CN116092812A - Preparation method of carbonyl iron powder soft magnetic core for hundred MHz high frequency - Google Patents
Preparation method of carbonyl iron powder soft magnetic core for hundred MHz high frequency Download PDFInfo
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- 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
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
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Abstract
The invention relates to a preparation method of carbonyl iron powder magnetic core for hundred MHz high frequency, which comprises the following steps: proportioning carbonyl iron powder with different granularities, and then uniformly mixing; pouring the phosphoric acid solution into carbonyl iron powder which is uniformly mixed, mixing and stirring the mixture to form dry powder, drying the dry powder to obtain powder, adding the following insulating binding materials, drying, sieving and granulating; adding zinc stearate into the sieved powder, uniformly mixing, and then performing compression molding; carrying out sectional heat treatment on the pressed magnetic powder cores in a furnace, wherein the heat treatment is carried out in 3-5 stages of heating treatment; and coating the epoxy plastic powder on the surface of the magnetic powder core by adopting a paint spraying process, and heating by an oven for curing. The invention adopts three or four auxiliary materials, the process method has simple steps, the used equipment is simple, the operability is strong, and the cost is low; the obtained product has the advantages of strong magnetic core saturation resistance, low temperature coefficient and good stability.
Description
Technical Field
The invention relates to a preparation method of a carbonyl iron powder soft magnetic core for hundred MHz high frequency, belonging to the technical field of iron powder magnetic cores.
Background
The high-frequency inductor is widely applied to the fields of radio frequency communication, cable televisions, broadband transformers, high-frequency antennas and the like, and plays roles of impedance transformation, power output, network filtering and the like. The core is used as a core component of the inductor and has decisive influence on the performance of the inductor, such as the working frequency band, the Q value, the anti-interference capability, the temperature coefficient and the like. Losses of a core operating at several tens to several hundreds MHz mainly result from eddy current losses and residual losses. The carbonyl iron powder has very fine granularity and has an onion lamellar special structure, so that the vortex is very small when the carbonyl iron powder works at hundred MHz; meanwhile, since the Snoek limit of iron is GHz, the residual loss has little effect on the loss of hundred MHz.
The magnetic cores currently used at the level of hundred MHz are mainly high resistivity nickel zinc ferrite and non-magnetic ceramic materials. Among them, nickel zinc ferrite has problems of low saturation magnetic flux density, poor anti-saturation capability, poor temperature stability, etc. Particularly, when the nickel-zinc ferrite is applied to the crystal filter, the pulse current of the crystal filter can generate a strong pulse magnetic field in the packaging process, the nickel-zinc core is easily magnetized to saturation due to the strong magnetic field outside, when the external strong magnetic field is not present after packaging, the core is also in a remanence state, and the magnetic permeability of the nickel-zinc ferrite core is different from the magnetic permeability of the nickel-zinc ferrite core before packaging, so that the filter performance is deviated, and failure is possibly caused. Meanwhile, the nickel zinc ferrite has high temperature coefficient, and the magnetic permeability can generate larger fluctuation in a wide temperature working range, so that the stability of the device is affected. The non-magnetic ceramic material has no problem of nickel zinc ferrite, but has magnetic permeability of only 1, has too low magnetic permeability, and is difficult to reduce in volume under the same inductance requirement.
Disclosure of Invention
First, the technical problem to be solved
In order to solve the problems in the prior art, the invention provides a preparation method of a carbonyl iron powder soft magnetic core for hundred MHz high frequency.
