CN104862609A - Method for pressurized induction smelting of high nitrogen stainless steel through pressure control in stages - Google Patents
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Abstract
The present invention discloses a method for pressurized induction smelting of high nitrogen stainless steel through pressure control in stages, and belongs to the technical field of high nitrogen stainless steel smelting. The high nitrogen stainless steel smelted by the method comprises less than or equal to 0.2% of C, 12-23% of Mn, 15-24% of Cr, less than or equal to 1% of Si, 0-4.5% of Mo, 0.7-2% of N, 0-4.5% of Ni, and the balance of Fe. The method specifically comprises: preparing materials and determining pressurization parameters in stages; loading the materials; vacuumizing to achieve 10 Pa, and then carrying out electrifying heating; filling nitrogen gas with a purity of more than or equal to 99.99% to achieve smelting pressure after the raw material is subjected to steelmaking, alloying, and carrying out thermal insulation for 10-15 min; and filling high purity nitrogen gas until achieving a casting pressure, and then casting. According to the present invention, the nitridized alloy addition amount is optimized and the smelting pressure and the casting pressure are reasonably controlled, such that the problems of serious nitrogen segregation, nitrogen precipitation, nitrogen gas pore formation and the like during the high nitrogen stainless steel solidification process are effectively solved.
Description
Technical field
The invention belongs to high nitrogen stainless steel technical field of smelting, be specifically related to a kind of method of pressurization induction smelting high nitrogen stainless steel of control by stages pressure.
Background technology
Nitrogen is widely applied to austenitic stainless steel as important alloying element, in duplex stainless steel and Martensite Stainless Steel, by with other alloying element as Mn, Cr, Mo, V, the acting in conjunction of Nb and Ti etc., not only significantly can improve the intensity of steel, toughness, creep resistance, the multiple performance such as wear resistance and erosion resistance, and nitrogen to add in austenitic stainless steel the also expensive Ni element of alternative part as the strong austenite former of one, therefore high nitrogen stainless steel becomes a kind of important engineering materials day by day, electric power will be widely used in, shipbuilding, railway, petrochemical complex, the fields such as medical Artificial bone material.But perfect not due to high nitrogen steel technology of preparing and technique, the development of high nitrogen steel is also subject to certain restrictions, and is therefore devoted to develop high nitrogen steel technology of preparing, and promoting China's height nitrogen steel scale operation is one of current urgent problem.
For the high nitrogen stainless steel that nitrogen content exceedes normal pressure nitrogen solubility, be difficult at ambient pressure prepare, for ensureing that molten steel obtains higher nitrogen content, its smelting process must be carried out in pressured atmosphere, particularly in casting cycle, need higher environmental stress, nitrogen uneven with the composition avoiding nitrogen in high nitrogen stainless steel process of setting causing due to phase transformation and segregation is separated out and the problem of stomatal limiting value.At present, the induction furnace that pressurizes is that the variety development of high nitrogen stainless steel provides important equipment guarantee.
Two hang-ups are faced with in utilization pressurization induction furnace smelting high nitrogen stainless steel process, namely how how fast nitrogen pick-up realize the accurate control of nitrogen in steel content, determine reasonably to cast pressure with the macrosegregation avoiding nitrogen in process of setting, precipitation and stomatal limiting value simultaneously.Due to the difference of nitrogen solubleness in solid phase (δ/γ phase) and molten steel, result in the smelting pressure in pressurization induction furnace and the different of pressure of casting, increase smelting pressure effectively can improve the nitrogen content in molten steel, improves casting pressure and is then conducive to avoiding the precipitation of nitrogen and the formation of pore in solidification of molten steel process.But at smelting pressure in casting pressure (higher than smelting pressure) transition process, higher casting pressure is while the solution precipitation of nitrogen and the formation of pore, accelerate gas nitriding process, cause nitrogen content in high nitrogen stainless steel to exceed standard, thus increase the difficulty of Control of Nitrogen Content in pressurization induction furnace melting high nitrogen stainless steel process.
