CN112466647A - Production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder - Google Patents
Production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder Download PDFInfo
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- CN112466647A CN112466647A CN202011353287.8A CN202011353287A CN112466647A CN 112466647 A CN112466647 A CN 112466647A CN 202011353287 A CN202011353287 A CN 202011353287A CN 112466647 A CN112466647 A CN 112466647A
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—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
- H01F1/14775—Fe-Si based alloys in the form of sheets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—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
Abstract
The invention provides a production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder, which comprises the following steps: A) mixing and ball-milling steel balls, grinding aids and Fe-Si-Al soft magnetic alloy raw material powder to obtain mixed slurry; the mass ratio of the steel ball, the grinding aid and the Fe-Si-Al soft magnetic alloy raw material powder is (3-6): (4-8): 1; the grinding aid is an alcohol organic solvent; the diameter of the steel ball is 4.0-8.0 mm; B) carrying out solid-liquid separation on the mixed slurry, and drying the solid to obtain dried powder; C) and annealing the dried powder at high temperature to obtain the Fe-Si-Al soft magnetic alloy flaky powder with high magnetic conductivity. The invention can improve the yield and the magnetic conductivity of the flaky powder by changing the proportion of the steel ball, the grinding aid, the raw material powder and the lubricant and the ball diameter of the steel ball. In addition, when the flaky powder is ground at low temperature and high rotating speed (the lubricant has an assistance effect), the brittleness of raw material powder with different shapes is effectively controlled, the ductility is improved, and the ground flaky powder has large flake diameter and thin thickness (the ratio of the diameter to the thickness is large).
Description
Technical Field
The invention belongs to the technical field of alloy preparation, and particularly relates to a production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder.
Background
The Fe-Si-Al soft magnetic alloy with high magnetic conductivity and low loss is a novel functional material and has excellent magnetic, electric conversion, energy storage and filtering functions. The alloy material has two uses: firstly, the iron-silicon-aluminum soft magnetic alloy powder is prepared into particle powder for producing magnetic cores of new-generation inductance devices, namely iron-silicon-aluminum soft magnetic alloy magnetic powder cores, and the iron-silicon-aluminum soft magnetic alloy magnetic powder cores are widely used in the electronic power industry. Secondly, preparing flaky powder for producing another new material: an absorbent of electromagnetic wave absorbing material. The new material still belongs to the starting stage at home at present.
The alloy has physical properties of large HRC hardness, large brittleness and poor plasticity, so the mechanical processing cannot directly process the alloy into electronic components. Therefore, the method which is generally adopted internationally is to prepare the alloy into granular powder and then prepare the alloy powder into various high-performance electronic devices by applying the powder metallurgy principle and process. The production method comprises the following steps: (1) the alloy is mechanically crushed and ball-milled to produce irregular particle powder by utilizing the brittleness of the alloy; (2) the melted liquid alloy is directly sprayed into spherical and nearly spherical particle powder at high temperature by adopting a water atomization/gas atomization process.
On the other hand, the iron-silicon-aluminum alloy has the electromagnetic characteristics of high saturation magnetic induction intensity and high resistivity, is further deeply processed on the basis of granular powder, is ground into flaky powder (also called flat, leaf-shaped and scaly), is a novel high-performance electromagnetic wave absorbent, and is used for solving the electromagnetic wave interference and greatly improving the wave absorbing performance. Can be widely applied to various electronic devices and electronic equipment.
The electromagnetic wave absorbing material with Fe-Si-Al alloy powder as absorbent is one kind of composite film formed through fusion and adhesion of base material and absorbent. The absorbent has the function of absorbing electromagnetic waves, and the matrix material (most of which has no wave absorbing function) has the functions of: 1) fusing and bonding the absorbent to form the wave-absorbing film material, and 2) transmitting electromagnetic waves. Namely: the electromagnetic wave incident to the surface of the wave-absorbing material effectively enters the absorber through the base material, and the electromagnetic wave is converted into heat energy (or energy in other forms or mutual interference and cancellation of the electromagnetic wave) and dissipated in the process of continuously attenuating the electromagnetic wave.
