2O5The sintering condition of the silver paste can be further improved, and the resistivity of the silver wire is 3.90 to 10-6Omega cm, so that the high-temperature-resistant sintered glass can obtain better sintering performance at relatively low sintering temperature and within short sintering time, and can meet the molding temperature (550-650 ℃) of the rear windshield of the passenger car.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
A preparation method of conductive silver paste for a chip inductor comprises the following steps:
(1) preparing an organic carrier: preparing 50Kg of carrier, weighing 10Kg of ethyl cellulose, 22Kg of butyl ether and 18Kg of terpineol, stirring to wet the cellulose, heating to 80 ℃ and keeping the temperature until the cellulose is completely dissolved, and filtering and removing impurities on a mesh fabric with 400 meshes of 300 meshes when the temperature is cooled to below 25 ℃ to obtain the carrier.
(2) Preparing materials according to the following components and contents:
the used metal silver powder is a compound formed by mixing spherical silver powder and flake silver powder according to the mass ratio of 5:1, the particle size of the spherical silver powder is 0.3 mu m, and the tap density is 3.2 g/ml; the silver flakes had a particle size of 0.5 μm and a tap density of 1.0 g/ml.
The glass powder is a mixture formed by mixing glass powder-L and glass powder-H according to the mass ratio of 2:1,
the glass powder-L is lead-free glass powder with the particle size of 0.5-2 mu m and the sintering temperature of 550-650 ℃, and comprises the following components in parts by weight: bi2O320、SiO210、B2O310、ZnO 5、TiO21、SrO 1、Al2O35、CuO 1、NiO1、V2O51，
The glass powder-H is lead-free glass powder with the particle size of 0.5 mu m and the sintering temperature of 650 ℃, and comprises the following components in parts by weight: bi2O350、B2O310、ZnO 5、SiO23、Sb2O33。
The organic solvent is butyl ether.
The leveling agent is polyether modified organic siloxane, and the plasticizer is dimethyl phthalate.
(3) Preparing silver paste: weighing metal silver powder, glass powder, a flatting agent and a plasticizer, fully mixing the metal silver powder, the glass powder, the flatting agent and the plasticizer with an organic carrier and a solvent in a mixer, and then dispersing at a high speed by using a high-speed dispersion machine to obtain uniform slurry;
(4) production of silver paste: grinding the slurry on a three-roll grinder, and finely adjusting by using a roller to control the fineness of the silver paste to be below 8 mu m and the viscosity to be 45Pa.S to prepare the conductive silver paste for the chip capacitor, wherein the performance test result is shown in Table 1.
Table 1 silver paste performance test results
Example 2
A preparation method of conductive silver paste for a chip inductor comprises the following steps:
(1) preparing an organic carrier: preparing 50Kg of carrier, weighing 10Kg of nitrocellulose, 22Kg of butyl ether and 18Kg of terpineol, stirring to wet the cellulose, heating to 80 ℃ and keeping the temperature until the cellulose is completely dissolved, and filtering and removing impurities on a mesh fabric with 400 meshes of 300 meshes when the temperature is cooled to below 25 ℃ to obtain the carrier.
(2) Preparing materials according to the following components in parts by weight:
the used metal silver powder is a compound formed by mixing spherical silver powder and flake silver powder according to the mass ratio of 6:1, the particle size of the spherical silver powder is 0.6 mu m, and the tap density is 4.8 g/ml; the silver flakes had a particle size of 0.7 μm and a tap density of 3.0 g/ml.
The glass powder is a mixture formed by mixing glass powder-L and glass powder-H according to the mass ratio of 2:1,
the glass powder-L is lead-free glass powder with the particle size of 2 mu m and the sintering temperature of 650 ℃, and comprises the following components in parts by weight: bi2O340、SiO220、B2O320、ZnO 15、TiO26、SrO5、Al2O320、 CuO5、NiO 5、V2O55，
The glass powder-H is lead-free glass powder with the particle size of 2 mu m and the sintering temperature of 750 ℃, and comprises the following components in parts by weight: bi2O370、B2O330、ZnO15、SiO210、Sb2O310、Al2O33、Na2O 3、Cr2O32、Fe2O31、ZrO21、NiO 1、Ag2O 1。
The organic solvent is 12 ester alcohol.
