CN116288007A - Low-loss high-molding-strength Fe-Si-Al powder and preparation method and application thereof - Google Patents
Low-loss high-molding-strength Fe-Si-Al powder and preparation method and application thereof Download PDFInfo
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- 229910002796 Si–Al Inorganic materials 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000956 alloy Substances 0.000 claims abstract description 96
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- 238000010438 heat treatment Methods 0.000 claims abstract description 46
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- -1 iron-silicon-aluminum Chemical compound 0.000 claims abstract description 31
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- 238000000227 grinding Methods 0.000 claims abstract description 25
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- 239000001301 oxygen Substances 0.000 claims abstract description 21
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 33
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- 239000010949 copper Substances 0.000 claims description 28
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
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- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0637—Accessories therefor
- B22D11/0697—Accessories therefor for casting in a protected atmosphere
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/16—Controlling or regulating processes or operations
- B22D11/18—Controlling or regulating processes or operations for pouring
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/10—Handling in a vacuum
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
-
- 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
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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
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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
- B22F2009/045—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling
Abstract
The invention belongs to the technical field of soft magnetic materials, and particularly relates to iron-silicon-aluminum powder with low loss and high forming strength, and a preparation method and application thereof. Iron-silicon aluminum powder, wherein the oxygen content of the iron-silicon aluminum powder is less than 730ppm; the granularity of the Fe-Si-Al powder is more than or equal to 200 meshes, the granularity of 200 meshes is less than or equal to 15-30% of 300 meshes, the granularity of 300 meshes is less than or equal to 35-50% of 400 meshes, and the granularity is more than or equal to 25-40% of 400 meshes. The raw materials for preparing the Fe-Si-Al powder comprise 9.0 to 10.0 percent of Si, 5.0 to 6.0 percent of Al and 84 to 86 percent of Fe according to the weight percentage. The preparation method comprises the following steps: vacuum smelting the raw material components to obtain molten alloy, throwing the molten alloy into an alloy thin belt, crushing the alloy thin belt, grinding the alloy thin belt into powder, sieving and performing heat treatment to obtain the Fe-Si-Al powder. The Fe-Si-Al powder has the advantages of low loss and high molding strength, and can meet the low loss and special-shaped requirements of devices.
Description
Technical Field
The invention belongs to the technical field of soft magnetic materials, and particularly relates to iron-silicon-aluminum powder with low loss and high forming strength, and a preparation method and application thereof.
Background
The metal soft magnetic powder core is a soft magnetic composite material produced by mixing metal soft magnetic alloy powder with an insulating medium and adopting a powder metallurgy process. At present, the metal soft magnetic powder core is widely applied at home and abroad, and the metal soft magnetic powder core with mature production process has five series: iron powder core, ferrosilicon magnetic powder core, ferrosilicon aluminum magnetic powder core, ferronickel Molybdenum (MPP) magnetic powder core, and ferronickel (HF) magnetic powder core.
Sendust powder cores, commonly referred to as Sendust powder cores, are made from Sendust powder. The sendust core is somewhat more expensive than the iron powder core, but the losses are much lower than the iron powder core and the sendust core is smaller in size than the iron powder core. In addition, the iron-silicon-aluminum magnetic powder core has good performance at high temperature, the temperature rise is far lower than that of the iron powder core, and the iron-silicon-aluminum magnetic powder core can form a composite part with other capacitors, so that the iron-silicon-aluminum magnetic powder core has good temperature compensation effect. Meanwhile, the saturation magnetic induction intensity of the Fe-Si-Al powder core is about 1.05T, the magnetic conductivity range is 26-125 mu, the magnetostriction coefficient of Fe-Si-Al is close to zero, no noise is generated when the Fe-Si-Al powder core works at different frequencies, and the Fe-Si-Al powder core can be manufactured into a low-noise filter. Noble metals such as Ni and Mo are not contained in the Fe-Si-Al alloy raw material, the cost is lower than that of a high-flux magnetic powder core containing Ni and a Fe-Ni-Mo magnetic powder core, and the cost performance is high. Finally, the Fe-Si-Al material has great flexibility and can be used for manufacturing magnetic cores with various different shapes and oversized sizes.
Along with the development of electronic technology and new energy technology, electronic components develop to miniaturization, high performance and abnormal shape, and higher requirements are also put forward on the Fe-Si-Al material, at least the following requirements are met: (1) The Fe-Si-Al material has low loss so as to improve the magneto-electric conversion efficiency and reduce the energy loss; (2) The sendust material has higher molding strength, so that the sendust material has good molding performance under the abnormal shape of the sendust powder core, improves the yield, and can be designed into more complex components.
At present, the preparation method of the ferrosilicon aluminum powder mainly comprises an air atomization method and a mechanical method, the ferrosilicon aluminum powder prepared by the air atomization method is spherical, the preparation cost is high, the magnetic conductivity is low, the forming strength is low, and the magnetic powder core with the special-shaped complex structure is difficult to form. The traditional mechanical method is to melt raw materials into an iron-silicon-aluminum alloy ingot in a non-vacuum environment, and then mechanically crush and ball mill the iron-silicon-aluminum alloy ingot to obtain the iron-silicon-aluminum alloy powder.
