CN103014477B - Method for smelting iron-based nanocrystalline master alloy - Google Patents
Method for smelting iron-based nanocrystalline master alloy Download PDFInfo
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- CN103014477B CN103014477B CN201310016199.2A CN201310016199A CN103014477B CN 103014477 B CN103014477 B CN 103014477B CN 201310016199 A CN201310016199 A CN 201310016199A CN 103014477 B CN103014477 B CN 103014477B
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Abstract
The invention relates to a method for smelting an iron-based nanocrystalline master alloy. The method comprises the following process steps of: putting raw materials in a furnace according to the process requirement; vacuumizing, transmitting power, adjusting heating power and time as well as adding residual pure iron into the furnace in the process; insulating for 15 minutes when the temperature reaches at 1520+/-10 DEG C, stopping power transmission and cooling to 1460 +/-10 DEG C, adding metallic silicon, adjusting the heating power to 100kW, smelting for 30 seconds, adding cathode copper into the furnace after the time is ended and guaranteeing the heating power of 100kW and the smelting time for 30 seconds at the same time; and stopping power transmission and cooling to 1360+/-10 DEG C, opening a furnace cover, continuously to heat to 1280+/-10 DEG C, tapping steel and pouring molten steel into a steel ingot mould. Through the reasonable material distribution and the control of heating power and time, the smelting efficiency is improved and the problems of great furnace lining damage, severe burning loss of beneficial elements, high impurity content in the master alloy and the like in the process of smelting nanocrystalline master alloy are effectively solved.
Description
Technical field
The present invention relates to smelting nut alloy technical field, relate in particular to a kind of method of smelting iron-based nanocrystalline mother alloy.
Background technology
Iron-base nanometer crystal alloy is taking Fe element as main, add a small amount of Nb, Cu, Si, B element to form alloy, form a kind of amorphous material through fast solidification technology, after thermal treatment, obtain the crystallite that diameter is 10-20nm, disperse is distributed on amorphous matrix, is called as iron based nano crystal or iron-base ultramicro-crystal material.Iron based nano crystal has excellent comprehensive soft magnetic performance: initial permeability can reach 100,000, maximum permeability can reach 500,000, saturation induction density is 1.0-1.2T, coercive force and cobalt base amorphous close, at 20～100kHz, there is the loss less than iron-nickel alloy, there are higher B second and desirable thermostability than ferrite, and different composition proportion can obtain the characteristics such as high squareness factor, high impulse magnetic permeability, low remanent magnetism, and technique is simple, cheap.Iron based nano crystal, because its excellent soft magnetic performance is widely used, can be applicable to current transformer, common mode inductance, high power switching power supply, inverter, magnetic amplifier, earth leakage circuit-breaker, high-frequency transformer, high-frequency converter, high-frequency chocke etc.
The starting material of iron based nano crystal are technically pure iron, Pure Silicon Metal, electrolytic copper, ferro-niobium, ferro-boron, wherein comparatively infusibility of ferro-niobium and ferro-boron, also have Pure Silicon Metal and the electrolytic copper of easy scaling loss, wherein ferro-niobium is expensive, the mother alloy of smelting with these starting material requires beneficial element to have higher recovery rate, composition is even, even particle distribution, and spray is with there being higher volume ratio (volume ratio=strip quality/raw material quality) in process.
Existing iron based nano crystal mother alloy smelting process is generally simple method for vacuum smelting or air induced melting method.In the general cloth situation of the nanocrystalline mother alloy of air induced melting, the highest smelting temperature is 1560-1600 DEG C, more serious to furnace lining injury, element degree of oxidation causes greatly impurity more (can cause preparing gained band embrittlement), beneficial element scaling loss is more serious, and the mother alloy composition fluctuation range of the furnace charge melting of identical proportioning is large (conference of composition fluctuation range causes preparing band unstable properties): Si fluctuation range reaches 0.15%, Cu fluctuation range reaches 0.06%, B fluctuation range reaches 0.1%, Nb fluctuation range reaches 0.1%, the recovery rate of Nb is lower is generally 95%.The nanocrystalline mother alloy of vacuum metling is longer tap to tap time, the nanocrystalline mother alloy of melting 200kg generally needs about 150 minutes, and general cloth situation requires the highest smelting temperature need reach 1560-1600 DEG C, larger to furnace lining injury, the fluctuation range of the mother alloy Cu of the furnace charge melting of identical proportioning reaches 0.1%.