(II) technical scheme
In order to achieve the above purpose, the main technical scheme adopted by the invention comprises the following steps:
a preparation method of carbonyl iron powder soft magnetic core for hundred MHz high frequency comprises the following steps:
s1, proportioning carbonyl iron powder with different granularities, and then uniformly mixing;
s2, adding phosphoric acid into a solvent to dilute the phosphoric acid into a phosphoric acid solution, pouring the phosphoric acid solution into carbonyl iron powder which is uniformly mixed, mixing and stirring the mixture until the mixture becomes dry powder, and drying the dry powder;
s3, adding the following insulating binding materials into the powder obtained in the step S2,
s4, drying, sieving and granulating;
s5, adding zinc stearate into the granulated powder sieved in the step S4, uniformly mixing, and then performing compression molding;
s6, carrying out sectional heat treatment on the pressed magnetic powder cores in a furnace, wherein the heat treatment is carried out in 3-5 stages;
and S7, coating the epoxy molding powder on the surface of the magnetic powder core by adopting a paint spraying process, and heating and curing the epoxy molding powder by using an oven.
In the above preparation method, preferably, in step S1, the carbonyl iron powder has a main component of C of 0.3 to 0.5%, an O content of 0.5 to 0.6%, and an Fe content of 97.8 to 99.2%.
In the above-described production method, preferably, in the step S1, the carbonyl iron powder is formulated such that D10.ltoreq.1.2. Mu.m, D50.ltoreq.2.0. Mu.m, and D90.ltoreq.4.5. Mu.m.
In the preparation method as described above, preferably, in step S2, the solvent is acetone, alcohol, or water, and the volume ratio of phosphoric acid to solvent is 1:200 to 300.
In the preparation method as described above, preferably, in the step S2, the phosphoric acid is used in an amount of 10% to 24% by weight of the carbonyl iron powder.
In the preparation method as described above, preferably, in step S2, the drying temperature is 80 to 120 ℃ and the drying time is 30 to 120min.
In the above preparation method, preferably, in step S3, the insulating adhesive material is one or more of epoxy resin, organic silicon resin, phenolic resin, water glass, nano silicon dioxide, kaolin, magnesium oxide, aluminum oxide or talcum powder, and the weight of the insulating adhesive material accounts for 6% -15% of the weight of the powder.
Further, the insulating adhesive material is preferably epoxy resin and acetone resin in a weight ratio of 1-3:1.
Further, the insulating bonding material is preferably water glass, organic silicon resin, kaolin and magnesium oxide according to the weight ratio of 4:4:2:1;
and dissolving water glass in water, dissolving organic silicon resin in alcohol, adding the water glass solution into the step S2 to obtain powder, adding the organic silicon resin solution, adding kaolin and magnesium oxide, and uniformly stirring.
In the above preparation method, preferably, in step S4, the sieving granulation is performed to obtain granules passing through a 40-60 mesh sieve; the drying temperature is 80-120 ℃ and the drying time is 30-60 min.
In the preparation method, preferably, in the step S5, the zinc stearate is used in an amount of 0.3-0.8% of the weight of the sieved granulated powder; the pressing pressure is 6 tons/cm 2 About 8 tons/cm 2 。
In the preparation method, in step S6, preferably, the step of heat treatment is to heat at a heating rate of 5-10 ℃/min, heat preservation is performed after heating from normal temperature to 60-80 ℃, heat preservation is performed after heating each time to 20-40 ℃, heat preservation time is 20-60 min, and heating is divided into 4-5 stages.
(III) beneficial effects
The beneficial effects of the invention are as follows:
according to the preparation method of the carbonyl iron powder soft magnetic core for hundred MHz high frequency, provided by the invention, by utilizing the characteristics of fine granularity and high activity of carbonyl iron powder, the diluted phosphoric acid solution is adopted to perform in-situ reaction on the surface of the powder, the reaction time and the uniformity of a surface insulating layer are precisely controlled by controlling the concentration of phosphoric acid and the temperature in the reaction process, and the phosphoric acid solution can ensure that each powder particle reacts, so that each particle is isolated, and the generation of eddy current loss among the particles is reduced to the greatest extent; the molding pressure is small in the pressing process, so that the possibility of insulation damage of the powder surface is avoided; the product obtained by the method has strong anti-saturation capacity, low temperature coefficient and good stability.
