CN102409137A - Method for controlling content of nitrogen in oriented silicon steel - Google Patents

Method for controlling content of nitrogen in oriented silicon steel Download PDF

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CN102409137A
CN102409137A CN2011103285038A CN201110328503A CN102409137A CN 102409137 A CN102409137 A CN 102409137A CN 2011103285038 A CN2011103285038 A CN 2011103285038A CN 201110328503 A CN201110328503 A CN 201110328503A CN 102409137 A CN102409137 A CN 102409137A
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nitrogen
silicon steel
oriented silicon
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CN102409137B (en
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刘和平
向睿
赵宇
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Central Iron and Steel Research Institute
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Abstract

The invention discloses a method for controlling the content of nitrogen in oriented silicon steel. The method comprises the following steps: placing pure iron used as the raw material and carbon in a crucible, placing accessories in a vacuum hopper according to the alloy raw material proportion and the charging sequence, wherein the alloy raw material proportion is calculated according to the content of each element in the oriented silicon steel; heating the furnace charge to melt, and refining the molten steel; adding aluminum to deoxidize after refinement, then adding metallic silicon or an alloy containing the nonvolatile elements of the oriented silicon steel to perform alloying; deciding whether to inject argon or nitrogen according to the content of nitrogen in the oriented silicon steel; adding nitrogen-containing ferromanganese to adjust nitrogen under the protective atmosphere, adding other alloy raw materials to meet the target contents; and performing the vacuum charged pouring of molten steel at a proper molten steel temperature. Therefore, the narrow component range control of nitrogen element in the oriented silicon steel can be realized by adopting the method for controlling the content of nitrogen in the oriented silicon steel.

Description

The control method of the nitrogen content in the oriented silicon steel
Technical field
The present invention relates to a kind of method of controlling the nitrogen content in the oriented silicon steel, more particularly, relate in particular to a kind of under the vacuum induction melting condition method of the nitrogen content in the narrow composition range control oriented silicon steel.
Background technology
Oriented silicon steel is a kind of functional metallic substance that is widely used in electric power, electromechanics, household electrical appliances manufacturing and war industry, and the production difficulty is bigger, and specification of quality is strict, is referred to as " steel artwork " in the industry.Oriented silicon steel is extremely strict to the requirement of chemical ingredients, and the composition range of regulation is very narrow, and composition slightly fluctuates just has very big influence to performance.In the oriented silicon steel production process, in order to obtain single Goss texture through secondary recrystallization, must effectively suppress first grain growth, wherein, what bring into play key effect is that phase particle or the crystal boundary tiny, that disperse is separated out gathers element (being called suppressor factor) partially.All have an optimum content scope, content to cross the low DeGrain that then suppresses as the Mn of suppressor factor forming element, S, Al, N etc., too high levels degenerates the subgrain growth and in finished product, is difficult for removing, and causes the reduction of silicon steel magnetic.
Different according to type, blank heating means and the cold rolling mode of suppressor factor; The oriented silicon steel of current production mainly contains: (1) is intrinsic suppressor factor with AlN+MnS; The HiB oriented silicon steel that adopts heat once cold rolling method to produce; Nitrogen content in the general requirement control steel is 0.008wt%-0.009wt%, and manganese content is 0.06wt%-0.09wt%; (2) be intrinsic suppressor factor with MnS, the common orientation silicon steel that adopts heat secondary cold-rolling method to produce, the manganese content in the general requirement control steel is 0.055wt%-0.061wt%, and nitrogen content<0.005wt%; (3) with the mode of " intrinsic inhibition+later stage nitriding ", with the HiB oriented silicon steel that low-temperature heat once cold rolling method is produced, the nitrogen content in the general requirement control steel is 0.005wt%-0.007wt%, and manganese content is 0.13wt%-0.16wt%; (4) with Cu 2S+AlN is intrinsic suppressor factor, produces common orientation silicon steel with low-temperature heat secondary cold-rolling method, and the nitrogen content in the general requirement control steel is 0.006wt%-0.008wt%, and manganese content is 0.20wt%-0.23wt%.It is thus clear that in the production of oriented silicon steel, the span of control of nitrogen content is extremely narrow, undulating quantity is merely 10ppm-20ppm, simultaneously, denitrogenates outside the element, also need carry out narrower Chemical Composition control to manganese in the oriented silicon steel.
