CN116189957A - Copper conductive paste for inductor and preparation method and application thereof - Google Patents
Copper conductive paste for inductor and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 11
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 9
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- 230000000052 comparative effect Effects 0.000 description 3
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- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
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- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
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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
- H01B1/14—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
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Conductive Materials (AREA)
Abstract
The invention relates to the technical field of conductive paste, in particular to a copper conductive paste for an inductor, and a preparation method and application thereof. The material comprises 50 to 95 weight percent of metal powder, 0.5 to 5 weight percent of ceramic powder, 1 to 15 weight percent of glass composition, 3 to 15 weight percent of organic binder and 0.5 to 20 weight percent of solvent, wherein the glass composition comprises 0.1 to 6 weight percent of Li 2 O、30～60wt％ZnO、0.1～6wt％Al 2 O 3 、1～8wt％Na 2 O、0.1～5wt％SrO、1～20wt％V 2 O 5 、20～60wt％B 2 O 3 、0.1～5wt％CuO、0.1～5wt％MnO 2 5 to 15wt% SiO 2 . The glass composition has lower glass transition temperature, and the prepared inductance conductive film body can be sintered at 650-750 ℃.
Description
Technical Field
The invention relates to the field of conductive paste, in particular to a conductive paste material for preparing an inductance film body.
Background
With the development of electronic products, the market has been developing toward miniaturization and thinning, and it is desired to have the advantages of high capacity and low energy consumption, while the inductor occupies about 10-15% of the passive component market.
The inductance component has two types of plug-in type and sheet type, wherein the sheet type can be divided into winding type and lamination type. The laminated inductor (MLCI) breaks through the limitation of the traditional inductor, realizes the advantages of lightness, thinness, low production cost and high reliability of an inductor product, and becomes the main stream of the chip inductor.
The inductance generates an electromotive force due to a change in the current passing therethrough, thereby resisting the change in the current. When the coil and the magnetic field move relatively or the coil generates an alternating magnetic field through alternating current, induced voltage is generated to resist the original magnetic field change, so that the characteristic of inhibiting the current change is achieved.
The structure of the inductor generally comprises a main carrier, a thick metal film layer, an external electrode and the like. The external electrodes commonly used in the prior art are thick film paste formed by mixing precious metals Pd/Ag/Au and lead-containing glass, and besides the thick film paste is expensive, and the lead-containing glass composition is regarded as a harmful component substance in electronic and electric equipment in the European Union RoHS specification.
Therefore, on the premise of keeping the temperature coefficient and the excellent electrical property, the resistor paste material which has excellent sintering matching property with metal powder and can meet the requirements of low cost and environmental protection regulations is provided, and is a target for continuous research and development of the current technicians in the field.
Disclosure of Invention
In order to solve the problems, the invention provides a copper conductive paste for an inductor, and a preparation method and application thereof.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a copper conductive paste for inductance comprises 50-95 wt% of metal powder, 0.5-5 wt% of ceramic powder, 1-15 wt% of glass composition, 3-15 wt% of organic binder and 0.5-20 wt% of solvent;
wherein the glass composition comprises 0.1 to 6wt% Li 2 O、30～60wt％ZnO、0.1～6wt％Al 2 O 3 、1～8wt％Na 2 O、0.1～5wt％SrO、1～20wt％V 2 O 5 、20～60wt％B 2 O 3 、0.1～5wt％CuO、0.1～5wt％MnO 2 5 to 15wt% SiO 2 。
Wherein the glass transition temperature Tg of the glass composition is 380-600 ℃.
Wherein the metal powder comprises Cu powder and Cu 2 At least one of the O powder and at least one of the NiO powder and the Ni powder.
Wherein the average grain diameter of the Cu powder is 0.3-10 mu m; the Cu is 2 The average grain diameter of the O powder is 0.5-5 mu m; the average particle size of the NiO powder is 0.5-3 mu m; the average grain diameter of the Ni powder is 0.2-3 mu m; the BaTiO 3 The average particle size of the powder is 0.05-3 mu m.
Wherein the ceramic powder has a perovskite structure and a general structural formula of ABO 3 Wherein A can be Ca, sr, bi, cs, la or any one of the other rare earth elements and alkaline earth elements; b can be Ti, fe, mn, co or one of the rest transition elements, and the average particle size of the ceramic powder is 0.05-3 mu m.
Further, the ceramic powder is BaTiO 3 。
Wherein the organic binder is a thermosetting resin, a thermoplastic resin or a mixture of the thermosetting resin and the thermoplastic resin.
