CN110718347B - Preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder - Google Patents
Preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder Download PDFInfo
- Publication number
- CN110718347B CN110718347B CN201911029890.8A CN201911029890A CN110718347B CN 110718347 B CN110718347 B CN 110718347B CN 201911029890 A CN201911029890 A CN 201911029890A CN 110718347 B CN110718347 B CN 110718347B
- Authority
- CN
- China
- Prior art keywords
- magnetic powder
- magnetic
- solvent
- ball milling
- scaly
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
-
- 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
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention belongs to the field of wave-absorbing materials, and discloses a preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder. The preparation method of the scaly iron-silicon-aluminum magnetic powder with high magnetic conductivity comprises the following steps: selecting Fe-Si-Al magnetic powder with the granularity of 80-180 mu m as raw material powder, and adding grinding balls, a solvent and the magnetic powder into a stirring ball mill, wherein the solvent is one of or a mixed solvent of dimethylformamide and dimethyl sulfoxide; heating the solvent and the magnetic powder to 80 ℃ by using a heating device of a ball mill, carrying out ball milling, keeping the temperature at 80-130 ℃ in the ball milling process, drying the magnetic powder after ball milling, carrying out particle size grading, and annealing treatment. The method optimizes the traditional ball milling process, improves the diameter-thickness ratio and the magnetic conductivity of the high diameter-thickness ratio flaky magnetic powder, and greatly improves the yield of the flaky magnetic powder.
Description
Technical Field
The invention relates to the field of wave-absorbing materials, in particular to a preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder.
Background
With the rapid development of electronic information technology, the problems of electromagnetic compatibility and electromagnetic interference are increasingly prominent. There are many ways to solve the problem of electromagnetic compatibility of electronic products, such as reasonable wiring, filtering, shielding, etc. The wave-absorbing magnetic sheet material is a flexible sheet material mainly compounded by scaly soft magnetic alloy magnetic powder and a high-molecular binder, and is also called a noise suppression sheet. In recent years, the wave-absorbing magnetic sheet has higher magnetic conductivity and convenient use, and is more and more favored by electronic engineers, and the wave-absorbing magnetic sheet material is more and more used in electronic products to solve the problem of electromagnetic interference.
The electromagnetic property of the scaly soft magnetic alloy powder in the wave-absorbing magnetic sheet material is the most critical factor influencing the performance of the noise suppression sheet, and the scaly soft magnetic alloy mainly uses an iron-silicon-aluminum alloy system at present. A large number of researches show that in order to ensure that the wave-absorbing magnetic sheet has high magnetic conductivity and loss characteristics, the thickness of the scaly magnetic powder is smaller than the skin depth of the material and is generally smaller than 1 mu m, and the magnetic conductivity of the magnetic sheet is higher when the radius-thickness ratio is larger. At present, the scaly iron-silicon-aluminum magnetic powder is mainly prepared by ball milling and heat treatment. Firstly, selecting proper raw material powder, then placing the raw material powder, grinding balls, a ball-milling medium (solvent, grinding aid and the like) and the like into a ball mill according to a certain proportion for ball milling, gradually changing isotropic magnetic powder into a sheet shape under the high-speed impact and rolling of the grinding balls, then screening the flaky ferrosilicon aluminum powder, and finally placing the flaky ferrosilicon aluminum powder into an annealing furnace with gas protection for heat treatment.
The sendust powder has high hardness, is brittle, and has poor plastic deformation capability. Under the action of repeated squeezing and impacting of the grinding balls, the magnetic powder is converted into a sheet shape on one hand, and is crushed into fine powder on the other hand. Therefore, the scale-like sendust magnetic powder after ball milling is very uneven, the magnetic powder with high aspect ratio (ratio of the diameter dimension to the thickness dimension of the scale-like magnetic powder) is less, and the yield is low. Meanwhile, the edges of the magnetic powder are not smooth enough and have burrs, so that the magnetic conductivity of the magnetic powder is greatly influenced. In addition, in order to improve the ball milling efficiency and promote the deformation of the sendust magnetic powder, auxiliary materials such as a dispersing agent or a grinding aid are generally required to be added in the ball milling process, and the materials are not easy to be completely removed in the subsequent treatment process and have adverse effects on the magnetic powder magnetic permeability.
