CN115602437B - Preparation method of inductance magnetic core - Google Patents
Preparation method of inductance magnetic core Download PDFInfo
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- CN115602437B CN115602437B CN202211304483.5A CN202211304483A CN115602437B CN 115602437 B CN115602437 B CN 115602437B CN 202211304483 A CN202211304483 A CN 202211304483A CN 115602437 B CN115602437 B CN 115602437B
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- 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
- H01F41/02—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 for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
- C23C24/085—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
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- 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
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- 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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Abstract
The invention belongs to the field of electronic parts and discloses a preparation method of an inductance magnetic core, which comprises the steps of sintering a conductive silver layer, an electroplated nickel layer and an electroplated tin layer on the surface of the magnetic core; the sintering method of the conductive silver layer comprises the following steps: the magnetic core coated with the conductive silver paste passes through a tunnel furnace, the tunnel furnace is divided into 7 continuous furnace bodies with the same length, and the sintering temperature of the furnace bodies from front to back is 300+/-20 ℃, 400+/-20 ℃, 500+/-20 ℃, 660+/-5 ℃, 685+/-2 ℃, 690+/-2 ℃ and 690+/-2 ℃ in sequence; the residence time of the magnetic core in the tunnel furnace is 75-80min; the thickness of the conductive silver layer is 2.8-3.7 mu m; the conductive silver paste comprises the following components: 60-65wt% of silver powder; 4-9wt% of lead-free glass; 1-4wt% of ethyl cellulose; the balance of organic solvent; the silver powder consists of nano silver powder with the particle size of less than 100nm, superfine silver powder and silver micro powder with the particle size of 1-5 mu m, wherein the particle size of the superfine silver powder is more than 100nm and less than 1 mu m; the weight ratio of the nanometer silver powder to the superfine silver powder to the silver micro powder is 1:2-4:5-7; the content of inorganic components in the conductive silver paste is 70+/-3 wt%. According to the method, the temperature control is optimized, and the prepared magnetic core silver layer has high yield.
Description
Technical Field
The invention relates to the field of electronic parts, in particular to a preparation method of an inductance magnetic core.
Background
CN201110461017.3 discloses a method for preparing conductive silver paste for ferrite core inductance, which comprises the following steps: preparing lead-free glass powder, wherein the lead-free glass powder contains an inorganic additive I accounting for 1-4% of the total amount of the lead-free glass powder, (2) preparing an organic carrier, (3) mixing superfine silver powder, flaky silver powder, the lead-free glass powder and the inorganic additive II, preparing powder, uniformly stirring, adding the organic carrier, stirring and dispersing at a high speed, rolling to a fineness of less than 10 mu m by a three-roller mill, and then sieving by a 200-mesh screen to obtain the conductive silver paste for ferrite magnetic core inductance.
The sintering temperature of the scheme is 650-720 ℃.
The company adopts silver paste provided by suppliers, and the sintering temperature is 670-680 ℃ under the guidance of the suppliers;
after the silver paste provided by the provider of the company is applied to the magnetic core of the company, the problems of silver spreading, silver dew body feeding, silver flowing, silver connection and the like are found.
Therefore, the technical problem solved by the scheme is as follows: how to alleviate the problems of upper silver diffusion, upper silver dew body, silver flowing, silver connection and the like in the process of sintering the silver layer of the magnetic core.
Disclosure of Invention
The invention aims to provide a preparation method of an inductance magnetic core, which is characterized in that the prepared magnetic core silver layer has high yield through optimizing temperature control.
In order to achieve the above purpose, the present invention provides the following technical solutions: the preparation method of the inductance magnetic core comprises the steps of sintering a conductive silver layer, an electroplated nickel layer and an electroplated tin layer on the surface of the magnetic core;
the sintering method of the conductive silver layer comprises the following steps:
the magnetic core coated with the conductive silver paste passes through a tunnel furnace, wherein the tunnel furnace is divided into 7 continuous furnace bodies with the same length, and the sintering temperature of the furnace bodies from front to back is 300+/-20 ℃, 400+/-20 ℃, 500+/-20 ℃, 660+/-5 ℃, 685+/-2 ℃, 690+/-2 ℃ and 690+/-2 ℃ in sequence;
the residence time of the magnetic core in the tunnel furnace is 75-80min;
the thickness of the conductive silver layer is 2.8-3.7 mu m;
the conductive silver paste comprises the following components:
60-65wt% of silver powder;
4-9wt% of lead-free glass;
1-4wt% of ethyl cellulose;
the balance of organic solvent;
the silver powder consists of nano silver powder with the particle size of less than 100nm, superfine silver powder and silver micro powder with the particle size of 1-5 mu m, wherein the particle size of the superfine silver powder is more than 100nm and less than 1 mu m; the weight ratio of the nanometer silver powder to the superfine silver powder to the silver micro powder is 1:2-4:5-7;
the content of inorganic components in the conductive silver paste is 70+/-3 wt%.