Wherein the thermosetting resin is at least one selected from epoxy resin, amine ester resin, vinyl ester resin, silicone resin, phenol resin, urea resin, melamine resin, unsaturated polyester resin, diallyl phthalate resin and polyimide resin; the thermoplastic resin is at least one selected from the group consisting of ethyl cellulose, acrylic resin, alkyd resin, saturated polyester resin, butyraldehyde resin, polyvinyl alcohol and hydroxypropyl fiber.
Wherein the solvent is at least one selected from organic acids, aromatic hydrocarbons, pyrrolidone, amides, ketones and cyclic carbonates. Wherein the organic acid can be, for example, diethylene glycol diethyl ether acetate, diethylene glycol butyl ether acetate, or ethyl acetate; the aromatic hydrocarbon may be, for example, toluene, or xylene; the pyrrolidone may be, for example, N-methyl-2-pyrrolidone (NMP); the amides may be, for example, N-Dimethylformamide (DMF); the ketone may be, for example, methyl Ethyl Ketone (MEK); the cyclic carbonate may be, for example, terpineol (Terpineol); or Butyl Carbitol (BC).
The preparation method of the copper conductive paste for the inductor comprises the following steps:
(1) Taking Li 2 O、ZnO、Al 2 O 3 、Na 2 O、SrO、V 2 O 5 、B 2 O 3 、CuO、MnO 2 SiO (silicon oxide) 2 Is subjected to melting and water quenching to obtain a glass composition;
the glass composition comprises 0.1 to 6wt% Li 2 O、30～60wt％ZnO、0.1～6wt％Al 2 O 3 、1～8wt％Na 2 O、0.1～5wt％SrO、1～20wt％V 2 O 5 、20～60wt％B 2 O 3 、0.1～5wt％CuO、0.1～5wt％MnO 2 5 to 15wt% SiO 2 ；
(2) The above glass composition is mixed with a metal powder, an organic binder and a solvent to obtain a copper electroconductive paste for inductance.
Wherein the melting temperature in the step (1) is 1000 ℃ to 1500 ℃.
Wherein, after the glass composition is obtained by the water quenching step, the method further comprises a grinding step, so that the glass composition forms powder with the average particle size of 1-5 mu m.
Wherein the glass transition temperature Tg of the glass composition is 380-600 ℃.
An inductance conductive film body is prepared from the copper conductive paste for the inductance.
The preparation method of the inductance conductive film body comprises the following steps: and sintering the copper conductive paste for the inductor in a reducing atmosphere to obtain an inductance conductive film body. Wherein the sintering temperature is 650-750 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the novel glass composition in the copper conductive paste for the inductor has lower glass transition temperature and can form optimal sintering matching property with metal powder, so that the paste can be sintered to form a film at 650-750 ℃.
The inductance conductive film body prepared from the copper conductive paste for the inductance can pass the sulfuration resistance test, and the inductance conductive film body can maintain excellent electrical characteristics for a long time.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The preparation method of the copper conductive paste for the inductor comprises the following steps:
(1) Taking Li 2 O、ZnO、Al 2 O 3 、Na 2 O、SrO、V 2 O 5 、B 2 O 3 、CuO、MnO 2 SiO (silicon oxide) 2 Based on the total weight, is stirred and mixed according to the following proportion: 0.1 to 6wt% Li 2 O、30～60wt％ZnO、0.1～6wt％Al 2 O 3 、1～8wt％Na 2 O、0.1～5wt％SrO、1～20wt％V 2 O 5 、20～60wt％B 2 O 3 、0.1～5wt％CuO、0.1～5wt％MnO 2 5 to 15wt% SiO 2 ；
(2) Mixing the powder, placing the powder into a crucible carrier, heating the powder and the crucible carrier together by a resistance furnace to 1000-1500 ℃ for melting, keeping the temperature for 2-4 hours, and then rapidly pouring the powder into deionized water for water extraction to obtain a bulk glass composition material;
(3) Wet grinding the bulk glass composition material for 24 hours to form powder with an average particle size of 1-5 mu m;
(4) Weighing metal powder, ceramic powder and powdered glass composition material, mixing, adding organic binder and solvent, and mixing according to the following proportion: 50 to 90wt% of the total weight of the metal powder, 1 to 15wt% of the glass composition material in powder form, 3 to 15wt% of the organic binder, and 10 to 20wt% of the solvent; fully mixing, dispersing by a three-roller mill and a dispersing grinder, and filtering and defoaming to obtain the copper conductive paste for the inductor.