Researches show that (1) the electromagnetic parameters of the absorbent are main factors influencing the electromagnetic wave absorption performance, wherein the magnetic permeability and the electrical resistivity of the material are 2 key indexes of the electromagnetic parameters. (2) The larger the magnetic permeability and the resistivity of the material are, the better the wave-absorbing performance is (the invention only relates to the influence of the magnetic permeability of the material on the wave-absorbing performance). (3) The magnetic permeability can be effectively improved by changing the shape of the sendust soft magnetic alloy powder. (4) Different geometrical sizes of the Fe-Si-Al soft magnetic alloy flake powder show different magnetic conductivity characteristics, namely: the magnetic permeability of the iron-silicon-aluminum alloy flake powder is increased along with the increase of the surface area of the powder. (5) When the geometric dimension of the Fe-Si-Al flaky powder reaches 50 mu m of sheet diameter (D) and 2 mu m of thickness (H), the magnetic conductivity begins to generate an ascending inflection point, and after the inflection point is exceeded, the larger the D/H ratio of the diameter thickness is, the larger the inclination angle of the magnetic conductivity is. (6) The flexibility, dispersion and fusion property, bonding lamination effect and the like of the iron-silicon-aluminum alloy flake powder in the base material are factors influencing the magnetic permeability. (7) The Fe-Si-Al alloy flake powder has poor corrosion resistance and is easy to oxidize. After the wave absorbing agent is prepared into the wave absorbing material, if the wave absorbing material is oxidized and rusted, the magnetic conductivity of the material can be reduced, so that the wave absorbing performance is reduced, and the service life of the wave absorbing material is shortened. (8) The sheet iron-silicon-aluminum alloy powder is subjected to rust resistance treatment, so that the high-quality wave absorber with good rust resistance can be obtained.
The physical characteristics of the Fe-Si-Al soft magnetic alloy, such as high hardness and brittleness and poor plasticity, increase the difficulty of preparing the alloy into flaky powder with large diameter-thickness ratio. In general, granulated powders having the same composition are used as a starting powder to conduct grinding tableting. Namely, raw material powder, solvent and grinding body are added into a grinder according to a proportion. The ball body is used as a grinding body, the solvent is used as a grinding aid, the ball body, the raw material powder and the solvent move in the same direction under the driving of the stirring device, and the ball body and the raw material powder are impacted, extruded and rubbed, so that the raw material powder is ground into pieces in the crushing and deformation processes. Because the alloy has poor plastic deformation capability, if advanced grinding equipment and production technology are not available, the flaky powder with normally distributed radius-thickness ratio and high magnetic conductivity is difficult to prepare.
Disclosure of Invention
The invention aims to provide a production process of high-permeability Fe-Si-Al soft magnetic alloy flaky powder.
The invention provides a production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder, which comprises the following steps:
A) mixing and ball-milling steel balls, grinding aids and Fe-Si-Al soft magnetic alloy raw material powder to obtain mixed slurry;
the mass ratio of the steel ball, the grinding aid and the Fe-Si-Al soft magnetic alloy raw material powder is (3-6): (4-8): 1; the grinding aid is an alcohol organic solvent; the diameter of the steel ball is 4.0-8.0 mm;
B) carrying out solid-liquid separation on the mixed slurry, and drying the solid to obtain dried powder;
C) and annealing the dried powder at high temperature to obtain the Fe-Si-Al soft magnetic alloy flaky powder with high magnetic conductivity.
Preferably, the grain size of the Fe-Si-Al soft magnetic alloy raw material powder is-60 meshes, and the chemical components are as follows: si: 8.5-10.0 wt%, Al: 5.0 to 7.0 wt%, and the balance Fe.
Preferably, the grinding aid is one or more of ethanol, isopropanol and methanol.
Preferably, a lubricant is also added in the step A) to be mixed and ball-milled,
the lubricant is one or more of stearic acid, zinc stearate and ethyl acetate; the mass of the lubricant is 0.01-2% of the total mass of the steel ball, the grinding aid and the Fe-Si-Al soft magnetic alloy raw material powder.