In the preparation method of the inductance core, the organic solvent is terpineol, ethylene glycol monomethyl ether or propylene glycol methyl ether acetate.
In the preparation method of the inductance core, the grain size of the lead-free glass is 2-5 mu m.
In the preparation method of the inductance core, the conductive silver paste further comprises a silane coupling agent, and the dosage of the silane coupling agent is 0.1-0.3wt%.
In the above method for manufacturing an inductor core, the electroplated nickel layer has an electroplated thickness of 2.9-3.9 μm, and the electroplated tin layer has an electroplated thickness of 2.1-2.45 μm.
Compared with the prior art, the invention has the beneficial effects that:
the invention combines the nanometer silver powder, the superfine silver powder and the silver micro powder, the silver micro powder and the ethyl cellulose are combined to be used as the main body of the silver layer, the superfine silver powder has larger specific surface area and has an improvement effect on conductivity, and gaps among the silver micro powder can be filled; although the nano silver powder is not easy to disperse, under the condition of small dosage, the nano silver powder can be matched with the superfine silver powder, and gaps of the silver micro powder are filled under the carrying of the superfine silver powder, so that the surface of the silver layer is more uniform.
The invention optimizes the suggestion of 670-680 ℃ sintering temperature provided by suppliers, and mainly comprises the following optimization steps:
1. a temperature rising section of 300-500 ℃ is arranged;
2. setting the sintering temperature at 685-690 ℃, and adding a 660 ℃ high-temperature section between the temperature rising section and the sintering section;
through the optimization, the problems of upper silver diffusion, upper silver dew body, silver flowing, silver connection and the like can be basically avoided.
Drawings
FIG. 1 is a graph of silver diffusion effects on rejects;
FIG. 2 is a pictorial view of the upper silver paste;
FIG. 3 is a flow silver image;
fig. 4 is a diagram of silver-attached phenomena.
Detailed Description
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.
Example 1
The preparation method of the inductance magnetic core comprises the steps of sintering a conductive silver layer, an electroplated nickel layer and an electroplated tin layer on the surface of the magnetic core from bottom to top;
the thickness of the conductive silver layer is 2.8-3.7 mu m; the electroplating thickness of the electroplated nickel layer is 2.9-3.9 mu m, and the electroplating thickness of the electroplated tin layer is 2.1-2.45 mu m;
1000 samples were prepared in this example 1, 10 samples were randomly selected, and the thickness parameters of each interlayer structure were as follows in table 1:
TABLE 1
| Sample numbering | Sn μm | Ni μm | Ag μm |
| 1 | 2.12 | 3.26 | 3.42 |
| 2 | 2.27 | 3.72 | 3.26 |
| 3 | 2.24 | 3.83 | 3.61 |
| 4 | 2.19 | 3.46 | 3.69 |
| 5 | 2.43 | 4.15 | 3.44 |
| 6 | 2.39 | 3.9 | 3.06 |
| 7 | 2.34 | 2.94 | 3.41 |
| 8 | 2.19 | 2.9 | 2.83 |
| 9 | 2.22 | 3.91 | 3.56 |
| 10 | 2.22 | 3.81 | 3.43 |
The sintering method of the conductive silver layer comprises the following steps:
the magnetic core coated with the conductive silver paste (dried and formed at 150 ℃) is passed through a tunnel furnace, the tunnel furnace is divided into 7 continuous furnace bodies with the same length, and the sintering temperature of the furnace bodies from front to back is 300 ℃, 400 ℃, 500 ℃, 660 ℃, 685 ℃, 690 ℃ and 690 ℃ in sequence;
the residence time of the magnetic core in the tunnel furnace is 80min;
the conductive silver paste comprises the following components:
65wt% of silver powder;
5wt% of lead-free glass with the particle size of 2-5 mu m;
3wt% of ethyl cellulose;
terpineol balance;
the silver powder consists of nano silver powder with the particle size of less than 100nm, superfine silver powder and silver micro powder with the particle size of 1-5 mu m, wherein the particle size of the superfine silver powder is more than 100nm and less than 1 mu m; the weight ratio of the nanometer silver powder to the superfine silver powder to the silver micro powder is 1:3:6.
