CN111524677A - 35 carbonyl iron powder core of magnetic conductivity - Google Patents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/42—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/005—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing gelatineous or gel forming binders, e.g. gelatineous Al(OH)3, sol-gel binders
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
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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
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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Abstract
The invention discloses a 35-carbonyl iron powder core with magnetic conductivity, which comprises the following raw materials: carbonyl iron, chromate, phosphoric acid, a component A, a component B and a lubricant. The magnetic conductivity 35 carbonyl iron powder core obtained by the technical scheme of the invention realizes that the performance of the magnetic conductivity 35 carbonyl iron powder core is kept in a basically unchanged state under the condition of 180 ℃ for 8760 hours, and no obvious thermal aging phenomenon occurs. Compared with the similar iron powder cores in the current market, the iron powder core loss is reduced by 30-50%.
Description
Technical Field
The invention relates to the field of materials, in particular to a 35 carbonyl iron core with magnetic conductivity.
Background
With the development of modern electronic information industry technology, the application market scale of the iron powder core is gradually increased, and the iron powder core is mainly applied to an electric appliance loop to solve the problem of electromagnetic compatibility (EMC). In practical application, various other substances can be added according to different requirements on filtering under different wave bands. The iron powder core is a common soft magnetic material and is one of the materials with lower market price at present. The material is composed of carbon-based ferromagnetic powder and resin carbon-based ferromagnetic powder, and due to low price, the iron powder core is still the magnetic powder core with the largest use amount so far, and the magnetic conductivity is between 10 and 100. The magnetic conductivity 35 carbonyl iron powder core is used as one kind of iron powder core and is widely applied to modern instruments and equipment.
Although the raw materials and the formula of the carbonyl iron powder core in the prior art are numerous, the magnetic conductivity 35 carbonyl iron powder core obtained by adopting the existing raw materials and the formula cannot meet the requirements of practical application, cannot resist high temperature in the using process, is easy to age and burn, seriously restricts the production efficiency and even the development of science and technology, and therefore, a new magnetic conductivity 35 carbonyl iron powder core is urgently needed to be researched.
Disclosure of Invention
The invention solves the problems that the existing 35 carbonyl iron powder core with magnetic conductivity cannot be used at a higher temperature in the application process and can burn due to aging after long-term use.
In order to solve the technical problem, the technical scheme is as follows: providing a 35-carbonyl iron powder core with magnetic permeability, wherein the iron powder core comprises the following raw materials: carbonyl iron, chromate, phosphoric acid, a component A, a component B and a lubricant.
On the basis of the raw materials, through further experimental study, the carbonyl iron powder core raw materials comprise: 100 parts of carbonyl iron, 0.18-0.6 part of chromate, 0.2-0.8 part of phosphoric acid, 0.5-1.2 parts of component A, 2-6 parts of component B and 0.3-0.6 part of lubricant.
In a specific embodiment of the present invention, the carbonyl iron powder core raw material includes: 100 parts of carbonyl iron, 0.3-0.6 part of chromate, 0.3-0.6 part of phosphoric acid, 0.5-1.2 parts of component A, 2-6 parts of component B and 0.3-0.6 part of lubricant.
In the invention, the carbonyl iron is carbonyl iron powder, and the granularity of the carbonyl iron powder is D10= 1.5-3.5 microns, D50= 3.0-5.5 microns, and D90= 6.0-9.5 microns.
In the present invention, the chromate includes potassium dichromate, sodium dichromate, calcium dichromate, etc., and preferably, the chromate is potassium dichromate.
In the present invention, the lubricant comprises: lithium stearate, zinc stearate, calcium stearate, barium stearate, and the like, and in one embodiment of the invention, the lubricant is lithium stearate.
In the present invention, the component a comprises: one or more of clay such as mica, kaolin, and diatomite.
The component A can play a role in supporting the carbonyl iron core, can help the carbonyl iron to form effective gaps in the carbonyl iron core manufactured after molding, is helpful to improve the direct current lamination characteristic of the carbonyl iron core, and is also beneficial to bearing higher sintering temperature of the carbonyl iron core during high-temperature heat treatment.
In the invention, the component A is powder, and the particle size of the component A is 0-15 microns (excluding an endpoint of 0).
In the present invention, the component B comprises: one or more of silica sol, aluminum sol and silicon-aluminum sol.