Therefore, it is needed to provide a sendust powder with low loss and high forming strength, which can meet the low loss and special-shaped requirements of devices.
Disclosure of Invention
The present invention is directed to solving one or more of the problems of the prior art and providing at least one of a beneficial choice or creation of conditions. The invention provides the Fe-Si-Al powder which has the properties of low loss and high forming strength and can meet the low loss and abnormal requirements of devices.
The invention is characterized in that: the invention controls the oxygen content in the Fe-Si-Al powder to be less than 730ppm, prevents the alloy material from being oxidized, improves the performance of the material and reduces the loss. In addition, the granularity of the Fe-Si-Al powder is more than or equal to 200 meshes, the granularity of the Fe-Si-Al powder is less than or equal to 200 meshes and less than or equal to 300 meshes and is 15-30 percent, the granularity of the Fe-Si-Al powder is less than or equal to 300 meshes and is 35-50 percent, the granularity of the Fe-Si-Al powder is more than or equal to 400 meshes and is 25-40 percent, the granularity distribution of the Fe-Si-Al powder has the performance of low loss and high forming strength, and when the Fe-Si-Al powder is manufactured into a magnetic core, the magnetic core with low loss and high forming strength can be obtained, and the low loss and abnormal requirements of a device are met.
Accordingly, the first aspect of the present invention provides a low-loss, high-forming-strength iron-silicon-aluminum powder.
Specifically, the oxygen content of the Fe-Si-Al powder is less than 730ppm; the granularity of the Fe-Si-Al powder is more than or equal to 200 meshes, the granularity of 200 meshes is less than or equal to 15-30% of 300 meshes, the granularity of 300 meshes is less than or equal to 35-50% of 400 meshes, and the granularity is more than or equal to 25-40% of 400 meshes.
Preferably, the oxygen content of the Fe-Si-Al powder is less than 700ppm; the granularity of the Fe-Si-Al powder is more than or equal to 200 meshes, the granularity of 200 meshes is less than or equal to 20-30% of 300 meshes, the granularity of 300 meshes is less than or equal to 40-45% of 400 meshes, and the granularity is more than or equal to 30-40% of 400 meshes.
Specifically, when oxygen is contained in a high amount, the purity of the material is lowered and the material is easily oxidized, so that the performance of the material is lowered and the loss is increased.
Specifically, the granularity of the Fe-Si-Al powder affects the molding strength and loss of the finally prepared magnetic core, and the granularity distribution of the Fe-Si-Al powder needs to meet certain requirements. When the granularity of the Fe-Si-Al powder is more than or equal to 200 meshes, the granularity of the Fe-Si-Al powder is less than or equal to 200 meshes and less than 300 meshes and is 15-30 percent, the granularity of the Fe-Si-Al powder is less than or equal to 300 meshes and is 35-50 percent, the granularity of the Fe-Si-Al powder is more than or equal to 400 meshes and is 25-40 percent, the Fe-Si-Al powder has good low-loss and high-forming strength performance, and when the Fe-Si-Al powder is manufactured into a magnetic core, the magnetic core with low-loss and high-forming strength can be obtained, and the low-loss and special-shaped requirements of a device are met.
Preferably, the raw materials for preparing the Fe-Si-Al powder comprise 9.0-10.0% of Si, 5.0-6.0% of Al and 84-86% of Fe in percentage by weight.
Further preferably, the raw materials for preparing the Fe-Si-Al powder are 9.2% -9.8% of silicon, 5.2% -5.8% of aluminum and 84.5% -85.6% of iron in percentage by weight.
The second aspect of the invention provides a preparation method of low-loss high-molding-strength Fe-Si-Al powder.
Specifically, the preparation method comprises the following steps:
vacuum smelting the raw material components to obtain molten alloy steel, throwing the molten alloy steel into an alloy thin belt, crushing the alloy thin belt, grinding the alloy thin belt into powder by ring grinding, screening and carrying out heat treatment to obtain the ferrosilicon aluminum powder.
Specifically, by adopting vacuum melting, the increase of the oxygen content of each raw material of the Fe-Si-Al alloy molten steel in the process of melting the raw material into the Fe-Si-Al alloy molten steel can be strictly controlled, thereby ensuring that the Fe-Si-Al alloy molten steel with high purity is obtained, and further ensuring that the low-loss Fe-Si-Al powder is obtained from the source.
Preferably, the alloy molten steel is spun into an alloy thin strip by adopting a vacuum melt-spun, and the vacuum melting and the vacuum melt-spun adopt integrated equipment.
