CN111590065B - Soft magnetic metal powder with negative thermal expansion coefficient and high insulation property and preparation method thereof - Google Patents
Soft magnetic metal powder with negative thermal expansion coefficient and high insulation property and preparation method thereof Download PDFInfo
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- 229910052743 krypton Inorganic materials 0.000 claims description 3
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
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- ZPLUZNXSYCCJOE-UHFFFAOYSA-N phosphoric acid;propan-2-one Chemical compound CC(C)=O.OP(O)(O)=O ZPLUZNXSYCCJOE-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 1
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- KJAZZOWIUGBRCT-UHFFFAOYSA-K aluminum;iron(2+);phosphate Chemical compound [Al+3].[Fe+2].[O-]P([O-])([O-])=O KJAZZOWIUGBRCT-UHFFFAOYSA-K 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- 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
- B22F1/16—Metallic particles coated with a non-metal
-
- 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
- H01F1/01—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
- H01F1/20—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 in the form of particles, e.g. powder
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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
- H01F41/0253—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 for manufacturing permanent magnets
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- Soft Magnetic Materials (AREA)
Abstract
The invention provides soft magnetic metal powder with negative thermal expansion coefficient and high insulation property and a preparation method thereof. The preparation method comprises the following steps: carrying out vacuum heat treatment on the soft magnetic metal powder; preparing a nano zirconium hydroxide solution, a nano aluminum tungstate solution and an aluminum dihydrogen phosphate solution, uniformly mixing, adding phosphoric acid for titration, and adjusting the pH value of the solution to 3-4 to obtain a mixed solution; adding the soft magnetic metal powder subjected to vacuum heat treatment into the mixed solution, carrying out ultrasonic treatment for 45-90 minutes, heating to 110 ℃, and stirring to obtain a preformed product; and (3) carrying out atmosphere protection heat treatment on the preformed product at the temperature of 500-650 ℃ for 3-6 hours, and cooling to room temperature to obtain the soft magnetic metal powder with the negative thermal expansion coefficient and the high insulation property. According to the invention, the soft magnetic metal powder with the negative thermal expansion coefficient is prepared through a composite reaction, so that the problem of thermal expansion of the powder and a product can be reduced, and meanwhile, a coating insulating layer is better formed on the surface of the powder, so that the insulating property of the powder is greatly improved.
Description
Technical Field
The invention belongs to the field of magnetic functional materials, and particularly relates to soft magnetic metal powder with negative thermal expansion coefficient and high insulation property and a preparation method thereof.
Background
The magnetic material is widely applied to electronic and electric products and is one of basic materials in the material industry. It has special functions of energy conversion, storage and the like. Compared with the traditional laminated rigid magnetic core, the soft magnetic composite material obtained by coating the insulating film on the surface of the ferromagnetic particles has a series of unique properties, such as three-dimensional isotropic magnetic property, extremely low eddy current loss, flexible magnetic core structure design and the like, and the soft magnetic composite material has wide application prospect due to the characteristics. However, electronic products made of soft magnetic materials are subjected to high temperature impact of 250 + -5 ℃ during the process of being soldered on the PCB, in the process of rapidly increasing the temperature, the danger of cracking of the product is caused due to the thermal expansion characteristics of the powder and the coating film, and a great deal of research is carried out at home and abroad to solve the problem, for example, the epoxy adhesive for the integrated molding technology of electronic components and the preparation method thereof with the publication number of CN103555246A invents an adhesive formula with higher body strength, high modulus, high Tg and high bonding strength than the traditional adhesive, the adhesive for the integrated molding of electronic components and the preparation method thereof with the publication number of CN107674625A also develops a new adhesive formula with high strength, however, these methods only place the center of gravity to improve the strength of the adhesive, and do not consider the essential problem of thermal expansion of the material.
Disclosure of Invention
Aiming at the problems, the invention provides soft magnetic metal powder with negative thermal expansion coefficient and high insulation property and a preparation method thereof, and aims to solve the problems that the soft magnetic metal powder prepared by the existing soft magnetic metal powder preparation method is easy to expand when heated, is easy to cause product cracking, and is poor in powder coating effect and insulation property.
