CN103938127B - Method for preparing iron-based amorphous broadband - Google Patents
Method for preparing iron-based amorphous broadband Download PDFInfo
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- CN103938127B CN103938127B CN201410165856.4A CN201410165856A CN103938127B CN 103938127 B CN103938127 B CN 103938127B CN 201410165856 A CN201410165856 A CN 201410165856A CN 103938127 B CN103938127 B CN 103938127B
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000003723 Smelting Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000007921 spray Substances 0.000 claims description 42
- 229910000831 Steel Inorganic materials 0.000 claims description 39
- 239000010959 steel Substances 0.000 claims description 39
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 16
- 239000010453 quartz Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052796 boron Inorganic materials 0.000 claims description 13
- 238000009413 insulation Methods 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 230000006698 induction Effects 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 6
- 241001062472 Stokellia anisodon Species 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- 239000003818 cinder Substances 0.000 claims description 3
- 229910000808 amorphous metal alloy Inorganic materials 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005507 spraying Methods 0.000 abstract description 4
- 206010039897 Sedation Diseases 0.000 abstract 1
- 238000007712 rapid solidification Methods 0.000 abstract 1
- 230000036280 sedation Effects 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 10
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 238000003475 lamination Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229920000742 Cotton Polymers 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 230000006641 stabilisation Effects 0.000 description 4
- 238000011105 stabilization Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000003245 working effect Effects 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000005300 metallic glass Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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Abstract
The invention belongs to the technical field of rapid solidification of amorphous alloy, and discloses a method for preparing an iron-based amorphous broadband. The method orderly comprises the following three steps: 1, smelting at low temperature; 2, insulated sedation; 3, spraying the band, and the like. The demands on raw materials can be properly reduced, good performance of the product can also be ensured, the cost is reduced, the manufactured band surface is even and consistent, the band production efficiency and banding forming rate are greatly improved, and the band with more excellent performance is obtained.
Description
Technical field
The invention belongs to non-crystaline amorphous metal flash set technology field, relate to a kind of preparation method of Fe-based amorphous broadband.
Background technology
Fe-based amorphous alloy is as a kind of novel green developed rapidly in recent years, energy-conservation novel material, usual use flash set technology, its preparation technology is: by each starting material of specific alloy components containing through melting, then the molten iron of the condition of high temperature is controlled to be ejected on the cooling roller of high speed rotating by the liquid level, temperature etc. of spray bag, make the amorphous thin ribbon that thickness is less than 0.03mm with the speed of cooling chilling of 106 DEG C.
There are problems in equipment and the technique of existing production iron-based amorphous-alloy broadband.Smelt top temperature and be generally greater than 1500 DEG C, one is that lining erosion is aggravated, and two is that the serious composition of molten steel scaling loss is difficult to control, and be unfavorable for the removal of impurity element, comprehensive consideration can make molten steel pollution level increase; In spray bag, molten steel liquid level is floated large, and nozzle ejection molten steel speed is out unstable, and cause weld pool unstable, cause the one-tenth band rate of band, zone face apparent form all undesirable, such band consistency of performance is poor, lamination coefficient is low; Even if spray the clean again minute impurities particle that also can remainingly affect spray and be with of molten steel process when smelting in bag, and spray bag also can with the contact process of molten steel in separate out impurity, these impurity can cause burr, do not become band by plug nozzle when spraying band, the even generation of the bad phenomenon such as vexed bag.
China Patent Publication No. CN102314985A proposes a kind of iron-based amorphous-alloy broadband and manufacture method thereof, its production technique still continues to use traditional method, nozzle seam width is still 0.4 ~ 0.7mm, this is because their smelting technology or spray bag structure cannot make the impurity particle in molten steel reach the spray band level of 0.3 ~ 0.4mm mouth seam, its iron-based amorphous-alloy broadband lamination coefficient produced can only reach the level being greater than 0.84.
China Patent Publication No. CN2882849Y proposes a kind of Ampere force pressure pocket builder, although its spraying pressure by nozzle place molten steel and speed can be constant, but the impurity in molten steel is still difficult to remove totally, and its spray bag heat insulation effect is poor, is not suitable for the iron-based amorphous-alloy broadband that disposable spray is greater than 1 ton.
