CN114242300A - Conductive copper paste for ferrite core inductance and preparation method thereof - Google Patents
Conductive copper paste for ferrite core inductance and preparation method thereof Download PDFInfo
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- CN114242300A CN114242300A CN202111532164.5A CN202111532164A CN114242300A CN 114242300 A CN114242300 A CN 114242300A CN 202111532164 A CN202111532164 A CN 202111532164A CN 114242300 A CN114242300 A CN 114242300A
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- copper powder
- ferrite core
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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
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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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- 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
Abstract
The invention provides conductive copper paste for ferrite core inductance and a preparation method thereof. The raw materials of the conductive copper paste comprise the following substances in mass ratio: 2-15%; copper powder: 61-84%; organic carrier: 5-25%; inorganic additives: 7-14%; wherein the copper powder is a mixture of flake copper powder and superfine spherical copper powder. The preparation method comprises the steps of mixing the solvent, the copper powder, the organic carrier and the inorganic additive according to a certain proportion, and mixing and rolling the uniformly mixed slurry again by using a three-roller machine. The ferrite conductive copper paste can effectively overcome the defects of similar products in the aspects of adhesive force, corrosivity, electroplating property and the like, can ensure the consistency and stability of the product process by using the copper paste prepared by the process, is far lower in price than silver paste products, and is an ideal substitute for lead-containing paste.
Description
Technical Field
The invention relates to the technical field of conductive paste, in particular to conductive copper paste for ferrite core inductance and a preparation method thereof.
Background
The conductive silver paste is widely used in various high-performance electronic products as a basic functional material in electronic information and electronic industries. At present, conductive silver paste is mature to be applied to ferrite core inductance components, mainly because metal silver has the advantages of high conductivity, excellent adhesion property, weldability and the like, but because the price of the ferrite core inductance components is continuously lowered due to the high cost of silver and the intense competition, the profits of the ferrite core inductance components are reduced more and more, and the application and popularization of the metal silver in the ferrite core inductance components are greatly limited. Meanwhile, the ferrite core inductance silver paste generally has certain defects, such as cracks, non-compact silver layer, more defects and the like easily generated after sintering, so that the chip inductance is lower in quality factor and higher in circuit noise.
Therefore, it is important to select a material with relatively good conductivity and adhesion and good solderability to replace metallic silver for the ferrite core inductor component.
The metal copper has a plurality of excellent performances, the copper has better high-frequency characteristics and conductivity than noble metal silver, meanwhile, the copper also has excellent weldability and lower cost, and the copper has good adhesiveness after being sintered with corresponding glass powder, so that the metal copper also has stronger application value in the field of ferrite core inductance components according to the characteristics.
In summary, it is important to provide a conductive paste made of copper metal.
Disclosure of Invention
According to the technical problems that the price of metal silver is high, and the prepared silver paste is easy to generate cracks, the silver layer is not compact and the like after sintering, the conductive copper paste for the ferrite core inductor and the preparation method thereof are provided. The copper paste is prepared by uniformly mixing flake copper powder, superfine spherical copper powder, an organic solvent, an inorganic additive and the like, and mixing and rolling the mixed paste again by using a three-roller machine. The ferrite conductive copper paste provided by the invention has the advantages of difficult cracking, corrosion resistance, strong adhesive force, higher compactness, excellent electroplating performance and the like, and can effectively overcome the defects of similar products in the aspects of adhesive force, corrosivity, electroplating performance and the like.
The technical means adopted by the invention are as follows:
the conductive copper paste for the ferrite core inductor comprises the following raw materials in percentage by mass:
solvent: 2-15%;
copper powder: 61-84%;
organic carrier solution: 5-25%;
inorganic additives: 7-14%;
wherein the copper powder is a mixture of flake copper powder and superfine spherical copper powder.
Furthermore, the flake copper powder accounts for 50-64% of the raw materials; 11-20% of the superfine spherical copper powder, wherein the grain diameter of the superfine spherical copper powder is 1.5-2 μm.
Further, the solvent is one or a mixture of more of terpineol, diethylene glycol monobutyl ether, butyl cellosolve, butyl carbitol, dibutyl phthalate and the like.
Further, the organic carrier in the organic carrier solution is one or a mixture of more of polyacrylate, cellulose resin, polyvinyl butyral and the like.
Further, the inorganic additive is one or a mixture of more of silicon oxide, zinc oxide, boron trioxide and potassium oxide.