A preparation method of soft magnetic metal powder with negative thermal expansion coefficient and high insulation property comprises the following steps:
carrying out vacuum heat treatment on the soft magnetic metal powder;
preparing 0.5-1% by mass of nano zirconium hydroxide solution, 0.5-1% by mass of nano aluminum tungstate solution, 0.5-2% by mass of aluminum dihydrogen phosphate solution and analytically pure phosphoric acid liquid;
uniformly mixing three solutions of nano zirconium hydroxide, nano aluminum tungstate and aluminum dihydrogen phosphate, adding phosphoric acid for titration, and adjusting the pH value of the solution to 3-4 to obtain a mixed solution;
adding the soft magnetic metal powder subjected to vacuum heat treatment into the mixed solution, carrying out ultrasonic treatment for 45-90 minutes, heating to 110 ℃, carrying out mechanical stirring while heating, and stopping heating and stirring until the reactants are completely dried to obtain a soft magnetic metal powder preform with negative thermal expansion coefficient and high insulation property;
and carrying out atmosphere protection heat treatment on the soft magnetic metal powder preform with the negative thermal expansion coefficient and the high insulation characteristic at the temperature of 500-650 ℃ for 3-6 hours, and cooling to room temperature to obtain the soft magnetic metal powder with the negative thermal expansion coefficient and the high insulation characteristic.
The product of the mixture and reaction of several materials such as nano zirconium hydroxide, nano aluminum tungstate, aluminum dihydrogen phosphate and the like has a negative thermal expansion coefficient, and the mass fraction of each material is controlled to be 0.5-2.0% because the coating effect is not ideal due to too little addition, and the magnetic permeability of the powder is reduced due to too much addition, so that the requirement of magnetic properties cannot be met.
Furthermore, the heat treatment conditions are 800-1000 ℃, the vacuum degree is 4 multiplied by 10 < -3 > Pa, and the temperature control precision is +/-0.1 ℃.
Furthermore, a magnetic field is added while the soft magnetic metal powder is subjected to heat treatment, and the magnetic field intensity is 0-4 kA/m.
Furthermore, the mass ratio of the nano zirconium hydroxide, the nano aluminum tungstate and the aluminum dihydrogen phosphate is (3-5): (2-8): (1-5).
Controlling the mass ratio of the nano zirconium hydroxide, the nano aluminum tungstate and the aluminum dihydrogen phosphate to be (3-5): (2-8): (1-5), the effect of the whole reaction system can be optimal, the reaction is more complete, and the reaction residual materials are less, so that the aims of saving the cost and efficiently producing are fulfilled.
Further, the soft magnetic metal powder has a mass 3 to 5 times that of the mixed solution.
In actual operation, if the amount of the mixed solution is too much, the waste of liquid and the difficulty of subsequent drying can be caused; if the amount of the mixed solution is too small, it may be difficult to sufficiently contact the powder with the solution, and uniform coating may not be achieved. The quality of the soft magnetic metal powder is controlled to be 3-5 times of the quality of the mixed solution, and meanwhile, the soft magnetic metal powder can be in more uniform contact with the substances in the mixed solution by matching with the ultrasonic treatment mode in the invention, so that the optimal coating effect is achieved.
Furthermore, the nano zirconium hydroxide solution is a nano zirconium hydroxide ethanol solution, the nano aluminum tungstate solution is a nano aluminum tungstate ethanol solution, and the aluminum dihydrogen phosphate solution is a distilled aluminum dihydrogen phosphate aqueous solution.
Further, the atmosphere is any one of helium, neon, argon, krypton, xenon, or nitrogen.
Furthermore, the soft magnetic metal powder is one or more of carbonyl iron powder, ferrosilicon-chromium alloy powder and ferrosilicon-aluminum alloy powder.
Further, the stirring speed during the mechanical stirring while heating is 30 to 50 rad/s.
The invention also provides soft magnetic metal powder with negative thermal expansion coefficient and high insulation property, which is prepared by the preparation method.
According to the soft magnetic metal powder with the negative thermal expansion coefficient and the high insulation characteristic and the preparation method thereof, disclosed by the invention, the soft magnetic metal powder with the negative thermal expansion coefficient is prepared through a composite reaction, so that the problem of thermal expansion of the powder and a product can be successfully reduced, meanwhile, an insulating layer is better coated on the surface of the powder, the insulation characteristic of the powder is greatly improved, and the preparation method is simple to operate and is suitable for industrial production. Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 is a schematic view showing a process for preparing a soft magnetic metal powder having a negative thermal expansion coefficient and high insulation property according to the present invention.
Detailed Description
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 some, but not all, embodiments of the present invention. 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.