The defect that Fe-based amorphous wide-band system Preparation Method described in above-mentioned each patent or spray carrying equipment exist because of self, causes ferrous alloy broadband to become band rate, lamination coefficient low, is unfavorable for that production in enormous quantities operates.Therefore, how to improve the preparation method in Fe-based amorphous broadband, increase substantially band and become band rate and lamination coefficient etc. to become the problem needing solution badly.
Summary of the invention
The object of this invention is to provide a kind of preparation method of Fe-based amorphous broadband, can produce zone face uniformity, reduce strip surface projection, acicular pores, scratch etc., lamination coefficient is greater than 0.9; Zone face width 80 ~ 213mm, tape thickness can be controlled in 25 ± 1m, can be excellent without comprehensive magnetic after magnetic-field annealing, saturation magnetic flux density Bs=1.56T, coercivity H≤2A/m, maximum permeability >=650000, Pc (50Hz, 1.4T)≤0.11W/kg.
For technical solution problem, the present invention adopts following technical scheme:
The preparation method in Fe-based amorphous broadband, its preparation process comprises successively:
Step one, low temperature smelting: adopt medium-frequency induction furnace to smelt, first pure iron is booked furnace bottom successively along furnace wall, again residue pure iron is booked one deck along furnace wall, then ferro-boron is poured in stove by 1/7 ~ 1/5 batching of pure iron in stove, like this, the mass ratio of boron and iron is about 3:97, now ferro-boron fusing point about 1250 DEG C, not only in stove, melting sources is fast, and also can realize cold melt, be conducive to removing high temperature furnace slag and low temperature slag, after raw material in stove has all melted and scarfing cinder is complete, add Pure Silicon Metal, obtain the molten steel smelted, in whole smelting process, temperature controls below 1380 DEG C, in tradition smelting requirements pure iron, Al, Ti are all less than 0.005%, and in ferro-boron, Al, Ti are all less than 0.05%, and in Pure Silicon Metal, Al is less than 0.05%, in low temperature smelting of the present invention, in pure iron, ferro-boron, Al, Ti content is only less than 0.1%, and in Pure Silicon Metal, Al content is only less than 0.3%,
Step 2, insulation calmness: the molten steel that medium-frequency induction furnace has been smelted is entered tundish inside holding, calmness by diversion trench, float to make residual impurities in molten steel, wherein, be incubated by the globars of heating in diversion trench and pass into argon gas protection, argon shield can reduce molten steel oxidation, is protected in tundish by Frequency Induction Heating; Diversion trench comprises insulation cover, flume and insulating shell, is filled with insulating cotton in insulation cover, inlays the globars of heating, and is provided with shielding gas ingress pipe; The bottom transverse cross section of flume is semicircle, and end has tap hole, is provided with insulating brick and insulating cotton outside flume;
Step 3, spray band: mix up nozzle exchange apparatus, wide 0.4 ~ the 0.6mm of nozzle seam, bandwidth 80 ~ 213mm, pressure spray bag heating temperatures is to after 1280 ~ 1380 DEG C, molten steel in tundish is poured in pressure spray bag, pressure spray bag is provided with quartz cover, quartz cover holds the molten steel be poured in pressure spray bag, the negative pressure of quartz cover is-20 ~-100kPa, reach after predetermined fluid level until molten steel, negative pressure becomes malleation value, this malleation value and liquid-level pressure value sum control at 0.1 ~ 1.0Mpa, molten steel in tundish constantly adds in pressure spray bag makes the liquid level in quartz cover and malleation value keep constant, after molten steel in tundish is most, the pressure change formula adjustment that in spray bag, malleation value sets according to liquid level change, keep constant to keep malleation value and liquid-level pressure value sum, under the effect of the pressure, band is obtained from nozzle ejection, wherein, predetermined fluid level height is 350 ~ 450mm.