The preparation method of the carbonyl iron powder soft magnetic core for hundred MHz high frequency provided by the invention only adopts three or four auxiliary materials, and has the advantages of simple process steps, simple equipment, strong operability and low cost.
Detailed Description
The invention provides a preparation method of a carbonyl iron powder soft magnetic core for hundred MHz high frequency, which comprises the following steps:
s1, proportioning carbonyl iron powder with different granularities, and then uniformly mixing;
s2, adding phosphoric acid into a solvent to dilute the phosphoric acid into a phosphoric acid solution, pouring the phosphoric acid solution into carbonyl iron powder which is uniformly mixed, mixing and stirring the mixture until the mixture becomes dry powder, and drying the dry powder; wherein the weight of the phosphoric acid is 10-24% of the weight of carbonyl iron powder;
s3, adding the powder obtained in the step S2 into one or more of the following insulating binding materials such as epoxy resin, organic silicon resin, phenolic resin, water glass, nano silicon dioxide, kaolin, magnesium oxide, aluminum oxide or talcum powder, and uniformly mixing; wherein the weight of the insulating binding material accounts for 6-15% of the weight of the powder;
s4, drying, sieving and granulating;
s5, adding the lubricant into the granulated powder sieved in the step S3, uniformly mixing, and then performing compression molding;
s6, carrying out heat treatment on the pressed magnetic powder cores in a furnace, wherein the heat treatment is carried out in 3-5 stages;
and S7, coating the epoxy molding powder on the surface of the magnetic powder core by adopting a paint spraying process, and heating and curing the epoxy molding powder by using an oven.
The preparation method is preferably carried out according to the preparation method that D10 is less than or equal to 1.2 mu m, D50 is less than or equal to 2.0 mu m and D90 is less than or equal to 4.5 mu m. In the above preparation method, the carbonyl iron powder preferably contains C0.3-0.5%, O0.5-0.6% and Fe 97.8-99.2%.
The weight of phosphoric acid in the preparation method is preferably 10-24% of that of carbonyl iron powder; the weight of the insulating binding material preferably accounts for 6-15% of the weight of the powder; in the step S2, the drying temperature is preferably 80-120 ℃ and the drying time is 30-120 min. It was found that the residual acetone solution was completely volatilized at a temperature of 80-120 ℃.
In the step S4, sieving and granulating to obtain granules which are sieved by a sieve with 40-60 meshes; drying at 80-120 deg.c for 30-60 min;
preferably, the lubricant is zinc stearate, and the dosage is preferably 0.3-0.8% of the weight of the granulated powder. The heat treatment is preferably carried out by gradient heating: heating from normal temperature to 60-80 ℃, then carrying out heat preservation, wherein the heating rate is 5-10 ℃/min, and after each heating to 20-40 ℃, the heat preservation is carried out, the time of each heat preservation is 20-60 min, and the heating is divided into 4-5 stages.
The invention will be described in detail by way of specific embodiments for better explaining the invention. The raw materials used in the invention can be commercially available products.
Example 1
S1, taking carbonyl iron powder according to the granularity ratio, d10=0.9 μm, d50=1.6 μm and d90=3.7 μm, and uniformly mixing the powder with different particle diameters. Wherein the main component of the carbonyl iron powder is C0.5%, O0.6% and Fe 98.5%.
S2, mixing phosphoric acid and acetone according to the volume ratio of 1:200 to obtain an acetone phosphate solution, and taking carbonyl iron powder prepared in the step S1 according to the weight of the phosphoric acid being 14% of the weight of the carbonyl iron powder; and adding the acetone phosphate solution into carbonyl iron powder, and stirring and insulating at normal temperature until the powder is dried. And then the insulated carbonyl iron powder is put into an oven for drying, wherein the drying temperature is 80 ℃ and the drying time is 120min.
S3, mixing the epoxy resin and the phenolic resin in a weight ratio of 3:1, dissolving in an acetone solution, weighing the epoxy resin and the phenolic resin which are 12% of the carbonyl iron powder in weight, adding the mixture into the insulated carbonyl iron powder, and uniformly stirring at normal temperature.