According to the invention, the carbonyl iron powder core raw material also comprises one or two of water and alcohol, the carbonyl iron powder core raw material also comprises water and alcohol, the water and chromate are prepared into 6-10 wt% of chromate water solution, and the alcohol and phosphoric acid are prepared into 2-4 wt% of phosphoric acid alcohol solution. The invention adopts the mixed solution of alcohol and water as the solvent to accelerate the generation of the chromium oxide film.
The reason for generating thermal aging is that the organic binder causes the characteristic failure of the material and the loss of the insulation effect due to the decomposition of organic functional groups under the high-temperature condition, thereby causing the reduction of the insulation effect among powder particles to be weak or disappear, causing the eddy current loss of the carbonyl iron powder core to be greatly increased, causing the temperature of the carbonyl iron powder core to be further increased, further aggravating the aging failure of the organic binder, causing the vicious circle to finally cause the over-high loss of the carbonyl iron powder core, causing the complete failure of the iron powder core and seriously causing the burning of the circuit board.
On the basis of the raw materials, the preparation method of the 35 carbonyl iron powder core with the magnetic conductivity is also researched, and the preparation method of the 35 carbonyl iron powder core with the magnetic conductivity comprises the following steps:
a. mixing carbonyl iron with 6-10% of chromate aqueous solution, and simultaneously continuously adding 2-4 wt% of phosphoric acid alcohol solution, wherein the weight ratio of the chromate aqueous solution to the carbonyl iron is 3-6%, preferably 5%, and the weight ratio of the phosphoric acid alcohol solution to the carbonyl iron is 10-15%, preferably 15%;
b. drying the material obtained in the step a at 70 ℃, and then treating the material for 90 minutes at 150 ℃;
c. adding an alcohol solution containing the component A into the material obtained in the step b, and stirring the mixture to a dry state, wherein the weight ratio of the component A to carbonyl iron is 0.5-1.2%, and the weight ratio of the alcohol to the carbonyl iron is 8-15%;
d. c, mixing the material obtained in the step c with a component B, and drying, wherein the weight ratio of the component B to carbonyl iron is 2-6%;
e. and d, adding a lubricant into the material obtained in the step d, wherein the weight of the lubricant is 0.3-0.6% of the weight of the material, and then performing compression molding to obtain the material.
The steps a to e ensure that the surface of each powder particle can be fully contacted with the component B, and the anti-aging effect is good.
In the step e, the condition of press forming is 5-18T/cm2Is pressed and molded under the pressure of (2), and further is 8-18T/cm2Preferably 10 to 18T/cm2Is press-formed under a pressure of (1).
The preparation method further comprises the step of carrying out heat treatment on the carbonyl iron powder core subjected to compression molding under the inert gas condition, wherein the heat treatment temperature is 400-600 ℃, and the time is 60-120 min.
The invention provides a 35 carbonyl iron powder core with low loss and high direct current superposition characteristic and no aging, which has better surface coating effect by adding non-aging high-temperature-resistant components and matching with an effective surface treatment process and a method, and ensures that each particle can be fully contacted with the added non-aging high-temperature-resistant components. Compared with the same type of carbonyl iron powder cores in the current market, the loss of the carbonyl iron powder cores is reduced by 30-50%.
Detailed Description
The technical solution of the present invention will be further specifically described below by way of specific examples.
In the present invention, all the raw materials and equipment used are commercially available unless otherwise specified.
Example one
Selecting carbonyl iron powder with purity of more than 97.5 percent as the iron powder of the raw material, wherein the granularity is as follows: d10= 1.5-3.5 microns, D50= 3.0-5.5 microns, D90= 6.0-9.5 microns, and is prepared with 2wt% phosphoric acid alcohol solution and 6wt% potassium dichromate water solution.
Mixing and stirring the potassium dichromate water solution and carbonyl iron powder, and meanwhile, slowly adding the phosphoric acid alcohol solution into the mixture, stirring the mixture for 1 hour, stirring the mixture at the temperature of 70 ℃ until the powder is dried, and then baking the mixture for 90 minutes at the temperature of 150 ℃. The proportion of the potassium dichromate water solution and the carbonyl iron powder is 5 percent. The proportion of the phosphoric acid alcohol solution and the carbonyl iron powder is 15 percent.