Wherein, conventional spout does not have nozzle current stabilization hole, only has circular hole or trapezoidal stable chute, and nozzle can be made like this to stitch the molten steel instability of outflow, and cause " weld pool " to fluctuate large, impact normally sprays band; Nozzle of the present invention adds round current stabilization hole, CO gas heating groove and " weld pool " protect air cleft, and with CO gaseous combustion heat release heated nozzle, when making spray band, nozzle temperature keeps constant, and the CO produced
2by " weld pool " discharge, and also can avoid nozzle high temperature oxidation, and the air-flow that isolation cooling roller high speed rotating produces makes " weld pool " stablize and reduces the oxidation of molten steel by protection air cleft.
Preferably, in described step 2, by the globars insulation of heating in diversion trench, temperature is 1200 ~ 1350 DEG C.
Preferably, in described step 3, the negative pressure of quartz cover is-45 ~-50kPa.
Preferably, in described step 3, malleation value and liquid-level pressure value sum are 0.67 ~ 0.69Mpa.
The present invention has following beneficial effect:
1. the present invention smelt molten steel more less than traditional method impurity, molten steel is purer, composition and temperature homogeneity more excellent, and smelting energy consumption low;
2. this technique diversion trench uses globars heating and thermal insulation and gas shield measure, decreases the oxidation of molten steel, improves the stability of temperature;
3. spraying turn-up mechanism has load coil, pressure to spray bag and device for nozzle swapping, line slideway charging carriage has installed sensor and setter additional, upper and lower, forward and backward skew can be regulated, improve automatic regulation level, decrease the impact of human factor; Globars heating compared by induction heating spray bag crucible, improves the handiness of spray bag heating, avoids the impact of the unfavorable conditions such as globars short circuit, short circuit on spray band; Pressure spray bag structure improves the stability of liquid level, it also avoid conventional spray band level fluctuation and causes greatly the situation that weld pool instability is even broken to occur, make " weld pool " more stable, thus improve the planarization of strip surface; Device for nozzle swapping not only makes spray bag improve work-ing life, and improves the speed changing spray bag, nozzle, and in general, make band production efficiency and become band rate greatly to improve, the cost caused because of refractory materials work-ing life obviously reduces.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the invention will be further described:
Fig. 1 is the structural representation of diversion trench in preparation method's step 2 in a kind of Fe-based amorphous broadband of the present invention;
Fig. 2 is the side-view of diversion trench in Fig. 1;
Fig. 3 is the structural representation of pressure spray bag in preparation method's step 3 in a kind of Fe-based amorphous broadband of the present invention.
Embodiment
As shown in Figures 1 to 3, preparation method's embodiment 1 in a kind of Fe-based amorphous broadband of the present invention, its preparation process comprises successively:
Step one, low temperature smelting: adopt medium-frequency induction furnace to smelt, first pure iron is booked furnace bottom successively along furnace wall, again residue pure iron is booked one deck along furnace wall, then ferro-boron is poured in stove by 1/7 ~ 1/5 batching of pure iron in stove, like this, the mass ratio of boron and iron is about 3:97, now ferro-boron fusing point about 1250 DEG C, not only in stove, melting sources is fast, and also can realize cold melt, be conducive to removing high temperature furnace slag and low temperature slag, after raw material in stove has all melted and scarfing cinder is complete, add Pure Silicon Metal, obtain the molten steel smelted, in whole smelting process, temperature controls below 1380 DEG C, in tradition smelting requirements pure iron, Al, Ti are all less than 0.005%, and in ferro-boron, Al, Ti are all less than 0.05%, and in Pure Silicon Metal, Al is less than 0.05%, in low temperature smelting of the present invention, in pure iron, ferro-boron, Al, Ti content is only less than 0.1%, and in Pure Silicon Metal, Al content is only less than 0.3%,
Step 2, insulation calmness: the molten steel that medium-frequency induction furnace has been smelted is entered tundish inside holding, calmness by diversion trench, float to make residual impurities in molten steel, wherein, be incubated by the globars 3 of heating and pass into argon gas protection in diversion trench, argon shield can reduce molten steel oxidation, is protected in tundish by Frequency Induction Heating; Diversion trench comprises insulation cover 1, flume 4 and insulating shell 6, is filled with insulating cotton 2 in insulation cover 1, inlays the globars of heating, and is provided with shielding gas ingress pipe 9; The bottom transverse cross section of flume is semicircle, and end has tap hole 8, is provided with insulating brick 5 and insulating cotton 7 outside flume;
