CN109202092B - Process for preparing iron-silicon-aluminum powder and manufacturing magnetic core by using non-vacuum gas atomization - Google Patents
Process for preparing iron-silicon-aluminum powder and manufacturing magnetic core by using non-vacuum gas atomization Download PDFInfo
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- CN109202092B CN109202092B CN201811079978.6A CN201811079978A CN109202092B CN 109202092 B CN109202092 B CN 109202092B CN 201811079978 A CN201811079978 A CN 201811079978A CN 109202092 B CN109202092 B CN 109202092B
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- 239000000843 powder Substances 0.000 title claims abstract description 57
- 238000009689 gas atomisation Methods 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- -1 iron-silicon-aluminum Chemical compound 0.000 title claims description 18
- 238000000137 annealing Methods 0.000 claims abstract description 24
- 238000000889 atomisation Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- 239000002893 slag Substances 0.000 claims abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 26
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 12
- 229910000702 sendust Inorganic materials 0.000 claims description 12
- 229910000519 Ferrosilicon Inorganic materials 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 239000010959 steel Substances 0.000 claims description 7
- 239000003822 epoxy resin Substances 0.000 claims description 6
- 239000003973 paint Substances 0.000 claims description 6
- 229920000647 polyepoxide Polymers 0.000 claims description 6
- 235000019353 potassium silicate Nutrition 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 5
- 239000000314 lubricant Substances 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 238000009529 body temperature measurement Methods 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000006247 magnetic powder Substances 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000010902 jet-milling Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229940072033 potash Drugs 0.000 claims description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 2
- 235000015320 potassium carbonate Nutrition 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims 1
- 238000003723 Smelting Methods 0.000 abstract description 8
- 229910002796 Si–Al Inorganic materials 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 238000000748 compression moulding Methods 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 229910018619 Si-Fe Inorganic materials 0.000 description 3
- 229910008289 Si—Fe Inorganic materials 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000001050 lubricating effect Effects 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- VAWNDNOTGRTLLU-UHFFFAOYSA-N iron molybdenum nickel Chemical compound [Fe].[Ni].[Mo] VAWNDNOTGRTLLU-UHFFFAOYSA-N 0.000 description 2
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- RLQWHDODQVOVKU-UHFFFAOYSA-N tetrapotassium;silicate Chemical compound [K+].[K+].[K+].[K+].[O-][Si]([O-])([O-])[O-] RLQWHDODQVOVKU-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Classifications
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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
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- 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
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- 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
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/241—Chemical after-treatment on the surface
- B22F2003/242—Coating
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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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
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0844—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Dispersion Chemistry (AREA)
- Power Engineering (AREA)
- Soft Magnetic Materials (AREA)
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Abstract
The invention relates to a process for preparing Fe-Si-Al powder and manufacturing a magnetic core by using non-vacuum gas atomization, which is characterized in that a large amount of slag formed by severe oxidation of aluminum at high temperature is reduced as much as possible by adding a proper additive and a proper smelting process, furnace blockage during atomization is avoided, powder can be continuously prepared, the prepared powder is sieved, subjected to high-temperature annealing treatment and insulating coating treatment, and subjected to compression molding and high-temperature annealing process to realize the 100K/100mT loss of a mu 60 Fe-Si-Al magnetic core of 500mW/cm3(ii) a Overlay performance 100 Oe: 63%; 50 Oe: 83 percent.
Description
Technical Field
The invention relates to a preparation method of low-cost and low-loss soft magnetic alloy powder, in particular to a preparation method of Fe-Si-Al powder by using non-vacuum gas atomization.
Background
The powder preparation is the first step of manufacturing the alloy magnetic powder core and is also the most critical part, the conventional preparation methods include an atomization method, a crushing method and the like, and the gas atomization is a common method for preparing metal powder, wherein the method can be divided into vacuum gas atomization and non-vacuum gas atomization according to different smelting equipment. When preparing high-value powder such as iron nickel and iron nickel molybdenum, part of powder manufacturers use a vacuum gas atomization mode to prepare high-quality iron nickel and iron nickel molybdenum powder, and the other is that when preparing gas atomized iron silicon aluminum, a lot of slag is generated due to high-temperature oxidation in the melting process of iron silicon aluminum, so that a leakage nozzle and a spray gun for atomization are easily blocked, and the powder is prepared by adopting a vacuum melting mode.