Specifically, the integrated equipment of vacuum melting and vacuum melt-spinning is adopted, an alloy steel ingot is not required to be prepared, the turnover of iron and silicon aluminum from the alloy steel liquid to the steel ingot can be reduced, the increase of oxygen content is prevented, and the purity of the alloy thin strip is ensured. Meanwhile, compared with the iron-silicon-aluminum alloy steel ingot obtained by the traditional casting method, the alloy thin strip prepared by the vacuum melt-spinning method has the advantages of high cooling speed, small segregation, fine grains, reduced hysteresis loss of the magnetic core and ensured low loss performance of iron-silicon-aluminum. In addition, the alloy thin strip is easier to mechanically crush, so that powder preparation is easier to carry out, the machining amount is reduced, the internal stress, grain dislocation and magnetic stage displacement difficulty of the material in the powder preparation process are reduced, the hysteresis loss of the magnetic core is further reduced, and the low-loss performance is ensured.
Specifically, the broken iron-silicon-aluminum alloy fragments are ground to a certain degree by adopting a ring grinding method, powder automatically flows out in gaps, excessive grinding of particles can be prevented, the forming strength of the magnetic core is improved, and the magnetic core with special shape and complex structure can be formed. And the vacuum melt-spinning and the annular grinding process are combined, so that the machining amplitude can be reduced, powder with proper granularity is easier to obtain after annular grinding, the powder preparation process is quick, the internal stress of the product is small, the internal stress of the powder generated by mechanical crushing can be well eliminated through lower heat treatment temperature and shorter heat treatment time, the magnetic performance of powder particles is released, the production cost can be saved, and the production efficiency is improved.
Preferably, each raw material component comprises pure iron, pure silicon and pure aluminum.
Preferably, the pure iron (wt%) is: fe is more than or equal to 99.9%, C is less than or equal to 0.003%, si is less than or equal to 0.03%, mn is less than or equal to 0.02%, P is less than or equal to 0.008%, S is less than or equal to 0.004%, O is less than or equal to 0.008%, and Cu is less than or equal to 0.02; the pure silicon (wt%) is: si is more than or equal to 99.7 percent, ca is less than or equal to 0.02 percent; the pure aluminum (wt%) is: al is more than or equal to 99.85 percent, cu is less than or equal to 0.01.
Specifically, the high-purity raw materials are adopted, so that the impurity content can be controlled at the source, high-purity Fe-Si-Al can be easily obtained, and low-loss Fe-Si-Al powder is further ensured to be obtained.
Preferably, the vacuum degree of the vacuum smelting is 8-55Pa.
Further preferably, the vacuum degree of the vacuum melting is 10-50Pa.
Preferably, during vacuum melt spinning, molten alloy steel is poured onto a rotating copper roller, the pouring temperature is 1480-1780 ℃, the rotating speed of the copper roller is 8-44m/s, and the copper roller is cooled by cooling water during pouring.
Further preferably, during vacuum melt-spinning, molten alloy steel is poured onto a rotating copper roller, the pouring temperature is 1580-1680 ℃, the rotating speed of the copper roller is 10-40m/s, and the copper roller is cooled by cooling water during pouring.
Preferably, the temperature of the cooling water is 0-30 ℃.
Further preferably, the temperature of the cooling water is 0-22 ℃.
Preferably, the vacuum melt-spinning is protected by inert gas.
Further preferably, the inert gas is selected from any one of 99.999% nitrogen and 99.999% argon.
Specifically, the high-purity inert gas is adopted for protection, and the purpose of protecting is mainly to reduce the increase of impurities, particularly the increase of oxygen content, in the process of vacuum melt-spinning as much as possible, so that the purity of the material is improved, the material is prevented from being oxidized, the material performance is improved, and the loss is reduced.
Preferably, the thickness of the alloy ribbon is 0.2mm-0.8mm.
Preferably, the alloy thin strip is crushed in a crusher to obtain Fe-Si-Al alloy fragments, and the diameters of the Fe-Si-Al alloy fragments are smaller than 10mm.
Preferably, placing the Fe-Si-Al alloy fragments into a ring mill for ring milling to prepare powder; the rotating speed of the ring mill is 450-850r/min; the nitrogen is introduced for protection during the grinding of the powder, and the flow rate of the nitrogen is 2-12m 3 /h。
Further preferably, the Fe-Si-Al alloy fragments are put into a ring mill for ring milling to prepare powder; the rotating speed of the ring mill is 500-800r/min; the nitrogen is introduced for protection during the grinding of the powder by the ring mill, and the flow of the nitrogen is 2-10m 3 /h。
Specifically, nitrogen is introduced, so as to reduce the increase of impurities, especially the increase of oxygen content, in the process of ring milling powder, thereby improving the purity of the material, preventing the material from being oxidized, improving the performance of the material and reducing the loss.
Preferably, the powder is placed in a sieving machine for sieving with 200 meshes to obtain the powder with the granularity of more than or equal to 200 meshes.
Preferably, the temperature of the heat treatment is 550-800 ℃, and the time of the heat treatment is 0.9-3.2h.
Further preferably, the temperature of the heat treatment is 600-750 ℃, and the time of the heat treatment is 1-3h.