Preferably, the ball milling speed is 350-700 r/min.
Preferably, the temperature of the mixed slurry in the ball milling process is controlled to be 30-60 ℃.
Preferably, the ball milling is carried out until the apparent density AD of the powder is less than 0.6g/cm3Discharging the materials.
Preferably, the high-temperature annealing temperature is 600-800 ℃; the high-temperature annealing time is 40-120 min.
Preferably, the high-temperature annealing is performed under a protective atmosphere, which is nitrogen and/or hydrogen.
Preferably, the Fe-Si-Al soft magnetic alloy flake powder after high-temperature annealing is subjected to air flow classification and vibration screening to obtain high-permeability Fe-Si-Al soft magnetic alloy flake powder with the grain size of-120 meshes.
The invention provides a production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder, which comprises the following steps: A) mixing and ball-milling steel balls, grinding aids and Fe-Si-Al soft magnetic alloy raw material powder to obtain mixed slurry; the mass ratio of the steel ball, the grinding aid and the Fe-Si-Al soft magnetic alloy raw material powder is (3-6): (4-8): 1; the grinding aid is an alcohol organic solvent; the diameter of the steel ball is 4.0-8.0 mm; B) carrying out solid-liquid separation on the mixed slurry, and drying the solid to obtain dried powder; C) and annealing the dried powder at high temperature to obtain the Fe-Si-Al soft magnetic alloy flaky powder with high magnetic conductivity.
The invention can improve the yield and the magnetic conductivity of the flaky powder (to produce high-magnetic conductivity wave-absorbing materials with various specifications) by changing the proportion of the steel ball/the grinding aid/the raw material powder/(the lubricant) and the ball diameter of the steel ball. Wherein, the yield of the flaky powder with the magnetic permeability of mu e 180-200-;
in addition, when the flaky powder is ground at low temperature and high rotating speed (the lubricant has an assistance effect), the brittleness of raw material powder with different shapes is effectively controlled, the ductility is improved, the powder is easier to flake, the radial surface of the flaky powder is smoother, and the defect phenomenon of the arc edge of the flaky powder is greatly reduced. Meanwhile, the proportion of small-diameter powder is greatly reduced, the cold welding overlapping phenomenon of small micro-piece powder (the piece diameter is nano-scale) on the large-diameter powder surface tends to disappear, and the ground flaky powder has large piece diameter and thin thickness (the diameter-thickness ratio is large). The testing laser granularity shows that: the ratio concentrated in normal distribution 50-200 μm is more than 85%, and the geometric size tested by a scanning electron microscope is as follows: the maximum thickness is less than 1 μm, and the maximum sheet diameter is more than 200 μm. The maximum diameter-thickness ratio is more than 200: 1.
Detailed Description
The invention provides a production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder, which comprises the following steps:
A) mixing and ball-milling steel balls, grinding aids and Fe-Si-Al soft magnetic alloy raw material powder to obtain mixed slurry;
the mass ratio of the steel ball, the grinding aid and the Fe-Si-Al soft magnetic alloy raw material powder is (3-6): (4-8): 1; the grinding aid is an alcohol organic solvent; the diameter of the steel ball is 4.0-8.0 mm;
B) carrying out solid-liquid separation on the mixed slurry, and drying the solid to obtain dried powder;
C) and annealing the dried powder at high temperature to obtain the Fe-Si-Al soft magnetic alloy flaky powder with high magnetic conductivity.
The invention adds the steel ball, the grinding aid and the Fe-Si-Al soft magnetic alloy raw material powder into a ball mill for ball milling, preferably, the invention can also add the lubricant into the ball milling raw material to assist the ball milling process.
In the invention, the grain size of the Fe-Si-Al soft magnetic alloy raw material powder is preferably-60 meshes, and the Fe-Si-Al soft magnetic alloy raw material powder comprises the following components: si: 8.5-10.0 wt%, Al: 5.0-7.0 wt%, and the balance of Fe, wherein the Fe-Si-Al soft magnetic alloy raw material powder is not oxidized and has no impurities.