Summary of the invention
How effectively and reasonably, at low cost prepare in the process of high nitrogen stainless steel in pressurized Induction Melting, control the smelting pressure in nitro-alloy add-on, induction furnace and casting pressure, be improve accurate core and the key with avoiding coagulation defect of Control of Nitrogen Content.Therefore, the invention discloses a kind of method of pressurization induction smelting high nitrogen stainless steel of control by stages pressure, the method is applicable to smelt all kinds of high nitrogen stainless steel steel grade, such as, the target component of high nitrogen stainless steel steel grade can be: C :≤0.2%, Mn:12 ~ 23%, Cr:15 ~ 24%, Si :≤1%, Mo:0 ~ 4.5%, N:0.7 ~ 2%, Ni:0 ~ 4.5%, Fe: be surplus.The present invention starts with from the angle of the smelting pressure controlled in nitrogen alloy addition, induction furnace and casting pressure, furnace pressure when furnace pressure when being smelted by optimization nitro-alloy add-on and conservative control and casting, invent a kind of nitrogen alloying method that more reasonable, efficient, economic high nitrogen stainless steel is smelted, have effectively achieved the Composition Control utilizing pressurization induction furnace melting high nitrogen stainless steel, solve the problems such as the macrosegregation of nitrogen in high nitrogen stainless steel process of setting, precipitation and nitrogen pore.
Pressurize and respond to a method for smelting high nitrogen stainless steel, the method comprises following concrete steps:
(1) batching and pressure parameter are determined: according to steel grade target component, 1. calculated the smelting pressure P in induction furnace by following formula
1, and 2. calculate the casting pressure P of coming out of the stove interior in conjunction with formula
2, 3. can obtain the actual of nitrogen in raw materials for metallurgy according to formula adds weight percent (wt%) simultaneously
1; Calculate the weight percent of required raw materials for metallurgy in conjunction with raw materials for metallurgy composition with this, preparation raw materials for metallurgy, add 1.0 ~ 2.0kg/t electrolytic aluminum, for deoxidation, wherein raw materials for metallurgy comprises: technically pure iron, chromium metal or ferrochrome, metal molybdenum or molybdenum-iron, metallic nickel, manganese metal, industrial silicon, chromium nitride, graphite etc.
Steel grade target component (by weight percentage) is: C :≤0.2%, Mn:12 ~ 23%, Cr:15 ~ 24%, Si :≤1%, Mo:0 ~ 4.5%, N:0.7 ~ 2%, Ni:0 ~ 4.5%, Fe: surplus.
Smelt pressure P
1calculation formula 1.:
A＝0.13[％N]+0.118[％C]+0.043[％Si]+0.011[％Ni]+3.5×10
-5[％Ni]
2
-0.024[％Mn]+3.2×10
-5[％Mn]
2-0.01[％Mo]+7.9×10
-5[％Mo]
2
-0.048[％Cr]+3.5×10
-4[％Cr]
2
。
In formula: P
1for smelting pressure, P
θfor standard atmospheric pressure, T is smelting temperature.
Casting pressure P 2 calculation formula 2.:
P
2＝[(0.25～0.40)P
1/P
θ+(0.15～0.65)]MPa。
In raw materials for metallurgy, the actual of nitrogen adds weight percent (wt%)
1calculation formula 3.:
(wt％)
1＝[-0.02P
1/P
θ+(0.66～0.76)]×(wt％)
N。
In formula: (wt%)
nfor the weight percentage of nitrogen in target steel grade.
(2) feed: technically pure iron, chromium metal or ferrochrome, metal molybdenum or molybdenum-iron, metallic nickel are put into crucible induction furnace, oxidizable or volatilization manganese metal, industrial silicon, chromium nitride, electrolytic aluminum, graphite etc. are placed in feeding chamber.
(3) load melting: to be evacuated to below 10Pa by induction furnace, and the furnace charge that energising is warming up in pressurization induction furnace in crucible all melts.
(4) alloying: in crucible induction furnace to be pressurised raw materials for metallurgy fully melt reach melting down after, high pure nitrogen to the pressure being filled with purity>=99.999% in induction furnace is P
1, then in crucible in stove, add industrial silicon successively by feeding chamber, manganese metal, chromium nitride, graphite carry out alloying, add electrolytic aluminum deoxidation simultaneously, and be incubated 10 ~ 15min at 1530 ~ 1600 DEG C of temperature.
(5) cast: high pure nitrogen to the furnace pressure being filled with purity>=99.999% in pressurization induction furnace is P
2, then cast; After casting terminates, cooling pressure release, take out ingot casting, wherein pouring temperature is 1530 ~ 1580 DEG C, and supercharging and pouring time are 8 ~ 15min altogether.
Theoretical analysis and result of study show:
1) affect nitrogen factor of solubleness in stainless steel and be mainly alloying constituent, temperature and pressure, under the condition that alloying constituent and smelting temperature are determined, for the high nitrogen stainless steel obtaining target nitrogen content need by the smelting pressure-controlling in stove within limits.Through nitrogen solubility thermomechanical analysis and experimental study, the present invention proposes to smelt pressure P
1calculation formula 1..