Preferably, 99.999% of nitrogen is introduced as a protective atmosphere during the heat treatment, and the cooling condition of the heat treatment is water cooling, cooling to below 50 ℃ and discharging.
Preferably, the preparation method further comprises a batch mixing, wherein the batch mixing is carried out in a mixer, and the mixing time of the batch mixing is 0.4-1.1h.
Further preferably, the mixing time of the batch is 0.5 to 1h.
The third aspect of the invention provides application of the ferro-silicon aluminum powder in the fields of electrons and new energy.
Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:
(1) The invention prevents the alloy material from being oxidized by the oxygen content in the Fe-Si-Al powder being less than 730ppm, improves the performance of the material and reduces the loss. In addition, the granularity of the Fe-Si-Al powder is more than or equal to 200 meshes, the granularity of 200 meshes is less than or equal to 15-30% of 300 meshes, the granularity of 300 meshes is less than or equal to 35-50% of 400 meshes, the granularity of 400 meshes is more than or equal to 25-40%, and the Fe-Si-Al powder with the granularity distribution has the properties of low loss and high forming strength, thereby meeting the low loss and special-shaped requirements of devices.
(2) The Fe-Si-Al powder prepared by combining the vacuum melting, the vacuum melt-spinning and the ring grinding method has the characteristics of low loss and high forming strength, and can meet the low loss and special-shaped requirements of devices. The increase of oxygen content in the smelting process can be effectively controlled by vacuum smelting, and the Fe-Si-Al alloy molten steel with high purity is obtained. Compared with an alloy steel ingot obtained by a casting method, the alloy thin strip prepared by the vacuum melt-spinning method has the advantages of high cooling speed, small segregation, fine grains, reduced hysteresis loss of a magnetic core and ensured low loss performance of Fe, si and Al; the powder preparation by the annular grinding method can prevent particles from being excessively ground, improves the forming strength of the magnetic core, and can form the magnetic core with special shape and complex structure; the vacuum melt-spun combines with the ring grinding method, because the alloy thin strip is thinner, the thickness is only 0.2-0.8mm, the powder process can be fast, the mechanical processing degree is low, the internal stress of the material is small, and meanwhile, the obtained powder particle size is thinner, so that the eddy current loss of the magnetic core is low, and the magnetic core loss can be reduced.
(3) The invention introduces inert gas in the vacuum melt-spinning, ring milling powder preparation and heat treatment processes, can effectively improve the purity of the material, prevent the material from being oxidized, further improve the material performance and reduce the loss.
(4) The powder obtained by the invention has small internal stress, so that the internal stress of the material can be better eliminated by adopting lower heat treatment temperature and shorter heat treatment time in the follow-up process, the resources can be saved, and the production efficiency can be improved.
Drawings
FIG. 1 is an SEM micrograph of powdered Fe-Si-Al powder prepared according to example 2 of the present invention;
fig. 2 is an SEM microstructure of the ferro-silicon aluminum powder prepared in comparative example 2 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples will be presented. It should be noted that the following examples do not limit the scope of the invention.
The starting materials, reagents or apparatus used in the following examples are all available from conventional commercial sources or may be obtained by methods known in the art unless otherwise specified.
Example 1
The preparation method of the Fe-Al-Si powder comprises the following steps:
(1) Preparing materials: weighing and preparing pure iron, pure silicon and pure aluminum respectively, wherein the weight percentages of the raw materials are as follows: 9.4% of silicon, 5.6% of aluminum and 85% of iron. Wherein, the purity of the raw materials is as follows: pure iron (wt%): fe is more than or equal to 99.9%, C is less than or equal to 0.003%, si is less than or equal to 0.03%, mn is less than or equal to 0.02%, P is less than or equal to 0.008%, S is less than or equal to 0.004%, O is less than or equal to 0.008%, and Cu is less than or equal to 0.02; pure silicon (wt%): si is more than or equal to 99.7 percent, ca is less than or equal to 0.02 percent; pure aluminum (wt%): al is more than or equal to 99.85 percent, cu is less than or equal to 0.01;
(2) Vacuum smelting and vacuum melt-spinning: putting the raw materials into an alloy furnace of vacuum melting and vacuum melt-spinning integrated equipment, vacuumizing to 50Pa, starting an alloy furnace power supply, and melting the raw materials into Fe-Si-Al alloy molten steel. Introducing 99.999% high-purity nitrogen into the alloy furnace, pouring the alloy molten steel onto a copper roller with the rotating speed of 40m/s when the temperature of the molten steel reaches 1600 ℃, cooling the copper roller by using cooling water with the temperature of 20 ℃ when pouring, rapidly cooling the alloy molten steel on the copper roller with low temperature and good heat conductivity, and throwing out the alloy molten steel under the action of centrifugal force to prepare an Fe-Si-Al alloy thin belt, wherein the thickness of the alloy thin belt is 0.2-0.5 mm;
(3) Crushing the alloy thin strip: crushing the thin strip of the Fe-Si-Al alloy in a universal crusher to obtain Fe-Si-Al alloy fragments, wherein the diameters of the Fe-Si-Al alloy fragments are mainly distributed between 2mm and 8mm;
(4) And (5) grinding into powder by ring grinding: filling thin fragments of Fe-Si-Al alloy into a blanking hopper of a ring mill, and introducing protective nitrogen with the flow rate of 8m 3 Starting a ring mill, wherein the rotating speed of the ring mill is 700r/min, starting a feeder, and ring-grinding the Fe-Si-Al alloy fragments into powder;
(5) And (3) screening: screening the powder obtained in the step (4) by adopting a screening machine to obtain 200 meshes, and taking the powder with the granularity of more than or equal to 200 meshes;
(6) And (3) heat treatment: placing the powder obtained in the step (5) into a boat box, carrying out annealing heat treatment in a mesh belt heat treatment furnace, wherein the heat treatment temperature is 750 ℃, the heat treatment time is 2.5h, 99.999% of high-purity nitrogen is introduced as a protective atmosphere, the cooling condition is water cooling, cooling to 40 ℃, and discharging the powder out of the furnace;
(7) Batch mixing: and (3) placing the powder subjected to heat treatment into a V-shaped mixer, closing a valve of a feed inlet, and mixing for 30min to obtain the iron-silicon-aluminum powder.