The leveling agent is polyether modified organic siloxane, and the plasticizer is dimethyl phthalate.
(3) Preparing silver paste: weighing metal silver powder, glass powder and other functional additives, fully mixing the metal silver powder, the glass powder and the other functional additives with an organic carrier and a solvent in a mixer, and then dispersing at a high speed by using a high-speed dispersion machine to obtain uniform slurry;
(4) production of silver paste: grinding the slurry on a three-roll grinder, and finely adjusting by using a roller to control the fineness of the silver paste to be below 8 mu m and the viscosity to be 35Pa.S to prepare the conductive silver paste for the chip capacitor, wherein the performance test result is shown in Table 2.
Table 2 silver paste performance test results
| Detecting items | Qualification standard | The result of the detection |
| Weldability | The tin coating rate is more than or equal to 90 percent | Qualified |
| Resistance to heat of welding | The tin coating rate is more than or equal to 75 percent | Qualified |
| End socket adhesion force F/N | ≥10 | 35 |
Example 3
A preparation method of conductive silver paste for a chip inductor comprises the following steps:
(1) preparing an organic carrier: preparing 50Kg of carrier, weighing 10Kg of nitrocellulose, 22Kg of ethylene glycol ether and 18Kg of terpineol, stirring to wet the cellulose, heating to 80 ℃ and keeping the temperature until the cellulose is completely dissolved, and filtering and removing impurities on a mesh fabric with 400 meshes after cooling to below 25 ℃ to obtain the carrier.
(2) Preparing materials according to the following components in parts by weight:
the used metal silver powder is a compound formed by mixing spherical silver powder and flake silver powder according to the mass ratio of 5.5:1, the particle size of the spherical silver powder is 0.5 mu m, and the tap density is 4.2 g/ml; the silver flakes had a particle size of 0.6 μm and a tap density of 2.0 g/ml.
The glass powder is a mixture formed by mixing glass powder-L and glass powder-H according to the mass ratio of 2:1,
the glass powder-L is lead-free glass powder with the particle size of 1 mu m and the sintering temperature of 600 ℃, and comprises the following components in parts by weight: bi2O330、SiO215、B2O315、ZnO10、TiO23、SrO 3、Al2O310、 CuO3、NiO 4、V2O53，
The glass powder-H is lead-free glass powder with the particle size of 1 mu m and the sintering temperature of 700 ℃, and comprises the following components in parts by weight: bi2O360、B2O320、ZnO 10、SiO28、Sb2O36、Al2O32、Na2O 2、 Cr2O31、Fe2O30.5、ZrO20.5、NiO 0.5、Ag2O 0.5。
The organic solvent is ethylene glycol ethyl ether.
The leveling agent is polyether modified organic siloxane, and the plasticizer is dimethyl phthalate.
(3) Preparing silver paste: weighing metal silver powder and glass powder, fully mixing the metal silver powder and the glass powder with an organic carrier, a solvent, a leveling agent and a plasticizer in a mixer, and then dispersing at a high speed by using a high-speed dispersion machine to obtain uniform slurry;
production of silver paste: grinding the slurry on a three-roll grinder, and finely adjusting by using a roller to control the fineness of the silver paste to be below 8 mu m and the viscosity to be 40Pa.S to prepare the conductive silver paste for the chip capacitor, wherein the performance test results are shown in Table 3.
