CN112207283A - Preparation method of flaky ferrosilicon aluminum powder with uniform particle size, micron-sized particles with large diameter-thickness ratio and particle morphology - Google Patents
Preparation method of flaky ferrosilicon aluminum powder with uniform particle size, micron-sized particles with large diameter-thickness ratio and particle morphology Download PDFInfo
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- 239000002245 particle Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910000519 Ferrosilicon Inorganic materials 0.000 title description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title description 8
- 239000000843 powder Substances 0.000 claims abstract description 93
- -1 iron-silicon-aluminum Chemical compound 0.000 claims abstract description 54
- 238000000498 ball milling Methods 0.000 claims abstract description 33
- 229910052751 metal Inorganic materials 0.000 claims abstract description 27
- 239000002184 metal Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- 229910000838 Al alloy Inorganic materials 0.000 claims description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 238000000889 atomisation Methods 0.000 claims description 24
- 238000000137 annealing Methods 0.000 claims description 20
- 238000005507 spraying Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910045601 alloy Inorganic materials 0.000 claims description 11
- 239000000956 alloy Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical group CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- RZRNAYUHWVFMIP-KTKRTIGZSA-N 1-oleoylglycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-KTKRTIGZSA-N 0.000 claims description 4
- 150000001408 amides Chemical class 0.000 claims description 4
- 229940075529 glyceryl stearate Drugs 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000007921 spray Substances 0.000 claims 1
- 230000035699 permeability Effects 0.000 abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910000702 sendust Inorganic materials 0.000 description 17
- 239000004902 Softening Agent Substances 0.000 description 10
- 229910002796 Si–Al Inorganic materials 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- PHYFQTYBJUILEZ-UHFFFAOYSA-N Trioleoylglycerol Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(OC(=O)CCCCCCCC=CCCCCCCCC)COC(=O)CCCCCCCC=CCCCCCCCC PHYFQTYBJUILEZ-UHFFFAOYSA-N 0.000 description 3
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- 238000004321 preservation Methods 0.000 description 3
- 238000003892 spreading Methods 0.000 description 3
- 230000007480 spreading Effects 0.000 description 3
- DCXXMTOCNZCJGO-UHFFFAOYSA-N Glycerol trioctadecanoate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 2
- 238000009689 gas atomisation Methods 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000009826 distribution Methods 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
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- 230000004907 flux Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920002545 silicone oil Polymers 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
- C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/008—Heat treatment of ferrous alloys containing Si
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
本发明公开了一种粒径均一的微米级大径厚比颗粒形貌片状的铁硅铝粉的制备方法，属于超细金属粉体制备技术领域。用本方法制备获得的片状铁硅铝粉，成片率高，厚度在1‑2μm之间，粒径大小均一，径厚比约为30‑38:1，具有良好的软磁性能。该方法通过在球磨前对铁硅铝粉料进行表面软化，在保证其磁性能的前提下，可以很大程度上提高铁硅铝粉料片化率。径厚比大的片状铁硅铝粉可进一步减少片状粉制成磁环内部气隙，同时，片状铁硅铝粉的形貌有利减少高频下的涡流，可以保证制成品在高频下仍具有较高的磁导率和较低损耗。
The invention discloses a preparation method of flake-shaped iron-silicon-aluminum powder with a uniform particle size and a large diameter-to-thickness ratio of particle shape, belonging to the technical field of ultrafine metal powder preparation. The flake iron-silicon-alumina powder prepared by the method has a high flake rate, a thickness of 1-2 μm, a uniform particle size, a diameter-to-thickness ratio of about 30-38:1, and good soft magnetic properties. The method can greatly improve the flake rate of the iron-silicon-aluminum powder by softening the surface of the iron-silicon-aluminum powder before ball milling, on the premise of ensuring its magnetic properties. The flake iron-silicon-aluminum powder with a large diameter-to-thickness ratio can further reduce the air gap inside the magnetic ring made of flake-like powder. It still has high permeability and low loss at high frequency.
Description
Technical Field
The invention belongs to the technical field of superfine metal powder preparation, and particularly relates to a preparation method of micron-sized large-diameter-thickness-ratio flaky ferrosilicon aluminum powder with high sheet forming rate and uniform particle size.