2) in casting cycle, high nitrogen stainless steel is in process of setting, and the formation of δ/γ phase, reduces the solubleness of nitrogen in system, very easily causes nitrogen to separate out gentle hole shape and is a problem, and the pressure improved when casting in stove is one of effective measure avoiding this problem to occur.Through lot of experiments research, the present invention draws aforesaid about casting pressure P
2experimental formula 2..
3) higher casting pressure, while the solution precipitation of nitrogen and the formation of pore, accelerates gas nitriding process, causes nitrogen content in high nitrogen stainless steel to exceed standard; The present invention revises the nitrogen add-on in raw material, and reduce the add-on of nitrogen alloy when preparing burden, realize effective control of nitrogen content, wherein 3. nitrogen alloy addition level is calculated by aforesaid experimental formula and determine.
The invention provides a kind of method of pressurization induction smelting high nitrogen stainless steel of control by stages pressure, its beneficial effect is: the composition effectively controlling high nitrogen stainless steel, and by smelting the conservative control of pressure and casting pressure, solve the problem of high nitrogen stainless steel nitrogen pore, also effectively can reduce production cost simultaneously.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
In illustrated embodiment of the present invention, smelting equipment is 25kg pressurized Induction Melting stove, and final vacuum is 0.1Pa, and power is 50kW, and batch is 20.0 ~ 21.5kg.Below for batching and pressure parameter calculate in the formula that will use, namely formula 1., formula 2., formula 3..
Formula is 1.:
A＝0.13[％N]+0.118[％C]+0.043[％Si]+0.011[％Ni]+3.5×10
-5[％Ni]
2
-0.024[％Mn]+3.2×10
-5[％Mn]
2-0.01[％Mo]+7.9×10
-5[％Mo]
2
-0.048[％Cr]+3.5×10
-4[％Cr]
2
。
In formula: P
1for smelting pressure, P
θfor standard atmospheric pressure, T is smelting temperature.
Formula is 2.:
P
2＝[(0.25～0.40)P
1/P
θ+(0.15～0.65)]MPa。
In formula: P
2for casting pressure.
Formula is 3.:
In formula: (wt%)
1for the actual of nitrogen in raw materials for metallurgy adds weight percentage, (wt%)
nfor the weight percentage of nitrogen in target steel grade.
In illustrated embodiment of the present invention, the main component of raw materials for metallurgy used is in table 1.
Table 1 raw materials for metallurgy main component (wt%)
| Kind | Fe | Cr | N | Mn | Ni | Mo | Si | Cu | Al | C | P | S |
| Technically pure iron | 99.9 | - | 0.0036 | - | - | - | - | - | 0.002 | 0.0024 | 0.01 | 0.0034 |
| Chromium metal | 0.19 | 9.17 | 0.032 | - | - | - | 0.23 | 0.002 | 0.14 | 0.008 | ≤0.003 | 0.0048 |
| Metal molybdenum | 0.0045 | - | 0.0001 | - | 0.0031 | 99.98 | 0.0007 | - | 0.0005 | 0.001 | 0.001 | - |
| Metallic nickel | 0.0019 | - | - | 0.0006 | 99.99 | - | 0.0016 | 0.0015 | - | 0.0015 | 0.0001 | 0.0005 |
| Manganese metal | 0.019 | - | - | 99.8 | - | - | 0.0072 | - | - | 0.036 | 0.0035 | 0.033 |
| Industrial silicon | ≤0.3 | - | - | - | - | - | 99.37 | - | ≤0.3 | - | - | - |
| Chromium nitride | 0.27 | 86.58 | 11.26 | - | - | - | 0.18 | - | 0.15 | 0.016 | 0.005 | 0.001 |
Embodiment 1
Target steel grade is 18Cr18Mn2Mo0.9N, and its Composition Control scope and smelting control objectives are in table 2.
Table 2 18Cr18Mn2Mo0.9N Composition Control scope and control objectives (wt%)
Concrete steps are as follows:
(1) batching is determined with pressure parameter: according to the elemental composition of target steel grade and formula 1., formula 2., 3. formula obtain: smelt pressure P
1for 0.18MPa, casting pressure P
2for 0.99MPa, in raw materials for metallurgy, the actual of nitrogen content adds weight percentage (wt%)
1be 0.65%; With the material composition preparation raw materials for metallurgy shown in this associative list 1, add 1.5kg/t electrolytic aluminum, for deoxidation, wherein raw materials for metallurgy comprises: 12044g technically pure iron, 2683g chromium metal, 400g metal molybdenum, 3954g manganese metal, 92g industrial silicon, 1154g chromium nitride, 17.21g graphite.