example 2
Substantially the same as in example 1, except that:
the sintering method of the conductive silver layer comprises the following steps:
the magnetic core coated with the conductive silver paste passes through a tunnel furnace, wherein the tunnel furnace is divided into 7 continuous furnace bodies with the same length, and the sintering temperature of the furnace bodies from front to back is 300 ℃, 400 ℃, 500 ℃, 665 ℃, 686 ℃, 692 ℃ and 688 ℃;
the residence time of the magnetic core in the tunnel furnace is 75min;
the conductive silver paste comprises the following components:
60wt% of silver powder;
9wt% of lead-free glass with the particle size of 2-5 mu m;
4wt% of ethyl cellulose;
terpineol balance;
the silver powder consists of nano silver powder with the particle size of less than 100nm, superfine silver powder and silver micro powder with the particle size of 1-5 mu m, wherein the particle size of the superfine silver powder is more than 100nm and less than 1 mu m; the weight ratio of the nanometer silver powder to the superfine silver powder to the silver micro powder is 1:2:7.
example 3
Substantially the same as in example 1, except that:
the sintering method of the conductive silver layer comprises the following steps:
passing the magnetic core coated with the conductive silver paste through a tunnel furnace, wherein the tunnel furnace is divided into 7 continuous furnace bodies with the same length, and the sintering temperature of the furnace bodies from front to back is 300 ℃, 400 ℃, 500 ℃, 655 ℃, 684 ℃, 688 ℃ and 692 ℃ in sequence;
the residence time of the magnetic core in the tunnel furnace is 80min;
the conductive silver paste comprises the following components:
63wt% of silver powder;
8wt% of lead-free glass with the particle size of 2-5 mu m;
3wt% of ethyl cellulose;
terpineol balance;
the silver powder consists of nano silver powder with the particle size of less than 100nm, superfine silver powder and silver micro powder with the particle size of 1-5 mu m, wherein the particle size of the superfine silver powder is more than 100nm and less than 1 mu m; the weight ratio of the nanometer silver powder to the superfine silver powder to the silver micro powder is 1:4:5.
example 4
Substantially the same as in example 1, except that:
the sintering method of the conductive silver layer comprises the following steps:
passing the magnetic core coated with the conductive silver paste through a tunnel furnace, wherein the tunnel furnace is divided into 7 continuous furnace bodies with the same length, and the sintering temperature of the furnace bodies from front to back is 300 ℃, 400 ℃, 500 ℃, 665 ℃, 687 ℃, 692 ℃ and 692 ℃ in sequence;
the residence time of the magnetic core in the tunnel furnace is 75min;
the conductive silver paste comprises the following components:
62wt% of silver powder;
7wt% of lead-free glass with the particle size of 2-5 mu m;
3wt% of ethyl cellulose;
0.2wt% of silane coupling agent KH-560;
terpineol balance;
the silver powder consists of nano silver powder with the particle size of less than 100nm, superfine silver powder and silver micro powder with the particle size of 1-5 mu m, wherein the particle size of the superfine silver powder is more than 100nm and less than 1 mu m; the weight ratio of the nanometer silver powder to the superfine silver powder to the silver micro powder is 1:4:5.
comparative example 1
Substantially the same as in example 1, except that the sintering temperature was different:
the magnetic core coated with the conductive silver paste was passed through a tunnel furnace which was divided into 7 continuous furnace bodies of the same length, and the sintering temperature from the front to the rear furnace bodies was 300 ℃, 400 ℃, 500 ℃, 660 ℃, 670 ℃, 680 ℃.
Comparative example 2
Substantially the same as in example 1, except that the sintering temperature was different:
the magnetic core coated with the conductive silver paste is passed through a tunnel furnace, and sintered for 15min at 670 ℃; sintering at 680 deg.c for 10min.
Performance testing
The magnetic cores of example 1, example 4, comparative example 1, comparative example 2 were observed for defects under a microscope after preparing a silver layer (not tin-nickel plated). 1000 samples were prepared for each example, and the number of times of occurrence of silver diffusion, silver exposure, silver flow, and silver connection phenomena was counted. Table 2 below:
TABLE 2
| Upper silver diffusion | Silver coating body | Silver flow | Silver connecting material | |
| Example 1 | 3 | 11 | 0 | 0 |
| Example 4 | 0 | 0 | 0 | 0 |
| Comparative example 1 | 15 | 42 | 3 | 7 |
| Comparative example 2 | 19 | 41 | 8 | 13 |
The upper silver diffusion phenomenon can be seen in fig. 1, the upper silver dew body phenomenon can be seen in fig. 2, the silver flowing phenomenon can be seen in fig. 3, and the silver connecting phenomenon can be seen in fig. 4.
