CN102181808B - Method for producing high-permeability amorphous nanocrystalline alloy - Google Patents
Method for producing high-permeability amorphous nanocrystalline alloy Download PDFInfo
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- CN102181808B CN102181808B CN 201110088357 CN201110088357A CN102181808B CN 102181808 B CN102181808 B CN 102181808B CN 201110088357 CN201110088357 CN 201110088357 CN 201110088357 A CN201110088357 A CN 201110088357A CN 102181808 B CN102181808 B CN 102181808B
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Abstract
The invention discloses a method for producing a high-permeability amorphous nanocrystalline alloy, which is characterized by comprising the following steps of: adding master alloy materials into a non-vacuum induction furnace for re-melting; after the master alloy materials begin to melt, adding materials to be supplemented, namely, calculating a weight difference between compositions of the used master alloy and required compositions, namely the amount of the materials to be supplemented; then adding perlite borax composite slag to isolate the alloy from the air; after the alloy and the composite slag are completely melted, when metal oxides are dissolved in the slag on the surface of the alloy feed liquid, removing the slag, then quickly covering composite slag on the surface of the alloy feed liquid, and removing the slag, and then covering composite slag on the surface of the alloy feed liquid, and repeating the operation until all the oxides floating in the alloy feed liquid are removed; then covering the composite slag on the surface of the alloy feed liquid, wherein the amount of the composite slag added for each time is 0.05 to 0.5 weight percent of the amount of the master alloy materials; and when the temperature of the alloy feed liquid reaches 1380 to 1410 DEG C, starting a band spraying machine for spraying a band. An amorphous band prepared by the method disclosed by the invention has stable contents of Si and B, and stable magnetic performance.
Description
Technical field
The present invention relates to a kind of production method of high permeability amorphous nanocrystalline alloy.
Background technology
The De Ji of FDAC metal Co., Ltd. swamp in 1988 gram benevolence finds to add the amorphous ribbon that a certain amount of NB and Cu make in the matrix of Fe Si B non-crystaline amorphous metal, through suitable temperature subsequent annealing, can obtain a kind of high magnetic conduction, the excellent non-retentive alloy with superfine crystal particle (nano level) of leading of performance, its typical composition is:
Fe73.5Cu1NB3 Si13.5B9 at％
The domestic 1K107 that is referred to as of this alloy.The industrialization production method of alloy as shown in Figure 1, first starting material such as pure iron, ferro-niobium, ferro-boron, industrial silicon and electrolytic copper are packed into by proportioning and melt in the vacuum induction furnace, cast mother alloy, again the mother alloy remelting in atmosphere in the non-vacuum induction furnace of packing into, when the alloy material liquid temp reaches 1380-1410 ℃, annotate on the cooling copper roller that rotates with the linear velocity of per second 20-30 rice, with 10 by nozzle
6℃/cooling of the speed of S makes the amorphous ribbon of 20-35 μ m.
Because 1K107 has high magnetic conduction, loss is little, it is of many uses, such as power current transformer, instrument precision current/voltage transformer, zero sequence current mutual inductor, sourdine, Laser Power Devices, accelerator pulse power magnetic part etc.Domestic this alloy year output reaches the 5000-6000 ton at present.
Fe is ferromagnetic element in the high permeability amorphous nanocrystalline alloy of FeCuNBSiB, and its content determines the size of alloy saturation magnetization Bs; Wherein Cu, NB are the elements of crystal grain thinning; Si, B are decrystallized elements, just are not easy to form amorphous if Si+B is less.Practice shows, in Fe73.5Cu1NB3 Si13.5B9 (at%) alloy, if Si+B＜22.5% is easy to occur Crystallization Phases in the amorphous ribbon, will affect significantly the magnetic property of alloy.Aforesaid amorphous alloy strip is when using, to form nanocrystalline through subsequent annealing, just can have good magnetic property, the variation of (Si+B) 1% will affect the variation of 5-10 ℃ of its crystallization temperature according to statistics, so the impact of the application performance of the fluctuation alloy of Si, B is very large in the alloy.Fig. 2 is the change curve of the variation 1K107 magnetic property u4 of the Si+B atomic percent drawn of the data of statistics 760 stove 1K107.
The domestic manufacturing enterprise that the amorphous nano-crystalline 1K107 alloy of certain scale arranged produced the 1-3 month in 2007 chemical analysis data of 1K107 band according to investigations, and the fluctuation of B is 7.87-10.5at%, and the fluctuation of Si is 12.92-14.12at%.Obviously the fluctuation of B is greater than the fluctuation of Si, so the fluctuation range of every series-produced amorphous nanocrystalline strip magnetic property u4 is very large, such as 110,000-330,000,110,000-360,000,110,000-460,000 do not wait, and the ratio of maximum and Schwellenwert is up to several times, and the so large fluctuation of magnetic property has caused great difficulty to the applying unit of band, even caused larger financial loss, also be the problem that 1K107 factory feels confused always.