Chinese patent CN103350225A discloses a method for multi-stage rod milling to flatten soft magnetic alloy magnetic powder, which can improve the diameter-thickness ratio of magnetic powder and increase the yield, but the production process is complex, requires multi-stage ball milling, and requires long-time ball milling, and the production efficiency is low. CN104249155A discloses a multistage ball milling method, which significantly improves the flattening rate of magnetic powder compared with the conventional process, however, the process also requires multistage ball milling, the ball milling time is long, the production efficiency is low, and the process parameters need to be accurately controlled, otherwise the flattening rate of magnetic powder is seriously affected. In conclusion, the traditional preparation process of the scaly iron-silicon-aluminum magnetic powder has the problems of low yield, shape defects and the like, and an efficient preparation method of the scaly iron-silicon-aluminum magnetic powder is urgently needed.
Disclosure of Invention
The invention aims to overcome the defects of the background technology and provides a preparation method of the scaly sendust magnetic powder with high magnetic conductivity.
In order to achieve the aim of the invention, the preparation method of the scaly iron-silicon-aluminum magnetic powder with high magnetic conductivity comprises the following steps:
(1) selecting Fe-Si-Al magnetic powder with the granularity of 80-180 mu m as raw material powder;
(2) adding grinding balls, a solvent and the magnetic powder in the step (1) into a stirring ball mill, wherein the solvent is one or a mixed solvent of dimethyl formamide and dimethyl sulfoxide;
(3) heating the solvent and the magnetic powder to 80 ℃ by using a heating device of a ball mill, and then carrying out ball milling, wherein the temperature of a mixed solution of the solvent and the magnetic powder is kept between 80 ℃ and 130 ℃ in the whole ball milling process, and drying the magnetic powder after ball milling;
(4) grading the magnetic powder in the step (3) in a particle size manner;
(5) and (4) annealing the magnetic powder graded in the step (4).
Further, the magnetic powder in the step (1) is spherical, blocky or irregular.
Preferably, the magnetic powder particle size in the step (1) is 100-150 μm.
Further, in the step (1), the sendust magnetic powder comprises the following alloy components in percentage by weight: 9% -10%, Al: 5 to 6 percent of Fe and the balance of impurities, and the content of impurity elements is less than 0.8 percent.
In the invention, the material of the grinding ball in the step (2) is not limited, preferably a steel ball or a zirconia ball, the size of the grinding ball is not limited, and preferably the grinding ball with the diameter of 2-7 mm.
Further, the mass ratio of the magnetic powder, the solvent and the grinding balls in the step (2) is 1: (3-5): (20 to 50).
The stirring ball mill in the step (2) has a heating function, can adopt a hot oil or other heating modes, has a temperature monitoring function, and can monitor the temperature of the solvent in real time, wherein the temperature monitoring range is required to reach 10-200 ℃, and preferably, the temperature of the mixed solution of the solvent and the magnetic powder in the step (3) is kept at 90-120 ℃, for example, 90-100 ℃ in the whole ball milling process.
Further, the ball milling time in the step (3) is not limited, and is preferably 1.5-2.5 h.
Further, the rotation speed of the ball mill in the step (3) is 100-200 rpm.
Further, the particle size classification in the step (4) is to adopt an air flow classification technology to respectively screen out a particle size-thickness ratio smaller than 50:1, ratio of diameter to thickness (50: 1) to (100: 1), and ratio of diameter to thickness greater than 100: 1 magnetic powder.
Further, the annealing temperature in the step (5) is 650-750 ℃; preferably, the annealing time is 30min to 90 min; further preferably, the annealing atmosphere is hydrogen or argon.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, high-polarity dimethylformamide and/or dimethyl sulfoxide are/is adopted as a solvent, and the solvent has high polarity, so that the solvent not only can play a role of the solvent, but also has a good grinding aid effect, and therefore, a grinding aid or a dispersing agent is not required to be used in the invention, thereby avoiding the phenomenon that the magnetic permeability is deteriorated due to the grinding aid or the dispersing agent remaining on the surface of the magnetic powder;
(2) according to the invention, dimethylformamide and dimethyl sulfoxide with high polarity and high boiling point are used as solvents to perform high-temperature ball milling on the sendust powder, and the ball milling temperature is controlled within a certain range, and the result shows that the sendust powder ball-milled at high temperature, especially at the temperature of 90-120 ℃, has the characteristics of high ratio of diameter to thickness, smooth edge, no burr, high yield and the like; meanwhile, the high-temperature ball milling can greatly shorten the ball milling time and improve the production efficiency.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
The technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Example 1
Step 1: selecting proper gas atomized spherical sendust magnetic powder as raw material powder, wherein the average particle size is 108 mu m; alloy composition (weight percent): 85.4% of Fe, 9.4% of Si and 5.2% of Al.