The invention preferably adopts a sphere with high hardness and good wear resistance as a grinding body (collectively called steel balls), and the sphere diameter is equal to or mixed with steel balls with the sphere diameter difference less than 10%. The hardness of the steel ball is preferably HRC > 58; the sphere diameter of the steel ball is preferably 4.0-8.0mm, and more preferably 5.0-6.9 mm.
In the invention, the grinding aid is preferably an alcohol organic solvent, such as one or more of methanol, ethanol and isopropanol; the invention preferably uses a mixture of two alcohol solvents as the grinding aid, and specifically, in the embodiment of the invention, ethanol and isopropanol can be used.
In the invention, the mass ratio of the steel ball, the grinding aid and the Fe-Si-Al soft magnetic alloy raw material powder is (3-6): (4-8): 1, preferably (4-5): (5-7): specifically, in the embodiment of the present invention, the ratio of 3: 5: 1. 5.5:6:1 or 4:8: 1.
In the invention, the lubricant is preferably one or more of stearic acid, zinc stearate and ethyl acetate; the mass of the lubricant is preferably 0.01-2%, more preferably 0.1-1.5%, and most preferably 0.5-1.0% of the total mass of the steel ball, the grinding aid and the sendust soft magnetic alloy raw material powder, and specifically, in the embodiment of the present invention, may be 0.5%.
In the invention, the ball milling speed is preferably 350-700 r/min, more preferably 400-650 r/min, and most preferably 450-600 r/min, specifically, in the embodiment of the invention, 600 r/min or 680 r/min. More preferably, the invention can also perform speed segmented stirring within the ball milling speed of 350-700 r/min, i.e. the ball milling speed is adjusted in segments, for example, the starting rotation speed is 350 r/min, the rotation speed is 700 r/min after 3 hours, and the rotation speed is 600 r/min after 8 hours.
In the stirring process, cooling water is preferably introduced into the ball mill to ensure that the temperature of the slurry is maintained in a low-temperature region of 30-60 ℃.
Ball-milling until the apparent density AD of the powder is less than 0.6g/cm3And discharging, and carrying out solid-liquid separation on the mixed slurry in the ball mill to obtain wet powder.
The method for solid-liquid separation is not particularly required in the invention, and a solid-liquid separation method well known in the art, such as centrifugal separation, can be adopted.
The invention dries wet powder obtained by solid-liquid separation to obtain dry powder. The drying method is preferably drying, and the drying process is a common process in the field, and the invention is not described herein again.
After the dry powder is obtained, the invention carries out high-temperature annealing on the dry powder under protective atmosphere to obtain the annealed flaky powder.
In the invention, the annealing temperature is preferably 600-800 ℃, more preferably 650-750 ℃, and preferably, the annealing in the invention is dual-temperature-zone annealing, that is, the annealing furnace has two temperature zones, a high-temperature zone and a low-temperature zone, specifically, in the embodiment of the invention, 680 ℃/780 ℃; 650 ℃/760 ℃; 600 ℃/800 ℃. The annealing time is preferably 40 to 120min, more preferably 50 to 110min, most preferably 60 to 100min, and specifically, in the embodiment of the present invention, the annealing time may be 60min, 80min or 120 min.
In the present invention, the protective atmosphere for the annealing is nitrogen and/or hydrogen.
After annealing, the obtained flaky powder is subjected to airflow classification and sieving in sequence, and the flaky powder with the particle size of-120 meshes is collected, namely the high-permeability Fe-Si-Al soft magnetic alloy flaky powder.