(2) feed: technically pure iron, chromium metal, metal molybdenum are put into crucible, manganese metal that is oxidizable or that volatilize, industrial silicon, chromium nitride, electrolytic aluminum, graphite are placed in feeding chamber.
(3) load melting: to be evacuated to 3.4Pa, energising heats up, and initial power is 6kW, progressively rises to 30kW.
(4) alloying: after raw materials for metallurgy in crucible is melting down, high pure nitrogen to the pressure filling purity >=99.999% is 0.18MPa, then add industrial silicon successively, manganese metal, chromium nitride, graphite carries out alloying, add electrolytic aluminum deoxidation simultaneously, and be incubated 12min, wherein temperature is 1550 DEG C.
(5) cast: the high pure nitrogen filling purity >=99.999% is pressurized to 0.99MPa, casts; Casting terminates rear cooling pressure release, takes out ingot casting; Wherein pouring temperature is 1570 DEG C, and supercharging and pouring time are 8min altogether.
Ingot structure is fine and close in nitrogen pore defect, and its chemical composition is as shown in table 3.
The chemical composition (wt%) of table 3 Finished Steel
Embodiment 2
Target steel grade is 18Cr14Mn3Mo0.9N, and its Composition Control scope and smelting control objectives are in table 4.
Table 4 18Cr14Mn3Mo0.9N Composition Control scope and control objectives (wt%)
Concrete steps are as follows:
(1) batching is determined with pressure parameter: according to the elemental composition of target steel grade and formula 1., formula 2., 3. formula obtain: smelt pressure P
1for 0.28MPa, casting pressure P
2for 1.15MPa, in raw materials for metallurgy, the actual of nitrogen content adds weight percentage (wt%)
1be 0.58%; With the material composition preparation raw materials for metallurgy shown in this associative list 1, add 1.5kg/t electrolytic aluminum, for deoxidation, wherein raw materials for metallurgy comprises: 13285g technically pure iron, 2931g chromium metal, 630g metal molybdenum, 3230g manganese metal, 97g industrial silicon, 1082g chromium nitride, 18.56g graphite.
(2) feed: technically pure iron, chromium metal, metal molybdenum are put into crucible, manganese metal that is oxidizable or that volatilize, industrial silicon, chromium nitride, electrolytic aluminum, graphite are placed in feeding chamber.
(3) load melting: to be evacuated to 6.8Pa, energising heats up, and initial power is 5kW, progressively rises to 32kW.
(4) alloying: after raw materials for metallurgy in crucible is melting down, high pure nitrogen to the pressure filling purity >=99.999% is 0.28MPa, then add industrial silicon successively, manganese metal, chromium nitride, graphite carries out alloying, add electrolytic aluminum deoxidation simultaneously, and be incubated 14min, wherein temperature is 1580 DEG C.
(5) cast: the high pure nitrogen filling purity >=99.999% is pressurized to 1.15MPa, casts; After casting terminates, cooling pressure release, takes out ingot casting; Wherein pouring temperature is 1570 DEG C, and supercharging and pouring time are 9min altogether.
Ingot structure is fine and close in nitrogen pore defect, and its chemical composition is as shown in table 5.
The chemical composition (wt%) of table 5 Finished Steel
Embodiment 3
Target steel grade is 18Cr14Mn3Mo1Ni0.7N, and its chemical composition is in table 6.
Table 6 18Cr14Mn3Mo1Ni0.7N Composition Control scope and control objectives (wt%)
Concrete steps are as follows:
(1) batching is determined with pressure parameter: according to the elemental composition of target steel grade and formula 1., formula 2., 3. formula obtain: smelt pressure P
1for 0.16MPa, casting pressure P
2for 0.92MPa, in raw materials for metallurgy, the actual of nitrogen content adds weight percentage (wt%)
1be 0.48%; With the material composition preparation raw materials for metallurgy shown in this associative list 1, add 1.5kg/t electrolytic aluminum, for deoxidation, wherein raw materials for metallurgy comprises: 13177g technically pure iron, 3035g chromium metal, 2943g manganese metal, 210g metallic nickel, 631g metal molybdenum, 105g industrial silicon, 851g chromium nitride, 21.02g graphite.