Current, to produce greatly in the smelting in industry, the close limit of nitrogen content control mainly is to adopt argon/nitrogen cycle or add method such as nitroalloy and realize through adding nitroalloy, RH behind converter control nitrogen, the stove in the oriented silicon steel.Compare with the big production of industry, when adopting the vacuum induction melting oriented silicon steel, the control of the close limit of nitrogen content is more difficult.This is that nitrogen partial pressure is low, and lacks top blast and bottom blowing system because the true vacuum tightness of holding induction furnace is higher, can not adopt the bottom blowing nitrogen flushing mentioned in some patents or the method control nitrogen content of nitrogen circulation; In addition, if only add the nitrogen pick-up alloy at vacuum induction furnace, then the fluctuation of the yield of nitrogen is big under vacuum, and composition is difficult to stable control.
Application number be 200810079428.4 Chinese invention patent application proposed a kind of in high vacuum induction furnace the method for nitrogen-containing steel smelting nitrogen pickup.That is the method that, under high vacuum, charges into nitrogen protection gas and add the nitrogen pick-up of nitrogen pick-up alloy.But the vacuum melting oriented silicon steel has its tangible steel grade characteristics, and the silicon material quantity that adds like oriented silicon steel is big; The high purity that molten steel requires; The nitrogen content of control in the steel relatively low (general≤110ppm), the narrow fluctuation range of nitrogen (within 10-20ppm), and filling under the situation of nitrogen; Also need consider the close limit control of other element (like manganese) in the oriented silicon steel, limit choosing and filling choosing of nitrogen pressure etc. of nitroalloy raw material.Especially; Vacuum induction furnace lack usually with the big production line of industry on similar sampling equipment, stokehold lack and also lack effectively control device such as the accurately multiple batches of function of adding alloy material at the line element quick analysis system, in vacuum hopper; And vacuum induction furnace itself also to exist heat size little; Slag gold reaction interface is little; A spot of alloy addition level just possibly cause big characteristics such as composition fluctuation, these all make the vacuum induction melting oriented silicon steel nitrogen composition close limit control and be not easy.But; Because on the big production line of industry, the molten steel amount of smelting a stove oriented silicon steel many (being generally 80-300 ton/stove) is carried out long flow path, the complex procedures of oriented silicon steel industrial experiment; And; If the control of the molten steel composition of oriented silicon steel is inaccurate, then produce of a high pricely, be necessary so utilize vacuum induction to smelt the research that experimentizes of qualified oriented silicon steel steel ingot.
Summary of the invention
The object of the present invention is to provide a kind of control method that reaches nitrogen content in the close limit control oriented silicon steel through rational Application to the vacuum tightness of vacuum induction furnace.
To achieve these goals; The control method of the nitrogen content in a kind of oriented silicon steel is provided; It is characterized in that: 1) pure iron raw material and carbon are put into crucible, and, will prepare burden and put into vacuum hopper by order of addition(of ingredients) by the alloy raw material proportioning that each constituent content in the orientation silicon steel calculates; 2) the heating furnace charge carries out refining to fusing to molten steel; 3) add aluminium deoxidation after the refining, the alloy that adds the not volatile element in Pure Silicon Metal or the oriented silicon steel composition subsequently carries out alloying; 4) whether determine applying argon gas or nitrogen according to the nitrogen content in the oriented silicon steel, when the nitrogen content requirement≤0.005wt% of oriented silicon steel, the charged pressure>=3KPa of argon gas; When the nitrogen content that requires oriented silicon steel surpasses 0.005wt%; In stove, charge into the nitrogen of purity>=99%, fill nitrogen pressure and an atmospheric ratio is calculated as follows:
lg [ % N ] = 0.5 lg P N 2 + lg K N - lg f [ N ] lg K N = - 188 T - 1.245 lg f [ N ] = ( 3280 T - 0.75 ) Σ i = 1 n e N i [ i ]
In the formula: K NBe the equilibrium constant of nitrogen solubilizing reaction, f [N]Be the non-dimensional activity quotient of nitrogen in molten steel, [%N] is the solubleness of nitrogen in steel, Be the interaction coefficient of oriented silicon steel interalloy element i to nitrogen, [i] is the content of steel interalloy element; 5) under protective atmosphere, add ferro-silicon nitride and transfer nitrogen, and it meets target content to add other alloy raw material adjustment; 6) by the time liquid steel temperature suitable after, the charged Pour Steel of vacuum.