The invention provides a production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder, which comprises the following steps: A) mixing and ball-milling steel balls, grinding aids and Fe-Si-Al soft magnetic alloy raw material powder to obtain mixed slurry; the mass ratio of the steel ball, the grinding aid and the Fe-Si-Al soft magnetic alloy raw material powder is (3-6): (4-8): 1; the grinding aid is an alcohol organic solvent; the diameter of the steel ball is 4.0-8.0 mm; B) carrying out solid-liquid separation on the mixed slurry, and drying the solid to obtain dried powder; C) and annealing the dried powder at high temperature to obtain the Fe-Si-Al soft magnetic alloy flaky powder with high magnetic conductivity.
The invention can improve the yield and the magnetic conductivity of the flaky powder (to produce high-magnetic conductivity wave-absorbing materials with various specifications) by changing the proportion of the steel ball/the grinding aid/the raw material powder/(the lubricant) and the ball diameter of the steel ball. Wherein, the yield of the flaky powder with the magnetic permeability of mu e 180-200-;
in addition, when the flaky powder is ground at low temperature and high rotating speed (the lubricant has an assistance effect), the brittleness of raw material powder with different shapes is effectively controlled, the ductility is improved, the powder is easier to flake, the radial surface of the flaky powder is smoother, and the defect phenomenon of the arc edge of the flaky powder is greatly reduced. Meanwhile, the proportion of small-diameter powder is greatly reduced, the cold welding overlapping phenomenon of small micro-piece powder (the piece diameter is nano-scale) on the large-diameter powder surface tends to disappear, and the ground flaky powder has large piece diameter and thin thickness (the diameter-thickness ratio is large). The testing laser granularity shows that: the ratio concentrated in normal distribution 50-200 μm is more than 85%, and the geometric size tested by a scanning electron microscope is as follows: the maximum thickness is less than 1 μm, and the maximum sheet diameter is more than 200 μm. The maximum diameter-thickness ratio is more than 200: 1.
in order to further illustrate the present invention, the following will describe the production process of a high permeability sendust soft magnetic alloy flake powder provided by the present invention in detail with reference to the examples, but it should not be construed as limiting the scope of the present invention.
Example 1
A. Selecting irregular Fe-Si-Al alloy raw material powder which is mechanically crushed by a 60-mesh sieve, wherein the chemical components (wt%) are as follows: 9.82% of Si, 5.21% of Al and the balance Fe, the powder is not oxidized and has no impurities, and the AD is 2.95g/cm3。
B. The grinding body is GCr15 steel ball, HRC > 60, and the ball diameter is 5.0-6.9 mm.
C. The grinding aid is mixed with 2 alcohol solvents of ethanol and isopropanol, and the lubricant is stearic acid.
D. And adding the steel ball, the grinding aid and the raw material powder into the ball mill in sequence. Steel ball: ethanol: raw material powder is 3: 5: 1, then 0.5% stearic acid is added.
E. The grinding stirring speed is 600 rpm, and the stirring is carried out at a constant speed.
F. Cooling water is introduced into the grinder during grinding, and the temperature of the slurry is kept between 30 and 60 ℃.
G. Grinding to obtain powder with apparent density AD less than 0.4g/cm3Discharging the materials.
H. And D, pumping the slurry prepared in the step G into a centrifugal machine, and putting wet powder into a dryer for drying after liquid-solid separation.
I. And D, feeding the dried powder baked in the step H into an annealing furnace for high-temperature annealing. The temperature is 680/780 ℃ (2 temperature zones) for 60 minutes, nitrogen is used as protective atmosphere, and the furnace is discharged after being cooled to less than 50 ℃.
J. And (4) putting the powder discharged from the furnace in the step I into an airflow classifier, and collecting flaky powder after classification.
K. And D, putting the flaky powder collected in the step J into a vibrating screen to be screened by 120 meshes, and collecting the flaky powder of-120 meshes.
And L, sampling from the flaky powder prepared in the step K, marking as No. 1 flaky powder, testing the particle size distribution by using a BT-93005 laser instrument, and observing the shape of the powder and the thickness h size of the marked powder by using SEM (the diameter-thickness ratio is the maximum h size marked by D98/SEM tested by using a laser particle sizer).