Example 2
The preparation method of the Fe-Al-Si powder comprises the following steps:
(1) Preparing materials: weighing and preparing pure iron, pure silicon and pure aluminum respectively, wherein the weight percentages of the raw materials are as follows: 9.4% of silicon, 5.6% of aluminum and the balance of Fe. Wherein, the purity of the raw materials is as follows: pure iron (wt%): fe is more than or equal to 99.9%, C is less than or equal to 0.003%, si is less than or equal to 0.03%, mn is less than or equal to 0.02%, P is less than or equal to 0.008%, S is less than or equal to 0.004%, O is less than or equal to 0.008%, and Cu is less than or equal to 0.02; pure silicon (wt%): si is more than or equal to 99.7 percent, ca is less than or equal to 0.02 percent; pure aluminum (wt%): al is more than or equal to 99.85 percent, cu is less than or equal to 0.01;
(2) Vacuum smelting and vacuum melt-spinning: putting the raw materials into an alloy furnace of vacuum melting and vacuum melt-spinning integrated equipment, vacuumizing to 30Pa, starting an alloy furnace power supply, and melting the raw materials into Fe-Si-Al alloy molten steel; introducing 99.999% high-purity nitrogen into the alloy furnace, pouring the alloy molten steel onto a copper roller with the rotating speed of 30m/s when the temperature of the alloy molten steel reaches 1620 ℃, cooling the copper roller by using cooling water with the temperature of 22 ℃ when pouring, rapidly cooling the alloy molten steel on the copper roller with low temperature and good heat conductivity, and throwing out the alloy molten steel under the action of centrifugal force to prepare an Fe-Si-Al alloy thin belt, wherein the thickness of the alloy thin belt is 0.3-0.6 mm;
(3) Crushing the alloy thin strip: crushing the thin strip of the Fe-Si-Al alloy in a universal crusher to obtain Fe-Si-Al alloy fragments, wherein the diameters of the Fe-Si-Al alloy fragments are mainly distributed between 2mm and 8mm;
(4) And (5) grinding into powder by ring grinding: filling the Fe-Si-Al alloy fragments into a discharge hopper of a ring mill, and introducing protective nitrogen with the flow rate of 6m 3 /h; starting a ring mill, wherein the rotating speed of the ring mill is 600r/min, starting a feeder, and ring-grinding the Fe-Si-Al alloy fragments into powder;
(5) And (3) screening: screening the powder obtained in the step (4) by adopting a screening machine to obtain 200 meshes, and taking the powder with the granularity of more than or equal to 200 meshes;
(6) And (3) heat treatment: placing the powder obtained in the step (5) into a boat box, and performing annealing heat treatment in a mesh belt heat treatment furnace; the temperature of the heat treatment is 700 ℃, the heat treatment time is 3 hours, 99.999 percent of high-purity nitrogen is introduced as protective atmosphere, the cooling condition is water cooling, the temperature is cooled to 30 ℃, and the powder is discharged from the furnace;
(7) Batch mixing: and (3) placing the powder subjected to heat treatment into a V-shaped mixer, closing a valve of a feed inlet, and mixing for 40min to obtain the iron-silicon-aluminum powder.