S4, when stirring is carried out until the mixture is dried, sieving the mixture by a 60-mesh sieve for granulation, and then drying the mixture in a drying oven at 80 ℃ for 60min; after drying, the particles smaller than 400 mesh were removed by sieving.
S5, adding zinc stearate lubricant accounting for 0.5% of the weight of the powder into the granulated powder, and enabling the granules to be 6 tons/cm 2 And (5) performing lower pressing molding.
S6, performing heat treatment on the pressed magnetic powder cores in air, and adopting a step heating mode. Specifically, the temperature is raised to 80 ℃ at the normal temperature, the heating rate is 5 ℃/min, and the temperature is kept at 80 ℃ for 30min; heating to 120deg.C at 80deg.C at a heating rate of 5deg.C/min, and maintaining at 120deg.C for 60min; heating to 160deg.C at 120deg.C at 8deg.C/min, and maintaining at 160deg.C for 60min.
S7, chamfering the heat-treated magnetic powder cores, and coating paint on the surfaces and curing.
Example 2
S1, proportioning according to granularity, wherein d10=0.7 mu m, d50=1.3 mu m and d90=2.8 mu m, and mixing the powder with different particle diameters uniformly, wherein the content of C in the main component of the carbonyl iron powder is 0.3%, the content of O is 0.5% and the content of Fe is 97.8%.
S2, taking materials according to the weight of phosphoric acid which is 18% of the weight of carbonyl iron powder, diluting phosphoric acid in alcohol according to the volume ratio of phosphoric acid to alcohol of 1:300, adding phosphoric acid alcohol solution into carbonyl iron powder, heating to 70 ℃, and stirring and insulating until the powder is dried. And then the insulated carbonyl iron powder is put into an oven for drying at 110 ℃ for 60min.
S3, taking materials according to the weight ratio of epoxy resin to acetone resin of 5% of the weight of carbonyl iron powder in 1:1, dissolving the epoxy resin and the acetone resin in an acetone solution, sequentially adding the epoxy resin and the acetone resin into the insulated carbonyl iron powder after complete dissolution, and uniformly stirring at normal temperature.
S4, stirring until the mixture is dried, sieving the mixture by a 40-mesh sieve, granulating, and drying the mixture in a drying oven at 80 ℃ for 30min. The granularity ratio after drying is 5% -10% below 400 meshes, 30% -50% between-400 meshes and-200 meshes, and the balance between-200 meshes and-40 meshes.
S5, adding 0.8% zinc stearate lubricant of the powder into the granulated powder, and granulating at 8 tons/cm 2 And (5) performing lower pressing molding.
S6, performing heat treatment on the pressed magnetic powder cores in air, and adopting a step heating mode. Specifically, the temperature is raised to 60 ℃ at the normal temperature, the heating rate is 5 ℃/min, and the temperature is kept at 60 ℃ for 20min; heating to 80deg.C at 60deg.C at a rate of 5deg.C/min, and maintaining at 80deg.C for 30min; heating to 120deg.C at 80deg.C at 10deg.C/min, and maintaining at 120deg.C for 60min; heating to 120deg.C to 150deg.C at 10deg.C/min, and maintaining at 150deg.C for 60min.
S7, chamfering the heat-treated magnetic powder cores, and coating paint on the surfaces and curing.
Example 3
S1, taking carbonyl iron powder according to the granularity ratio, d10=0.5 μm, d50=1.25 μm and d90=2.63 μm, and uniformly mixing the powder with different particle diameters. Wherein the content of C in the carbonyl iron powder is 0.3%, the content of O is 0.5%, and the content of Fe is more than or equal to 98.6%.