Adding mica powder into alcohol liquid, mixing to obtain uniform suspension etching solution, adding the mixed solution into the dried powder, and stirring until the powder is dried. Wherein the weight ratio of the mica powder to the carbonyl iron powder is 1.2 percent, and the weight ratio of the alcohol to the carbonyl iron powder is 12 percent. Adding the silica-alumina sol into the dried powder, stirring for 20 minutes, then sieving the powder in a semi-wet state by a 60-mesh sieve, and then drying the powder in a baking oven at 80 ℃. The ratio of the silicon-aluminum sol to the carbonyl iron powder is 3 percent.
And adding 0.3% of lithium stearate serving as a lubricant into the dried carbonyl iron powder, and uniformly mixing. At 8T/cm2Pressed into an iron powder core under the pressure of the press.
And carrying out heat treatment on the blank iron powder core under the nitrogen condition, wherein the heat treatment temperature is 400 ℃ and the time is 60 minutes.
The inductance and Q value are tested by using HP4284A under the test conditions of 100kHz1V and N =20 turn, 18.6uH of inductance, Q =227, and 998mW/cm of loss3(50 kHz/100 mT). Placing the iron powder core for 8760 hours at 180 ℃, wherein the electric inductance of the iron powder core is 18.3uH, the Q value is 224, and the loss is 987 mW/cm3(50kHz/100mT)。
Example two
The difference between this example and the first example is that the mica powder is replaced by kaolin and diatomite, the weight ratio of kaolin to carbonyl iron powder is 0.6%, and the weight ratio of diatomite to carbonyl iron powder is 0.6%. Silica sol is used to replace silica-alumina sol, and the ratio of silica sol to carbonyl iron powder is 4%. 0.3% lithium stearate was added as a lubricant.
At 10/cm2Pressed into an iron powder core under the pressure of the press. The heat treatment conditions are nitrogen, the heat treatment temperature is 500 ℃, and the time is 60 minutes.
The inductance and the Q value are tested by using HP4284A under the test condition of 100kHz1V, N =20 turns, the inductance is 19.4uH, Q =206 and the loss is 963mW/cm3(50 kHz/100 mT). Placing the iron powder core for 8760 hours at 180 ℃, wherein the electric inductance of the iron powder core is 19.6uH, the Q value is 207, and the loss is 947 mW/cm3(50kHz/100mT)。
EXAMPLE III
The difference between the example and the first example is that the mica powder is replaced by diatomite, and the weight ratio of the diatomite to the carbonyl iron powder is 0.9%. Silica sol is used to replace silica-alumina sol, and the weight ratio of silica sol to carbonyl iron powder is 5%. 0.3% lithium stearate was added as a lubricant.
At 12/cm2Pressed into an iron powder core under the pressure of the press. The heat treatment conditions are nitrogen, the heat treatment temperature is 600 ℃, and the time is 60 minutes.
The inductance and the Q value are tested by using HP4284A under the test conditions of 100kHz1V, N =20 turns, the inductance is 19.2uH, Q =201, and the loss is 910mW/cm3(50 kHz/100 mT). Placing the iron powder core for 8760 hours at 180 ℃, wherein the electric inductance of the iron powder core is 19.5uH, the Q value is 195, and the loss is 923 mW/cm3(50kHz/100mT)。
Example four
Selecting carbonyl iron powder with purity of more than 97.5 percent as the iron powder of the raw material, wherein the granularity is as follows: d10= 1.5-3.5 microns, D50= 3.0-5.5 microns, D90= 6.0-9.5 microns,
3wt% concentration alcohol solution of phosphoric acid and 8wt% concentration water solution of potassium dichromate.
Mixing and stirring the potassium dichromate water solution and carbonyl iron powder, and meanwhile, slowly adding a phosphoric acid alcohol solution into the mixture for 2 hours, then stirring the mixture at 70 ℃ until the powder is dried, and then baking the powder for 90 minutes at 150 ℃. The ratio of the potassium dichromate water solution to the carbonyl iron powder is 3 percent. The proportion of the phosphoric acid alcohol solution and the carbonyl iron powder is 12 percent.
Adding mica powder into alcohol liquid, mixing to obtain uniform suspension etching solution, adding the mixed solution into the dried powder, and stirring until the powder is dried. Wherein the weight ratio of the mica powder to the carbonyl iron powder is 0.8 percent, and the weight ratio of the alcohol to the carbonyl iron powder is 8.0 percent.