The invention also discloses a preparation method of the conductive copper paste for the ferrite core inductor, which comprises the steps of mixing the solvent, the copper powder, the organic carrier solution and the inorganic additive according to a certain proportion, and mixing and rolling the uniformly mixed paste again by using a three-roller machine for 8-15 min, wherein the rotating speed is 450-600 rpm/min, and the rolling frequency is within the range of 6-8 pass.
Further, the method specifically comprises the following steps:
s1, mixing a certain proportion of solvent and organic carrier, heating and dissolving to obtain an organic solution adhesive, namely an organic carrier solution;
s2, adding the organic carrier solution prepared in the step S1 in the preset proportion into the inorganic additive in the preset proportion after uniformly stirring, and stirring and dispersing at high speed;
s3, adding the flake copper powder and the superfine spherical copper powder in a preset proportion into the step S2, and stirring and dispersing at a high speed to prepare viscous slurry;
and S4, rolling the slurry by a three-roller machine, fully mixing, extruding and shearing, namely dispersing at a high speed (preferably, mixing for about 10min, rotating speed of 500rpm/min, rolling times within a range of 6-8 pass) to uniformly mix copper powder in a solvent, and screening by a 200-mesh screen to obtain the conductive copper slurry for the ferrite core inductor.
Further, in the step S1, the solvent accounts for 75-90% and the organic carrier accounts for 10-25%, and the organic carrier solution is obtained after mixing, heating and dissolving.
Compared with the prior art, the invention has the following advantages:
1. the invention uses two copper powders with different shapes as raw materials for ferrite core inductance, and the two copper powders compensate the incompactness of the slurry of the copper powder with a single shape after sintering under a specific proportion.
2. According to the invention, through a specific preparation process, the slurry is dispersed more uniformly, the sintered slurry is more compact, and the defects of the slurry in the aspects of corrosivity, electroplating property and the like are effectively overcome.
In conclusion, the conductive copper paste for the ferrite core inductor and the specific preparation process provided by the invention solve the defects of the similar products in the aspects of adhesive force, corrosivity, electroplating property and the like, are far lower in price than silver paste products, and are ideal substitutes of lead-containing paste.
Based on the reasons, the invention can be widely popularized in the field of conductive paste.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is an SEM picture of the surface of the ferrite core plated with nickel in the first embodiment of the present invention.
Fig. 2 is an SEM picture of the surface of the ferrite core plated with nickel in example two of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The invention provides conductive copper paste for ferrite core inductance, which comprises the following raw materials in percentage by mass:
solvent: 2-15%; the flake copper powder accounts for 50-64%; 11-20% of superfine spherical copper powder, wherein the particle size of the superfine spherical copper powder is 1.5-2 μm; organic carrier solution: 5-25%; inorganic additives: 7-14%;
the solvent is one or a mixture of more of terpineol, diethylene glycol butyl ether, butyl cellosolve, butyl carbitol, dibutyl phthalate and the like.
The organic carrier is one or a mixture of more of polyacrylate, cellulose resin, polyvinyl butyral and the like.
The inorganic additive is one or a mixture of more of silicon oxide, zinc oxide, boron trioxide and potassium oxide.
The conductive copper paste for the ferrite core inductor is prepared by the following method,
the method specifically comprises the following steps:
s1, mixing and heating a solvent (75-90%) and an organic carrier (10-25%) in a certain proportion for dissolving to obtain an organic solution adhesive, namely an organic carrier solution;
s2, adding the organic carrier solution prepared in the step S1 in the preset proportion into the inorganic additive in the preset proportion after uniformly stirring, and stirring and dispersing at high speed;
s3, adding the flake copper powder and the superfine spherical copper powder in a preset proportion into the step S2, and stirring and dispersing at a high speed to prepare viscous slurry;
and S4, rolling the slurry by a three-roller machine, fully mixing, extruding and shearing, namely dispersing at a high speed (the mixing is about 10min, the rotating speed is 500rpm/min, and the rolling times are within the range of 6-8 pass) to uniformly mix the copper powder in the solvent, and sieving by a 200-mesh sieve to obtain the conductive copper slurry for the ferrite core inductor.
Example 1
1. Preparing an organic solution adhesive:
15% of butyl carbitol, 30% of terpineol, 30% of diethylene glycol monobutyl ether and 25% of polyacrylate, and the materials are mixed and heated and dissolved at 85-95 ℃ to obtain an organic solution adhesive serving as an organic carrier solution.