Si, B are easy oxidation elements.As mentioned above, because the spray amorphous ribbon must carry out under atmosphere, and the 1K107 alloy will stay for some time under 1200-1400 ℃ liquid state, so that homogenization of composition, so the oxidation of Si, B is inevitable, this is to cause Si in the alloy, B fluctuation, so that make the major cause of alloy magnetic property fluctuation.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, a kind of technique of producing the amorphous nano crystal zone is provided, reach Si, the B stable content of amorphous ribbon, the purpose that the magnetic property of 1K107 is stable improves the quality of magnetic property and the product of 1K107 effectively.
Technical scheme of the present invention is: a kind of production method of high permeability amorphous nanocrystalline alloy, described method joins remelting in the non-vacuum induction furnace with the mother alloy material, after the mother alloy material begins fusing, add and add material, that is: calculate the composition of the mother alloy that uses and the weight difference of desired composition, be the amount of the material that need to add; Then add the compound slag charge of perlite borax, make alloy and air insulated; After alloy and compound slag charge all melt, when being dissolved with metal oxide in the slag on alloy feed liquid surface, scarfing cinder, add compound slag charge in alloy feed liquid surface cover rapidly again, again scarfing cinder, add compound slag charge in alloy feed liquid surface cover again, repetitive operation is until remove all oxides that floats in the alloy material; Add compound slag charge in alloy feed liquid surface cover again; The amount of each compound slag charge that adds is the 0.05-0.5wt% of mother alloy material amount; When the alloy material liquid temp reaches 1380-1410 ℃, start spray band machine, the spray band.
Preferably, the weight of the compound slag charge of described perlite borax consists of borax: perlite=1: 1.5-2.5, compound slag charge is removed moisture through baking.
Preferably, mother alloy contains Al greater than 0.005%, less than 0.1%.
Preferably, the mother alloy material is broken for less than 10cm
3Lumpy material.
The present invention selects rational slag system, constantly is stained with oxide compound in the steel with the slag of thickness, has reduced the impurity in the steel; Calculate subtly aborning and add material, add, guarantee that alloying constituent is stable, particularly Si, B content; Al content in the control mother alloy has guaranteed successfully spray band.
Description of drawings
Fig. 1 is the equipment flowsheet schematic diagram of preparation 1K107 alloy;
Fig. 2 is that the Si+B atomic percent changes and magnetic property u4 change curve in the 1K107 alloy.
Among the figure: 1. nozzle 2. nozzle bags 3. bronze medal rollers 4. amorphous ribbons 5. are peeled off tuyere 6. crucibles 7. induction coils 8. molten steel 9. slags
Embodiment
Under atmosphere, during remelting 1K107 mother alloy, select perlite and the slag making of borax compound material, the one, reduce the oxidation of Si, B, the 2nd, the adding that reduces fluctuation, the especially borax of Si, B makes the content of boron more stable, so that the 1K107 magnetic property is stable.
Perlitic composition is:
SiO2 (silicon-dioxide) 〉=73% Ai2O3 (aluminium sesquioxide) 12-14% NaO (sodium oxide) 〉=3.5% FeO (ferric oxide)≤2% Fe2O3 (ferric oxide)＜2% CaO (calcium oxide) 〉=0.5%
Perlite can sharply expand in the time of 1300 ℃ and become the thickness attitude, has the effect of poly-slag, also plays the effect of the anti-oxidation of covering alloy feed liquid.
The composition of borax is Na2B4O710H20, can be dehydrated into anhydrous sodium tetraborate, is molten into glassyly at 878 ℃, contains acidic oxide B2O3 in the melt, oxide compound that can dissolution of metals.
Owing in the composite slag of perlite and borax more SiO2 and B2O3 being arranged, because the oxide compound in the alloy feed liquid and the oxide compound in the slag have poising action, compare with only adopting perlitic effect among the patent ZL200810085015.7, poly-slag successful, more can stabilized steel in Si, B content.
Further, for guaranteeing good spray band efficient, need the Al content in the control mother alloy.
Owing to containing more NB and B in the 1K107 alloy, and NB and B add with ferro-niobium NBFe, ferro-boron BFe, NBFe contains Al can be up to 1.5% (Wt), and BFe contains Al can reach 0.45% (Wt), is inevitable so contain a certain amount of Al in the alloy.
The width of the nozzle seam among Fig. 1 is usually less than 0.7mm, and the distance of nozzle 1 and copper roller 3 is usually less than 0.3mm.So in the process of spray band, happen occasionally owing to the impurity in the alloy material causes the situation of gaging somebody.