Although the quality of the powder prepared by vacuum atomization is good, the equipment investment is large, the process is complex, the powder yield is limited by equipment, and the cost is high.
Although the existing non-vacuum gas atomization has advantages in equipment productivity and cost, the oxygen content in powder is increased in the smelting and atomization processes, aluminum in aluminum-containing molten steel can react with oxygen in the atmosphere at high temperature violently to generate a large amount of slag through oxidation, and severe oxidation slag easily generated in the process of preparing gas atomization sendust is excessive, so that furnace blockage is easy to occur, and the blockage is caused for normal production of gas atomization sendust.
Disclosure of Invention
The invention aims to provide low-loss and high-superposition mu 60 gas-atomized ferrosilicon aluminum powder and a magnetic core preparation method. According to the invention, by adding a proper additive and a proper smelting process, the formation of a large amount of slag caused by severe oxidation of aluminum at high temperature is reduced as much as possible, furnace blockage during atomization is avoided, powder can be continuously prepared, and the prepared powder is sieved and then subjected to high temperature treatmentAnnealing treatment and insulating coating treatment, and realizing 500mW/cm loss of 100K/100mT of the mu 60 iron-silicon-aluminum magnetic core through compression molding and high-temperature annealing process3(ii) a Overlay performance 100 Oe: 85 percent; 50 Oe: 95 percent.
In order to achieve the purpose, the invention adopts the following technical scheme:
a process for preparing a ferrosilicon aluminum powder and fabricating a magnetic core using non-vacuum gas atomization, the process comprising the steps of:
1) taking main materials of pure iron, ferrosilicon and aluminum particles, and auxiliary materials of a deslagging agent and carbon powder;
2) putting pure iron into an intermediate frequency furnace, heating, putting ferrosilicon into the medium frequency furnace when the pure iron is about to melt, uniformly stirring, and then reducing the frequency for first slag fishing;
3) opening a protective atmosphere gas curtain after slag fishing, pouring aluminum particles, quickly stirring, starting temperature measurement, and preparing for atomization;
4) controlling the initial temperature of the tundish to be above 1400 ℃, pouring molten steel to start atomization, and keeping the atomization pressure;
5) adjusting the heating of the intermediate frequency furnace and the tundish to keep the temperature of the molten steel to be more than 1700 ℃, and forming a protective atmosphere on the exposed part of the molten steel during atomization; 6) after atomization, screening, pin milling and jet milling are carried out on the raw powder, and after nitrogen protection and high-temperature annealing, the pin milling is carried out again, and then mixing is carried out for standby;
7) taking powder for physical and chemical detection, and adding a phosphoric acid solution diluted by water;
8) reacting the iron-silicon-aluminum powder in a phosphoric acid solution for 1-2 hours, and drying at 80-130 ℃ after the reaction is finished;
9) carrying out high-temperature annealing on the ferrosilicon aluminum powder for 1-2 hours in a nitrogen annealing furnace after phosphating, wherein the temperature is higher than 500 ℃;
10) after the iron-silicon-aluminum powder is insulated, adding one or more of high-temperature-resistant binders such as water glass, potassium water glass, composite phosphate and SiO2 sol, wherein the addition amount is 0.5-2%;
11) adding zinc stearate as a lubricant after the iron-silicon-aluminum powder is insulated and bonded, and pressing the mixed magnetic powder into an iron-silicon-aluminum core magnetic core;
12) magnetic core with iron powder core in N2Annealing heat treatment is carried out in the atmosphere;
13) spraying epoxy resin paint on the magnetic core;
14) mu 026 iron silicon aluminum magnetic core prepared by the method has 100K/100mT loss of 500-450 mW/cm3(ii) a Overlay performance 100 Oe: 61-63%; 50 Oe: 80-83%.