In view of the foregoing, in the urgent need to the method for the nanocrystalline mother alloy of smelting that the highest a kind of smelting temperature is lower, beneficial element fluctuation range is less, mother alloy foreign matter content is lower, efficiency is higher is provided.
Summary of the invention
The object of the present invention is to provide a kind of method of smelting nanocrystalline mother alloy, be intended to solve the problems such as in nanocrystalline mother alloy process, furnace lining infringement is large, beneficial element scaling loss is serious, mother alloy foreign matter content is high, efficiency is low of smelting.
For achieving the above object, the invention provides a kind of method of smelting nanocrystalline mother alloy.Its processing step comprises: a certain amount of Pure Silicon Metal is laid on to stove bottom, several technically pure irons are vertically placed in stove, and ensure between each technically pure iron to be impartial space, then the half amount of starting material ferro-boron is sprinkled in stove in Lower Half space, ferro-niobium is sprinkled into space, middle part in stove, and residue ferro-boron is sprinkled into first half space in stove; Cover bell, start to vacuumize, power transmission, regulate heating power and heat-up time until clothization is warmed up to 1520 ± 10 DEG C after clear, in the continuous melting process of furnace charge, by feeding chamber, residue technically pure iron is added in stove, heating power remains 200kW; In the time that reaching 1520 ± 10 DEG C, temperature is incubated 15 minutes, then regulate heating power to cool to 1460 ± 10 DEG C to 0kW, with smashing material bar, molten steel surface bits layer is abolished, add residual metallic silicon by feeding chamber, regulate heating power to 100kW, melt 30 seconds, after fusing time finishes, add electrolytic copper, ensure that heating power is that 100kW fusing time is 30 seconds simultaneously; Regulating power cools to 1360 ± 10 DEG C of vacuum breakers to 0kW, opens bell, continues to cool to 1280 ± 10 DEG C, destroys bits, and then tapping, pours into molten steel in steel ingot die.
The present invention has the following advantages and feature compared with existing technology: the present invention, by rational cloth, control heating power and heat-up time, has improved efficiency; Higher by the smelting iron-based nanocrystalline mother alloy smelting efficiency of present method, total smelting time is 105 ± 5 minutes, and this smelting process melting top temperature is 1530 DEG C, and top temperature is lower, can effectively protect furnace lining and improve its life-span, also may for using quartz sand lining to provide; Institute's master alloy melting composition is even, and the fluctuation of beneficial element composition is less: Si fluctuation range≤0.1%, and Cu fluctuation range≤0.04%, B fluctuation range≤0.05%, Nb fluctuation range≤0.04%, the recovery rate of Nb reaches more than 97%, can be effectively cost-saving; In mother alloy, impurity is less, impurity plug nozzle can not cause spray band time, and the volume ratio of spray band reaches more than 83%, and spray band toughness is better.
Brief description of the drawings
Fig. 1 is according to the method flow diagram of the nanocrystalline mother alloy of smelting of the embodiment of the present invention.
Embodiment
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Fig. 1 is according to the method flow diagram of the nanocrystalline mother alloy of smelting of the embodiment of the present invention.
In step 101,3～5kg Pure Silicon Metal is laid on to stove bottom, a technically pure iron is vertically placed in stove and touches furnace bottom, again 6～7 technically pure irons are vertically placed on the Pure Silicon Metal that is layered on stove bottom, and ensure between each technically pure iron to be impartial space, then the half amount of starting material ferro-boron is sprinkled in stove in Lower Half space, ferro-niobium is sprinkled into space, middle part in stove, and residue ferro-boron is sprinkled into first half space in stove.