Step 2: and (3) adding the magnetic powder, the grinding balls and the solvent in the step (1) into a stirring type ball mill. The solvent is dimethylformamide, the stirring type ball mill has a hot oil heating function, the grinding balls are steel balls, and the diameter of the grinding balls is 6.3 mm; the mass ratio of the magnetic powder to the solvent to the grinding balls is 1: 4: 25.
and step 3: heating the solvent and the magnetic powder to 80 ℃ for ball milling, regulating and controlling the temperature of the mixed solution of the solvent and the magnetic powder, keeping the temperature at 90-100 ℃ in the whole ball milling process, controlling the rotating speed of the ball mill at 150 revolutions per minute, and drying the ball-milled magnetic powder in an oven for 2.1 hours.
And 4, step 4: and (3) grading the magnetic powder in the step (3) in a granularity way, and screening out the magnetic powder with a diameter-thickness ratio of less than 50:1, (50: 1) - (100: 1) and a diameter-thickness ratio of more than 100: 1 magnetic powder.
And 5: and (4) annealing the magnetic powder graded in the step (4), wherein the annealing temperature is 650 ℃, the annealing time is 60 minutes, and the annealing atmosphere is hydrogen.
Comparative example 1
As a comparative example of example 1, the temperature of the mixed solution of the solvent and the magnetic powder was maintained at 130 ℃ to 140 ℃ throughout the ball milling process.
Comparative example 2
As a comparative example of example 1, the mixed solution of the solvent and the magnetic powder was not heated and the temperature was precisely controlled, and the ball milling time was 2.1 hours.
Comparative example 3
As a comparative example of example 1, the mixed solution of the solvent and the magnetic powder was not heated and the temperature was precisely controlled, and the ball milling time was 3 hours.
Comparative example 4
As a comparative example of example 1, the mixed solution of the solvent and the magnetic powder was not heated and the temperature was precisely controlled, and the ball milling time was 4 hours.
Comparative example 5
As a comparative example of example 1, the mixed solution of the solvent and the magnetic powder was not heated and the temperature was precisely controlled, and the ball milling time was 5 hours.
And weighing the magnetic powder after the granularity grading, and calculating the proportion of the magnetic powder with various granularities. And simultaneously, carrying out morphology characterization on the magnetic powder with the diameter-thickness ratio of more than 100 by using a scanning electron microscope, and observing the morphology and uniformity of the magnetic powder. Mixing magnetic powder, ethyl acetate and polyurethane uniformly according to a weight ratio of 9:12:1, then uniformly casting slurry on a PET film, drying and heating the casting film, completely removing ethyl acetate, taking down a casting sheet, cutting, putting the casting sheet on a flat vulcanizing machine, carrying out multilayer laminating, wherein the hot pressing temperature, the hot pressing time and the hot pressing pressure are respectively 150 ℃, 6 minutes and 20MPa, die-cutting the pressed magnetic sheet into a circular ring with the outer diameter of 14mm and the inner diameter of 8.5mm, and testing the magnetic conductivity of the magnetic ring by using an Agilent E991A impedance analyzer and an 16454A clamp, wherein the magnetic conductivity is used for representing the magnetic powder, and the diameter-thickness ratio is less than 50:1, the magnetic powder has lower magnetic permeability, so that the magnetic permeability is tested only on the magnetic powder with the diameter-thickness ratio of more than 50:1 without test analysis. The results are shown in Table 1.