The Al amount that contains in the mother alloy and relation such as the following table of spray band:
| Contain Al% (Wt) in the mother alloy | Spray band situation |
| ＜0.003 | Very difficult spray band, often plug nozzle |
| ＜0.005 | Not too easily spray is with |
| 0.024 | Easily spray is with |
| 0.026 | Easily spray is with |
| 0.03 | Easily spray is with |
| 0.1 | The alloy feed liquid is sticking, is difficult for the spray band |
If Al content is excessively low in the alloy, illustrate that Al by a large amount of scaling loss, must have a large amount of oxygen to exist in the alloy.Many alloys of Al feed liquid is sticking, also is not suitable for the spray band.Therefore the mother alloy of spray 1K107 band contains the Al requirement greater than 0.005%, less than 0.1%.Therefore in the selection of ferro-niobium and ferro-boron, to pay attention to very much the height of Al content.
Processing step of the present invention is as follows:
1, prepares compound slag charge
With one-level perlite and borax in borax: the ratio of perlite=1: 1.5-2.5 is made the mixing slag charge, then removes moisture.Remove moisture and can adopt ordinary method, as put into baking box, baking is 1.5-2.5 hour under the temperature about 600 ℃.Then place dry place.
2, mother alloy remelting
Mother alloy is broken into less than 10cm
3Piece, purpose is to burst when preventing rapid heating, then pack in the crucible of non-vacuum induction furnace, the high-power electricity that send, when alloy material begins to melt, add and add material, that is: calculate the composition of the mother alloy that uses and the weight difference of desired composition, be the amount of the material that need to add, then add the compound slag charge of perlite borax, its amount is the 0.5-0.05% of alloy material liquid measure, after alloy and compound slag charge all melt for some time, to be seen when being dissolved with metal oxide in the slag, carry out scarfing cinder, cover rapidly again composite slag, slag is covered in again scarfing cinder again, and the purpose of repetitive operation is to utilize the characteristics of composite slag to remove oxide compound in the steel like this.The amount of each compound slag charge that adds is the 0.5-0.05% of alloy material liquid measure.When the alloy material liquid temp reaches 1380-1410 ℃, start spray band machine, the spray band, as shown in Figure 1.
Embodiment 1
1. equipment
200kg non-vacuum induction furnace, and amorphous spray band machine.
2. raw material, each embodiment mother alloy charging capacity is 200kg.
(1) mother alloy composition
Fe83.737Cu1.22NB5.32Si7.7B2 Al0.023 wt％
(2) realize that composition is desired composition:
Fe83.37Cu1.29NB5.66Si7.7B1.98 wt％
Fe73.5Cu1NB3Si13.5B9 at％
(3) add material: pure iron, electrolytic copper, Cu99.97, ferro-niobium: Fe29.7NB66.4 Si1.53, industrial silicon: Si99.6, ferro-boron Fe80.857Si0.5B18.19 wt%
(4) the compound slag charge of borax and perlite
Borax: perlite=1: 1.5
3. adding material calculates
According to the difference that realizes between composition and mother alloy composition, in conjunction with the content of each composition in the starting material, calculate mother alloy and need add material weight.
It should be noted that for adding in the material calculating of pure iron and industrial silicon weight and also should consider added Fe, Si amount when adding ferro-niobium and ferro-boron.
The calculating of adding material can be summarized as substantially:
Component content in (realizing composition-mother alloy composition)/starting material
Each composition of this example need be added material weight and be specially: (unit: Kg)
Pure iron 0.951 electrolytic copper 0.164 ferro-niobium 0.781 industrial silicon 0.144
4. working method
Enter in the crucible mother alloy is packaged, send 150 kilowatts of electricity, add when beginning to melt and add material, then add the compound slag charge of 0.5kg, scarfing cinder after 10 minutes is stained with slag with iron plate, adds the compound slag charge of 0.25kg in mother alloy liquid surface cover rapidly again, 0.5 after minute, again slag is removed, added the compound slag charge of 0.25kg in mother alloy liquid surface cover again, again slag is stained with after 0.5 minute, be repeated to like this oxide-free above the alloy feed liquid, add the 0.5kg composite slag, full power is sent electricity again, thermometric, when temperature reaches 1390 ℃, open spray band machine, turndown spray band.
In general, because the mother alloy fusing needs the regular hour, the first scarfing cinder time is longer, is reinforced rear 8-12 minute; Mother alloy melts, and the scarfing cinder time that again adds behind the compound slag charge is shorter, is 0.3-0.8 minute; The scarfing cinder number of times is generally 3-5 time.Scarfing cinder time and scarfing cinder number of times are not had strict regulation, operator can be according to the observation to the situation that melts out of alloy feed liquid oxide on surface, rationally grasp the scarfing cinder time, the scarfing cinder number of times, in a word till the feed liquid surface observation is less than metal oxide.The embodiment of back adopts the working method identical with the present embodiment, and detailed process no longer describes in detail.