Referring to fig. 1, fig. 1 is a schematic view showing a process for preparing a soft magnetic metal powder having a negative thermal expansion coefficient and high insulation property according to the present invention. As shown in fig. 1, the method for preparing the soft magnetic metal powder having the negative thermal expansion coefficient and the high insulation property includes the steps of:
carrying out vacuum heat treatment on the soft magnetic metal powder, wherein the heat treatment condition is 800-1000 ℃, and the vacuum degree is 4 multiplied by 10 -3 Pa, the temperature control precision is +/-0.1 ℃; adding a magnetic field while carrying out heat treatment on the soft magnetic metal powder, wherein the magnetic field intensity is 0-4 kA/m.
Preparing 0.5-1% by mass of nano zirconium hydroxide solution, 0.5-1% by mass of nano aluminum tungstate solution, 0.5-2% by mass of aluminum dihydrogen phosphate solution and analytically pure phosphoric acid liquid;
wherein the nano zirconium hydroxide solution is a nano zirconium hydroxide ethanol solution, the nano aluminum tungstate solution is a nano aluminum tungstate solution ethanol solution, and the aluminum dihydrogen phosphate solution is a distilled aluminum dihydrogen phosphate aqueous solution;
uniformly mixing three solutions of nano zirconium hydroxide, nano aluminum tungstate and aluminum dihydrogen phosphate, adding phosphoric acid for titration, and adjusting the pH value of the solution to 3-4 to obtain a mixed solution, wherein the mass ratio of the nano zirconium hydroxide to the nano aluminum tungstate to the aluminum dihydrogen phosphate is (3-5): (2-8): (1-5);
adding the heat-treated soft magnetic metal powder into the mixed solution, wherein the mass of the soft magnetic metal powder is 3-5 times of that of the mixed solution, performing ultrasonic treatment for 45-90 minutes, heating to 110 ℃, heating while performing mechanical stirring at a stirring speed of 30-50rad/s, and stopping heating and stirring until reactants are completely dried to obtain a soft magnetic metal powder preform with a negative thermal expansion coefficient and high insulation property;
and carrying out atmosphere protection heat treatment on the soft magnetic metal powder preform with the negative thermal expansion coefficient and the high insulation characteristic at the temperature of 500-650 ℃ for 3-6 hours, and cooling to room temperature to obtain the soft magnetic metal powder with the negative thermal expansion coefficient and the high insulation characteristic.
Wherein the atmosphere includes, but is not limited to, helium, neon, argon, krypton, xenon, or nitrogen.
The soft magnetic metal powder with negative thermal expansion coefficient and high insulation property is prepared by the preparation method, and the performance of the soft magnetic metal powder is detected.
Example one
2500g of carbonyl iron powder was subjected to a vacuum heat treatment at 800 ℃ under a vacuum of 4X 10 - 3 Pa, controlling the temperature precision to +/-0.1 ℃, and adding a magnetic field while carrying out heat treatment on the soft magnetic metal powder, wherein the magnetic field intensity is 3 kA/m;
500g of nano zirconium hydroxide ethanol solution with the mass fraction of 0.5%, 500g of nano aluminum tungstate ethanol solution with the mass fraction of 0.6%, 500g of distilled aluminum dihydrogen phosphate aqueous solution with the mass fraction of 0.5% and 100g of analytically pure phosphoric acid liquid are prepared;
uniformly mixing three solutions, namely 400g of nano zirconium hydroxide, 200g of nano aluminum tungstate and 100g of aluminum dihydrogen phosphate, adding phosphoric acid for titration, and adjusting the pH value of the solution to 3 to obtain a mixed solution;
adding the carbonyl iron powder after heat treatment into the mixed solution, performing ultrasonic treatment for 90 minutes, heating to 110 ℃, mechanically stirring at a stirring speed of 30-50rad/s while heating, stopping heating and stirring until reactants are completely dried, and obtaining a soft magnetic metal powder preform with a negative thermal expansion coefficient and high insulation property;
and (3) carrying out atmosphere protection heat treatment on the soft magnetic metal powder preform with the negative thermal expansion coefficient and high insulation property at 550 ℃ for 4 hours, and cooling to room temperature to obtain the soft magnetic metal powder with the negative thermal expansion coefficient and high insulation property.
In this embodiment, the nano zirconium hydroxide, the nano aluminum tungstate, and the aluminum dihydrogen phosphate react with the carbonyl iron powder to form a composite reaction film of aluminum iron phosphate and zirconium phosphotungstate under the phosphoric acid solution condition, and the film is a negative thermal expansion material and an insulating material with good performance, has good chemical and thermal stability, high-temperature mechanical stability and insulating property, has an obvious negative thermal expansion property in a large temperature range, and has no phase change and no water absorption in a negative thermal expansion temperature range. Therefore, the powder can be well insulated and coated, and the composite material has the characteristic of negative thermal expansion coefficient.
