CN103014477A - Method for smelting iron-based nanocrystalline master alloy - Google Patents
Method for smelting iron-based nanocrystalline master alloy Download PDFInfo
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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 the 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 take the Fe element as main, add a small amount of Nb, Cu, Si, B element formation alloy, form a kind of amorphous material through fast solidification technology, obtaining diameter after the thermal treatment is the crystallite of 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, the loss less than iron-nickel alloy arranged, than ferrite higher B second and desirable thermostability are arranged, 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 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. owing to its excellent soft magnetic performance is widely used.
The starting material of iron based nano crystal are technically pure iron, Pure Silicon Metal, electrolytic copper, ferro-niobium, ferro-boron, ferro-niobium and ferro-boron infusibility comparatively wherein, the Pure Silicon Metal and the electrolytic copper that also have easy scaling loss, wherein ferro-niobium is expensive, the mother alloy of smelting with these starting material requires beneficial element that higher recovery rate is arranged, homogeneous chemical composition, even particle distribution, spray is with higher volume ratio (volume ratio=strip quality/raw material quality) is arranged in the process.
Existing iron based nano crystal mother alloy smelting process is generally simple method for vacuum smelting or air induced melting method.The highest smelting temperature is 1560-1600 ℃ in the general cloth situation of the nanocrystalline mother alloy of air induced melting, more serious to the furnace lining injury, the element degree of oxidation causes greatly impurity more (can cause preparing gained band embrittlement), the 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 the band unstable properties): the Si fluctuation range reaches 0.15%, the Cu fluctuation range reaches 0.06%, the B fluctuation range reaches 0.1%, the recovery rate that the Nb fluctuation range reaches 0.1%, Nb is low to be 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 ℃, larger to the 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, the beneficial element fluctuation range is less, the 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 the furnace lining infringement is large in the nanocrystalline mother alloy process, the beneficial element scaling loss is serious, the 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 the stove bottom, several technically pure irons are vertically placed in the stove, and guarantee between each technically pure iron to be impartial space, then half amount of starting material ferro-boron is sprinkled in the stove in the Lower Half space, ferro-niobium is sprinkled into space, middle part in the stove, and the residue ferro-boron is sprinkled into first half space in the stove; Cover bell, begin to vacuumize, send electricity, regulate heating power and heat-up time until clothization is warmed up to 1520 ± 10 ℃ after clear, will remain in the technically pure iron adding stove by feeding chamber in the continuous melting process of furnace charge, heating power remains 200kW; When reaching 1520 ± 10 ℃, temperature is incubated 15 minutes, then regulate heating power and cool to 1460 ± 10 ℃ to 0kW, with smashing the material bar molten steel surface bits layer is abolished, add residual metallic silicon by feeding chamber, regulate heating power to 100kW, melted 30 seconds, and after the fusing time finishes, added electrolytic copper, guarantee that simultaneously heating power is that the 100kW fusing time is 30 seconds; Regulating power cools to 1360 ± 10 ℃ of vacuum breakers to 0kW, opens bell, continues to cool to 1280 ± 10 ℃, destroys bits, and then tapping pours into molten steel in the steel ingot die.
The present invention compares with existing technology and has the following advantages and characteristics: the present invention has improved efficiency by rational cloth, control heating power and heat-up time; Higher with 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 ℃, 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 homogeneous chemical composition, the fluctuation of beneficial element composition is less: 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%, can effectively save cost; Impurity is less in the mother alloy, impurity plug nozzle in the time of can not causing the spray band, and the volume ratio of spray band reaches more than 83%, and spray band toughness is better.
Description of drawings
Fig. 1 is the method flow diagram according to the nanocrystalline mother alloy of smelting of the embodiment of the invention.
Embodiment
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Fig. 1 is the method flow diagram according to the nanocrystalline mother alloy of smelting of the embodiment of the invention.
In step 101,3～5kg Pure Silicon Metal is laid on the stove bottom, be vertically placed on a technically pure iron in the stove and touch furnace bottom, again 6～7 technically pure irons are vertically placed on the Pure Silicon Metal that is layered on the stove bottom, and guarantee between each technically pure iron to be impartial space, then half amount of starting material ferro-boron is sprinkled in the stove in the Lower Half space, ferro-niobium is sprinkled into space, middle part in the stove, and the residue ferro-boron is sprinkled into first half space in the stove.