5. chemically examine the composition of amorphous ribbon
Fe73.01Cu0.93NB3.0Si13.5B9.56at％
6. magnetic test
U4=44 ten thousand
(1) mother alloy composition
Fe84.17 Cu1.2 NB5.24 Si7.38 B1.98 Al0.03 wt％
(2) material (kg) is added in calculating
Pure iron 0.009 electrolytic copper 0.203 ferro-niobium 0.943 industrial silicon 0.768 ferro-boron 0.043
Borax: perlite=1: 1.8
(3) working method is with embodiment 1
(4) band composition analysis
Cu0.96NB2.93Si13.4B9.35 at％
(5) magnetic property u4=35 ten thousand
(1) mother alloy composition
Fe84.354 Cu1.24 NB5.24 Si7.3 B1.84 Al0.026 wt％
(2) material (kg) is added in calculating
Pure iron 0.004 electrolytic copper 0.129 ferro-niobium 0.976 industrial silicon 0.957 ferro-boron 0.323
Borax: perlite=1: 2
(3) working method is with embodiment 1
(4) band composition analysis
Cu0.98NB2.96Si13.61B9.6Fe72.85 at％
(5) magnetic property u4=40 ten thousand
Embodiment 4
(1) mother alloy composition
Fe83.82 Cu1.13 NB5.28 Si7.7 B2.05 Al0.02 Wt％
(2) material (kg) is added in calculating
Pure iron 4.926 electrolytic coppers 0.397 ferro-niobium 1141 industrial silicons 0.512
Borax: perlite=1: 2.3
(3) working method is with embodiment 1
(4) band composition analysis
Fe73.83 Cu0.96 NB3.02 Si13.63 B9.01 Wt％
(5) magnetic property μ 4,=35 ten thousand
(1) mother alloy composition Wt%
Fe83.384 Cu1.28 Si7.69 B1.97 NB5.65 Al0.026
(2) material (kg) is added in calculating
Electrolytic copper 0.02 ferro-niobium 0.027 industrial silicon 0.022 ferro-boron 0.02
Borax: perlite=1: 2.5
(3) working method is with embodiment 1
(4) band composition analysis
Fe73.08 Cu0.91 NB2.95 Si13.46 B9.60at％
(5) magnetic property μ 4,=35 ten thousand
The method that more than proposes by the present invention, spray 1K107 amorphous ribbon, when antivacuum remelting mother alloy, in stove, adopt perlite to add the borax slag making, by the operating procedure of implementing 1, under meticulous operation, implement the experiment of five stoves, realization/standard analysis of 1K107 is Fe73.5Cu1NB3Si13.5B9 (at%), and the Si average assay of testing in five stoves is 13.514%, fluctuation 0.1; The B average assay is 9.42 fluctuations 0.25; 37.8 ten thousand fluctuations 4.1 ten thousand of magnetic property u4 average out to.The result shows, adopts perlite of the present invention to add the technique of borax slag making, has effectively stablized the content of Si, B in the alloy, has also stablized the magnetic property of 1K107, owing to effectively reducing the impurity in the alloy, magnetic property u4 also is significantly improved.
Claims (4)
1. the production method of a high permeability amorphous nanocrystalline alloy, it is characterized in that the mother alloy material is joined remelting in the non-vacuum induction furnace, after the mother alloy material begins fusing, add and add material, that is: calculate the composition of the mother alloy that uses and the weight difference of desired composition, be the amount of the material that need to add; Then add the compound slag charge of perlite borax, make alloy and air insulated; After alloy and compound slag charge all melt, when being dissolved with metal oxide in the slag on alloy feed liquid surface, scarfing cinder, add compound slag charge in alloy feed liquid surface cover rapidly again, again scarfing cinder, add compound slag charge in alloy feed liquid surface cover again, repetitive operation is until remove all oxides that floats in the alloy material; Add compound slag charge in alloy feed liquid surface cover again; The amount of each compound slag charge that adds is the 0.05-0.5wt% of mother alloy material amount; When the alloy material liquid temp reaches 1380-1410 ℃, start spray band machine, the spray band.
2. the production method of high permeability amorphous nanocrystalline alloy claimed in claim 1, it is characterized in that the weight of the compound slag charge of described perlite borax consists of borax: perlite=1: 1.5-2.5, compound slag charge is removed moisture through baking.
3. the production method of high permeability amorphous nanocrystalline alloy claimed in claim 1 is characterized in that mother alloy contains Al greater than 0.005%, less than 0.1%.
4. the production method of the described high permeability amorphous nanocrystalline alloy of any one among the claim 1-3 is characterized in that the mother alloy material is less than 10cm
3Lumpy material.
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