CN111128438A - Dip-soldering tin-free environment-friendly silver paste and preparation method thereof - Google Patents
Dip-soldering tin-free environment-friendly silver paste and preparation method thereof Download PDFInfo
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- CN111128438A CN111128438A CN201911422391.5A CN201911422391A CN111128438A CN 111128438 A CN111128438 A CN 111128438A CN 201911422391 A CN201911422391 A CN 201911422391A CN 111128438 A CN111128438 A CN 111128438A
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- China
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- free environment
- soldering tin
- raw materials
- silver paste
- dip
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Classifications
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- 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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
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- 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
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C1/00—Details
- H01C1/14—Terminals or tapping points or electrodes specially adapted for resistors; Arrangements of terminals or tapping points or electrodes on resistors
- H01C1/142—Terminals or tapping points or electrodes specially adapted for resistors; Arrangements of terminals or tapping points or electrodes on resistors the terminals or tapping points being coated on the resistive element
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/228—Terminals
- H01G4/252—Terminals the terminals being coated on the capacitive element
Abstract
The invention relates to dip soldering tin-free environment-friendly silver paste and a preparation method thereof. The silver electrode slurry comprises the following components in percentage by weight: 60-80% of silver conductive powder, 0.2-4% of inorganic glass binder, 0.2-2% of titanium and its oxide and 20-40% of organic carrier. The titanium and the titanium oxide are added into the environment-friendly silver paste, so that the silver surface except the lead wire can be effectively prevented from being coated with tin during dip soldering, the tin consumption is greatly reduced, and the cost is saved; the obvious dip soldering tin-hanging prevention effect of titanium and the oxide thereof is universally applied to various base materials, and the solderability, the adhesive force and other properties of the product are not influenced.
Description
Technical Field
The invention relates to the technical field of electronic materials, in particular to dip soldering tin-free environment-friendly silver paste and a preparation method thereof.
Background
The dip soldering tin coating means that the silver surface of the printed and sintered substrate is coated with tin except the lead during dip soldering.
The working environment of the electronic ceramic component is mostly high-temperature high-humidity condition, the tin is more hung, the tin is easy to melt and seep, and the welding spot has defects; under the impact of large current, the silver surface is coated with tin more, and short circuit is easy to occur. Most of the existing tin-coating prevention technologies can affect other performances of the silver paste, such as weldability, adhesive force, stacking adhesion and the like, and the actual performances are not perfect.
Disclosure of Invention
The invention aims to provide an immersion welding tin-hanging-free environment-friendly silver paste and a preparation method thereof.
The technical scheme of the invention is as follows: the dip-soldering tin-free environment-friendly silver paste comprises the following components in percentage by weight:
a preparation method of dip-soldering tin-free environment-friendly silver paste comprises the following steps: a. preparation of organic vehicle
Weighing 3-5% of the macromolecular thickening agent and 15-37% of the solvent, heating the mixed system to 90-120 ℃, fully stirring at the stirring speed of 60-120 r/min for 300 min, completely dissolving the macromolecular thickening agent in the solvent, and adding the organic auxiliary agent in an amount of 0.1-3% of the weight of the raw materials, and uniformly stirring to obtain the organic carrier.
b. Preparation of inorganic glass binder
Mechanically mixing the raw materials according to a given proportion, heating the mixture to be molten at 1300 ℃ in a muffle furnace, preserving heat for 10 minutes, pouring the mixture into cold water for quenching, carrying out ball milling in a water medium for 48 hours until the granularity of the powder is less than or equal to 10 mu m, and drying the powder at 120 ℃.
c. Preparation of slurry
Mixing and stirring the silver conductive powder 60-80% of the weight of the raw materials, the prepared organic carrier and the prepared inorganic glass binder 0.2-4% of the weight of the raw materials.
d. Manufacture of slurries
And c, grinding the mixed raw materials obtained in the step c on a three-roll grinder, obtaining uniformly dispersed slurry through a certain grinding process, wherein the granularity of the slurry is less than or equal to 10 mu m, adding titanium and oxides thereof accounting for 0.2-2% of the weight of the raw materials, and uniformly mixing to obtain the dip-soldering tin-free environment-friendly silver slurry.