2. Preparing 5% of silicon oxide, 1.5% of zinc oxide, 2% of boron trioxide and 1.5% of potassium oxide into powder, uniformly stirring, adding 15% of organic carrier solution, stirring and dispersing at a high speed, adding 60% of flake copper powder and 15% of superfine spherical copper powder, stirring and dispersing at a high speed again, rolling by a three-roll machine, and sieving by a 200-mesh screen to obtain the conductive copper paste for the ferrite core inductor.
And transferring the copper paste to the surface of the ferrite core by using the prepared paste through a pad printing or spraying method to form a film with a required shape.
After sintering at 760 ℃, putting the surface of the ferrite magnetic core into a nickel-plating corrosive liquid, if the surface of the magnetic core does not crack, as shown in fig. 1, the surface is an SEM picture after nickel plating, namely, the surface shows corrosion resistance, and a tension meter is used for testing the adhesion of the product, as shown in 1-3 in table 1.
Example 2
1. Preparing an organic solution adhesive:
50% of terpineol, 25% of diethylene glycol monobutyl ether and 25% of polyacrylate, and the organic solution adhesive is obtained by mixing the materials and heating and dissolving at 85-95 ℃.
2. Preparing 5% of silicon oxide, 1.5% of zinc oxide, 2% of boron trioxide and 1.5% of potassium oxide into powder, uniformly stirring, adding 20% of organic carrier solution, stirring and dispersing at a high speed, adding 60% of flake copper powder and 10% of superfine copper powder, stirring and dispersing at a high speed again, rolling by a three-roll machine, and sieving by a 200-mesh screen to obtain the conductive copper paste for ferrite core inductance.
And transferring the copper paste to the surface of the ferrite core by using the prepared paste through a pad printing or spraying method to form a film with a required shape.
After sintering at 760 ℃, the surface of the ferrite core is subjected to nickel plating corrosion solution, if the surface of the core is not cracked, fig. 2 shows an SEM picture of the sintered ferrite core after being subjected to the surface nickel plating corrosion solution, namely corrosion resistance is shown, and a product is tested for adhesion by using a tension meter, as shown in 4-6 in table 1.
Table 1 adhesion test using a tensile tester for the products of examples 1 and 2
| Serial number | 1 | 2 | 3 | 4 | 5 | 6 |
| Adhesion (N) | 42 | 45.5 | 44 | 50 | 49 | 48.5 |
As can be seen from table 1, good adhesion is exhibited in example two relative to the test values of example one when the vehicle loading is increased.
Example 3
On the basis of the embodiment 1, the proportion of the inorganic additive is adjusted, 5% of silicon oxide, 1.5% of zinc oxide, 1% of boron trioxide and 2.5% of potassium oxide are selected to prepare powder, organic carrier solution under the same conditions is added for gathering, after high-speed stirring and dispersion, 60% of flake copper powder and 10% of superfine copper powder are added, after high-speed stirring and dispersion again, the mixture is rolled by a three-roller machine and then passes through a 200-mesh screen to prepare the conductive copper paste for ferrite core inductance.
And transferring the copper paste to the surface of the ferrite core by using the prepared paste through a pad printing or spraying method to form a film with a required shape. And sintering at 760 ℃ and then carrying out nickel plating on the surface of the ferrite core by using the corrosive liquid. This example increases the content of organic potassium oxide, lowers the softening temperature of the organic material during high-temperature sintering, and makes it possible to make the surface of the ferrite core denser, to make the surface of the core free from cracks, and to exhibit good corrosion resistance and adhesion.
Example 4
On the basis of the embodiment 2, the proportion of the inorganic additive is adjusted, 5% of silicon oxide, 1.5% of zinc oxide, 1% of boron trioxide and 2.5% of potassium oxide are selected and selected to prepare powder, organic carrier solution under the same conditions is added for gathering, after high-speed stirring and dispersion, 60% of flake copper powder and 10% of superfine copper powder are added, after high-speed stirring and dispersion again, after rolling by a three-roll machine, the mixture is sieved by a 200-mesh screen to prepare the conductive copper paste for ferrite core inductance.
And transferring the copper paste to the surface of the ferrite core by using the prepared paste through a pad printing or spraying method to form a film with a required shape. After sintering at 760 ℃, the surface of the ferrite core is plated with nickel corrosive liquid, and if the surface of the core is not cracked, the ferrite core also has good corrosion resistance and adhesiveness.