Step 3, spray band: mix up nozzle exchange apparatus 12, nozzle 13 stitches wide 0.4 ~ 0.6mm, bandwidth 80 ~ 213mm, pressure spray bag heating temperatures is to after 1280 ~ 1380 DEG C, molten steel in tundish is poured in pressure spray bag, pressure spray bag is provided with quartz cover 11, quartz cover 11 holds the molten steel be poured in pressure spray bag, the negative pressure of quartz cover 11 is-20 ~-100kPa, reach after predetermined fluid level until molten steel, negative pressure becomes malleation value, this malleation value and liquid-level pressure value sum control at 0.1 ~ 1.0Mpa, molten steel in tundish constantly adds in pressure spray bag makes the liquid level in quartz cover 11 and malleation value keep constant, after molten steel in tundish is most, the pressure change formula adjustment that in spray bag, malleation value sets according to liquid level change, keep constant to keep malleation value and liquid-level pressure value sum, under the effect of the pressure, band is obtained from nozzle 13 ejection, wherein, predetermined fluid level height is 350 ~ 450mm.
Wherein, conventional spout does not have nozzle current stabilization hole, only has circular hole or trapezoidal stable chute, and nozzle can be made like this to stitch the molten steel instability of outflow, and cause " weld pool " to fluctuate large, impact normally sprays band; Nozzle of the present invention adds round current stabilization hole, CO gas heating groove and " weld pool " protect air cleft, and with CO gaseous combustion heat release heated nozzle, when making spray band, nozzle temperature keeps constant, and the CO produced
2by " weld pool " discharge, and also can avoid nozzle high temperature oxidation, and the air-flow that isolation cooling roller high speed rotating produces makes " weld pool " stablize and reduces the oxidation of molten steel by protection air cleft.
Get 5 groups of samples to the band obtained in embodiment 1 below, detect the impurity contained by it and various performance, detected result is as table 1:
Table 1
Learn from detected result, the thickness of strip that the embodiment of the present invention 1 obtains is even, can be controlled in 25 ± 1m, and density improves, and reduce strip surface projection, acicular pores, scratch etc., band rolled product lamination coefficient >=0.9, prepared band can be excellent without comprehensive magnetic after magnetic-field annealing, saturation magnetic flux density Bs=1.56T, coercivity H≤2A/m, maximum permeability >=620000, Pc (50Hz, 1.4T)≤0.11W/kg.
The foregoing is only specific embodiments of the invention, but technical characteristic of the present invention is not limited thereto, any those skilled in the art is in the field of the invention, and the change done or modification are all encompassed among the scope of the claims of the present invention.
Claims (4)
1. the preparation method in Fe-based amorphous broadband, is characterized in that: its preparation process comprises successively:
Step one, low temperature smelting: adopt medium-frequency induction furnace to smelt, first pure iron is booked furnace bottom successively along furnace wall, again residue pure iron is booked one deck along furnace wall, then ferro-boron is poured in stove by 1/7 ~ 1/5 batching of pure iron in stove, the mass ratio of boron and iron is about 3:97, has all melted and after scarfing cinder completely, add Pure Silicon Metal until raw material in stove, obtain the molten steel smelted, in whole smelting process, temperature controls below 1380 DEG C; Wherein, in pure iron, ferro-boron, Al, Ti foreign matter content is less than 0.1%, and in Pure Silicon Metal, Al content is less than 0.3%;
Step 2, insulation calmness: the molten steel that medium-frequency induction furnace has been smelted is entered tundish inside holding, calmness by diversion trench, wherein, pass through the globars insulation of heating and pass into argon gas protection in diversion trench, tundish is interior to be protected by Frequency Induction Heating;
Step 3, spray band: the wide 0.4 ~ 0.6mm of nozzle seam, bandwidth 80 ~ 213mm, pressure spray bag heating temperatures is to after 1280 ~ 1380 DEG C, molten steel in tundish is poured in pressure spray bag, pressure spray bag is provided with quartz cover, quartz cover holds the molten steel be poured in pressure spray bag, the negative pressure of quartz cover is-20 ~-100kPa, reach after predetermined fluid level until molten steel, negative pressure becomes malleation value, this malleation value and liquid-level pressure value sum control at 0.1 ~ 1.0MPa, the liquid level in quartz cover and malleation is kept to be worth constant, malleation value and liquid-level pressure value sum is kept to keep constant, under the effect of the pressure, band is obtained from nozzle ejection, wherein, predetermined fluid level height is 350 ~ 450mm.