Background
Iron-silicon-aluminum alloys, also known as Sendust alloys, were first developed in 1932 in japan. The saturated magnetostriction coefficient and the magnetocrystalline anisotropy constant of the soft magnetic alloy of Fe-9.6% Si-5.4% Al are almost zero at the same time, so that the iron-silicon-aluminum alloy has high magnetic conductivity and low coercive force, the maximum magnetic conductivity can reach 120000, and the saturated magnetic flux density can reach 1.05T. And has high resistivity and low cost, and is an ideal material for magnetic head cores. However, the magnetic performance of the Fe-Si-Al alloy is sensitive to fluctuation of components, and the Fe-Si-Al alloy has high brittleness and poor processing performance.
Since the advent of sendust, research into sendust has been increasingly conducted, and the field of sendust applications, such as uninterruptible power supplies and high frequency filters, has been expanding. However, most of the sendust powder used for production and processing is prepared by an atomization method or a crushing method. The shape of the alloy powder is spherical or irregular, so that the contact area between the powder is small, and the requirements of the wave-absorbing material cannot be met. And because the skin effect exists when the metal micropowder receives the electromagnetic wave, the particle can not be too large, otherwise, the reflection of the electromagnetic wave can be rapidly increased. Therefore, the spherical or irregular powder is processed into a sheet shape by changing the shape of the powder, so that the effective magnetic conductivity and the resistivity can be improved by utilizing the shape anisotropy, and the eddy current loss can be effectively reduced when the thickness is smaller than the skin depth. Therefore, in order to expand the application field of iron-silicon-aluminum alloy development, the research on the preparation method of the micron-sized large-diameter-thickness-ratio flaky iron-silicon-aluminum powder with high sheet forming rate and uniform particle size has important significance.
Disclosure of Invention
In order to overcome the technical defects that the ferrosilicon aluminum alloy is hard and brittle, is easy to break and break in the ball milling process and is difficult to form flaky appearance, the invention provides a preparation method of micron-sized flaky ferrosilicon aluminum powder with large diameter-thickness ratio and uniform particle size.
The preparation operation steps of the flaky ferrosilicon aluminum powder with uniform particle size, micron-sized large diameter-thickness ratio and particle morphology are as follows:
(1) cleaning the iron-silicon-aluminum alloy powder with acetone, drying, uniformly spreading on a screen, uniformly spraying a metal softening agent solution on the iron-silicon-aluminum powder with atomization equipment, wherein the atomization spraying time interval is 10-60min, and the atomization frequency is 3-8 times; the single atomization spraying amount is 5% -18% of the amount of the alloy powder;
(2) after the metal softener is sprayed for 20-60min for the last time, putting the iron-silicon-aluminum powder into an annealing furnace, annealing under the protection of nitrogen, wherein the annealing temperature is 400-500 ℃, and the heat preservation time is 3 h;
(3) ultrasonically dispersing the annealed iron-silicon-aluminum alloy powder by using ethanol as a medium;
(4) performing primary ball milling, namely adding 2-5 parts of hard amide by taking ethylene glycol as a ball milling medium, wherein the ball-material ratio is 5-16:1, and the ball milling time is 3-6 h; taking out the iron-silicon-aluminum alloy powder, washing with acetone, and drying in an oven;
(5) soaking the iron-silicon-aluminum powder obtained in the step (4) in a metal softener solution for 2-12 hours at the soaking temperature of 50-80 ℃, taking out and drying;
(6) performing secondary ball milling, namely taking 100 parts of the iron-silicon-aluminum powder obtained in the step (5), 1-2 parts of glyceryl oleate and 50-100 parts of ethanol, taking ethylene glycol as a ball milling medium, wherein the ball-material ratio is 8-20:1, and the ball milling time is 6-18 h;
(7) and (3) ultrasonically cleaning the powder obtained in the step (6) by using acetone, drying in vacuum, and annealing in vacuum at the annealing temperature of 700-800 ℃ for 2-3h to obtain the flaky iron-silicon-aluminum alloy powder with uniform particle size and the diameter-thickness ratio of 30-38: 1.
The technical scheme for further limiting is as follows:
in the step (1) or the step (5), the metal softener is glyceryl stearate or glyceryl stearate and polydimethylsiloxane oil according to a volume ratio of 2:1, mixing the mixture.
In the step (1), the atomizing equipment is a small-sized electric sprayer.
In the step (1), the first metal softener is sprayed on the surface of the sendust powder through an atomization device, the atomization spraying time interval is 10-60min, the atomization frequency is 3-8 times, and the single atomization spraying amount is 5% -18% of the alloy powder amount.
In the step (5), the soaking time for the second softening is 2-12h, and the soaking temperature is 50-80 ℃.