TABLE 1 magnetic powder obtained in example 1 and comparative examples 1 to 5 and magnetic permeability test results
The scaly iron-silicon-aluminum magnetic powder is an excellent electromagnetic wave absorbent, and the diameter-thickness ratio, the morphology and the like of the magnetic powder have important influences on the magnetic conductivity. The higher the diameter-thickness ratio, the smoother the magnetic powder edge, the less impurities, and the higher the magnetic permeability. By comparison, example 1 more easily obtained a magnetic powder with a high aspect ratio and a high magnetic permeability.
The data of comparative example 1 show that the ball milling temperature is not too high and needs to be controlled within a certain range. The results of the series of experiments in comparative examples 2 to 5, in which no heating was performed and the ball milling temperature was not controlled, show that the magnetic powder prepared in comparative example 4 has a higher aspect ratio, and thus the optimal ball milling time was 4 hours.
However, it was found by comparing with example 1 that even though the ball milling time is optimal, the magnetic powder with high aspect ratio can be obtained more easily by high temperature and temperature controlled ball milling, and meanwhile, the ball milling time can be greatly shortened, which is beneficial to the improvement of production efficiency.
In addition, through the analysis of a scanning electron microscope, the magnetic powder in the example 1 has more uniform appearance, smooth edges and no burrs, while the magnetic powder in the comparative examples 1 to 5 has poorer uniformity, and more importantly, the magnetic powder has rough edges and obvious burrs, which is the reason that the magnetic permeability of the same diameter-thickness ratio in the following example 1 is obviously higher than that of other magnetic powders.
Example 2
Step 1: selecting proper gas atomized spherical sendust magnetic powder as raw material powder, wherein the average particle size is 100.4 mu m, and the alloy components (weight percentage) are as follows: 84.3 percent of Fe, 9.8 percent of Si and 5.9 percent of Al.
Step 2: and (3) adding the magnetic powder, the grinding balls and the solvent in the step (1) into a stirring type ball mill. The solvent is dimethyl sulfoxide, the stirring type ball mill has a hot oil heating function, the grinding balls are steel balls, and the diameter of the grinding balls is 5.6 mm; the mass ratio of the magnetic powder to the solvent to the grinding balls is 1: 4.5: 35;
and step 3: heating the solvent and the magnetic powder to 80 ℃ for ball milling, regulating and controlling the temperature of the mixed solution of the solvent and the magnetic powder, keeping the temperature at 110-120 ℃ in the whole ball milling process, controlling the rotating speed of the ball mill at 200 r/min, and drying the ball-milled magnetic powder in an oven for 1.7 hours.
And 4, step 4: and (3) grading the magnetic powder in the step (3) in a granularity way, and screening out the magnetic powder with the diameter-thickness ratio of less than 50:1, (50: 1) to (100: 1), greater than 100: 1 magnetic powder.
And 5: and (4) annealing the magnetic powder graded in the step (4), wherein the annealing temperature is 650 ℃, the annealing time is 60 minutes, and the annealing atmosphere is argon.
And weighing the magnetic powder after the granularity grading, and calculating the proportion of the magnetic powder with various granularities. And simultaneously, carrying out morphology characterization on the magnetic powder with the diameter-thickness ratio of more than 100 by using a scanning electron microscope, and observing the morphology and uniformity of the magnetic powder. Mixing magnetic powder, ethyl acetate and polyurethane uniformly according to a weight ratio of 9:12:1, then uniformly casting slurry on a PET film, drying and heating the casting film, completely removing ethyl acetate, taking down a casting sheet, cutting, putting the casting sheet on a flat vulcanizing machine, carrying out multilayer laminating, wherein the hot pressing temperature, the hot pressing time and the hot pressing pressure are respectively 150 ℃, 6 minutes and 20MPa, die-cutting the pressed magnetic sheet into a circular ring with the outer diameter of 14mm and the inner diameter of 8.5mm, and testing the magnetic conductivity of the magnetic ring by using an Agilent E991A impedance analyzer and an 16454A clamp, wherein the magnetic conductivity is used for representing the magnetic powder, and the diameter-thickness ratio is less than 50:1, the magnetic powder has lower magnetic permeability, so that the magnetic permeability is tested only on the magnetic powder with the diameter-thickness ratio of more than 50:1 without test analysis. The results are shown in Table 2.