Meanwhile, the magnetic conductivity of the metal powder is increased, and the coercive force is reduced, so that the comprehensive magnetic performance of the soft magnetic metal powder is improved.
Comparative example 1
And passivating and insulating carbonyl iron powder by using a phosphoric acid acetone solution, performing heat treatment at 550 ℃ after insulating coating, and then cooling to room temperature along with a furnace.
Performance detection
The soft magnetic metal powder prepared in the first embodiment and the first comparative embodiment is respectively pressed into magnetic rings, the specifications of the magnetic rings are 8mm in inner diameter and 14mm in outer diameter, the mass of the powder is 2g, the pressing pressure is 3t, and then the magnetic rings are heated to 200 ℃, kept warm for 3h and cooled to room temperature. And respectively testing the heights of the magnetic ring before and after baking, observing the appearance and testing the insulation characteristic of the baked magnetic ring. The test results are shown in Table 1.
TABLE 1 comparison of carbonyl iron coated powders obtained in example one and comparative example one
| Test items | Insulation resistance | Thickness difference before and after baking | Appearance after baking |
| Example one | 8.2MΩ | 0 | Without cracks |
| Comparative example 1 | 3.6MΩ | 0.03mm | Individual very fine cracks |
From the results of the performance test, it can be seen that the soft magnetic metal powder obtained in example one is superior to that of comparative example one in both thermal stability and insulation.
Example two
8000g of iron-silicon-chromium alloy powder is subjected to vacuum heat treatment, and the heat treatment condition is 1000 ℃, and the vacuum degree is 4 multiplied by 10 -3 Pa, controlling the temperature precision to be +/-0.1 ℃, adding a magnetic field while carrying out heat treatment on the soft magnetic metal powder, wherein the magnetic field intensity is 4 kA/m;
preparing 1000g of nano zirconium hydroxide ethanol solution with the mass fraction of 0.8%, 1000g of nano aluminum tungstate ethanol solution with the mass fraction of 1%, 500g of distilled water solution of aluminum dihydrogen phosphate with the mass fraction of 2% and 100g of analytically pure phosphoric acid liquid;
uniformly mixing three solutions of 500g of nano zirconium hydroxide, 800g of nano aluminum tungstate and 500g of aluminum dihydrogen phosphate, adding phosphoric acid for titration, and adjusting the pH value of the solution to 3 to obtain a mixed solution;
adding the heat-treated iron-silicon-chromium alloy powder into the mixed solution, performing ultrasonic treatment for 90 minutes, heating to 110 ℃, mechanically stirring at a stirring speed of 30-50rad/s while heating, and stopping heating and stirring until reactants are completely dried to obtain a soft magnetic metal powder preform with a negative thermal expansion coefficient and high insulation property;
and (3) carrying out atmosphere protection heat treatment on the soft magnetic metal powder preform with the negative thermal expansion coefficient and high insulation property at 650 ℃ for 5.5 hours, and cooling to room temperature to obtain the soft magnetic metal powder with the negative thermal expansion coefficient and high insulation property.
Comparative example No. two
Passivating and insulating the iron-silicon-chromium alloy powder by using an acetone phosphate solution, performing heat treatment at 650 ℃ after insulating and coating, and then cooling to room temperature along with a furnace.
Performance detection
And (3) respectively pressing the soft magnetic metal powder prepared in the second embodiment and the second embodiment into magnetic rings, wherein the specifications of the magnetic rings are 8mm in inner diameter and 14mm in outer diameter, the mass of the powder is 2g, the pressing pressure is 3t, and then heating to 200 ℃, keeping the temperature for 3h, and cooling to room temperature. And respectively testing the heights of the magnetic ring before and after baking, observing the appearance and testing the insulation characteristic of the baked magnetic ring. The test results are shown in Table 2.
Table 2, comparison of the properties of the alloy powders obtained in example two and comparative example two
| Test item | Insulation resistance | Thickness difference before and after baking | Appearance after baking |
| Example two | 7.7MΩ | 0 | Without cracks |
| Comparative example No. two | 3.1MΩ | 0.02mm | Individual very fine cracks |
The results of the performance tests show that the alloy powder obtained in example two has better thermal stability and insulation than those of comparative example two.