According to exemplary embodiment of the present invention, in step 2) fusing and refining process in, close stove evacuation to stove during pressure<15Pa; Send the electrically heated furnace charge, during rubescent and a large amount of splash Mars, close vacuum pump when furnace charge; After treating that furnace charge melts clearly; The open vacuum pump, vacuum tightness<20Pa, refining 10min-15min.
According to exemplary embodiment of the present invention, in the alloying step of step 3), after the Pure Silicon Metal of waiting to be added or the alloy of the not volatile element in the oriented silicon steel composition melt fully, restart vacuum system, send electricity, vacuumize 2min.
According to exemplary embodiment of the present invention, in step 5), adding the time that other alloy raw material carries out alloying is 4-7min.In addition, in the alloying latter stage that has a power failure before waiting for tapping, the alloying of transferring manganese or transferring aluminium.
According to exemplary embodiment of the present invention, when charging into argon gas or nitrogen, add the nitrogen content of ferro-silicon nitride with the narrow composition scope in the control oriented silicon steel.In addition, after filling nitrogen and in the early stage of alloying, add ferro-silicon nitride in the process, can fusing fully during alloying to guarantee ferro-silicon nitride.
Embodiment
Below, will specify embodiments of the invention.
The present invention smelts in the process of oriented silicon steel at high vacuum induction furnace; Through rational Application, utilize the principles of chemistry such as dissolving of reaction between carbon and oxygen, aluminium deoxidation reaction and nitrogen in steel content, adjustment alloy addition sequence to the vacuum tightness of vacuum induction furnace; Control melting power and time; Under the condition of vacuum induction furnace, reach the purpose of nitrogen content in the close limit control oriented silicon steel, and satisfy the requirement of oriented silicon steel purity.
The present invention comprises the steps: successively
(1) charging: pure iron raw material after the clean dry and carbon are put into crucible together; And by the alloy proportion that is orientated each constituent content calculating in the silicon steel; Batching is put into the vacuum hopper of vacuum induction furnace by order of addition(of ingredients); Wherein, in order to smelt the oriented silicon steel of high purity, composition narrow range, the overall principle of order of addition(of ingredients) of the present invention is: aluminium deoxidation after the first carbon deoxidation; Add Pure Silicon Metal (or not Volatile Elements, like Cu etc.); After the inflation, add ferro-silicon nitride (carbon or FeS alloying) again; Then at alloying manganese addition in latter stage or aluminium etc.;
(2) close the fusing of stove evacuation and furnace charge: close stove evacuation and to stove, during pressure<15Pa, send the electrically heated furnace charge, rubescent and when beginning a large amount of splash Mars when furnace charge, close vacuum pump;
(3) refining: after treating that furnace charge melts clearly, open vacuum pump, vacuum tightness<20Pa; Refining 10min-15min under high vacuum, carries out reaction between carbon and oxygen; Fully remove oxygen and gas and impurity element in the steel; This is because high vacuum has reduced the dividing potential drop of reaction product CO, impels reaction between carbon and oxygen acutely to carry out, and the generation of CO bubble more helps fully removing oxygen and gas and the impurity element in the steel;
(4) add aluminium and Pure Silicon Metal etc.: the power failure termination of pumping adds aluminium deoxidation, to reduce the oxide inclusion in the steel as far as possible, avoids forming silicate to be mingled with; Behind the 2min-3min, add the alloy of the not Volatile Elements in Pure Silicon Metal or the oriented silicon steel composition, after the fusing, restart vacuum system fully, send electricity, vacuumize 2min;