Preferably, the mass fractions of the raw materials in the step 1) are respectively as follows: 80-82% of main material pure iron, 9.5-10% of ferrosilicon, 5-6% of aluminum particles, 0.2 thousandth of deslagging agent as auxiliary material, 0.5 thousandth of carbon powder and the balance of inevitable impurities.
Preferably, the temperature measured in step 3) reaches 1750-1800 ℃ and atomization is started.
Preferably, the atomization pressure in step 4) is maintained at 3.0 MPa.
Preferably, the adding amount of the lubricant in the step 11) is 0.2-0.5% of the iron-silicon-aluminum powder, and the pressing pressure is 20T/cm3。
Preferably, the temperature of the heat treatment in the step 12) is 600-750 ℃, and the oxygen content is controlled below 50ppm during annealing.
Preferably, the thickness of the epoxy resin varnish in the step 13) is 0.3 to 0.5 mm.
The invention has the beneficial effects that: according to the invention, by adding a proper additive and a proper smelting process, severe oxidation of aluminum at high temperature is reduced as much as possible to form a large amount of furnace slag, furnace blockage during atomization is avoided, powder can be continuously prepared, the prepared powder is sieved, subjected to high-temperature annealing treatment and insulating coating treatment, and subjected to compression molding and high-temperature annealing process to realize 100K/100mT loss of the mu 60 iron-silicon-aluminum magnetic core of 500mW/cm3(ii) a Overlay performance 100 Oe: 63%; 50 Oe: 83 percent.
Detailed Description
The invention is further described below in conjunction with specific embodiments, the following examples are intended to illustrate the invention but not to limit it further, and the invention may be practiced in any of the ways described in this summary.
In order to avoid repetition, the raw materials and related process parameters related to the present embodiment are uniformly described in the following embodiments, which are not repeated.
Example 1
According to 100% of mass fraction, 9.5% of Si-Fe alloy with the concentration of 75%, 5% of aluminum particles, 0.2% of carbon powder, 0.5% of deslagging agent and 99.9% of pure iron are taken, gas atomization Fe-Si-Al is prepared according to a smelting process, a 6.0 leakage nozzle is selected, the atomization pressure is 3.0MPa, the powder yield of prepared powder is 75%, and the physicochemical test results of the powder are shown in Table 1;
taking 1kg of 200-mesh sendust to a temperature-controllable stirring pot, adding 100ml of 30% phosphoric acid aqueous solution, wherein the addition amount of phosphoric acid accounts for 2% of the weight of the sendust, continuously stirring for 1 hour, raising the temperature of the stirring pot to 120 ℃, baking to dry, sieving, putting the powder into a nitrogen-protected annealing furnace for high-temperature annealing for 2 hours, adding 50g of high-temperature binder water glass, and continuously stirring until the powder is dried. Adding 30g of zinc stearate lubricating powder, stirring uniformly, and adding 20 tons/cm of powder3Pressing under pressure to obtain standard magnetic rings with OD27.0, ID14.8 and HT11.0, annealing at 750 deg.C under nitrogen protection with oxygen content controlled at 20ppm for 180 min, and spraying with epoxy resin paint.
The copper wire is phi 0.5mm, the number of coil turns is 20, and an HP4284 inductance analyzer is used for testing inductance L and quality factor Q under the conditions of 100kHz and 1V. The copper wire adopts phi 0.8mm, the number of coil turns is 25, 0A inductance and 20A (namely 100Oe) direct current superposition inductance are tested under the conditions of 10kHz and 0.05V by using an HP4284 inductance analyzer, and the superposition percentage under the condition of 100Oe is calculated. The power loss is measured by a copper wire with phi of 0.5mm in a mode of adding 5 turns to 30 turns, the inductance L is 29.26-30.05 mu H, the 200KhzQ value is 61-65, and the loss value of the power loss at 100kHz and 100mT is 466.86mW/cm 3; overlay performance 100 Oe: 62.55 percent; 50 Oe: 82.91 percent.