Table 2 magnetic powder obtained in example 2 and magnetic permeability test results
Through observation of a scanning electron microscope, the magnetic powder of the embodiment 2 has uniform appearance and smooth and flat edges, and the above results show that the magnetic powder with high aspect ratio has very high proportion and high magnetic conductivity.
Example 3
Step 1: selecting proper gas atomized spherical sendust magnetic powder as raw material powder, wherein the average particle size is 95.6 mu m, and the alloy components (weight percentage) are as follows: 85.7% of Fe, 9.1% of Si and 5.2% of Al.
Step 2: adding the magnetic powder, the grinding balls and the solvent in the step 1 into a stirring ball mill, wherein the solvent is a mixed solution of dimethylformamide and dimethyl sulfoxide, and the volume ratio of the dimethylformamide to the dimethyl sulfoxide is 1: 1, the stirring ball mill has a hot oil heating function, the grinding balls are steel balls, and the diameter of the grinding balls is 6.3 mm; the mass ratio of the magnetic powder to the solvent to the grinding balls is 1: 3.5: 20.
and step 3: heating the solvent and the magnetic powder to 80 ℃ for ball milling, regulating and controlling the temperature of the mixed solution of the solvent and the magnetic powder, keeping the temperature at 90-100 ℃ in the whole ball milling process, controlling the rotating speed of the ball mill at 130 r/min, and drying the ball-milled magnetic powder in an oven for 2.2 hours.
And 4, step 4: and (3) grading the magnetic powder in the step (3) in a granularity way, and screening out the magnetic powder with the diameter-thickness ratio of less than 50:1, (50: 1) to (100: 1), greater than 100: 1 magnetic powder.
And 5: and (4) annealing the magnetic powder graded in the step (4), wherein the annealing temperature is 650 ℃, the annealing time is 60 minutes, and the annealing atmosphere is argon.
And weighing the magnetic powder after the granularity grading, and calculating the proportion of the magnetic powder with various granularities. And simultaneously, carrying out morphology characterization on the magnetic powder with the diameter-thickness ratio of more than 100 by using a scanning electron microscope, and observing the morphology and uniformity of the magnetic powder. Mixing magnetic powder, ethyl acetate and polyurethane uniformly according to a weight ratio of 9:12:1, then uniformly casting slurry on a PET film, drying and heating the casting film, completely removing ethyl acetate, taking down a casting sheet, cutting, putting the casting sheet on a flat vulcanizing machine, carrying out multilayer laminating, wherein the hot pressing temperature, the hot pressing time and the hot pressing pressure are respectively 150 ℃, 6 minutes and 20MPa, die-cutting the pressed magnetic sheet into a circular ring with the outer diameter of 14mm and the inner diameter of 8.5mm, and testing the magnetic conductivity of the magnetic ring by using an Agilent E991A impedance analyzer and an 16454A clamp, wherein the magnetic conductivity is used for representing the magnetic powder, and the diameter-thickness ratio is less than 50:1, the magnetic powder has low magnetic permeability, so that the magnetic powder is not tested and analyzed, and only the ratio of the diameter to the thickness is more than 50:1 magnetic powder was subjected to magnetic permeability test. The results are shown in Table 3.
Table 3 magnetic powder obtained in example 3 and magnetic permeability test results
The magnetic powder of example 3 has uniform morphology and smooth edge observed by a scanning electron microscope, and the results in table 3 show that the magnetic powder with high aspect ratio has very high proportion and high magnetic permeability.
It will be understood by those skilled in the art that the foregoing is merely exemplary of the present invention, and is not intended to limit the invention to the particular forms disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. The preparation method of the scaly iron silicon aluminum magnetic powder with high magnetic conductivity is characterized by comprising the following steps:
(1) selecting Fe-Si-Al magnetic powder with the granularity of 80-180 mu m as raw material powder;
(2) adding grinding balls, a solvent and the magnetic powder in the step (1) into a stirring ball mill, wherein the solvent is one or a mixed solvent of dimethyl formamide and dimethyl sulfoxide;
(3) heating the solvent and the magnetic powder to 80 ℃ by using a heating device of a ball mill, and then carrying out ball milling, wherein the temperature of a mixed solution of the solvent and the magnetic powder is kept between 80 ℃ and 130 ℃ in the whole ball milling process, and drying the magnetic powder after ball milling;
(4) grading the magnetic powder in the step (3) in a particle size manner;
(5) annealing the magnetic powder graded in the step (4);
the mass ratio of the magnetic powder to the solvent to the grinding balls in the step (2) is 1: (3-5): (20 to 50).