(5) in stove, charge into argon gas or nitrogen: whether determine applying argon gas or nitrogen according to the nitrogen content in the oriented silicon steel, when the nitrogen content requirement≤0.005wt% of oriented silicon steel, the charged pressure>=3KPa of argon gas; When the nitrogen content of oriented silicon steel requires to surpass 0.005wt%; In stove, charge into the nitrogen of purity>=99%, fill nitrogen pressure and an atmospheric ratio is calculated as follows:
lg [ % N ] = 0.5 lg P N 2 + lg K N - lg f [ N ] lg K N = - 188 T - 1.245 lg f [ N ] = ( 3280 T - 0.75 ) Σ i = 1 n e N i [ i ]
In the formula: K NBe the equilibrium constant of nitrogen solubilizing reaction, T is a liquid steel temperature, f [N]Be the non-dimensional activity quotient of nitrogen in molten steel, [%N] is the solubleness of nitrogen in steel, Be the interaction coefficient of oriented silicon steel interalloy element i to nitrogen, [i] is the content of steel interalloy element;
(6) alloying: under protective atmosphere, add ferro-silicon nitride and transfer nitrogen, simultaneously; Adjust other composition and meet the steel grade requirement; Alloying time 4-7min in the alloying latter stage that has a power failure before waiting for tapping, adds the alloy that manganese metal is transferred the Volatile Elements in manganese or the oriented silicon steel composition; Wherein, under the high vacuum, aluminium and manganese all belong to volatile element, if add in early stage, the yield fluctuation of manganese and aluminium greatly, and is wayward, so the present invention is behind inflated with nitrogen/argon gas, in alloying latter stage, carry out the alloying of above-mentioned element;
(7) steel tapping casting: after waiting until that liquid steel temperature is suitable, the charged cast of vacuum.
Furnace charge melting process among the present invention is: in the furnace charge melting process, be to prevent that splash or furnace charge that fierce reaction between carbon and oxygen produces from building bridge, and rubescent and when beginning a large amount of splash Mars when furnace charge, close vacuum pump.Therefore, the trace harmful elements of fully degassing, remove high vapour pressure of molten steel etc. is to utilize the reaction between carbon and oxygen in refining period to remove.
The present invention requires to confirm to charge into argon gas or nitrogen according to the nitrogen content in the oriented silicon steel.When the nitrogen content requirement≤0.005wt% of oriented silicon steel, then charge into argon gas.When the nitrogen content of oriented silicon steel requires to surpass 0.005wt%, then in stove, charge into nitrogen, fill the dissolution equilibrium equation of nitrogen pressure by nitrogen in the gas phase and nitrogen in steel
Figure BDA0000102053790000051
Obtaining, is 1% during as standard state when be dissolved in the steel concentration with nitrogen, then has:
Figure BDA0000102053790000052
And the equilibrium constant lgK of nitrogen solubilizing reaction NCan be expressed as with the relation of temperature T:
Figure BDA0000102053790000053
f [N]Be activity quotient, obtain according to smelting steel grades and molten steel temperature.
When nitrogen content in the oriented silicon steel≤0.005wt%, press following formula and calculate, fill nitrogen pressure during the melting oriented silicon steel and be generally less than 3KPa.According to pertinent literature; If inflation pressure too small (<3KPa), the volatile quantity that is prone to cause have the manganese element of high vapour pressure in the steel increases, and is unfavorable for stablizing the yield of manganese; Think that realization is to the control of the close limit of manganese element content in the oriented silicon steel; When this steel grade of melting, should not charge into nitrogen, need charge into argon gas, and pressure be greater than 3KPa at least.