S2, taking materials with the weight of phosphoric acid accounting for 12% of the weight of the carbonyl iron powder, mixing the phosphoric acid and deionized water according to the volume ratio of 1:250, adding the phosphoric acid aqueous solution into the carbonyl iron powder, heating to 80 ℃, and stirring and insulating until the powder is dried. And then the insulated carbonyl iron powder is put into an oven for drying at the drying temperature of 150 ℃ for 30min.
S3, dissolving water glass in water, dissolving organic silicon resin in alcohol, adding the completely dissolved water glass into the insulated carbonyl iron powder, and uniformly stirring at 80 ℃ until the mixture is dried; adding the organic silicon resin dissolved in alcohol into the powder for stirring; adding kaolin and magnesium oxide, and stirring uniformly. Wherein, the water glass, the organic silicon resin, the kaolin and the magnesia are weighed according to the weight ratio of 4:4:2:1, and the total weight of the water glass, the organic silicon resin, the kaolin and the magnesia accounts for 8.5 percent of the weight of the carbonyl iron powder.
S4, stirring until the mixture is dried, sieving the mixture by a 80-mesh sieve, granulating, and drying the mixture in a drying oven at 120 ℃ for 60min. The granularity ratio after drying is 10-20% between-400 mesh and-200 mesh, and the rest is-200 mesh to-40 mesh.
S5, adding 0.4% zinc stearate lubricant into the granulated powder, and granulating at 6.5 tons/cm 2 And (5) performing lower pressing molding.
S6, performing heat treatment on the pressed magnetic powder cores in air, and adopting a step heating mode. Specifically, the temperature is raised to 80 ℃ at the normal temperature, the heating rate is 10 ℃/min, and the temperature is kept at 80 ℃ for 60min; heating to 100deg.C at 80deg.C, heating rate of 8deg.C/min, and maintaining at 100deg.C for 60min; heating to 120deg.C at 100deg.C at 8deg.C/min, and maintaining at 120deg.C for 60min; heating to 160deg.C at 120deg.C at 10deg.C/min, and maintaining at 160deg.C for 60min.
S7, chamfering the heat-treated magnetic powder cores, and coating paint on the surfaces and curing.
The magnetic powder cores in the above examples were pressed to have dimensions of Φ3.18mm×Φ1.7mm×1.27mm, and 9 turns of enameled wire of Φ0.27mm was wound on the magnetic ring. Measuring inductance value and Q value by adopting an Agilent E4991A table, and calculating magnetic permeability through the inductance value; measuring the direct current superposition characteristics of the magnetic core by adopting an Agilent E4980A LCR table and an Agilent 42841A bias current source; the core power consumption was measured using a SY-8232B-H analyzer. A magnet ring with the size of phi 26.9mm multiplied by phi 14.5mm multiplied by 11.1mm is prepared, 100 turns of enameled wire with the size of phi 0.51mm are wound on the magnet ring, the temperature coefficient of magnetic permeability between minus 60 ℃ and 150 ℃ is measured by using an Agilent E4991A meter and a high and low temperature test box, and meanwhile, similar products purchased from Micrometals company in the United states are detected in different batches, and the results are shown in the following table 1.
TABLE 1 detection results
The result shows that the material prepared by the embodiment of the invention can be used in a circuit with the frequency of tens of MHz to hundreds of MHz, and has the functions of filtering, resonance and the like in the circuit. High Q value, high DC superposition characteristic and low magnetic permeability temperature coefficient, so that the magnetic resonance frequency is high in wide temperature range the magnetic material has strong stability under complex electromagnetic environment.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any person skilled in the art may make modifications or alterations to the above disclosed technical content to equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the carbonyl iron powder soft magnetic core for hundred MHz high frequency is characterized by comprising the following steps:
s1, proportioning carbonyl iron powder with different granularities, and then uniformly mixing;
s2, adding phosphoric acid into a solvent to dilute the phosphoric acid into a phosphoric acid solution, pouring the phosphoric acid solution into carbonyl iron powder which is uniformly mixed, mixing and stirring the mixture until the mixture becomes dry powder, and drying the dry powder;
s3, adding the following insulating binding materials into the powder obtained in the step S2,
s4, drying, sieving and granulating;
s5, adding zinc stearate into the granulated powder sieved in the step S4, uniformly mixing, and then performing compression molding;
s6, carrying out sectional heat treatment on the pressed magnetic powder cores in a furnace, wherein the heat treatment is carried out in 3-5 stages;
and S7, coating the epoxy molding powder on the surface of the magnetic powder core by adopting a paint spraying process, and heating and curing the epoxy molding powder by using an oven.