2. the preparation method in a kind of Fe-based amorphous broadband as claimed in claim 1, is characterized in that: in described step 2, and by the globars insulation of heating in diversion trench, temperature is 1200 ~ 1350 DEG C.
3. the preparation method in a kind of Fe-based amorphous broadband as claimed in claim 1, is characterized in that: in described step 3, and the negative pressure of quartz cover is-45 ~-50kPa.
4. the preparation method in a kind of Fe-based amorphous broadband as claimed in claim 1, is characterized in that: in described step 3, and malleation value and liquid-level pressure value sum are 0.67 ~ 0.69MPa.
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| CN104200986A (en) * | 2014-09-15 | 2014-12-10 | 安徽蓝海机电设备有限公司 | Transformer core and production method thereof |
| US9733017B2 (en) * | 2014-09-26 | 2017-08-15 | Crucible Intellectual Property, LLC. | Quartz pouring and casting system for non-wetting amorphous alloys |
| CN105728676B (en) * | 2016-04-05 | 2018-06-08 | 江苏国能合金科技有限公司 | Amorphous thin ribbon equipment molten iron whole process gas protection system |
| CN105935748B (en) * | 2016-04-05 | 2018-05-08 | 江苏国能合金科技有限公司 | A kind of amorphous thin ribbon equipment nozzle nonstorage calorifier |
| CN106975733A (en) * | 2017-03-27 | 2017-07-25 | 江苏驰睿新材料科技有限公司 | One kind production amorphous band compound nozzle cup |
| CN107385363A (en) * | 2017-07-09 | 2017-11-24 | 兆晶股份有限公司 | A kind of Fe-based amorphous broadband and preparation method thereof |
| CN113005325B (en) * | 2021-02-25 | 2022-03-25 | 宁波中超新材料有限公司 | Copper-iron alloy strip with microcrystalline structure and high iron content and preparation method thereof |
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| JPH09263914A (en) * | 1996-03-29 | 1997-10-07 | Nippon Steel Corp | Inexpensive Fe-based master alloy for amorphous ribbon |
| CN1854322A (en) * | 2002-03-28 | 2006-11-01 | 新日本制铁株式会社 | High-purity ferroboron |
| CN103014477A (en) * | 2013-01-16 | 2013-04-03 | 青岛云路新能源科技有限公司 | Method for smelting iron-based nanocrystalline master alloy |
| CN103602931A (en) * | 2013-11-07 | 2014-02-26 | 同济大学 | Iron-based amorphous nanocrystalline soft magnetic alloy and preparation method thereof |
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| CN102314985B (en) * | 2011-09-29 | 2013-01-09 | 安泰科技股份有限公司 | Iron-based amorphous-alloy broadband and manufacturing method thereof |
| CN102909327B (en) * | 2012-10-25 | 2015-03-25 | 江苏锴博材料科技有限公司 | Device and process for producing amorphous strips |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09263914A (en) * | 1996-03-29 | 1997-10-07 | Nippon Steel Corp | Inexpensive Fe-based master alloy for amorphous ribbon |
| CN1854322A (en) * | 2002-03-28 | 2006-11-01 | 新日本制铁株式会社 | High-purity ferroboron |
| CN103014477A (en) * | 2013-01-16 | 2013-04-03 | 青岛云路新能源科技有限公司 | Method for smelting iron-based nanocrystalline master alloy |
| CN103602931A (en) * | 2013-11-07 | 2014-02-26 | 同济大学 | Iron-based amorphous nanocrystalline soft magnetic alloy and preparation method thereof |
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