When nitrogen content in the oriented silicon steel surpassed 0.005%wt, the present invention's employing was filled nitrogen and is controlled with the narrow composition that the mode that adds ferro-silicon nitride is implemented in the interior nitrogen of vacuum induction furnace.Use nitrogenize ferromanganese if do not adopt ferro-silicon nitride, then because of the nitrogen content in the nitrogenize ferromanganese very low (general ≯ 5%), and manganese content is high, so can not be used for the low oriented silicon steel melting of manganese content.If fill the nitrogen insufficient pressure, then nitrogen partial pressure is low in the vacuum, and denitrogenation will take place the nitrogen that ferro-silicon nitride is dissolved in the steel.If fill the nitrogen hypertonia, possibly cause the dissolved nitrogen in the steel high.Do not fill nitrogen if only add ferro-silicon nitride, then because ferro-silicon nitride density is light, melting temperature (Tm) is high, the recovery of nitrogen is unstable.Do not add ferro-silicon nitride if only charge into nitrogen, then because the heat size of vacuum induction furnace is little, the reaction interface that nitrogen pick-up takes place is little, will cause nitrogen element skewness in molten steel, also is unfavorable for realizing the stable control of close limit of nitrogen.
Therefore, the present invention is according to the composition and the nitrogen content requirement of oriented silicon steel, calculate nitrogen in steel activity quotient and under smelting temperature the solubleness of nitrogen, confirm to charge into nitrogen gas pressure and ferro-silicon nitride add-on in the stove according to the target nitrogen content.And the alloying early stage process adding of ferro-silicon nitride need after filling nitrogen, can melt fully during alloying to guarantee it.Alloying time too weak point will influence the fusing of ferro-silicon nitride, and oversize alloying time will cause element loss and increase the weight of melt and refractory materials reaction and corroding.
Inflation atmosphere is maintained to the cast end in the stove, simultaneously, adopts charged cast to influence the ingot quality of oriented silicon steel to avoid slag, sull etc. to sneak into beam.
The invention has the advantages that through vacuum induction furnace and under the high vacuum situation, melt out qualified oriented silicon steel steel ingot; Be reduced in the sky high cost that carries out industrial experiment on the production line; Can lack under the situation of effective control device at vacuum induction furnace, realize the narrow composition scope control requirement of oriented silicon steel the nitrogen element.
Embodiment:
Embodiment 1
Equipment adopts 50kg vacuum induction furnace, power 160KW, voltage rating 380V, 1700 ℃ of top temperatures, frequency 2500Hz.Batch 40kg, ([N]≤0.005wt%), its composition span of control and target call such as table 1 show melting 1 stove oriented silicon steel QX1, feed proportioning (not counting deoxidation with carbon and aluminium) as shown in table 2.Wherein, the Chemical Composition of pure iron is Mn:0.042wt%, N:0.037wt%, and P:0.0086wt%, S:0.035wt%, Cu:0.034wt%, other is the impurity of Fe and trace; Nitrogenous in the ferro-silicon nitride is 26wt%.
Composition span of control and the controlled target of table 1 oriented silicon steel QX1
Figure BDA0000102053790000061
The feed proportioning table of table 2 melting oriented silicon steel QX1
Pure iron Carbon Pure Silicon Metal Manganese metal Iron sulfuret Ferro-silicon nitride Copper
38.573kg 13.6g 1294g 12g 32.4g 8.0g 67g
Target components according to this oriented silicon steel QX1; In the time of 1600 ℃; Draw it and fill nitrogen pressure by filling nitrogen calculation of pressure formula less than 2.5KPa, because too low inflation pressure (<3KPa) be unfavorable for stablizing the yield of manganese, so; Employing charges into argon gas and the auxilliary mode that adds ferro-silicon nitride is controlled nitrogen in desired composition scope, and the chemical ingredients of QX1 Finished Steel is as shown in table 3.