Example 2
According to 100% of mass fraction, 9.8% of Si-Fe alloy with the concentration of 75%, 5.8% of aluminum particles, 0.2% of carbon powder, 0.5% of deslagging agent and the balance of 99.9% of pure iron are taken, gas atomization Fe-Si-Al is prepared according to a smelting process, a 6.0 leakage nozzle is selected, the atomization pressure is 3.0Mpa, and the powder yield of prepared powder is 76%;
taking 1kg to 200 meshes of ferrum-silicon-aluminum powderAnd (3) adding 100ml of 30% phosphoric acid aqueous solution into a stirring pot with controllable temperature, wherein the adding amount of phosphoric acid accounts for 2% of the weight of the iron, silicon and aluminum powder, continuously stirring for 1.5 hours, raising the temperature of the stirring pot to 80 ℃, baking to dry, sieving, putting the powder into an annealing furnace under the protection of nitrogen for annealing at 1000 ℃ for 2 hours, adding 25g of composite phosphate and 25g of silicon dioxide sol, and continuously stirring until the mixture is dried. Adding 30g of zinc stearate lubricating powder, stirring uniformly, and adding 20 tons/cm of powder3Pressing under pressure to obtain standard magnetic rings with OD27.0, ID14.8 and HT11.0, annealing at 750 + -5 deg.C under nitrogen protection with oxygen content controlled at 20ppm for 180 min, and spraying with epoxy resin paint.
The copper wire is phi 0.5mm, the number of coil turns is 20, and an HP4284 inductance analyzer is used for testing inductance L and quality factor Q under the conditions of 100kHz and 1V. The copper wire adopts phi 0.8mm, the number of coil turns is 25, 0A inductance and 20A (namely 100Oe) direct current superposition inductance are tested under the conditions of 10kHz and 0.05V by using an HP4284 inductance analyzer, and the superposition percentage under the condition of 100Oe is calculated. The power loss is measured by a copper wire with phi of 0.5mm in a mode of adding 5 turns to 30 turns, the inductance L is 29.26-30.05 mu H, the 200KhzQ value is 61-65, and the loss value of the power loss at 100kHz and 100mT is 450mW/cm 3; overlay performance 100 Oe: 61%; 50 Oe: 80 percent.
Example 3
Taking 10% of Si-Fe alloy with the concentration of 75%, 6% of aluminum particles, 0.2% of carbon powder, 0.5% of deslagging agent and 99.9% of pure iron according to 100% of mass fraction, preparing gas atomization Fe-Si-Al according to a smelting process, selecting a 6.0 leakage nozzle, enabling the atomization pressure to be 3.0Mpa, and enabling the powder yield of prepared powder to be 77%;
taking 1kg of 200-mesh sendust to a temperature-controllable stirring pot, adding 100ml of 30% phosphoric acid aqueous solution, wherein the addition amount of phosphoric acid accounts for 2% of the weight of the sendust, continuously stirring for 2 hours, raising the temperature of the stirring pot to 130 ℃, baking to dry, sieving, putting the powder into a nitrogen-protected annealing furnace at 800 ℃ for annealing for 2 hours, adding 25g of potash water glass and 25g of silica sol, and continuously stirring until the powder is dried. Adding 30g of zinc stearate lubricating powder, stirring uniformly, and adding 20 tons/cm of powder3Pressing into standard magnetic ring with OD27.0, ID14.8, and HT11.0 under pressure, and maintaining in nitrogen at 750 + -5 deg.CAnnealing under protection, controlling the oxygen content at 20ppm during annealing, performing heat treatment for 180 minutes, and finally spraying epoxy resin paint.
The copper wire is phi 0.5mm, the number of coil turns is 20, and an HP4284 inductance analyzer is used for testing inductance L and quality factor Q under the conditions of 100kHz and 1V. The copper wire adopts phi 0.8mm, the number of coil turns is 25, 0A inductance and 20A (namely 100Oe) direct current superposition inductance are tested under the conditions of 10kHz and 0.05V by using an HP4284 inductance analyzer, and the superposition percentage under the condition of 100Oe is calculated. The power loss is measured by a copper wire with phi of 0.5mm in a mode of adding 5 turns to 30 turns, the inductance L is 29.26-30.05 mu H, the 200KhzQ value is 61-65, and the loss value of the power loss at 100kHz and 100mT is 500mW/cm 3; overlay performance 100 Oe: 63%; 50 Oe: 83 percent.