Example 3
The preparation method of the Fe-Al-Si powder comprises the following steps:
(1) Preparing materials: weighing and preparing pure iron, pure silicon and pure aluminum respectively, wherein the weight percentages of the raw materials are as follows: 9.4% of silicon, 5.6% of aluminum and the balance of Fe. Wherein, the purity of the raw materials is as follows: pure iron (wt%): fe is more than or equal to 99.9%, C is less than or equal to 0.003%, si is less than or equal to 0.03%, mn is less than or equal to 0.02%, P is less than or equal to 0.008%, S is less than or equal to 0.004%, O is less than or equal to 0.008%, and Cu is less than or equal to 0.02; pure silicon (wt%): si is more than or equal to 99.7 percent, ca is less than or equal to 0.02 percent; pure aluminum (wt%): al is more than or equal to 99.85 percent, cu is less than or equal to 0.01;
(2) Vacuum smelting and vacuum melt-spinning: putting the raw materials into an alloy furnace of vacuum melting and vacuum melt-spinning integrated equipment, vacuumizing to 20Pa, starting an alloy furnace power supply, and melting the raw materials into Fe-Si-Al alloy molten steel; introducing 99.999% high-purity nitrogen into the alloy furnace, pouring the alloy molten steel onto a copper roller with the rotating speed of 20m/s when the temperature of the alloy molten steel reaches 1630 ℃, cooling the copper roller by cooling water with the temperature of 25 ℃ when pouring, rapidly cooling the alloy molten steel on the copper roller with low temperature and good heat conductivity, and throwing out the alloy molten steel under the action of centrifugal force to prepare an Fe-Si-Al alloy thin belt, wherein the thickness of the alloy thin belt is 0.5-0.8 mm;
(3) Crushing the alloy thin strip: crushing the thin strip of the Fe-Si-Al alloy in a universal crusher to obtain Fe-Si-Al alloy fragments, wherein the diameters of the thin alloy fragments are mainly distributed between 2mm and 8mm;
(4) And (5) grinding into powder by ring grinding: filling the Fe-Si-Al alloy fragments into a discharge hopper of a ring mill, and introducing protective nitrogen with the flow rate of 10m 3 /h; starting a ring mill, wherein the rotating speed of the ring mill is 800r/min, starting a feeder, and ring-grinding the Fe-Si-Al alloy fragments into powder;
(5) And (3) screening: screening the powder obtained in the step (4) by adopting a screening machine to obtain 200 meshes, and taking the powder with the granularity of more than or equal to 200 meshes;
(6) And (3) heat treatment: placing the powder obtained in the step (5) into a boat box, and performing annealing heat treatment in a mesh belt heat treatment furnace; the heat treatment temperature is 720 ℃, the heat treatment time is 2 hours, 99.999 percent of high-purity nitrogen is introduced as protective atmosphere, the cooling condition is water cooling, the temperature is cooled to 25 ℃, and the powder is discharged from the furnace;
(7) Batch mixing: and (3) placing the powder subjected to heat treatment into a V-shaped mixer, closing a valve of a feed inlet, and mixing for 45min to obtain the iron-silicon-aluminum powder.
Comparative example 1
The preparation method of the Fe-Al-Si powder comprises the following steps:
(1) Preparing materials: weighing and preparing pure iron, pure silicon and pure aluminum respectively, wherein the weight percentages of the raw materials are as follows: 9.4% of silicon, 5.6% of aluminum and the balance of Fe. Wherein, the purity of the raw materials is as follows: pure iron (wt%): fe is more than or equal to 99.9%, C is less than or equal to 0.003%, si is less than or equal to 0.03%, mn is less than or equal to 0.02%, P is less than or equal to 0.008%, S is less than or equal to 0.004%, O is less than or equal to 0.008%, and Cu is less than or equal to 0.02; pure silicon (wt%): si is more than or equal to 99.7 percent, ca is less than or equal to 0.02 percent; pure aluminum (wt%): al is more than or equal to 99.85 percent, cu is less than or equal to 0.01;
(2) Smelting and casting: and (3) putting the raw materials into an alloy intermediate frequency furnace, starting a power supply of the intermediate frequency furnace, melting the raw materials into Fe-Si-Al alloy molten steel in an atmospheric environment, pouring the alloy molten steel into a mould, and pouring to obtain the Fe-Si-Al alloy steel ingot.
(3) Crushing alloy steel ingots: mechanically crushing the iron-silicon-aluminum alloy steel ingot into iron-silicon-aluminum granules;
(4) Ball milling and pulverizing: putting the Fe-Si-Al granules into a ball mill protected by nitrogen, and ball milling to obtain powder;
(5) And (3) screening: screening the powder obtained in the step (4) by adopting a screening machine to obtain 200 meshes, and taking the powder with the granularity of more than or equal to 200 meshes;
(6) And (3) heat treatment: placing the powder obtained in the step (5) into a boat box, and performing annealing heat treatment in a mesh belt heat treatment furnace; the temperature of the heat treatment is 750 ℃, the heat treatment time is 3 hours, 99.999 percent of high-purity nitrogen is introduced as protective atmosphere, the cooling condition is water cooling, the temperature is cooled to 30 ℃, and the powder is discharged from the furnace;
(7) Batch mixing: and (3) placing the powder subjected to heat treatment into a V-shaped mixer, closing a valve of a feed inlet, and mixing for 30min to obtain the iron-silicon-aluminum powder.