In conclusion, it can be shown from the examples 1 and 2 that the obtained copper paste has good sintering and corrosion resistance properties by only changing the proportion of the organic carrier under the condition that the proportion of the inorganic additive is not changed.
It can be seen from examples 1 and 3 and examples 2 and 4 that the copper pastes prepared by adding inorganic additives in different proportions have good sintering property and corrosion resistance without changing the proportion of the organic carrier.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. The conductive copper paste for the ferrite core inductor is characterized by comprising the following raw materials in percentage by mass:
solvent: 2-15%;
copper powder: 61-84%;
organic carrier solution: 5-25%;
inorganic additives: 7-14%;
wherein the copper powder is a mixture of flake copper powder and superfine spherical copper powder.
2. The conductive copper paste for the inductance of the ferrite core according to claim 1, wherein the flake copper powder accounts for 50-64% of the raw materials; 11-20% of the superfine spherical copper powder, wherein the grain diameter of the superfine spherical copper powder is 1.5-2 μm.
3. The conductive copper paste for ferrite core inductors according to claim 1, wherein the solvent is one or a mixture of more of terpineol, butyl diglycol, butyl cellosolve, butyl carbitol and dibutyl phthalate.
4. The conductive copper paste for the inductance of the ferrite magnetic core as claimed in claim 1, wherein the organic carrier in the organic carrier solution is one or a mixture of polyacrylate, cellulose resin and polyvinyl butyral.
5. The conductive copper paste for ferrite core inductors according to claim 1, wherein said inorganic additive is one or a mixture of silicon oxide, zinc oxide, boron trioxide and potassium oxide.
6. A method for preparing the conductive copper paste for ferrite core inductance according to any one of claims 1 to 5, characterized in that: mixing a certain proportion of solvent, copper powder, organic carrier solution and inorganic additive, and mixing and rolling the uniformly mixed slurry again by using a three-roller machine for 8-15 min, wherein the rotating speed is 450-600 rpm/min, and the rolling frequency is 6-8 pass.
7. The method for preparing the conductive copper paste for the ferrite core inductor according to claim 6, which comprises the following steps:
s1, mixing a certain proportion of solvent and organic carrier, heating and dissolving to obtain an organic carrier solution;
s2, uniformly stirring the inorganic additive in a preset proportion, adding the organic carrier solution prepared in the step S1 in the preset proportion, and stirring at a high speed for dispersing;
s3, adding the flake copper powder and the superfine spherical copper powder in a preset proportion into the step S2, and stirring and dispersing at a high speed to prepare viscous slurry;
and S4, rolling the slurry by a three-roller machine, and screening by a 200-mesh screen to obtain the conductive copper slurry for the ferrite core inductor.
8. The method for preparing the conductive copper paste for the ferrite core inductor according to claim 6, wherein in the step S1, the solvent accounts for 75-90%, the organic carrier accounts for 10-25%, and the organic carrier solution is obtained after mixing, heating and dissolving.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114883103A (en) * | 2022-04-28 | 2022-08-09 | 广州三则电子材料有限公司 | Method for manufacturing low-temperature sintered copper electrode alloy iron powder core power inductor |
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| CN103310870A (en) * | 2012-03-12 | 2013-09-18 | 深圳市圣龙特电子有限公司 | Lead-free copper slurry applied to silicon solar battery electrode and preparation method thereof |
| CN106981324A (en) * | 2017-04-26 | 2017-07-25 | 上海安缔诺科技有限公司 | A kind of copper electrocondution slurry and its production and use |
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2021
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Patent Citations (5)
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| US20070209475A1 (en) * | 2004-04-28 | 2007-09-13 | Mitsui Mining & Smelting Co., Ltd. | Flaky Copper Powder, Method For Producing The Same, And Conductive Paste |
| CN102610326A (en) * | 2011-12-31 | 2012-07-25 | 肇庆市羚光电子化学品材料科技有限公司 | Conductive silver paste for ferrite core inductance and method for producing same |
| CN103310870A (en) * | 2012-03-12 | 2013-09-18 | 深圳市圣龙特电子有限公司 | Lead-free copper slurry applied to silicon solar battery electrode and preparation method thereof |
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| CN114883103A (en) * | 2022-04-28 | 2022-08-09 | 广州三则电子材料有限公司 | Method for manufacturing low-temperature sintered copper electrode alloy iron powder core power inductor |
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