In step 102; after the cloth of completing steps 101; cover bell; start to vacuumize, power transmission; regulate heating power and heat-up time; if vacuum induction furnace furnace lining is normal temperature, regulate heating power and heat-up time to be: 30KW:30 minute → 60KW:20 minute → 120kW:10 minute → 160kW:5 minute → 200kW: until clothization is warmed up to 1520 ± 10 DEG C after clear; If vacuum induction furnace furnace lining red heat regulates heating power and heat-up time to be: 70kW:5 minute → 100kW:5 minute → 140kW:10 minute → 180kW:5 minute → 200kW: until clothization is warmed up to 1520 ± 10 DEG C after clear.In the continuous melting process along with furnace charge, by feeding chamber, residue technically pure iron is added in stove, heating power remains 200kW.
In step 103, in the time that reaching 1520 ± 10 DEG C, temperature is incubated 15 minutes, then regulate heating power to cool to 1460 ± 10 DEG C to 0kW, with smashing material bar, molten steel surface bits layer is abolished, add residual metallic silicon by feeding chamber, adjusting adds power to 100kW fusing 30 seconds, and adds electrolytic copper in this fusing time, ensures that heating power is that 100kW fusing time is 30 seconds simultaneously.
In step 104, regulating power cools to 1360 ± 10 DEG C of vacuum breakers to 0kW, opens bell, continues to cool to 1280 ± 10 DEG C, destroys bits, and then tapping, pours into molten steel in steel ingot die.
In embodiments of the present invention, 3～5kg Pure Silicon Metal is put for avoiding heavier technically pure iron will damage furnace bottom in stove bottom, pure iron is selected vertically to place and is avoided furnace charge under vacuum environment to put up a bridge, ferro-boron, ferro-niobium can effectively utilize furnace inner space between technically pure iron space, ferro-niobium can ensure the higher position of ferro-niobium temperature in stove in stove medium position, in the space of ferro-boron Lower Half and first half in stove.Fe-B is that 5wt% left and right exists a dark eutectic point at B content, and ferro-boron fully contacts with iron, contributes to furnace charge to occur early molten bath, and in the embodiment of the present invention, the clear temperature of clothization is 1360 ± 10 DEG C, and cloth expects that the clear time of clothization is 50 ± 5 minutes.
Heating power adjustment process in the embodiment of the present invention is in order to have ensured furnace charge melting efficiency, also ensures that lining life is unaffected simultaneously.
In whole melting process, ferro-niobium is the process of dissolving, but also needs certain temperature, is therefore set in embodiments of the present invention 1520 ± 10 DEG C of insulations 15 minutes.If temperature lower than 15 minutes, will there will be ferro-niobium to dissolve insufficient lower than 1510 DEG C or soaking time, part ferro-niobium is deposited on furnace bottom; If temperature causes the lost of life or furnace lining to damage higher than 1530 DEG C can be caused burning furnace lining, overlong time can cause B element evaporation, and recovery rate declines.In the embodiment of the present invention, be set in 1460 ± 10 DEG C and add Pure Silicon Metal, be conducive to improve the recovery rate of Si, be chosen in and add the volatilization that adds electrolytic copper after silicon and reduced Cu, make Si, two kinds of element fluctuation ranges of Cu less.
The embodiment of the present invention occurs that at molten steel it is to be the process of carrying out melting below 15Pa in vacuum tightness that molten bath to temperature is 1360 ± 10 DEG C, can be reduced in oxidation or the amount of impurities of high temperature section molten alloy by this operation; Be to adopt non-vacuum condition to water steel between 1360 ± 10 DEG C to 1280 ± 10 DEG C in temperature, be conducive to accelerate cooling rate, improve efficiency.