Analytical test data were as follows:
TABLE 1 laser particle size distribution and diameter-thickness ratio d/h
M, taking the-120 flaky powder obtained in the step K, and mixing the flaky powder with the weight of 1: (5-10) putting the mixture into the prepared liquid silica sol (namely the matrix material), and stirring the mixture for 30-120 minutes at normal temperature to prepare uniform slurry.
And N, pumping the slurry prepared in the step M into a feed inlet of a coating machine by using a pump, adjusting the height of a spraying seam, uniformly coating the slurry on the PE film to form a coating with the thickness of 50 microns, and baking and removing the coating with the PE film by using a solvent of silica sol in each heating section (normal temperature/60 ℃/80 ℃/100 ℃/120 ℃) of the coating machine to obtain the high-permeability wave-absorbing material film.
O, using 40-80kg/cm of the wave-absorbing material film prepared in the step N2Pressure calendering.
P, randomly taking 3 point positions of the wave-absorbing material film prepared in the step P, cutting the wave-absorbing material film into an annular sample with the outer diameter of 20mm, and marking the sample as: loop # 1, loop # 2, loop # 3.
And Q, testing the magnetic permeability of the ring No. 1, the ring No. 2 and the ring No. 3 prepared in the step P, and testing the anti-corrosion function by soaking in salt water.
Analytical test data were as follows:
table 2 magnetic permeability μ e test of wave-absorbing material:
example 2
A. Selecting gas atomized spherical Fe-Si-Al alloy raw material powder with a particle size of-60 meshes, wherein the chemical components (wt%) are as follows: 9.21% of Si, 6.95% of Al and the balance Fe, the powder is not oxidized and has no impurities, and the AD is 4.06g/cm3。
B. The grinding body is a GCr15 steel ball, the HRC is more than 58, and the diameter of the ball is 6.0 mm.
C. The grinding aid is 95% industrial ethanol.
D. Adding the steel balls, the ethanol and the raw material powder into a ball mill in sequence. Steel ball: ethanol: raw material powder is 5.5:6:1
E. The grinding stirring speed is 680 r/min, and the stirring is carried out at a constant speed.
F. Cooling water is introduced into the grinder during grinding, and the temperature of the slurry is kept between 30 and 60 ℃.
G. Grinding to obtain powder with apparent density AD less than 0.5g/cm3Discharging the materials.
H. And D, pumping the slurry prepared in the step G into a centrifugal machine, and putting wet powder into a dryer for drying after liquid-solid separation.
I. And D, feeding the dried powder baked in the step H into an annealing furnace for high-temperature annealing. The temperature is 650/760 ℃ (2 temperature zones) for 80 minutes, nitrogen is used as protective atmosphere, and the temperature is cooled to be less than 50 ℃ and then the product is discharged.
J. And (4) putting the powder discharged from the furnace in the step I into an airflow classifier, and collecting flaky powder after classification.
K. And D, putting the flaky powder collected in the step J into a vibrating screen to be screened by a 120-mesh sieve, and collecting the flaky powder of-120 meshes.
And L, sampling from the-120 flaky powder prepared in the step K, marking as # 2 flaky powder, testing the particle size distribution by using a BT-93005 laser instrument, and observing the shape of the powder and the thickness h size of the marked powder by using SEM (the diameter-thickness ratio is the maximum h size marked by D98/SEM tested by using a laser particle sizer).
Analytical test data were as follows:
TABLE 3 laser particle size distribution to diameter-thickness ratio d/h
M, taking the-120 flaky powder obtained in the step K, and mixing the flaky powder with the weight of 1: (5-10) putting the mixture into the prepared liquid silica sol (namely the matrix material), and stirring the mixture for 30-120 minutes at normal temperature to prepare uniform slurry.
And N, pumping the slurry prepared in the step M into a feed inlet of a coating machine by using a pump, adjusting the height of a spraying seam, uniformly coating the slurry on a PE film to form a coating film layer with the thickness of 50 microns, and baking and removing the coating film layer with the PE film forward through a solvent of silica sol in each heating section (normal temperature/60 ℃/80 ℃/100 ℃/120 ℃) of the coating machine to obtain the high-permeability wave-absorbing material film.