Comparative example 2
The preparation method of the Fe-Al-Si powder comprises the following steps:
(1) Preparing materials: weighing and preparing pure iron, pure silicon and pure aluminum respectively, wherein the weight percentages of the raw materials are as follows: 9.4% of silicon, 5.6% of aluminum and the balance of Fe. Wherein, the purity of the raw materials is as follows: pure iron (wt%): fe is more than or equal to 99.9%, C is less than or equal to 0.003%, si is less than or equal to 0.03%, mn is less than or equal to 0.02%, P is less than or equal to 0.008%, S is less than or equal to 0.004%, O is less than or equal to 0.008%, and Cu is less than or equal to 0.02; pure silicon (wt%): si is more than or equal to 99.7 percent, ca is less than or equal to 0.02 percent; pure aluminum (wt%): al is more than or equal to 99.85 percent, cu is less than or equal to 0.01;
(2) Vacuum smelting and vacuum melt-spinning: putting the raw materials into an alloy furnace of vacuum melting and vacuum melt-spinning integrated equipment, vacuumizing to 30Pa, starting an alloy furnace power supply, and melting the raw materials into Fe-Si-Al alloy molten steel; introducing 99.999% high-purity nitrogen into the alloy furnace, pouring the alloy molten steel onto a copper roller with the rotating speed of 30m/s when the temperature of the alloy molten steel reaches 1620 ℃, cooling the copper roller by using cooling water with the temperature of 22 ℃ when pouring, rapidly cooling the alloy molten steel on the copper roller with low temperature and good heat conductivity, and throwing out the alloy molten steel under the action of centrifugal force to prepare an Fe-Si-Al alloy thin belt, wherein the thickness of the alloy thin belt is 0.3-0.6 mm;
(3) Crushing the alloy thin strip: crushing the thin strip of the Fe-Si-Al alloy in a universal crusher to obtain Fe-Si-Al alloy fragments, wherein the diameters of the Fe-Si-Al alloy fragments are mainly distributed between 2mm and 8mm;
(4) Ball milling and pulverizing: putting the thin iron-silicon-aluminum fragments into a ball mill, and ball-grinding the thin iron-silicon-aluminum fragments into iron-silicon-aluminum powder under the protection of nitrogen;
(5) And (3) screening: screening the powder obtained in the step (4) by adopting a screening machine to obtain 200 meshes, and taking the powder with the granularity of more than or equal to 200 meshes;
(6) And (3) heat treatment: placing the powder obtained in the step (5) into a boat box, and performing annealing heat treatment in a mesh belt heat treatment furnace; the heat treatment temperature is 700 ℃, the heat treatment time is 3 hours, 99.999 percent of high-purity nitrogen is introduced as protective atmosphere, the cooling condition is water cooling, the temperature is cooled to 30 ℃, and the powder is discharged from the furnace;
(7) Batch mixing: and (3) placing the powder subjected to heat treatment into a V-shaped mixer, closing a valve of a feed inlet, and mixing for 40min to obtain the iron-silicon-aluminum powder.
Performance testing
SEM test of ferrosilicon aluminum powder: SEM analysis was performed on the Fe-Si-Al powder prepared in example 2 and comparative example 2, as shown in FIGS. 1-2. Comparing fig. 1 and 2, it can be seen that the powder of example 2 using vacuum belt and ring mill is finer and more uniform in particle size than the powder of comparative example 2 using vacuum belt and ball mill.
Oxygen content test: taking the mixed iron-silicon-aluminum powder, and measuring the oxygen content of the iron-silicon-aluminum powder by using an ONH-3000 oxygen-nitrogen-hydrogen tester produced by the steel Nake company. Specifically, iron silicon aluminum powder is placed in a crucible, and under the protection of inert atmosphere, a pulse is adopted to heat and melt a sample, and carbon element is reacted with oxygen element to generate CO because the crucible contains the carbon element 2 Measurement of CO produced by infrared absorption 2 Further, the oxygen content in the ferrosilicon aluminum powder is converted.
Particle size testing: taking the iron-silicon-aluminum powder after the batch mixing, adopting a slapping type standard vibration sieve machine to carry out the granularity test of the iron-silicon-aluminum powder, putting screens with different meshes on the slapping type standard vibration sieve machine, and measuring the powder weight of each layer of screen.
The oxygen content and the particle size distribution of the ferrosilicon aluminum powder are shown in table 1.
Magnetic core performance test:
(1) And (3) testing the molding strength of the magnetic core: and (3) insulating and coating the mixed ferro-silicon aluminum powder into powder with magnetic permeability mu 60, and pressing and forming the powder to prepare a 106-specification magnetic core with the outer diameter of 26.90mm, the inner diameter of 14.70mm and the height of 11.15mm, and measuring the forming strength of the magnetic core by adopting a pointer type pulling and pressing force measuring instrument. Examples 1-3, comparative examples 1-2 each had 5 test samples, and the average was taken and the test results are shown in Table 2.