The beneficial technical effects of the invention are embodied in the following aspects:
1. according to the invention, before ball milling, the metal softener is added to the iron-silicon-aluminum alloy powder in an atomization spraying manner before primary ball milling, so that the hard brittleness of the powder is improved, and the hardness of the powder is further reduced and the hard brittleness of the iron-silicon-aluminum alloy powder is improved through subsequent annealing. And the powder is soaked in the metal softener before the secondary ball milling, so that the hardness and brittleness of the powder are reduced for the second time, and partial internal stress is released. The problems of low sheet forming rate and small diameter-thickness ratio caused by particle breakage due to overhigh external energy in the ball milling process of the sendust are effectively avoided.
2. The iron-silicon-aluminum powder prepared by the invention has flaky particles with uniform particle size and larger diameter-thickness ratio of 30-38: 1. As shown by comparing fig. 1 and fig. 2: after ball milling, the shape of the iron-silicon-aluminum powder is changed, the original irregular shape is changed into a sheet shape, and the thickness of the sheet is about 1 mu m. And the metal softening agent can be removed by high-temperature annealing, so that the finally obtained ferrum-silicon-aluminum is free from pollution. Compared with the traditional gas atomization sendust and broken sendust, after the gas atomization sendust and the broken sendust are pressed and formed, the flaky sendust particles are arranged layer by layer, air gaps in a magnetic ring made of the powder can be effectively reduced, and the density is improved. The sheet Fe-Si-Al with large diameter-thickness ratio can further reduce the air gap inside the magnetic ring made of the powder. Meanwhile, the shape of the sheet sendust is favorable for reducing eddy current at high frequency, and can ensure that a magnetic ring made of the powder still has higher magnetic conductivity and lower loss at high frequency.
TABLE 1
| Material | Saturation magnetization | Particle size |
| Raw powder | 1.07T | 60.22μm |
| Flaky powder | 1.28T | 32.79μm |
TABLE 2
| Material | Magnetic permeability (100 kHz) | Loss (100 kHz/100 mT) | Density of |
| Raw powder | 58 | 489.67 mw/cm3 | 5.58 g/cm3 |
| Flaky powder | 70 | 376.54 mw/cm3 | 5.89 g/cm3 |
From table 1, it can be seen that the saturation magnetization of the flaky ferrosilicon aluminum powder prepared by the present invention is increased from 1.07T to 1.28T by changing the shape anisotropy of the powder, which is significantly improved. Secondly, due to the addition of the metal softening agent, the particle size of the powder is reduced from 60.22 mu m to 32.79 mu m through short-time ball milling, and the particle size distribution of the powder is concentrated. The ratio of the particle size to the thickness of the powder is about 32: 1.
The sheet sendust powder and the raw powder prepared by the invention are prepared into a test magnetic ring for testing the magnetic performance. As can be seen from Table 2, the sheet sendust utilizes shape anisotropy to reduce the air gap inside the magnetic ring and increase the density, so that the magnetic permeability is increased from 58 to 70. In addition, the sheet sendust powder prepared by the invention has the thickness of about 1 μm, higher resistance and smaller skin depth, so the loss is reduced from 489.67 mw/cm3 to 376.54 mw/cm3 in high frequency compared with the original powder. From the above data, it is understood that the sheet sendust powder having excellent magnetic energy can be prepared by the present invention.
Drawings
FIG. 1 is an SEM topography of the Fe-Si-Al alloy powder before ball milling.
FIG. 2 is an SEM topography of the flaky ferrosilicon aluminum alloy powder obtained in example 1.
Detailed Description
The present invention will be described with reference to specific examples.
Example 1
The specific operation steps for preparing the micron-sized flaky ferrosilicon aluminum powder with large diameter-thickness ratio and uniform particle size are as follows:
(1) washing 500g of crushed iron-silicon-aluminum alloy powder with the particle size of 50-80 microns by using acetone, drying, uniformly spreading on a screen, wherein the metal softening agent is stearin, uniformly spraying the metal softening agent on the iron-silicon-aluminum powder by using an atomizing device, the atomizing device is a small electric sprayer, the atomizing spraying time interval is 15min, and the atomizing frequency is 4 times; the single atomization spraying amount is 6% of the amount of the alloy powder.
(2) And 30min after the metal softener solution is sprayed for the last time, putting the iron-silicon-aluminum powder into an annealing furnace, annealing under the protection of nitrogen, wherein the annealing temperature is 400 ℃, and the heat preservation time is 3 h.