It can be found by the above test that:
1. the defects can be obviously reduced by adopting three silver powder combinations and combining the optimization of the sintering temperature of the scheme;
2. the addition of the silane coupling agent is beneficial to promoting the strength of the combination of the silver micro powder, the superfine silver powder and the organic phase; avoiding the phenomenon of exposing the body.
3. The formula needs to accurately control the heating sintering temperature.
Claims (4)
1. The preparation method of the inductance magnetic core is characterized in that the method comprises the steps of sintering a conductive silver layer, an electroplated nickel layer and an electroplated tin layer on the surface of the magnetic core;
the sintering method of the conductive silver layer comprises the following steps:
the magnetic core coated with the conductive silver paste passes through a tunnel furnace, wherein the tunnel furnace is divided into 7 continuous furnace bodies with the same length, and the sintering temperature of the furnace bodies from front to back is 300+/-20 ℃, 400+/-20 ℃, 500+/-20 ℃, 660+/-5 ℃, 685+/-2 ℃, 690+/-2 ℃ and 690+/-2 ℃ in sequence;
the residence time of the magnetic core in the tunnel furnace is 75-80min;
the thickness of the conductive silver layer is 2.8-3.7 mu m;
the conductive silver paste comprises the following components:
60-65wt% of silver powder;
4-9wt% of lead-free glass;
1-4wt% of ethyl cellulose;
the balance of organic solvent;
the silver powder consists of nano silver powder with the particle size of less than 100nm, superfine silver powder and silver micro powder with the particle size of 1-5 mu m, wherein the particle size of the superfine silver powder is more than 100nm and less than 1 mu m; the weight ratio of the nanometer silver powder to the superfine silver powder to the silver micro powder is 1:2-4:5-7;
the content of inorganic components in the conductive silver paste is 70+/-3 wt%;
the conductive silver paste also comprises a silane coupling agent, wherein the dosage of the silane coupling agent is 0.1-0.3wt%.
2. The method for manufacturing an inductor core according to claim 1, wherein the organic solvent is terpineol, ethylene glycol monomethyl ether or propylene glycol methyl ether acetate.
3. The method of manufacturing an inductor core according to claim 1, wherein the lead-free glass has a particle size of 2-5 μm.
4. The method for manufacturing an inductor core according to claim 1, wherein the electroplated nickel layer has an electroplating thickness of 2.9 to 3.9 μm and the electroplated tin layer has an electroplating thickness of 2.1 to 2.45 μm.
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| CN102262941B (en) * | 2011-07-19 | 2012-09-19 | 彩虹集团公司 | Method for preparing environment-friendly terminal electrode dipping silver paste for chip inductor |
| CN102610326B (en) * | 2011-12-31 | 2014-06-18 | 广东羚光新材料股份有限公司 | Conductive silver paste for ferrite core inductance and method for producing same |
| CN106098150A (en) * | 2016-08-30 | 2016-11-09 | 中国振华集团云科电子有限公司 | The inductor ends of low-temperature sintering low silver content is coated with formula of silver slurry and preparation method thereof |
| CN107892563A (en) * | 2017-11-14 | 2018-04-10 | 中山市东晨磁性电子制品有限公司 | A kind of manufacture method of high pendulum folding intensity nickel zinc soft magnetic core |
| CN109215843A (en) * | 2018-11-05 | 2019-01-15 | 肇庆市辰业电子有限公司 | A kind of inductance is with exempting to plate termination electrode silver paste |
| CN111627590A (en) * | 2020-02-29 | 2020-09-04 | 上海宝银电子材料有限公司 | Conductive silver paste for chip inductor and preparation method thereof |
| CN112028615A (en) * | 2020-09-18 | 2020-12-04 | 深圳振华富电子有限公司 | Low-temperature co-fired ceramic material, laminated chip inductor and preparation method thereof |
| CN114171255A (en) * | 2021-11-16 | 2022-03-11 | 南通强生光电科技有限公司 | Composite conductive functional silver paste and preparation method thereof |
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