Concrete steps are following:
(1) pure iron and carbon 12g are put into crucible, aluminium, Pure Silicon Metal, copper, carbon, Iron sulfuret, ferro-silicon nitride, manganese metal are put into vacuum hopper by the material alloying order;
(2) close that vacuum tightness is 12Pa in stove evacuation to the stove, send electrically heated, power 30KW progressively is sent to superpower 70KW, and is rubescent and when beginning a large amount of splash Mars when furnace charge, closes vacuum pump, molten clear to furnace charge;
(3) open vacuum pump, vacuum tightness is low to moderate 9Pa most, refining 12min;
(4) the power failure termination of pumping adds aluminium 12g deoxidation, adds Pure Silicon Metal and copper, and electricity is given in the fusing back, vacuumizes 2min; Applying argon gas 8KPa adds ferro-silicon nitride, and carbon, Iron sulfuret send power 50KW, alloying time 5min, and in alloying latter stage, 2min adds manganese metal before having a power failure.
(5) under argon filling atmosphere, steel tapping casting.
The steel ingot Chemical Composition of table 3 oriented silicon steel QX1
C,wt% Si,wt% Mn,wt% S,wt% N,wt% Cu,wt% P,wt%
0.039 3.15 0.060 0.027 0.0044 0.18 0.0087
Comparative Examples 1: under same proportioning raw materials and operation steps, an applying argon gas but when not adding the ferro-silicon nitride alloy, the Chemical Composition of its Finished Steel is following:
The Finished Steel chemical ingredients of the reference examples of table 4 melting oriented silicon steel QX1
C,wt% Si,wt% Mn,wt% S,wt% N,wt% Cu,wt% P,wt%
0.041 3.10 0.056 0.028 0.0031 0.17 0.0084
The result is illustrated under the situation of argon filling and adds ferro-silicon nitride, and the yield of nitrogen is low in the ferro-silicon nitride, only is applicable to the oriented silicon steel melting of the low nitrogen content of control.
Embodiment 2
Equipment adopts 50kg vacuum induction furnace, power 160KW, voltage rating 380V, 1700 ℃ of top temperatures, frequency 2500Hz.Batch 40kg, ([N]=0.008wt%-0.009wt%), its composition span of control and target call such as table 5 show melting 1 stove oriented silicon steel QX2, feed proportioning (not counting deoxidation with carbon and aluminium) as shown in table 6.
Composition span of control and the controlled target of table 5 oriented silicon steel QX2
Figure BDA0000102053790000071
The feed proportioning table of table 6 melting oriented silicon steel QX2
Figure BDA0000102053790000081
Concrete steps are following:
(1) pure iron and carbon 12g are put into crucible, aluminium, Pure Silicon Metal, carbon, Iron sulfuret, tin, ferro-silicon nitride, manganese metal are put into vacuum hopper by the material alloying order;
(2) close that vacuum tightness is 9Pa in stove evacuation to the stove, send electrically heated, power 30KW progressively is sent to superpower 70KW, and is rubescent and when beginning a large amount of splash Mars when furnace charge, closes vacuum pump, clear to furnace chargeization;
(3) open vacuum pump, vacuum tightness is low to moderate 8.9Pa most, refining 12min;
(4) the power failure termination of pumping adds aluminium 12g deoxidation, adds Pure Silicon Metal/copper, and the fusing back vacuumizes 2min to electricity.Inflated with nitrogen 8.2KPa adds ferro-silicon nitride, and carbon, Iron sulfuret, tin are given electric power 50KW, alloying time 5min, and in alloying latter stage, 2min adds manganese metal and aluminium before having a power failure.
(5) under the inflated with nitrogen atmosphere, steel tapping casting.
Target components according to this oriented silicon steel QX2; In the time of 1600 ℃; By filling nitrogen calculation of pressure formula, drawing it, to fill nitrogen pressure be 8.2KPa, at this moment; Employing charges into nitrogen 8.2KPa and the auxilliary mode that adds ferro-silicon nitride is controlled nitrogen in desired composition scope, and Chemical Composition such as the table 7 of Finished Steel QX2 show.