TABLE 1 powder physicochemical test results
Claims (5)
1. A process for preparing sendust powder and making a magnetic core using non-vacuum gas atomization, the process comprising the steps of:
1) taking main materials of pure iron, ferrosilicon and aluminum particles, and auxiliary materials of a deslagging agent and carbon powder; the slag removing agent accounts for 0.5 per mill of the total mass of the raw materials, and the carbon powder accounts for 0.2 per mill of the total mass of the raw materials;
2) putting pure iron into an intermediate frequency furnace, heating, putting ferrosilicon into the medium frequency furnace when the pure iron is about to melt, uniformly stirring, and then reducing the frequency for first slag fishing;
3) opening a protective atmosphere gas curtain after slag fishing, pouring aluminum particles, quickly stirring, starting temperature measurement, and preparing for atomization; the temperature of the temperature measurement reaches 1750-1800 ℃, and atomization is started;
4) controlling the initial temperature of the tundish to be above 1400 ℃, pouring molten steel to start atomization, and keeping the atomization pressure to be 3.0 Mpa;
5) adjusting the heating of the intermediate frequency furnace and the tundish to keep the temperature of the molten steel to be more than 1700 ℃, and forming a protective atmosphere on the exposed part of the molten steel during atomization;
6) after atomization, screening, pin milling and jet milling are carried out on the raw powder, and after nitrogen protection high-temperature annealing, pin milling is carried out again, and then mixing is carried out for standby;
7) taking powder for physical and chemical detection, and adding a phosphoric acid solution diluted by water; the concentration of the phosphoric acid solution is 30%, and the addition amount of the phosphoric acid solution accounts for 2wt% of the iron-silicon-aluminum powder;
8) reacting iron-silicon-aluminum powder in a phosphoric acid solution for 1-2 hours, and drying at 80-130 ℃ after the reaction is finished;
9) carrying out high-temperature annealing on the ferrosilicon aluminum powder for 1-2 hours in a nitrogen annealing furnace after phosphating, wherein the temperature is higher than 500 ℃;
10) adding high-temperature resistant binders such as water glass, potash water glass, composite phosphate and SiO after the iron-silicon-aluminum powder is insulated2One or more sol with the addition amount of 5%;
11) adding zinc stearate as a lubricant after the iron-silicon-aluminum powder is insulated and bonded, and pressing the mixed magnetic powder into an iron-silicon-aluminum core magnetic core; the pressing pressure is 20T/cm3；
12) Magnetic core with iron powder core in N2Annealing heat treatment is carried out in the atmosphere;
13) spraying epoxy resin paint on the magnetic core;
14) the mu 60 iron-silicon-aluminum magnetic core prepared by the method has the loss of 500-450 mW/cm at the temperature of 100K/100mT3(ii) a Overlay performance 100 Oe: 61-63%; 50 Oe: 80-83%.
2. The process for preparing the sendust powder and manufacturing the magnetic core by using non-vacuum gas atomization according to claim 1, wherein the mass fractions of the raw materials in the step 1) are respectively as follows: 80-82% of pure iron as a main material, 9.5-10% of ferrosilicon, 5-6% of aluminum particles and the balance of auxiliary materials and inevitable impurities.
3. The process for preparing a sendust powder and making a magnetic core using non-vacuum gas atomization as claimed in claim 1, wherein the lubricant is added in an amount of 3% of the sendust powder in step 11).
4. The process for preparing sendust powder and making magnetic core using non-vacuum gas atomization as claimed in claim 1, wherein the temperature of the heat treatment in step 12) is 600-750 ℃, and the oxygen content during annealing is controlled below 50 ppm.
5. The process for preparing sendust powder and making magnetic cores using non-vacuum gas atomization as claimed in claim 1, wherein the thickness of the epoxy paint in step 13) is 0.3-0.5 mm.
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