The starting material of same proportioning are smelted many stoves iron based nano crystal mother alloy by this smelting process, the composition that detects every stove with direct-reading spectrometer can obtain many stoves mother alloy beneficiating ingredient fluctuation range: Si fluctuation range≤0.1%, Cu fluctuation range≤0.04%, B fluctuation range≤0.05%, Nb fluctuation range≤0.04%, the recovery rate of Nb reaches more than 97%, with this smelting process smelt the suitable spray band technique of mother alloy spray band, band volume ratio can reach more than 83%, fully ensured the volume ratio of spray band by improving mother alloy homogeneity, because more than 1360 DEG C temperature section in smelting process carries out under vacuum environment, reduce the generation of impurity, reduced forming core point, so impurity plug nozzle can not cause spray band with the mother alloy that this method is smelted time, the volume ratio of spray band reaches more than 83%, spray band toughness is better, more be conducive to processing welding.
The nanocrystalline mother alloy data sheet of smelting of table 1 embodiment of the present invention.
Can be obtained by above result: this smelting process melting top temperature is 1530 DEG C, and top temperature is lower, can effectively protect furnace lining and improve its life-span, also may for using quartz sand lining to provide; Institute's master alloy melting composition is even, and the fluctuation of beneficial element composition is less: Si fluctuation range≤0.1%, and Cu fluctuation range≤0.04%, B fluctuation range≤0.05%, Nb fluctuation range≤0.04%, the recovery rate of Nb reaches more than 97%, can be effectively cost-saving; In mother alloy, impurity is less, impurity plug nozzle can not cause spray band time, and the volume ratio of spray band reaches more than 83%, and spray band toughness is better.
It should be noted that the present invention carries out on ZG-0.2L vacuum induction furnace, it will be understood by those of skill in the art that to adopt in 50-500kg vacuum oven or intermediate frequency furnace adopts distributing mode and smelting flow process in present method also can carry out smelting iron-based nanocrystalline mother alloy.
Above-described embodiment; object of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only the specific embodiment of the present invention; the protection domain being not intended to limit the present invention; within the spirit and principles in the present invention all, any amendment of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. a method for smelting iron-based nanocrystalline mother alloy, its processing step is:
A certain amount of Pure Silicon Metal is laid on to stove bottom, several technically pure irons are vertically placed in stove, and ensure between each technically pure iron to be impartial space, then the half amount of starting material ferro-boron is sprinkled in stove in Lower Half space, ferro-niobium is sprinkled into space, middle part in stove, and residue ferro-boron is sprinkled into first half space in stove;
Cover bell, start to vacuumize, power transmission, regulate heating power and heat-up time until clothization is warmed up to 1520 ± 10 DEG C after clear, in the continuous melting process of furnace charge, by feeding chamber, residue technically pure iron is added in stove, heating power remains 200kW;
In the time that reaching 1520 ± 10 DEG C, temperature is incubated 15 minutes, then regulate heating power to cool to 1460 ± 10 DEG C to 0kW, with smashing material bar, molten steel surface bits layer is abolished, add residual metallic silicon by feeding chamber, regulate heating power to 100kW, melt 30 seconds, after fusing time finishes, add electrolytic copper, ensure that heating power is that 100kW fusing time is 30 seconds simultaneously;
Regulating power cools to 1360 ± 10 DEG C of vacuum breakers to 0kW, opens bell, continues to cool to 1280 ± 10 DEG C, destroys bits, and then tapping, pours into molten steel in steel ingot die.
2. the method for smelting iron-based nanocrystalline mother alloy according to claim 1, it is characterized in that, several technically pure irons are vertically placed in stove and are comprised: first a technically pure iron is vertically placed in stove and touches furnace bottom, then 6～7 technically pure irons are vertically placed on the Pure Silicon Metal that is layered on stove bottom.
3. the method for smelting iron-based nanocrystalline mother alloy according to claim 1, it is characterized in that, the stove of described smelting iron-based nanocrystalline mother alloy is the vacuum induction furnace of ZG-0.2L, and the working vacuum degree of vacuum oven is 3～15Pa, and furnace charge fusing initial vacuum degree is below 15Pa.