The above first embodiment and the second embodiment are only two preferred embodiments for exemplary illustration, and actually, in the implementation process of the present invention, each parameter can be adjusted within a reasonable range according to actual needs, as long as the purpose of the present invention can be achieved.
In addition, various raw materials used in the above examples of the present invention are as follows: z104424 nm zirconium hydroxide (Shanghai Alatin Biotechnology Co., Ltd.), 15123-82-7 nm aluminum tungstate (Shandong West Asia chemical industry Co., Ltd.), A165289 aluminum dihydrogen phosphate (Shanghai Alatin Biotechnology Co., Ltd.), ZB0005 distilled water (Shanghai Huancao environmental protection technology Co., Ltd.), E298791 ethanol (Shanghai Alatin Biotechnology Co., Ltd.), P120547 phosphoric acid (Shanghai Huancao environmental protection technology Co., Ltd.), FeSiCr-A iron-silicon-chromium alloy powder (Antai technology Co., Ltd.), RTE carbonyl iron powder (Jiangsu Tian-ultra-fine metal powder Co., Ltd.). Other commercially available products having the same performance parameters can also be used for the above-mentioned raw materials.
Although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A method for preparing soft magnetic metal powder with negative thermal expansion coefficient and high insulation property is characterized by comprising the following steps:
carrying out vacuum heat treatment on the soft magnetic metal powder;
preparing 0.5-1% by mass of nano zirconium hydroxide solution, 0.5-1% by mass of nano aluminum tungstate solution, 0.5-2% by mass of aluminum dihydrogen phosphate solution and analytically pure phosphoric acid solution, wherein the mass ratio of the nano zirconium hydroxide to the nano aluminum tungstate to the nano aluminum dihydrogen phosphate is (3-5): (2-8): (1-5);
uniformly mixing three solutions of nano zirconium hydroxide, nano aluminum tungstate and aluminum dihydrogen phosphate, adding phosphoric acid for titration, and adjusting the pH value of the solution to 3-4 to obtain a mixed solution;
adding the soft magnetic metal powder subjected to vacuum heat treatment into the mixed solution, performing ultrasonic treatment for 45-90 minutes, heating to 110 ℃, and mechanically stirring while heating until reactants are completely dried, and stopping heating and stirring to obtain a soft magnetic metal powder preform with a negative thermal expansion coefficient and high insulation property;
and carrying out atmosphere protection heat treatment on the soft magnetic metal powder preform with the negative thermal expansion coefficient and the high insulation characteristic at the temperature of 500-650 ℃ for 3-6 hours, and cooling to room temperature to obtain the soft magnetic metal powder with the negative thermal expansion coefficient and the high insulation characteristic.
2. The method for producing a soft magnetic metal powder having a negative thermal expansion coefficient and high insulating properties as claimed in claim 1, wherein the vacuum heat treatment is carried out under conditions of 800 to 1000 ℃ and a degree of vacuum of 4X 10 -3 Pa, temperature control precision +/-0.1 ℃.
3. A method of manufacturing soft magnetic metal powder with negative thermal expansion coefficient and high insulation property according to claim 1 or 2, characterized in that a magnetic field is added while heat treating the soft magnetic metal powder, and the magnetic field strength of the magnetic field is 0 to 4 kA/m.
4. A method for producing a soft magnetic metal powder with a negative thermal expansion coefficient and high insulation property as claimed in claim 1, wherein the mass of the soft magnetic metal powder is 3 to 5 times the mass of the mixed solution.
5. The method for preparing a soft magnetic metal powder with negative thermal expansion coefficient and high insulation property according to claim 4, wherein the nano zirconium hydroxide solution is a nano zirconium hydroxide ethanol solution, the nano aluminum tungstate solution is a nano aluminum tungstate ethanol solution, and the aluminum dihydrogen phosphate solution is a distilled aluminum dihydrogen phosphate solution.
6. A method of manufacturing a soft magnetic metal powder with negative thermal expansion coefficient and high insulation characteristics as claimed in claim 1, wherein the atmosphere is any one of helium, neon, argon, krypton, xenon or nitrogen.
7. A method for preparing soft magnetic metal powder with negative thermal expansion coefficient and high insulation property as claimed in claim 1, wherein the soft magnetic metal powder is one or more of carbonyl iron powder, ferrosilicon alloy powder, ferrosilicon chromium alloy powder and ferrosilicon aluminum alloy powder.