The steel ingot Chemical Composition of table 7 oriented silicon steel QX2
Figure BDA0000102053790000082
Embodiment 3
Equipment adopts 50kg vacuum induction furnace, power 160KW, voltage rating 380V, 1700 ℃ of top temperatures, frequency 2500Hz.Batch 40kg, ([N]=0.006wt%-0.008wt%), its composition span of control and target call such as table 8 show melting 1 stove oriented silicon steel QX3, feed proportioning (not counting deoxidation with carbon and aluminium) as shown in table 9.
Composition span of control and the controlled target of table 8 oriented silicon steel QX3
Figure BDA0000102053790000091
The feed proportioning table of table 9 melting oriented silicon steel QX3
Figure BDA0000102053790000092
According to the target components of this oriented silicon steel QX3, in the time of 1600 ℃, by filling nitrogen calculation of pressure formula; Draw that to fill nitrogen pressure be 5.0KPa; At this moment, employing charges into nitrogen 5KPa and the auxilliary mode that adds ferro-silicon nitride is controlled nitrogen in desired composition scope, and Chemical Composition such as the table 10 of Finished Steel QX3 show.
Concrete steps are following:
(1) pure iron and carbon 12g are put into crucible, aluminium, Pure Silicon Metal, ferrophosphorus, carbon, ferro-silicon nitride, chromium, aluminium, manganese metal are put into vacuum hopper by the material alloying order;
(2) close vacuum tightness 9Pa in stove evacuation gas to the stove, send electricity, power 30KW progressively is sent to superpower 70KW, and is rubescent and when beginning a large amount of splash Mars when furnace charge, closes vacuum pump, clear to furnace chargeization;
(3) open vacuum pump, vacuum tightness is low to moderate 13Pa most, refining 12min;
(4) the power failure termination of pumping adds aluminium 12g deoxidation, adds Pure Silicon Metal/ferrophosphorus, and the fusing back vacuumizes 2min to electricity, and inflated with nitrogen 5KPa adds ferro-silicon nitride, and carbon, chromium are given electric power 50KW, alloying time 5min, and in alloying latter stage, 2min adds manganese metal and aluminium before having a power failure;
(5) under the inflated with nitrogen atmosphere, steel tapping casting.
The steel ingot Chemical Composition of table 10 oriented silicon steel QX3
Figure BDA0000102053790000093
Data according to the foregoing description can be found out; Under the high vacuum situation, melt out qualified oriented silicon steel steel ingot through vacuum induction furnace; Be reduced in the sky high cost that carries out industrial experiment on the production line; Can lack under the situation of effective control device at vacuum induction furnace, realize the narrow composition scope control requirement of oriented silicon steel the nitrogen element.
Although described the present invention, the invention is not restricted to the foregoing description with reference to specific embodiment of the present invention.Without departing from the present invention, can carry out various distortion and modification.Scope of the present invention is limited claim and equivalent thereof.

Claims (7)

1. the control method of the nitrogen content in the oriented silicon steel is characterized in that:
1) pure iron raw material and carbon are put into crucible, and, will prepare burden and put into vacuum hopper by order of addition(of ingredients) by the alloy raw material proportioning that each constituent content in the orientation silicon steel calculates;
2) the heating furnace charge carries out refining to fusing to molten steel;
3) add aluminium deoxidation after the refining, the alloy that adds the not volatile element in Pure Silicon Metal or the oriented silicon steel composition subsequently carries out alloying;
4) whether determine applying argon gas or nitrogen according to the nitrogen content in the oriented silicon steel, when the nitrogen content requirement≤0.005wt% of oriented silicon steel, the charged pressure>=3KPa of argon gas; When the nitrogen content that requires oriented silicon steel surpasses 0.005wt%; In stove, charge into the nitrogen of purity>=99%, fill nitrogen pressure and an atmospheric ratio
Figure FDA0000102053780000011
is calculated as follows:
lg [ % N ] = 0.5 lg P N 2 + lg K N - lg f [ N ] lg K N = - 188 T - 1.245 lg f [ N ] = ( 3280 T - 0.75 ) Σ i = 1 n e N i [ i ]
In the formula: K NBe the equilibrium constant of nitrogen solubilizing reaction, f [N]Be the non-dimensional activity quotient of nitrogen in molten steel, [%N] is the solubleness of nitrogen in steel,
Figure FDA0000102053780000013
Be the interaction coefficient of oriented silicon steel interalloy element i to nitrogen, [i] is the content of steel interalloy element;
5) under protective atmosphere, add ferro-silicon nitride and transfer nitrogen, and it meets target content to add other alloy raw material adjustment;
6) by the time liquid steel temperature suitable after, the charged Pour Steel of vacuum.