2. The method according to claim 1, wherein in the step S1, the carbonyl iron powder has a C content of 0.3 to 0.5%, an O content of 0.5 to 0.6%, and an Fe content of 97.8 to 99.2%.
3. The method according to claim 1, wherein in step S1, the carbonyl iron powder is formulated with D10.ltoreq.1.2. Mu.m, D50.ltoreq.2.0. Mu.m, D90.ltoreq.4.5. Mu.m.
4. The method according to claim 1, wherein in step S2, the solvent is acetone, alcohol, or water, and the volume ratio of phosphoric acid to solvent is 1:200 to 300.
5. The method of claim 1, wherein the phosphoric acid is used in an amount of 10% to 24% by weight of the carbonyl iron powder in step S2.
6. The method according to claim 1, wherein in step S2, the drying is performed at 80 to 120 ℃ for 30 to 120 minutes.
7. The preparation method of claim 1, wherein in the step S3, the insulating adhesive material is one or more of epoxy resin, organic silicon resin, phenolic resin, water glass, nano silicon dioxide, kaolin, magnesia, alumina or talcum powder, and the weight of the insulating adhesive material accounts for 6% -15% of the weight of the powder.
8. The preparation method according to claim 1, wherein in step S4, sieving and granulating are performed by sieving and granulating through a 40-60 mesh sieve; the drying temperature is 80-120 ℃ and the drying time is 30-60 min.
9. The preparation method according to claim 1, wherein in the step S5, the zinc stearate is used in an amount of 0.3 to 0.8% by weight of the sieved granulated powder; the pressing pressure is 6 tons/cm 2 About 8 tons/cm 2 。
10. The method according to claim 1, wherein in step S6, the step of heat treatment is to heat at a heating rate of 5 to 10 ℃/min, heat is preserved after heating from room temperature to 60 to 80 ℃, heat is preserved after heating each time to 20 to 40 ℃, heat is preserved for 20 to 60min, and the heating is divided into 4 to 5 stages.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU765891A1 (en) * | 1978-07-07 | 1980-09-23 | Предприятие П/Я А-1216 | Method of manufacturing magneto-dielectric cores on the base of carbonyl iron |
| CN109545537A (en) * | 2018-12-28 | 2019-03-29 | 东莞铭普光磁股份有限公司 | A kind of powder core and preparation method thereof |
| CN111063501A (en) * | 2019-12-26 | 2020-04-24 | 深圳市艺感科技有限公司 | Preparation method of low-loss powder for producing integrally-formed inductor |
| CN115083758A (en) * | 2021-12-22 | 2022-09-20 | 华萃微感电子(江苏)有限公司 | Organic resin coating preparation method of nano iron-based inductance soft magnetic material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU765891A1 (en) * | 1978-07-07 | 1980-09-23 | Предприятие П/Я А-1216 | Method of manufacturing magneto-dielectric cores on the base of carbonyl iron |
| CN109545537A (en) * | 2018-12-28 | 2019-03-29 | 东莞铭普光磁股份有限公司 | A kind of powder core and preparation method thereof |
| CN111063501A (en) * | 2019-12-26 | 2020-04-24 | 深圳市艺感科技有限公司 | Preparation method of low-loss powder for producing integrally-formed inductor |
| CN115083758A (en) * | 2021-12-22 | 2022-09-20 | 华萃微感电子(江苏)有限公司 | Organic resin coating preparation method of nano iron-based inductance soft magnetic material |
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