The metal powder used in the preparation of the copper conductive paste for inductance may be Cu metal powder having an average particle diameter of 0.3 to 10 μm or Cu metal powder having an average particle diameter of 0.5 to 5 μm 2 O metal powder, niO metal powder with average particle diameter of 0.05-3 μm and average particle diameter of 0.5-3 μm, ni metal powder with average particle diameter of 0.2-3 μm or any combination of two or more metal powders.
The ceramic powder used in the preparation of the copper conductive paste for inductance may be BaTiO having an average particle diameter of 0.05 to 3 μm 3 And (3) powder.
In this example, terpineol as a solvent, ethylcellulose as an organic binder, and a dispersant, an adhesive, a leveling agent, and a thixotropic agent, which may be additives, were sufficiently mixed and stirred for about five hours. It should be noted that the composition of the additive suitable for the present invention is not limited thereto, and those skilled in the art can increase or decrease the composition of the additive according to actual needs, which are well known in the art, and will not be further discussed herein.
A preparation method of an inductance conductive film body comprises the following steps: the inductance copper conductive paste prepared by the method is screen printed on a proper substrate, such as a ceramic substrate, dried for 20 minutes in the environment of about 200 ℃, and finally sintered in the reducing atmosphere to obtain the inductance conductive film body. Wherein sintering is performed in an atmosphere furnace at a temperature of 700 ℃ for about 10 minutes.
Inductance and sulfuration resistance test of the inductance conductive film body prepared by the method:
in order to more clearly show the specific composition of the glass composition used in the present invention, which does contribute to the excellent electrical properties of pastes and films, the following will be directed to comparative examples of films not containing the glass composition of the present invention, and a plurality of sets of "metal powders" in different proportions: glass composition: organic binder: solvent "examples were compared and the values of inductance and resistance to vulcanization were recorded for the ultra-low temperature coefficient conductive pastes of the comparative examples and examples after the same was sintered at 700 c to form a film. The vulcanization resistance test is carried out by using a vulcanization tester with the model of ASTMB809-95, wherein water, potassium nitrate and vulcanized powder are used as mediums, a thick film chip sample is placed in the vulcanization tester, and the temperature is raised to 60-90 ℃ for 800-1000 hours for life test. The compositions of the electroconductive paste components of the comparative examples and examples are shown in table 1. The test results are shown in Table 2 below.
TABLE 1
TABLE 2
Note that: x represents no passage, and O represents passage.
From the above preparation process and test results, it can be seen that the novel glass composition in the copper conductive paste for inductor provided by the invention has a low glass transition temperature and can have an optimal sintering matching property with metal powder, so that the paste can be sintered to form a film at 650-750 ℃, and the prepared conductive film (examples 1-4) of the inductor can pass the vulcanization resistance test and can maintain excellent electrical characteristics for a long time.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (14)
1. A copper conductive paste for an inductor, characterized in that: comprises 50 to 95 weight percent of metal powder, 0.5 to 5 weight percent of ceramic powder, 1 to 15 weight percent of glass composition, 3 to 15 weight percent of organic binder and 0.5 to 20 weight percent of solvent;
wherein the glass composition comprises 0.1 to 6wt% Li 2 O、30～60wt％ZnO、0.1～6wt％Al 2 O 3 、1～8wt％Na 2 O、0.1～5wt％SrO、1～20wt％V 2 O 5 、20～60wt％B 2 O 3 、0.1～5wt％CuO、0.1～5wt％MnO 2 5 to 15wt% SiO 2 。
2. The copper electroconductive paste for inductance according to claim 1, wherein: the glass transition temperature Tg of the glass composition is 380-600 ℃.
3. The copper electroconductive paste for inductance according to claim 1, wherein: the metal powder comprises Cu powder, cu 2 At least one of the O powder and at least one of the NiO powder and the Ni powder.
4. A copper electroconductive paste for inductance according to claim 3, wherein: the average grain diameter of the Cu powder is 0.3-10 mu m; the Cu is 2 The average grain diameter of the O powder is 0.5-5 mu m; the average particle size of the NiO powder is 0.5-3 mu m; the Ni powder has an average particle diameter of 0.2 to 3 μm.
5. The copper electroconductive paste for inductance according to claim 1, wherein: the ceramic powder has a perovskite structure and a general structural formula of ABO 3 Wherein A can be Ca, sr, bi, cs, la or any one of the other rare earth elements and alkaline earth elements; b can be Ti, fe, mn, co or one of the rest transition elements, and the average particle size of the ceramic powder is 0.05-3 mu m.