2. the control method of the nitrogen content in the oriented silicon steel according to claim 1 is characterized in that in step 2) fusing and refining process in, close stove evacuation to stove during pressure<15Pa; Send the electrically heated furnace charge, during rubescent and a large amount of splash Mars, close vacuum pump when furnace charge; After treating that furnace charge melts clearly; The open vacuum pump, vacuum tightness<20Pa, refining 10min-15min.
3. the control method of the nitrogen content in the oriented silicon steel according to claim 1; It is characterized in that in the alloying step of step 3); After the Pure Silicon Metal of waiting to be added or the alloy of the not volatile element in the oriented silicon steel composition melt fully; Restart vacuum system, send electricity, vacuumize 2min.
4. the control method of the nitrogen content in the oriented silicon steel according to claim 1 is characterized in that in step 5), and adding the time that other alloy raw material carries out alloying is 4-7min.
5. the control method of the nitrogen content in the oriented silicon steel according to claim 4 is characterized in that in the alloying latter stage that has a power failure before waiting for tapping the alloying of transferring manganese or transferring aluminium.
6. the control method of the nitrogen content in the oriented silicon steel according to claim 1 is characterized in that when charging into argon gas or nitrogen, adds the nitrogen content of ferro-silicon nitride with the narrow composition scope in the control oriented silicon steel.
7. the control method of the nitrogen content in the oriented silicon steel according to claim 6 is characterized in that after filling nitrogen and in the early stage of alloying, adding ferro-silicon nitride in the process, can fusing fully during alloying to guarantee ferro-silicon nitride.
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Cited By (5)

* Cited by examiner, † Cited by third party
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CN104419801A (en) * 2013-08-23 2015-03-18 上海重型机器厂有限公司 Nitrogen content control method for FB2 steel smelted by vacuum induction furnace
CN105543448A (en) * 2015-12-25 2016-05-04 江苏省沙钢钢铁研究院有限公司 Method for increasing yield of antimony element in RH vacuum refining
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CN110093582A (en) * 2019-05-14 2019-08-06 东北大学 A method of gas nitriding smelts COST-FB2 steel under condition of negative pressure
CN114295435A (en) * 2021-11-26 2022-04-08 东北大学 Method for measuring Mg interaction mother coefficient in Sn-based alloy

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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN104419801A (en) * 2013-08-23 2015-03-18 上海重型机器厂有限公司 Nitrogen content control method for FB2 steel smelted by vacuum induction furnace
CN105543448A (en) * 2015-12-25 2016-05-04 江苏省沙钢钢铁研究院有限公司 Method for increasing yield of antimony element in RH vacuum refining
CN105543448B (en) * 2015-12-25 2017-12-29 江苏省沙钢钢铁研究院有限公司 A kind of method of raising RH vacuum refining antimony element recovery rates
CN106048134A (en) * 2016-07-08 2016-10-26 首钢总公司 Intermediate test method of smelted silicon steel
CN106048134B (en) * 2016-07-08 2017-11-17 首钢总公司 A kind of intermediate experiment method of smelting silicon steel
CN110093582A (en) * 2019-05-14 2019-08-06 东北大学 A method of gas nitriding smelts COST-FB2 steel under condition of negative pressure
CN110093582B (en) * 2019-05-14 2020-05-01 东北大学 Method for smelting COST-FB2 steel by gas phase nitriding under negative pressure condition
CN114295435A (en) * 2021-11-26 2022-04-08 东北大学 Method for measuring Mg interaction mother coefficient in Sn-based alloy

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