Adding the aluminum sol into the dried powder, stirring for 20 minutes, then sieving the semi-wet powder with a 60-mesh sieve, and then drying the powder in a baking oven at 80-100 ℃. The ratio of the alumina sol to the carbonyl iron powder is 5%.
Lithium stearate is added into the dried carbonyl iron powder as a lubricant, the weight ratio of the lithium stearate to the dried carbonyl iron powder is 0.6%, and the lithium stearate and the dried carbonyl iron powder are uniformly mixed. At 18/cm2Pressed into an iron powder core under the pressure of the press.
And (3) carrying out heat treatment on the blank iron powder core under the nitrogen condition, wherein the heat treatment temperature is 600 ℃, and the time is 90 minutes.
The inductance and the Q value are tested by using HP4284A under the test condition of 100kHz1V, N =20 turns, the inductance is 19.9uH, Q =198, and the loss is 824mW/cm3(50 kHz/100 mT). Placing the iron powder core for 8760 hours at 180 ℃, wherein the electric inductance of the iron powder core is 19.5uH, the Q value is 192, and the loss is 812 mW/cm3(50kHz/100mT)。
EXAMPLE five
Selecting carbonyl iron powder with purity of more than 97.5 percent as the iron powder of the raw material, wherein the granularity is as follows: d10= 1.5-3.5 microns, D50= 3.0-5.5 microns, D90= 6.0-9.5 microns,
preparing phosphoric acid alcohol solution with the concentration of 4wt%, and preparing potassium dichromate water solution with the concentration of 10 wt%.
Mixing and stirring the potassium dichromate water solution and carbonyl iron powder, and meanwhile, slowly adding the phosphoric acid alcohol solution into the mixture for 1.5 hours, then stirring the mixture at 70 ℃ until the powder is dried, and then baking the powder for 90 minutes at 150 ℃. The proportion of the potassium dichromate water solution and the carbonyl iron powder is 6 percent. The proportion of the phosphoric acid alcohol solution and the carbonyl iron powder is 15 percent.
Adding mica powder into alcohol liquid, mixing to obtain uniform suspension etching solution, adding the mixed solution into the dried powder, and stirring until the powder is dried. Wherein the weight ratio of the mica powder to the carbonyl iron powder is 0.5 percent, and the weight ratio of the alcohol to the carbonyl iron powder is 10.0 percent.
Adding the aluminum sol into the dried powder, stirring for 20 minutes, then sieving the powder in a semi-wet state through a 60-mesh sieve, and then drying the powder in a 80-DEG oven. The ratio of the alumina sol to the carbonyl iron powder is 4%.
Lithium stearate is added into the dried carbonyl iron powder as a lubricant, and the lithium stearate and the dried carbonyl iron powder are uniformly mixed according to the weight ratio of 0.4%. At 15/cm2Pressed into an iron powder core under the pressure of the press.
And carrying out heat treatment on the blank iron powder core under the nitrogen condition, wherein the heat treatment temperature is 500 ℃, and the time is 75 minutes.
The inductance and the Q value are tested by using HP4284A under the test condition of 100kHz1V, N =20 turns, the inductance is 18.8uH, Q =205 and the loss is 858mW/cm3(50 kHz/100 mT). Placing the iron powder core for 8760 hours at 180 ℃, wherein the electric inductance of the iron powder core is 18.9uH, the Q value is 198, and the loss is 867 mW/cm3(50kHz/100mT)。
Comparative example
Selecting carbonyl iron powder with purity of more than 97.5 percent as the iron powder of the raw material, wherein the granularity is as follows: d10= 1.5-3.5 microns, D50= 3.0-5.5 microns, and D90= 6.0-9.5 microns, and preparing a phosphoric acid acetone solution, wherein the weight ratio of phosphoric acid to carbonyl iron powder is 0.3%, and the weight ratio of acetone to carbonyl iron powder is 10%. Adding the phosphoric acid acetone solution into carbonyl iron powder, and uniformly stirring for 1 hour. Then adding an epoxy resin acetone solution, wherein the weight ratio of the epoxy resin to the carbonyl iron powder is 0.8 percent, and the weight ratio of the acetone to the carbonyl iron powder is 8 percent, stirring for 20 minutes, taking out the powder, sieving by a 40-mesh sieve, and airing.
And adding 0.3% of lithium stearate serving as a lubricating agent into the aired carbonyl iron powder, and uniformly mixing. At 5/cm2Pressed into carbonyl iron powder core.