In step 102, behind the cloth of completing steps 101, cover bell, begin to vacuumize, send electricity, regulate heating power and heat-up time, if the vacuum induction furnace furnace lining is normal temperature, regulates heating power and heat-up time and be: 30KW:30 minute → 60KW:20 minute → 120kW:10 minute → 160kW:5 minute → 200kW: until clothization is warmed up to 1520 ± 10 ℃ after clear; If vacuum induction furnace furnace lining red heat is regulated heating power and heat-up time and is: 70kW:5 minute → 100kW:5 minute → 140kW:10 minute → 180kW:5 minute → 200kW: until clothization is warmed up to 1520 ± 10 ℃ after clear.To remain technically pure iron by feeding chamber and add in the stove in along with the continuous melting process of furnace charge, heating power remains 200kW.
In step 103, when reaching 1520 ± 10 ℃, temperature is incubated 15 minutes, then regulate heating power and cool to 1460 ± 10 ℃ to 0kW, with smashing the 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, guarantees that simultaneously heating power is that the 100kW fusing time is 30 seconds.
In step 104, regulating power cools to 1360 ± 10 ℃ of vacuum breakers to 0kW, opens bell, continues to cool to 1280 ± 10 ℃, destroys bits, and then tapping pours into molten steel in the steel ingot die.
In embodiments of the present invention, the stove bottom is put 3～5kg Pure Silicon Metal and is used for avoiding heavier technically pure iron will damage furnace bottom, pure iron selects vertically placement to avoid furnace charge bridging under the vacuum environment, ferro-boron, ferro-niobium are between the technically pure iron space can effectively utilize furnace inner space, ferro-niobium is in the stove medium position can guarantee that ferro-niobium is in the higher position of temperature in the stove, and ferro-boron is in the space of the interior Lower Half of stove and the first half.Fe-B is to have a dark eutectic point about 5wt% at B content, and ferro-boron fully contacts with iron, helps furnace charge the molten bath to occur early, and the clear temperature of clothization is 1360 ± 10 ℃ in the embodiment of the invention, and cloth expects that the clear time of clothization is 50 ± 5 minutes.
Heating power adjustment process in the embodiment of the invention is in order to have guaranteed the furnace charge melting efficiency, to have guaranteed that also lining life is unaffected simultaneously.
Ferro-niobium is the process of dissolving in whole melting process, but also needs certain temperature, therefore is set in embodiments of the present invention 1520 ± 10 ℃ of insulations 15 minutes.If temperature is lower than 1510 ℃ or soaking time and is lower than 15 minutes, it is insufficient the ferro-niobium dissolving to occur, and the part ferro-niobium is deposited on furnace bottom; Can cause the burning furnace lining and cause the lost of life or furnace lining to damage if temperature is higher than 1530 ℃, overlong time can cause the B element evaporation, and recovery rate descends.Be set in 1460 ± 10 ℃ in the embodiment of the invention and add Pure Silicon Metals, be conducive to improve the recovery rate of Si, be chosen in and add the volatilization that electrolytic copper has reduced Cu after adding silicon, make two kinds of element fluctuation ranges of Si, Cu less.
The embodiment of the invention molten bath to temperature occurs at molten steel, and to be 1360 ± 10 ℃ be to be the process of carrying out melting below the 15Pa in vacuum tightness, 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 ℃ to 1280 ± 10 ℃ 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 with 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%, the mother alloy of smelting with this smelting process sprays band with suitable spray band technique, the band volume ratio can reach more than 83%, fully ensured the volume ratio of spray band by improving the mother alloy homogeneity, since in the smelting process more than 1360 ℃ temperature section under vacuum environment, carry out, reduced the generation of impurity, namely reduced the forming core point, impurity plug nozzle when so the mother alloy of smelting with this method can not cause the spray band, the volume ratio of spray band reaches more than 83%, and spray band toughness is better, more is conducive to the processing welding.
The nanocrystalline mother alloy data sheet of the smelting of table 1 embodiment of the invention.
Can be got by above result: this smelting process melting top temperature is 1530 ℃, and top temperature is lower, can effectively protect furnace lining and improves its life-span, also may for using quartz sand lining to provide; Institute's master alloy melting homogeneous chemical composition, the fluctuation of beneficial element composition is less: 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%, can effectively save cost; Impurity is less in the mother alloy, impurity plug nozzle in the time of can not causing the spray band, and the volume ratio of spray band reaches more than 83%, and spray band toughness is better.
Need to prove that the present invention carries out at the ZG-0.2L vacuum induction furnace, it will be understood by those of skill in the art that and adopt the distributing mode and the smelting flow process that adopt in 50-500kg vacuum oven or the intermediate frequency furnace in present method also can carry out smelting iron-based nanocrystalline mother alloy.