8. A method for preparing a soft magnetic metal powder with negative thermal expansion coefficient and high insulating property as claimed in claim 1, wherein the stirring speed during the mechanical stirring while heating is 30 to 50 rad/s.
9. A soft magnetic metal powder having a negative thermal expansion coefficient and high insulation characteristics, which is obtained by the production method according to any one of claims 1 to 8.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5919720A (en) * | 1997-04-15 | 1999-07-06 | State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Oregon State University | Materials with low or negative thermal expansion |
| CN1518011A (en) * | 2002-12-26 | 2004-08-04 | ������������ʽ���� | Metal powder and powder magnetic core using same |
| CN103065786A (en) * | 2011-10-22 | 2013-04-24 | 湖南康力新材料科技有限责任公司 | Manufacturing method of high permeability low power consumption Fe-Si-AI magnetic powder cores |
| JP2014122406A (en) * | 2012-12-21 | 2014-07-03 | Nihon Ceratec Co Ltd | Metal-ceramic composite material, and method for manufacturing the same |
| KR20140137175A (en) * | 2013-05-22 | 2014-12-02 | 목포대학교산학협력단 | Method for synthesis of Zr2WP2O12 ceramics |
| CN104974523A (en) * | 2015-05-21 | 2015-10-14 | 郑州大学 | A low thermal expansion coefficient Zr2WP2O12/polyimide composite material and its preparation method |
| CN108074878A (en) * | 2016-11-16 | 2018-05-25 | Tdk株式会社 | Composite magnetic sealing material and use its electronic circuit package body |
| CN108145151A (en) * | 2017-11-28 | 2018-06-12 | 合肥博微田村电气有限公司 | A kind of in-situ reaction preparation method of corrosion resistance high magnetic permeability insulated metal powder |
| CN108461247A (en) * | 2018-04-27 | 2018-08-28 | 合肥博微田村电气有限公司 | A kind of method that inorganic insulation cladding prepares soft magnetic metal powder |
| CN109326405A (en) * | 2018-09-26 | 2019-02-12 | 合肥博微田村电气有限公司 | A kind of preparation method and soft magnetic metal powder of high heat conductive insulating soft magnetic metal powder |
| CN109411175A (en) * | 2018-12-19 | 2019-03-01 | 合肥博微田村电气有限公司 | A kind of inductance of high magnetic permeability soft magnetic powder production method and soft magnetic powder |
-
2020
- 2020-04-14 CN CN202010290472.0A patent/CN111590065B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5919720A (en) * | 1997-04-15 | 1999-07-06 | State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Oregon State University | Materials with low or negative thermal expansion |
| CN1518011A (en) * | 2002-12-26 | 2004-08-04 | ������������ʽ���� | Metal powder and powder magnetic core using same |
| CN103065786A (en) * | 2011-10-22 | 2013-04-24 | 湖南康力新材料科技有限责任公司 | Manufacturing method of high permeability low power consumption Fe-Si-AI magnetic powder cores |
| JP2014122406A (en) * | 2012-12-21 | 2014-07-03 | Nihon Ceratec Co Ltd | Metal-ceramic composite material, and method for manufacturing the same |
| KR20140137175A (en) * | 2013-05-22 | 2014-12-02 | 목포대학교산학협력단 | Method for synthesis of Zr2WP2O12 ceramics |
| CN104974523A (en) * | 2015-05-21 | 2015-10-14 | 郑州大学 | A low thermal expansion coefficient Zr2WP2O12/polyimide composite material and its preparation method |
| CN108074878A (en) * | 2016-11-16 | 2018-05-25 | Tdk株式会社 | Composite magnetic sealing material and use its electronic circuit package body |
| CN108145151A (en) * | 2017-11-28 | 2018-06-12 | 合肥博微田村电气有限公司 | A kind of in-situ reaction preparation method of corrosion resistance high magnetic permeability insulated metal powder |
| CN108461247A (en) * | 2018-04-27 | 2018-08-28 | 合肥博微田村电气有限公司 | A kind of method that inorganic insulation cladding prepares soft magnetic metal powder |
| CN109326405A (en) * | 2018-09-26 | 2019-02-12 | 合肥博微田村电气有限公司 | A kind of preparation method and soft magnetic metal powder of high heat conductive insulating soft magnetic metal powder |
| CN109411175A (en) * | 2018-12-19 | 2019-03-01 | 合肥博微田村电气有限公司 | A kind of inductance of high magnetic permeability soft magnetic powder production method and soft magnetic powder |
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