And carrying out heat treatment on the blank carbonyl iron powder core under the air condition, wherein the heat treatment temperature is 160 ℃, and the time is 60 minutes.
The inductance and the Q value are tested by using HP4284A under the test condition of 100kHz1V, N =20 turns, the inductance is 18.5uH, Q =223, and the loss is 1581mW/cm3(50 kHz/100 mT). After the carbonyl iron powder core is placed for 8760 hours at the temperature of 180 ℃, the electric inductance of the carbonyl iron powder core is 15.6uH, the Q value is 34, and the loss is 2356 mW/cm3(50kHz/100mT)。
The test data for the first to fifth examples and comparative examples are as follows:
TABLE 1 test data
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. The magnetic permeability 35 carbonyl iron powder core is characterized in that the raw materials of the carbonyl iron powder core comprise: carbonyl iron, chromate, phosphoric acid, a component A, a component B and a lubricant, wherein the component A comprises: one or more of mica, kaolin and diatomite, wherein the component B comprises: silica sol, alumina sol, silica-alumina sol, or a mixture thereof.
2. The carbonyl iron powder core of claim 1, wherein the carbonyl iron powder core feedstock comprises: 100 parts of carbonyl iron, 0.18-0.6 part of chromate, 0.2-0.8 part of phosphoric acid, 0.5-1.2 parts of component A, 2-6 parts of component B and 0.2-0.8 part of lubricant.
3. The carbonyl iron powder core of claim 2, wherein the carbonyl iron powder core feedstock comprises: 100 parts of carbonyl iron, 0.3-0.6 part of chromate, 0.3-0.6 part of phosphoric acid, 0.5-1.2 parts of component A, 2-6 parts of component B and 0.3-0.6 part of lubricant.
4. The carbonyl iron powder core according to any one of claims 1 to 3, wherein the carbonyl iron is carbonyl iron powder, and the particle size of the carbonyl iron powder is D10= 1.5-3.5 microns, D50= 3.0-5.5 microns, and D90= 6.0-9.5 microns.
5. Carbonyl iron powder core according to any one of claims 1 to 3, characterized in that the chromate comprises potassium dichromate, potassium dichromate or calcium dichromate, preferably the chromate is potassium dichromate.
6. Carbonyl iron powder core according to any one of claims 1 to 3, characterized in that the lubricant comprises: lithium stearate, zinc stearate, barium stearate or calcium stearate, preferably, the lubricant is lithium stearate.
7. Carbonyl iron powder core according to any one of claims 1 to 3, characterized in that said component A comprises: one or more of mica, kaolin and diatomite.
8. A carbonyl iron powder core according to any one of claim 7, characterized in that, said component A is powder with particle size of 0-15 μm (excluding end 0).
9. Carbonyl iron powder core according to any one of claims 1 to 3, characterized in that said component B comprises: one or more of silica sol, aluminum sol and silicon-aluminum sol.
10. The carbonyl iron powder core according to any one of claims 1 to 3, wherein the raw material for the carbonyl iron powder core further comprises water and alcohol, the water and chromate form an aqueous solution of 6 to 10wt% of chromate, and the alcohol and phosphoric acid form an alcoholic solution of 2 to 4wt% of phosphoric acid.
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JP2006144096A (en) * | 2004-11-24 | 2006-06-08 | Jfe Steel Kk | Magnetic steel sheet with chromic acid-based insulating film |
CN101127269A (en) * | 2007-07-13 | 2008-02-20 | 李上奎 | Preparation method of high performance metal magnetic powder core for high frequency nonpolar lamp circuit |
CN103700460A (en) * | 2013-09-03 | 2014-04-02 | 横店集团东磁股份有限公司 | Preparation method of iron powder core with low loss and without heat aging |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2006144096A (en) * | 2004-11-24 | 2006-06-08 | Jfe Steel Kk | Magnetic steel sheet with chromic acid-based insulating film |
CN101127269A (en) * | 2007-07-13 | 2008-02-20 | 李上奎 | Preparation method of high performance metal magnetic powder core for high frequency nonpolar lamp circuit |
CN103700460A (en) * | 2013-09-03 | 2014-04-02 | 横店集团东磁股份有限公司 | Preparation method of iron powder core with low loss and without heat aging |
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Application publication date: 20200811 |