(2) Magnetic core magneto-electric performance test: sintering the prepared magnetic core at 700 ℃ for 1.5 hours, and winding 50Ts by adopting copper wires with the thickness of 0.8mm after sintering. The inductance and Q value of the magnetic core are measured by a TH2829C instrument, and the loss of the magnetic core is measured by a BST-2A power consumption tester. Examples 1-3, comparative examples 1-2 each had 5 test samples, and the average was taken and the test results are shown in Table 2.
TABLE 1
TABLE 2
As can be seen from Table 1, the oxygen content of the Fe-Si-Al powder in the examples 1-3 of the invention is less than 700ppm, and the oxygen content of the Fe-Si-Al powder in the comparative examples 1-2 is more than 700ppm, which indicates that the Fe-Si-Al powder prepared by the invention has low oxygen content, the material is not easy to oxidize, the material performance can be improved, and the loss is further reduced.
As can be seen from Table 1, the particle size of the Fe-Si-Al powder in the examples 1-3 of the present invention is not less than 200 meshes, and in the examples 1-3, the particle size of not less than 200 meshes is less than 300 meshes and is respectively 23.2%, 24.1% and 23.7%, the particle size of not less than 300 meshes and is less than 400 meshes and is respectively 41.3%, 41.6% and 38.9%, and the particle size of not less than 400 meshes and is respectively 35.5%, 34.2% and 37.3%. In comparative examples 1 to 2, the particle size of 200 meshes or less was 47.6% and 35.8% respectively, the particle size of 300 meshes or less was 27.7% and 34.6% respectively, the particle size of 300 meshes or less was 400 meshes or more was 24.7% and 29.1% respectively. In examples 1-3, the proportion of 300 mesh.ltoreq.particle size <400 mesh was the largest, whereas in comparative documents 1-2, the proportion of 200 mesh.ltoreq.particle size <300 mesh was the largest.
As can be seen from Table 2, the molding strength and Q value of the magnetic core prepared from the sendust powder of the embodiment 1-3 of the present invention are higher than those of the comparative example 1-2, and the magnetic core loss is significantly lower than those of the comparative example 1-2, which indicates that the sendust powder of the present invention has the properties of low loss and high molding strength, and can meet the requirements of low loss and special-shaped devices.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. The Fe-Si-Al powder is characterized in that the oxygen content of the Fe-Si-Al powder is less than 730ppm; the granularity of the Fe-Si-Al powder is more than or equal to 200 meshes, the granularity of 200 meshes is less than or equal to 15-30% of 300 meshes, the granularity of 300 meshes is less than or equal to 35-50% of 400 meshes, and the granularity is more than or equal to 25-40% of 400 meshes.
2. The ferrosilicon aluminum powder of claim 1 having an oxygen content of less than 700ppm; the granularity of the Fe-Si-Al powder is more than or equal to 200 meshes, the granularity of 200 meshes is less than or equal to 20-30% of 300 meshes, the granularity of 300 meshes is less than or equal to 40-45% of 400 meshes, and the granularity is more than or equal to 30-40% of 400 meshes.
3. The iron-silicon-aluminum powder according to claim 1, wherein the iron-silicon-aluminum powder is prepared from 9.0% -10.0% of silicon, 5.0% -6.0% of aluminum and 84% -86% of iron by weight.
4. The ferrosilicon aluminum powder of claim 3, wherein the raw materials for preparing the ferrosilicon aluminum powder are 9.2% -9.8% of silicon, 5.2% -5.8% of aluminum and 84.5% -85.6% of iron in percentage by weight.
5. The method for preparing the ferrosilicon aluminum powder as claimed in any one of claims 1 to 4, comprising the steps of:
vacuum smelting the raw material components to obtain molten alloy steel, throwing the molten alloy steel into an alloy thin belt, crushing the alloy thin belt, grinding the alloy thin belt into powder by ring grinding, screening and carrying out heat treatment to obtain the ferrosilicon aluminum powder.
6. The preparation method according to claim 5, wherein the molten alloy steel is spun into an alloy thin strip by vacuum spinning; pouring the molten alloy steel onto a rotating copper roller during the vacuum melt-spinning; the casting temperature is 1480-1780 ℃, the rotation degree of the copper roller is 8-44m/s, and the copper roller is cooled by cooling water during casting.
7. The method according to claim 5, wherein the ring milling is performed in a ring mill to obtain powder; the rotating speed of the ring mill powder is 450-850r/min; the nitrogen is introduced for protection during the grinding of the powder, and the flow rate of the nitrogen is 2-12m 3 /h。
8. The preparation method according to claim 7, wherein the powder is subjected to 200 mesh sieving in a sieving machine to obtain powder with a particle size of not less than 200 mesh.
9. The method according to claim 4, wherein the temperature of the heat treatment is 550 to 800 ℃, and the time of the heat treatment is 0.9 to 3.2 hours; the preparation method also comprises batch mixing; the mixing time of the batch is 0.4-1.1h.
10. Use of the ferro-silicon aluminium powder of any one of claims 1-4 in the field of electronics, new energy.
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CN111029076A (en) * | 2020-01-15 | 2020-04-17 | 合肥工业大学 | Gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss |
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