(3) Ultrasonically dispersing the annealed iron-silicon-aluminum alloy powder by using ethanol as a medium; ultrasonic power 360W and time 15 min.
(4) Performing primary ball milling, namely taking ethylene glycol as a ball milling medium, taking 400g of iron-silicon-aluminum alloy powder, 10g of hard amide and 200g of ethylene glycol, wherein the ball-material ratio is 8:1, and the ball milling time is 3 hours; taking out the iron-silicon-aluminum alloy powder, washing with acetone, and drying in an oven.
(5) And (3) soaking the iron-silicon-aluminum powder obtained in the step (4) in a metal softening agent for 3 hours, wherein the dosage of the metal softening agent is 20% of the powder, the soaking temperature is 50 ℃, and taking out and drying.
(6) And (3) performing secondary ball milling, namely taking 350g of the iron-silicon-aluminum powder obtained in the step (5), 3g of glyceryl oleate and 300g of ethanol, and taking ethylene glycol as a ball milling medium, wherein the ball-material ratio is 8:1, and the ball milling time is 6 hours.
(7) And (3) ultrasonically cleaning the powder obtained in the step (6) by using acetone, carrying out vacuum drying at the ultrasonic power of 360W for 10min, and carrying out vacuum annealing at the annealing temperature of 700 ℃ for 2h to obtain the sheet iron-silicon-aluminum alloy powder with uniform particle size and the average diameter-thickness ratio of 38:1, wherein the thickness is 1-2 mu m as shown in figure 2.
Example 2:
the specific operation steps for preparing the micron-sized flaky ferrosilicon aluminum powder with large diameter-thickness ratio and uniform particle size are as follows:
(1) washing 500g of crushed iron-silicon-aluminum alloy powder with the particle size of 50-80 mu m by using acetone, drying, uniformly spreading on a screen, wherein the metal softener is prepared by mixing the following components in percentage by volume: 1, mixing stearin and polydimethyl silicone oil, uniformly spraying a metal softening agent on iron-silicon-aluminum powder by using atomization equipment, wherein the atomization equipment is a small electric sprayer, the atomization spraying time interval is 30min, and the atomization frequency is 3 times; the single atomization spraying amount is 10% of the amount of the alloy powder.
(2) And 30min after the metal softener solution is sprayed for the last time, putting the iron-silicon-aluminum powder into an annealing furnace, annealing under the protection of nitrogen, wherein the annealing temperature is 500 ℃, and the heat preservation time is 3 h.
(3) Ultrasonically dispersing the annealed iron-silicon-aluminum alloy powder by using ethanol as a medium; ultrasonic power 360W and time 15 min.
(4) Performing primary ball milling, namely taking ethylene glycol as a ball milling medium, taking 400g of iron-silicon-aluminum alloy powder, 15g of hard amide and 250g of ethylene glycol, wherein the ball-material ratio is 11:1, and the ball milling time is 4 hours; taking out the iron-silicon-aluminum alloy powder, washing with acetone, and drying in an oven.
(5) And (3) soaking the iron-silicon-aluminum powder obtained in the step (4) in a metal softening agent for 9 hours, wherein the dosage of the metal softening agent is 10% of the powder, the soaking temperature is 70 ℃, and taking out and drying.
(6) And (3) performing secondary ball milling, namely taking 350g of the iron-silicon-aluminum powder obtained in the step (5), 5g of glyceryl oleate and 300g of ethanol, and taking ethylene glycol as a ball milling medium, wherein the ball-material ratio is 15:1, and the ball milling time is 6 hours.
(7) And (3) ultrasonically cleaning the powder obtained in the step (6) by using acetone, carrying out ultrasonic power 360W for 10min, carrying out vacuum drying, carrying out vacuum annealing at the annealing temperature of 750 ℃ for 2.5h to obtain the sheet iron-silicon-aluminum alloy powder with uniform particle size and the average diameter-thickness ratio of 36:1, wherein the thickness is 1-1.5 mu m.
It will be understood by those skilled in the art that the foregoing is merely a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included within the scope of the present invention.
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| CN113936906A (en) * | 2021-09-30 | 2022-01-14 | 安徽瑞德磁电科技有限公司 | Sphericizing preparation method of broken iron-silicon-aluminum magnetic powder particles |
| CN116900322A (en) * | 2022-12-07 | 2023-10-20 | 绵阳西磁科技有限公司 | High-flattening Fe-Si-Al alloy wave-absorbing magnetic powder and preparation method thereof |
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