2. The method for preparing scaly sendust magnetic powder with high magnetic permeability according to claim 1, wherein the magnetic powder in step (1) is spherical, blocky or irregular; the particle size of the magnetic powder in the step (1) is 100-150 μm.
3. The method for preparing the scale-shaped sendust magnetic powder with high permeability according to claim 1, wherein the sendust magnetic powder in step (1) comprises the following alloy components in percentage by weight: 9% -10%, Al: 5 to 6 percent of Fe and the balance of impurities, and the content of impurity elements is less than 0.8 percent.
4. The method for preparing the scaly ferrosilicoaluminophosphate magnetic powder with high magnetic conductivity according to claim 1, wherein the grinding ball in the step (2) is a steel ball or a zirconia ball, and the diameter of the grinding ball is 2-7 mm.
5. The method for preparing scaly sendust magnetic powder with high magnetic permeability according to claim 1, wherein the temperature of the mixed solution of the solvent and the magnetic powder in the step (3) is maintained at 90-120 ℃ during the whole ball milling process.
6. The method for preparing scaly sendust magnetic powder with high magnetic permeability according to claim 1, wherein the ball milling time in step (3) is 1.5-2.5 h.
7. The method for preparing the scaly sendust magnetic powder with high magnetic permeability according to claim 1, wherein the rotation speed of the ball mill in the step (3) is 100-200 rpm.
8. The method for preparing the scaly sendust magnetic powder with high magnetic permeability according to claim 1, wherein the step (4) of particle size classification is to select the magnetic powder with the ratio of diameter to thickness of less than 50:1, ratio of diameter to thickness (50: 1) to (100: 1), and ratio of diameter to thickness greater than 100: 1 magnetic powder.
9. The method for preparing the scaly sendust magnetic powder with high magnetic permeability according to claim 1, wherein the annealing temperature in the step (5) is 650 ℃ to 750 ℃; the annealing time is 30min-90 min; the annealing atmosphere is hydrogen or argon.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911029890.8A CN110718347B (en) | 2019-10-28 | 2019-10-28 | Preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911029890.8A CN110718347B (en) | 2019-10-28 | 2019-10-28 | Preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder |
Publications (2)
Publication Number | Publication Date |
---|---|
CN110718347A CN110718347A (en) | 2020-01-21 |
CN110718347B true CN110718347B (en) | 2021-03-26 |
Family
ID=69214383
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201911029890.8A Active CN110718347B (en) | 2019-10-28 | 2019-10-28 | Preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110718347B (en) |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112250345B (en) * | 2020-09-29 | 2022-04-26 | 绵阳西磁科技有限公司 | FeSiAl sheet-shaped wave-absorbing material and preparation method thereof |
CN112207283B (en) * | 2020-10-22 | 2022-05-20 | 合肥工业大学 | Preparation method of flaky iron-silicon-aluminum powder with uniform particle size and micron-sized large diameter-thickness ratio particles |
CN112466647A (en) * | 2020-11-26 | 2021-03-09 | 成都慧磁电子材料有限公司 | Production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder |
CN114045435B (en) * | 2021-11-11 | 2022-12-20 | 泉州天智合金材料科技有限公司 | Iron-based amorphous nanocrystalline wave-absorbing material and preparation method thereof |
CN116900322B (en) * | 2022-12-07 | 2024-07-19 | 绵阳西磁科技有限公司 | High-flattening Fe-Si-Al alloy wave-absorbing magnetic powder and preparation method thereof |
CN117457371A (en) * | 2023-11-30 | 2024-01-26 | 襄阳睿新鹏电子科技有限公司 | Flat wire type inductor manufacturing method |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5256326A (en) * | 1988-07-12 | 1993-10-26 | Idemitsu Kosan Co. Ltd. | Methods for preparing magnetic powder material and magnet, process for prepartion of resin composition and process for producing a powder molded product |
CN108962521A (en) * | 2018-07-13 | 2018-12-07 | 吴江市聚盈电子材料科技有限公司 | A kind of electromagnetic shielding preparation method of magnetic material |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105834440B (en) * | 2016-06-12 | 2018-02-13 | 横店集团东磁股份有限公司 | A kind of preparation method of high magnetic permeability sheet soft-magnetic alloy powder |