Compared with the prior art, the dip-soldering tin-free environment-friendly silver paste prepared by the invention is coated on the surface of a dielectric substrate of an electronic ceramic component by a silk screen printing method, and is sintered to be used as an electrode, so that the silver electrode paste is an important material of the electronic ceramic component, and has the advantages that:
the silver surface except the lead is effectively prevented from being tin-coated during dip soldering, the tin consumption is greatly reduced, and the cost is saved; when the composite wave-absorbing material is applied to the field of piezoresistors, the impact performance is ensured under the impact of large current and combined waves; when the titanium-titanium composite material is applied to the field of capacitors, the titanium and the titanium oxide enable the adhesive force between the silver layer and a substrate to be enhanced; meanwhile, the phenomenon of sticking of the products in multiple fields can be prevented.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Example 1: a preparation method of dip-soldering tin-free environment-friendly silver paste comprises the following basic steps:
step A: preparation of organic vehicle
Weighing the following raw materials in percentage by weight:
weighing 3-5 parts of macromolecular thickening agent and 15-37 parts of organic solvent, mixing, heating the mixed system to 90-120 ℃, and fully stirring at the stirring speed of 60-120 r/min for 300 min so as to completely dissolve the macromolecular thickening agent in the solvent.
Adding the organic auxiliary agent which accounts for 0.1-3% of the weight of the raw materials into a mixed system of a macromolecular thickening agent and an organic solvent, and uniformly stirring to obtain the organic carrier.
And B: preparation of inorganic glass binder
Mechanically mixing the raw materials according to a given proportion, heating the mixture to be molten at 1300 ℃ in a muffle furnace, preserving heat for 10 minutes, pouring the mixture into cold water for quenching, carrying out ball milling in a water medium for 48 hours until the granularity of the powder is less than or equal to 10 mu m, and drying the powder at 120 ℃.
And C: preparation of slurry
Mixing and stirring 60-80 parts of silver conductive powder, A, prepared organic carrier and 0.2-4 parts of B, prepared inorganic glass binder.
Step D: manufacture of slurries
And c, grinding the mixed raw materials obtained in the step c on a three-roll grinder, obtaining uniformly dispersed slurry through a certain grinding process, wherein the granularity of the slurry is less than or equal to 10 mu m, adding titanium and oxides thereof accounting for 0.2-2% of the weight of the raw materials, and uniformly mixing to obtain the dip-soldering tin-free environment-friendly silver slurry.
The solvent in the step A comprises one or a combination of more of terpineol, butyl carbitol acetate and a film forming auxiliary agent. And in the step A, the macromolecular thickening agent is ethyl cellulose. The organic auxiliary agent is one or a combination of more of RE610, digao 655, BYK111 and BYK 410.
The inorganic glass binder in the step B comprises the following raw materials in percentage by weight: 330-50% of B2O, 330-60% of Bi2O, 78-5% of SiO 20, 0-5% of ZnO, 0-5% of CuO and 0-5% of NiO. The particle size is preferably 500-1200 mesh.2
The silver conductive powder in the step C consists of coarse and fine spherical powder in a certain proportion (weight percentage): fine spherical powder: coarse spherical powder (30-100): (70-0), the specific surface area of the fine spherical powder is more than 7m2/g, the specific surface area of the coarse spherical powder is 1.5-4m2/g, the purity is 99.9, and the ignition weight loss is less than or equal to 1%.
The titanium and the titanium oxide in the step C are composed of titanium powder and titanium dioxide in a certain proportion, one or two of the titanium powder and the titanium dioxide are adopted, and the granularity is preferably 400 meshes.
Example 2: the preparation method is consistent with that of the example 1, only the mixture ratio of the raw materials is different, and the raw materials are shown in the table 1;
example 3: the preparation method is consistent with the previous examples, only the mixture ratio of the raw materials is different, and the raw materials are shown in table 1;
comparative example 1: the preparation method is consistent with the previous examples, only the mixture ratio of the raw materials is different, and the raw materials are shown in table 1;
comparative example 2: the preparation method is consistent with the previous examples, only the mixture ratio of the raw materials is different, and the raw materials are shown in table 1;
comparative example 3: the preparation method is consistent with the previous examples, only the mixture ratio of the raw materials is different, and the raw materials are shown in table 1;
TABLE 1
Inorganic glass binder formulation (100 g): b is2O345g、Bi2O340g、SiO26g、ZnO 4g、 CuO 1g、NiO4g。
The results are shown in Table 2
TABLE 2
The experimental results show that: the titanium or the titanium oxide and the inorganic glass binder form a synergistic effect, so that the surface activity of the silver layer is improved, and the adhesive property, the adhesive force and the tin hanging performance of the silver layer are improved.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (7)
1. The utility model provides a dip soldering does not hang tin environment-friendly silver thick liquids which characterized in that: comprises the following components in percentage by weight:
2. the dip soldering tin-free environment-friendly silver paste according to claim 1, which is characterized in that: the silver conductive powder comprises fine spherical powder and coarse spherical powder, and the ratio of the fine spherical powder to the coarse spherical powder is as follows: 30-100: 70-0.