O, using 40-80kg/cm of the wave-absorbing material film prepared in the step N2Pressure calendering.
And P, randomly taking 3 point positions on the wave-absorbing material film prepared in the step O, cutting into an annular sample with the outer diameter of 20mm, and marking as: loop # 4, loop # 5, loop # 6.
Analytical test data were as follows:
table 4 wave-absorbing material permeability μ e test:
example 3
A. Selecting raw material powder of an irregular Fe-Si-Al alloy crushed by 80 meshes, wherein the raw material powder comprises the following chemical components in percentage by weight: 9.25% of Si, 5.93% of Al and the balance Fe, the powder is not oxidized and has no impurities, and the AD is 2.86g/cm3。
B. The grinding body is GCr15 steel ball, HRC is more than 58, and the ball diameter is 4.0-8.0 mm.
C. The grinding aid is a mixture of 3 alcohol solvents of methanol, ethanol and isopropanol, and the lubricant is zinc stearate.
D. And adding the steel ball, the grinding aid and the raw material powder into the ball mill in sequence. Steel ball: ethanol: raw material powder is 4:8:1
E. The grinding stirring speed is 350-700 r/min, and the stirring speed is adjusted in stages.
F. Cooling water is introduced into the grinder during grinding, and the temperature of the slurry is kept between 30 and 60 ℃.
G. Grinding to obtain powder with apparent density AD less than 0.6g/cm3Discharging the materials.
H. And D, pumping the slurry prepared in the step G into a centrifugal machine, and putting wet powder into a dryer for drying after liquid-solid separation.
I. And D, feeding the dried powder baked in the step H into an annealing furnace for high-temperature annealing. The temperature is 600/800 ℃ (2 temperature zones) for 120 minutes, nitrogen is used as protective atmosphere, and the furnace is discharged after being cooled to 50 ℃.
J. And (4) putting the powder discharged from the furnace in the step I into an airflow classifier, and collecting flaky powder after classification.
K. And D, putting the flaky powder obtained in the step J into a vibrating screen, screening by a 120-mesh sieve, and collecting the flaky powder of-120 meshes.
And L, sampling from the-120 flaky powder prepared in the step M, marking as 3# flaky powder, testing the particle size distribution by using a BT-93005 laser instrument, and observing the morphology of the powder and marking the thickness h size of the powder by using SEM (the diameter-thickness ratio is the maximum h size marked by D98/SEM tested by using a laser particle sizer).
Analytical test data were as follows:
TABLE 5 laser particle size distribution to diameter-thickness ratio d/h
M, taking the-120 flaky powder obtained in the step K, and mixing the flaky powder with the weight of 1: (5-10) putting the mixture into the prepared liquid silica sol (namely the matrix material), and stirring the mixture for 30-120 minutes at normal temperature to prepare uniform slurry.
And N, pumping the slurry prepared in the step M into a feed inlet of a coating machine by using a pump, adjusting the height of a spraying seam, uniformly coating the slurry on the PE film to form a coating with the thickness of 50 microns, and baking and removing the coating with the PE film by using a solvent of silica sol in each heating section (normal temperature/60 ℃/80 ℃/100 ℃/120 ℃) of the coating machine to obtain the high-permeability wave-absorbing material film.
O, using 40-80kg/cm of the wave-absorbing material film prepared in the step N2Pressure calendering.
And P, randomly taking 3 point positions of the wave-absorbing material film prepared in the step O, cutting the wave-absorbing material film into an annular sample with the outer diameter of 20mm, and marking the sample as: 7# ring, 8# ring, 9# ring.