CN107507689B (en) * | 2016-06-14 | 2019-08-13 | 有研稀土新材料股份有限公司 | The preparation method of high magnetic permeability absorbing material |
JP6864498B2 (en) * | 2017-02-28 | 2021-04-28 | 山陽特殊製鋼株式会社 | A soft magnetic flat powder having high magnetic permeability and high weather resistance and a soft magnetic resin composition containing the same. |
CN109175384A (en) * | 2018-08-01 | 2019-01-11 | 四川大学 | A kind of preparation method of flake micron grade iron aluminum silicon powder |
CN110060834B (en) * | 2019-05-16 | 2021-06-08 | 常州威斯双联科技有限公司 | Soft magnetic alloy powder, wave absorbing plate, preparation method of soft magnetic alloy powder, electronic component and electronic equipment |
-
2019
- 2019-10-28 CN CN201911029890.8A patent/CN110718347B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5256326A (en) * | 1988-07-12 | 1993-10-26 | Idemitsu Kosan Co. Ltd. | Methods for preparing magnetic powder material and magnet, process for prepartion of resin composition and process for producing a powder molded product |
CN108962521A (en) * | 2018-07-13 | 2018-12-07 | 吴江市聚盈电子材料科技有限公司 | A kind of electromagnetic shielding preparation method of magnetic material |
Also Published As
Publication number | Publication date |
---|---|
CN110718347A (en) | 2020-01-21 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110718347B (en) | Preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder | |
CN105834440A (en) | Method for preparing high-permeability flaky soft magnetic alloy powder | |
CN107445605B (en) | A kind of preparation method of high-performance permanent magnetic ferrite material | |
CN104538143B (en) | Flat soft magnet powder and preparation method thereof | |
CN106735254B (en) | A kind of metal powder and its preparation method and application | |
CN109400139B (en) | Preparation process of low-cost permanent magnetic ferrite material | |
CN110085385A (en) | A kind of high magnetic permeability composite powder and preparation method thereof | |
CN110340345B (en) | Nano-phase reinforced copper-based diamond tool matrix powder and matrix preparation method | |
CN105702410A (en) | Method for preparing soft magnetic powder core | |
CN110270683B (en) | Fe/ZrH2 nanocrystalline composite particle and preparation method and application thereof | |
CN111545763B (en) | Preparation method of modified copper-gold powder | |
KR102369149B1 (en) | Magnetic flat powder and magnetic sheet containing same | |
CN114855055B (en) | Low-crack-sensitivity high-entropy alloy powder material and preparation method and application thereof | |
CN113579237B (en) | Preparation method for reducing apparent density of copper-tin alloy powder | |
CN112662930A (en) | High-entropy die steel material and preparation method thereof | |
CN111607745A (en) | High-density and high-hardness vacuum sintering stainless steel material and processing technology thereof | |
CN110253028A (en) | A kind of self-lubricating 3D printing alloy powder and preparation method thereof | |
CN109837441B (en) | Novel tungsten nickel cobalt material and preparation method thereof | |
CN111097916B (en) | Preparation method of superfine high-purity rhenium powder | |
CN113073178A (en) | Preparation method of GHz-frequency-band high-wave-absorption-performance iron-based nanocrystalline alloy | |
CN107287472B (en) | A kind of viscose staple fibre cutoff tool that the powder metallurgic method mixed with pure powder manufactures | |
CN114855056B (en) | Preparation method of heterojunction sintering alnico doped with casting alnico | |
CN112466647A (en) | Production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder | |
CN113601407B (en) | Diamond grinding wheel and preparation method thereof | |
CN114000025B (en) | WC-Co-based alloy with high wear resistance and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A preparation method of high permeability flake iron silicon aluminum magnetic powder Effective date of registration: 20220621 Granted publication date: 20210326 Pledgee: Dongyang Branch of China Construction Bank Co.,Ltd. Pledgor: HENGDIAN GROUP DMEGC MAGNETICS Co.,Ltd. Registration number: Y2022330001027 |