3. The dip soldering tin-free environment-friendly silver paste according to claim 1 or 2, which is characterized in that: the inorganic glass binder comprises the following components in percentage by weight: b is2O330-50％、Bi2O330-60％、SiO20-5％、ZnO 0-5％、CuO 0-5％、NiO 0-5％。
4. The dip soldering tin-free environment-friendly silver paste according to claim 3, which is characterized in that: the titanium and the oxide thereof are one or the mixture of two of titanium powder and titanium dioxide.
5. The dip soldering tin-free environment-friendly silver paste according to claim 4, which is characterized in that: the organic carrier is a mixture of an organic solvent, a macromolecular thickener and an organic auxiliary agent.
6. The dip soldering tin-free environment-friendly silver paste according to claim 5, which is characterized in that: the organic solvent is one or a combination of more of terpineol, butyl carbitol acetate and a film forming auxiliary agent; the macromolecular thickener is ethyl cellulose.
7. A preparation method of dip-soldering tin-free environment-friendly silver paste is characterized by comprising the following steps: the method comprises the following steps: a. preparation of organic vehicle
Weighing 3-5% of the macromolecular thickening agent and 15-37% of the solvent, heating the mixed system to 90-120 ℃, fully stirring at the stirring speed of 60-120 r/min for 300 min, completely dissolving the macromolecular thickening agent in the solvent, and adding the organic auxiliary agent in an amount of 0.1-3% of the weight of the raw materials, and uniformly stirring to obtain the organic carrier.
b. Preparation of inorganic glass binder
Mechanically mixing the raw materials according to a given proportion, heating the mixture to be molten at 1300 ℃ in a muffle furnace, preserving heat for 10 minutes, pouring the mixture into cold water for quenching, carrying out ball milling in a water medium for 48 hours until the granularity of the powder is less than or equal to 10 mu m, and drying the powder at 120 ℃.
c. Preparation of slurry
Mixing and stirring the silver conductive powder 60-80% of the weight of the raw materials, the prepared organic carrier and the prepared inorganic glass binder 0.2-4% of the weight of the raw materials.
d. Manufacture of slurries
And c, grinding the mixed raw materials obtained in the step c on a three-roll grinder, obtaining uniformly dispersed slurry through a certain grinding process, wherein the granularity of the slurry is less than or equal to 10 mu m, adding titanium and oxides thereof accounting for 0.2-2% of the weight of the raw materials, and uniformly mixing to obtain the dip-soldering tin-free environment-friendly silver slurry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911422391.5A CN111128438A (en) | 2019-12-31 | 2019-12-31 | Dip-soldering tin-free environment-friendly silver paste and preparation method thereof |
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| CN201911422391.5A CN111128438A (en) | 2019-12-31 | 2019-12-31 | Dip-soldering tin-free environment-friendly silver paste and preparation method thereof |
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| CN111128438A true CN111128438A (en) | 2020-05-08 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117711668A (en) * | 2024-02-06 | 2024-03-15 | 晶澜光电科技(江苏)有限公司 | N-type solar cell P+ emitter conductive paste and N-type solar cell |
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| JP2003151859A (en) * | 2001-08-22 | 2003-05-23 | Showa Denko Kk | Solid-state electrolytic capacitor and method of manufacturing the same |
| CN1637957A (en) * | 2003-11-19 | 2005-07-13 | E.I.内穆尔杜邦公司 | Thick film conductor case compositions for LTCC tape |
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2019
- 2019-12-31 CN CN201911422391.5A patent/CN111128438A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS50146898A (en) * | 1974-05-16 | 1975-11-25 | ||
| JP2003151859A (en) * | 2001-08-22 | 2003-05-23 | Showa Denko Kk | Solid-state electrolytic capacitor and method of manufacturing the same |
| CN1637957A (en) * | 2003-11-19 | 2005-07-13 | E.I.内穆尔杜邦公司 | Thick film conductor case compositions for LTCC tape |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117711668A (en) * | 2024-02-06 | 2024-03-15 | 晶澜光电科技(江苏)有限公司 | N-type solar cell P+ emitter conductive paste and N-type solar cell |
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Application publication date: 20200508 |
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