Above-described embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the above only is the specific embodiment of the present invention; the protection domain that is not intended to limit the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. the method for a smelting iron-based nanocrystalline mother alloy, its processing step is:
A certain amount of Pure Silicon Metal is laid on the stove bottom, several technically pure irons are vertically placed in the stove, and guarantee between each technically pure iron to be impartial space, then half amount of starting material ferro-boron is sprinkled in the stove in the Lower Half space, ferro-niobium is sprinkled into space, middle part in the stove, and the residue ferro-boron is sprinkled into first half space in the stove;
Cover bell, begin to vacuumize, send electricity, regulate heating power and heat-up time until clothization is warmed up to 1520 ± 10 ℃ after clear, will remain in the technically pure iron adding stove by feeding chamber in the continuous melting process of furnace charge, heating power remains 200kW;
When reaching 1520 ± 10 ℃, temperature is incubated 15 minutes, then regulate heating power and cool to 1460 ± 10 ℃ to 0kW, with smashing the material bar molten steel surface bits layer is abolished, add residual metallic silicon by feeding chamber, regulate heating power to 100kW, melted 30 seconds, and after the fusing time finishes, added electrolytic copper, guarantee that simultaneously heating power is that the 100kW fusing time is 30 seconds;
Regulating power cools to 1360 ± 10 ℃ of vacuum breakers to 0kW, opens bell, continues to cool to 1280 ± 10 ℃, destroys bits, and then tapping pours into molten steel in the 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 the stove comprise: at first be vertically placed on a technically pure iron in the stove and touch furnace bottom, again 6～7 technically pure irons are vertically placed on the Pure Silicon Metal that is layered on the 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 that quartz sand, magnesia or magnesium-aluminium spinel preset crucible.
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 ℃ after clear comprises: if the vacuum induction furnace furnace lining is normal temperature, regulates heating power and heat-up time and be: 30KW:30 minute → 60KW:20 minute → 120kW:10 minute → 160kW:5 minute → 200kW: until clothization is warmed up to 1520 ± 10 ℃ after clear; If vacuum induction furnace furnace lining red heat is regulated heating power and heat-up time and is: 70kW:5 minute → 100kW:5 minute → 140kW:10 minute → 180kW:5 minute → 200kW: until clothization is warmed up to 1520 ± 10 ℃ 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 oxidation or the amount of impurities at the high temperature section molten alloy; Under non-vacuum condition, water steel, be used for accelerating cooling rate, improve 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 the square billet shape, and size is 70mm*70mm*300mm; It is 65 ± 3wt% that described ferro-niobium contains the Nb amount, and surplus is mainly Fe, contains the impurity such as a small amount of Si, Al, Ta, C, second, P, and granularity is 5 ~ 50mm; Described ferro-boron contains the B amount and is 17-18wt%, 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 contains Cu amount 〉=99wt%, and entering stove starting material total amount is 200 ± 5kg.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN103667856A (en) * | 2013-12-13 | 2014-03-26 | 青岛云路新能源科技有限公司 | Method for smelting Fe-based nanocrystalline mother alloy by recovering scratch tape |
| CN103667855A (en) * | 2013-12-13 | 2014-03-26 | 青岛云路新能源科技有限公司 | Method for smelting iron-based amorphous master alloy with waste strips |
| CN103674652A (en) * | 2013-12-18 | 2014-03-26 | 青岛云路新能源科技有限公司 | Preparation method of standard spectrum sample of Fe-based nanocrystalline |
| CN103937928A (en) * | 2014-04-23 | 2014-07-23 | 兆晶股份有限公司 | Smelting process of alloy molten steel for preparing iron-based amorphous broadband |
| CN103938127A (en) * | 2014-04-23 | 2014-07-23 | 兆晶股份有限公司 | Method for preparing iron-based amorphous broadband |
| 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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| CN103643106A (en) * | 2013-08-27 | 2014-03-19 | 安徽新天瑞电气有限公司 | Mother alloy smelting method |
| CN103667856A (en) * | 2013-12-13 | 2014-03-26 | 青岛云路新能源科技有限公司 | Method for smelting Fe-based nanocrystalline mother alloy by recovering scratch tape |
| CN103667855A (en) * | 2013-12-13 | 2014-03-26 | 青岛云路新能源科技有限公司 | Method for smelting iron-based amorphous master alloy with waste strips |
| 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 |
| CN103674652A (en) * | 2013-12-18 | 2014-03-26 | 青岛云路新能源科技有限公司 | Preparation method of standard spectrum sample of Fe-based nanocrystalline |
| 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 |
| CN103937928A (en) * | 2014-04-23 | 2014-07-23 | 兆晶股份有限公司 | Smelting process of alloy molten steel for preparing iron-based amorphous broadband |
| CN103938127A (en) * | 2014-04-23 | 2014-07-23 | 兆晶股份有限公司 | Method for preparing iron-based amorphous broadband |
| 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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