Analytical test data were as follows:
table 6 magnetic permeability μ e test of wave-absorbing material:
the foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A production process of high-permeability Fe-Si-Al soft magnetic alloy flake powder comprises the following steps:
A) mixing and ball-milling steel balls, grinding aids and Fe-Si-Al soft magnetic alloy raw material powder to obtain mixed slurry;
the mass ratio of the steel ball, the grinding aid and the Fe-Si-Al soft magnetic alloy raw material powder is (3-6): (4-8): 1; the grinding aid is an alcohol organic solvent; the diameter of the steel ball is 4.0-8.0 mm;
B) carrying out solid-liquid separation on the mixed slurry, and drying the solid to obtain dried powder;
C) and annealing the dried powder at high temperature to obtain the Fe-Si-Al soft magnetic alloy flaky powder with high magnetic conductivity.
2. The production process of claim 1, wherein the grain size of the Fe-Si-Al soft magnetic alloy raw material powder is-60 meshes, and the chemical components are as follows: si: 8.5-10.0 wt%, Al: 5.0 to 7.0 wt%, and the balance Fe.
3. The production process of claim 1, wherein the grinding aid is one or more of ethanol, isopropanol and methanol.
4. The production process according to claim 1, wherein a lubricant is further added in the step A) to mix and ball mill,
the lubricant is one or more of stearic acid, zinc stearate and ethyl acetate; the mass of the lubricant is 0.01-2% of the total mass of the steel ball, the grinding aid and the Fe-Si-Al soft magnetic alloy raw material powder.
5. The production process according to claim 1, wherein the ball milling rate is 350 to 700 rpm.
6. The production process according to claim 1, wherein the temperature of the mixed slurry in the ball milling process is controlled to be 30-60 ℃.
7. The process according to claim 1, wherein the powder is ball-milled to a bulk density AD < 0.6g/cm3Discharging the materials.
8. The production process according to claim 1, wherein the temperature of the high-temperature annealing is 600-800 ℃; the high-temperature annealing time is 40-120 min.
9. The production process according to claim 1, characterized in that the high-temperature annealing is carried out under a protective atmosphere, which is nitrogen and/or hydrogen.
10. The production process according to any one of claims 1 to 9, wherein the Fe-Si-Al soft magnetic alloy flake powder after the high-temperature annealing is subjected to air flow classification and vibration screening to obtain the Fe-Si-Al soft magnetic alloy flake powder with the high magnetic permeability and the grain size of-120 meshes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114260455A (en) * | 2021-12-28 | 2022-04-01 | 苏州铂韬新材料科技有限公司 | Ball milling process of low-cost high-permeability wave-absorbing powder |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030081738A (en) * | 2002-04-12 | 2003-10-22 | 휴먼일렉스(주) | Method of manufacturing soft magnetic powder and inductor using the same |
| CN107414089A (en) * | 2017-07-20 | 2017-12-01 | 上海交通大学 | A kind of Fe-Si-Al magnetic and preparation method thereof |
| 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 |
| CN110060834A (en) * | 2019-05-16 | 2019-07-26 | 常州威斯双联科技有限公司 | Magnetically soft alloy powder inhales wave plate, preparation method, electronic component and electronic equipment |
| CN110718347A (en) * | 2019-10-28 | 2020-01-21 | 横店集团东磁股份有限公司 | Preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder |
-
2020
- 2020-11-26 CN CN202011353287.8A patent/CN112466647A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030081738A (en) * | 2002-04-12 | 2003-10-22 | 휴먼일렉스(주) | Method of manufacturing soft magnetic powder and inductor using the same |
| CN107414089A (en) * | 2017-07-20 | 2017-12-01 | 上海交通大学 | A kind of Fe-Si-Al magnetic and preparation method thereof |
| 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 |
| CN110060834A (en) * | 2019-05-16 | 2019-07-26 | 常州威斯双联科技有限公司 | Magnetically soft alloy powder inhales wave plate, preparation method, electronic component and electronic equipment |
| CN110718347A (en) * | 2019-10-28 | 2020-01-21 | 横店集团东磁股份有限公司 | Preparation method of high-permeability scaly iron-silicon-aluminum magnetic powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114260455A (en) * | 2021-12-28 | 2022-04-01 | 苏州铂韬新材料科技有限公司 | Ball milling process of low-cost high-permeability wave-absorbing powder |
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Application publication date: 20210309 |