6. The copper electroconductive paste for inductance according to claim 1, wherein: the organic binder is a thermosetting resin, a thermoplastic resin or a mixture of the thermosetting resin and the thermoplastic resin.
7. The copper electroconductive paste for inductance according to claim 1, wherein: the solvent is at least one selected from organic acids, aromatic hydrocarbons, pyrrolidone, amide, ketone and cyclic carbonate.
8. A method for producing the copper electroconductive paste for inductance according to any one of claims 1 to 7, comprising the steps of:
(1) Taking Li 2 O、ZnO、Al 2 O 3 、Na 2 O、SrO、V 2 O 5 、B 2 O 3 、CuO、MnO 2 SiO (silicon oxide) 2 Is subjected to melting and water quenching to obtain a glass composition;
the glass composition comprises 0.1 to 6wt% Li 2 O、30～60wt％ZnO、0.1～6wt％Al 2 O 3 、1～8wt％Na 2 O、0.1～5wt％SrO、1～20wt％V 2 O 5 、20～60wt％B 2 O 3 、0.1～5wt％CuO、0.1～5wt％MnO 2 5 to 15wt% SiO 2 ；
(2) The above glass composition is mixed with metal powder, ceramic powder, organic binder and solvent to obtain copper conductive paste for inductor.
9. The method for preparing a copper electroconductive paste for inductance according to claim 8, wherein: the melting temperature in step (1) is 1000 ℃ to 1500 ℃.
10. The method for preparing a copper electroconductive paste for inductance according to claim 8, wherein: after the glass composition is obtained through the water quenching step, the method further comprises a grinding step, so that the glass composition forms powder with the average particle size of 1-5 mu m.
11. The method for preparing a copper electroconductive paste for inductance according to claim 8, wherein: the glass transition temperature Tg of the glass composition is 380-600 ℃.
12. An inductance conductive film body prepared by using the copper conductive paste for inductance according to any one of claims 1 to 7.
13. The method for producing an inductive conductive film body according to claim 12, characterized in that: sintering the copper conductive paste for inductance according to any one of claims 1 to 6 under a reducing atmosphere to obtain an inductance conductive film body.
14. The method for manufacturing an inductance conductive film according to claim 13, wherein: the sintering temperature is 650-750 ℃.
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| CN202310330299.6A CN116189957A (en) | 2023-03-30 | 2023-03-30 | Copper conductive paste for inductor and preparation method and application thereof |
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Citations (5)
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|---|---|---|---|---|
| US4714570A (en) * | 1984-07-17 | 1987-12-22 | Matsushita Electric Industrial Co., Ltd. | Conductor paste and method of manufacturing a multilayered ceramic body using the paste |
| JP2006089310A (en) * | 2004-09-22 | 2006-04-06 | Shoei Chem Ind Co | Glass powder and conductor paste containing the same |
| CN111028975A (en) * | 2019-12-03 | 2020-04-17 | 南京汇聚新材料科技有限公司 | Low-temperature coefficient resistor paste and preparation method and application thereof |
| CN113782251A (en) * | 2021-09-09 | 2021-12-10 | 南京汇聚新材料科技有限公司 | Electrode paste, electrode thick film and preparation method thereof |
| CN114212995A (en) * | 2021-12-27 | 2022-03-22 | 中建材蚌埠玻璃工业设计研究院有限公司 | Preparation method suitable for OLED sealing solder |
-
2023
- 2023-03-30 CN CN202310330299.6A patent/CN116189957A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4714570A (en) * | 1984-07-17 | 1987-12-22 | Matsushita Electric Industrial Co., Ltd. | Conductor paste and method of manufacturing a multilayered ceramic body using the paste |
| JP2006089310A (en) * | 2004-09-22 | 2006-04-06 | Shoei Chem Ind Co | Glass powder and conductor paste containing the same |
| CN111028975A (en) * | 2019-12-03 | 2020-04-17 | 南京汇聚新材料科技有限公司 | Low-temperature coefficient resistor paste and preparation method and application thereof |
| CN113782251A (en) * | 2021-09-09 | 2021-12-10 | 南京汇聚新材料科技有限公司 | Electrode paste, electrode thick film and preparation method thereof |
| CN114212995A (en) * | 2021-12-27 | 2022-03-22 | 中建材蚌埠玻璃工业设计研究院有限公司 | Preparation method suitable for OLED sealing solder |
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