4. the method for smelting iron-based nanocrystalline mother alloy according to claim 3, is characterized in that, described smelting iron-based nanocrystalline mother alloy vacuum induction furnace lining material is the preset crucible of quartz sand, magnesia or magnesium-aluminium spinel.
5. the method for smelting iron-based nanocrystalline mother alloy according to claim 1; it is characterized in that; described adjusting heating power and heat-up time are until clothization is warmed up to 1520 ± 10 DEG C after clear comprises: if vacuum induction furnace furnace lining is normal temperature, regulate heating power and heat-up time to be: 30KW:30 minute → 60KW:20 minute → 120kW:10 minute → 160kW:5 minute → 200kW: until clothization is warmed up to 1520 ± 10 DEG C after clear; If vacuum induction furnace furnace lining red heat regulates heating power and heat-up time to be: 70kW:5 minute → 100kW:5 minute → 140kW:10 minute → 180kW:5 minute → 200kW: until clothization is warmed up to 1520 ± 10 DEG C after clear.
6. the method for smelting iron-based nanocrystalline mother alloy according to claim 1, is characterized in that, described smelting iron-based nanocrystalline mother alloy from cloth to the tapping time be 105 ± 5 minutes, from cloth to the clear time of cloth materialization be 50 ± 5 minutes.
7. the method for smelting iron-based nanocrystalline mother alloy according to claim 1, is characterized in that, described smelting iron-based nanocrystalline mother alloy is smelted under vacuum condition, for reducing the oxidation at high temperature section molten alloy or amount of impurities; Under non-vacuum condition, water steel, for accelerating cooling rate, improving efficiency.
8. the method for smelting iron-based nanocrystalline mother alloy according to claim 1, it is characterized in that, the starting material of described smelting iron-based nanocrystalline mother alloy are technically pure iron, ferro-niobium, ferro-boron, Pure Silicon Metal, electrolytic copper, and described technically pure iron is shaped as square billet shape, and size is 70mm*70mm*300mm; Described ferro-niobium is 65 ± 3wt% containing Nb amount, and surplus is mainly Fe, contains the impurity such as a small amount of Si, Al, Ta, C, P, and granularity is 5～50mm; Described ferro-boron is 17-18wt% containing B amount, and surplus is mainly Fe, contains a small amount of impurity element, and granularity is 2～40mm; Described Pure Silicon Metal si content >=99wt%, granularity is 5～100mm; Described electrolytic copper is containing Cu amount >=99wt%, and entering stove starting material total amount is 200 ± 5kg.
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| CN103643106A (en) * | 2013-08-27 | 2014-03-19 | 安徽新天瑞电气有限公司 | Mother alloy smelting method |
| CN103667856B (en) * | 2013-12-13 | 2015-10-21 | 青岛云路新能源科技有限公司 | A kind of method reclaiming the smelting iron-based nanocrystalline master alloy of scratch tape |
| CN103667855B (en) * | 2013-12-13 | 2015-10-21 | 青岛云路新能源科技有限公司 | A kind of method of scratch tape material smelting iron-based amorphous master alloy |
| CN103674652B (en) * | 2013-12-18 | 2016-01-20 | 青岛云路新能源科技有限公司 | Iron based nano crystal standard sample for spectrochemical analysis preparation method |
| CN103938127B (en) * | 2014-04-23 | 2015-06-17 | 兆晶股份有限公司 | Method for preparing iron-based amorphous broadband |
| CN103937928B (en) * | 2014-04-23 | 2015-11-25 | 兆晶股份有限公司 | The smelting technology of a kind of Fe-based amorphous wide-band system alloy molten steel for subsequent use |
| CN110923586A (en) * | 2019-11-22 | 2020-03-27 | 河北锴盈新材料有限公司 | Microalloyed ultrahigh magnetic conductivity iron-based nanocrystalline alloy strip and preparation method thereof |
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