Table 3 silver paste performance test results
| Detecting items | Qualification standard | The result of the detection |
| Weldability | The tin coating rate is more than or equal to 90 percent | Qualified |
| Resistance to heat of welding | The tin coating rate is more than or equal to 75 percent | Qualified |
| End socket adhesion force F/N | ≥10 | 39 |
。
Claims (9)
1. The conductive silver paste for the chip inductor is characterized by comprising the following components in parts by weight: 75-85 parts of metal silver powder; 3-8 parts of glass powder; 15-31 parts of organic carrier; 1-20 parts of organic solvent.
2. The conductive silver paste for the chip inductor according to claim 1, wherein the silver powder is a composite of spherical silver powder and the silver powder in a mass ratio of 5-6: 1, the spherical silver powder has a particle size of 0.3-0.6 μm and a tap density of 3.2-4.8 g/ml; the flake silver powder has a particle diameter of 0.5-0.7 μm and a tap density of 1.0-3.0 g/ml.
3. The conductive silver paste for chip inductors according to claim 1, wherein the glass frit is a mixture of glass frit-L and glass frit-H mixed according to a mass ratio of 2:1,
the glass powder-L is lead-free glass powder with the particle size of 0.5-2 mu m and the sintering temperature of 550-650 ℃, and comprises the following components in parts by weight: bi2O320-40、SiO210-20、B2O310-20、ZnO 5-15、TiO21-6、SrO 1-5、Al2O35-20、CuO 1-5、NiO 1-5、V2O51-5，
The glass powder-H is lead-free glass powder with the particle size of 0.5-2 mu m and the sintering temperature of 650-750 ℃, and comprises the following components in parts by weight: bi2O350-70、B2O310-30、ZnO 5-15、SiO23-10、Sb2O33-10、Al2O30-3、Na2O0-3、Cr2O30-2、Fe2O30-1、ZrO20-1、NiO 0-1、Ag2O 0-1。
4. The conductive silver paste for the chip inductor according to claim 1, wherein the organic vehicle comprises the following components in parts by weight: 10-30 parts of high molecular resin and 70-90 parts of organic solvent.
5. The conductive silver paste for the chip inductor according to claim 1, wherein the polymer resin is one or more of ethyl cellulose, nitrocellulose and rosin.
6. The conductive silver paste for chip inductors according to claim 1, wherein the organic solvent is one or a mixture of butyl ether, 12-ester alcohol, ethylene glycol ethyl ether, turpentine, cyclohexanone and terpineol mixed in any proportion.
7. The conductive silver paste for chip inductors according to claim 1, wherein the raw materials further comprise 0.2-0.3 parts by weight of leveling agent polyether modified organosiloxane and 0.2-0.3 parts by weight of plasticizer dimethyl phthalate.
8. The preparation method of the conductive silver paste for the chip inductor according to any one of claims 1 to 7, comprising the following steps:
(1) preparing an organic carrier: weighing the polymer resin and the organic solvent, heating the polymer resin and the organic solvent to 80 ℃, keeping the temperature constant until the polymer resin is completely dissolved, and filtering and removing impurities on a 300-400-mesh screen cloth when the polymer resin is cooled to below 25 ℃ to obtain an organic carrier;
(2) preparing silver paste: weighing metal silver powder and glass powder, fully mixing the organic solvent and the organic carrier in a mixer, and dispersing at high speed by using a high-speed dispersion machine to obtain uniform slurry;
(3) production of silver paste: and grinding the slurry in a three-roll mill, and finely adjusting by using a roller to control the fineness of the silver paste to be below 8 mu m and the viscosity to be 35-45 Pa.S, thus preparing the conductive silver paste for the chip inductor.
9. The method for preparing conductive silver paste for chip inductors according to claim 8, wherein the dispersion speed of the high speed dispersion machine in step (2) is 65-70 rpm.
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| CN112635124A (en) * | 2020-09-29 | 2021-04-09 | 陕西彩虹新材料有限公司 | High-identification-degree conductive silver paste and preparation method thereof |
| CN115602437A (en) * | 2022-10-24 | 2023-01-13 | 清远市海之澜电子科技有限公司（Cn） | Preparation method of inductance magnetic core |
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