(2) feed: technically pure iron, chromium metal, metal molybdenum, metallic nickel are put into crucible, manganese metal that is oxidizable or that volatilize, industrial silicon, chromium nitride, electrolytic aluminum, graphite are placed in feeding chamber.
(3) load melting: to be evacuated to 7.8Pa, energising heats up, and initial power is 6kW, progressively rises to 28kW.
(4) alloying: after raw materials for metallurgy in crucible is melting down, high pure nitrogen to the pressure filling purity >=99.999% is 0.16MPa, then add industrial silicon successively, manganese metal, chromium nitride, graphite carries out alloying, add electrolytic aluminum deoxidation simultaneously, and be incubated 12min, wherein temperature is 1580 DEG C.
(5) cast: the high pure nitrogen filling purity >=99.999% is pressurized to 0.92MPa, casts; After casting terminates, cooling pressure release, takes out ingot casting; Wherein pouring temperature is 1570 DEG C, and supercharging and pouring time are 10min altogether.
Ingot structure is fine and close in nitrogen pore defect, and its chemical composition is as shown in table 7.
The chemical composition (wt%) of table 7 Finished Steel
Claims (2)
1. a method for the pressurization induction smelting high nitrogen stainless steel of control by stages pressure, is characterized in that said method comprising the steps of:
(1) batching and pressure parameter are determined: according to the target component of high nitrogen stainless steel steel grade, 1. calculate the smelting pressure P in pressurization induction furnace by following formula
1, 2. calculate the casting pressure P in pressurization induction furnace by formula
2, 3. calculate the actual of nitrogen in raw materials for metallurgy according to formula and add weight percent (wt%)
1composition in conjunction with raw materials for metallurgy determines the weight percent of required raw materials for metallurgy, thus preparation raw materials for metallurgy, and add the electrolytic aluminum for deoxidation of 1.0 ~ 2.0kg/t, wherein, raw materials for metallurgy comprises technically pure iron, chromium metal or ferrochrome, metal molybdenum or molybdenum-iron, metallic nickel, manganese metal, industrial silicon, chromium nitride and graphite
Smelt pressure P
1calculation formula 1.,
Formula 1. in, P
1represent and smelt pressure, P
θrepresent standard atmospheric pressure, T represents smelting temperature, and A is obtained by following formulae discovery,
A＝0.13[％N]+0.118[％C]+0.043[％Si]+0.011[％Ni]+3.5×10
-5[％Ni]
2
-0.024[％Mn]+3.2×10
-5[％Mn]
2-0.01[％Mo]+7.9×10
-5[％Mo]
2
-0.048[％Cr]+3.5×10
-4[％Cr]
2
Casting pressure P
2calculation formula 2.,
P
2＝[(0.25～0.40)P
1/P
θ+(0.15～0.65)]MPa ②
Formula 2. in, P
2represent casting pressure,
In raw materials for metallurgy, the actual of nitrogen adds weight percent (wt%)
1calculation formula 3.,
③
Formula 3. in, (wt%)
1represent that in raw materials for metallurgy, the actual of nitrogen adds weight percent, (wt%)
nrepresent the weight percent of nitrogen in the target component of high nitrogen stainless steel steel grade;
(2) feed: crucible chromium metal or ferrochrome, metal molybdenum or molybdenum-iron, technically pure iron and metallic nickel being put into the induction furnace that pressurizes, manganese metal that is oxidizable or that volatilize, industrial silicon, chromium nitride, electrolytic aluminum and graphite are placed in feeding chamber;
(3) load melting: the pressure in pressurization induction furnace is evacuated to below 10Pa, and the energising furnace charge be warming up in crucible all melts;
(4) alloying: the furnace charge in the crucible of induction furnace to be pressurised fully melt reach melting down after, high pure nitrogen to the pressure being filled with purity>=99.999% in pressurization induction furnace is P
1, then in the crucible in pressurization induction furnace, add industrial silicon successively by feeding chamber, manganese metal, chromium nitride, graphite carry out alloying, add electrolytic aluminum deoxidation simultaneously, and be incubated 10 ~ 15min at 1530 ~ 1600 DEG C of temperature;
(5) cast: high pure nitrogen to the furnace pressure being filled with purity>=99.999% in pressurization induction furnace is P
2, then cast, after casting terminates, cooling pressure release, take out ingot casting, wherein, pouring temperature is 1530 ~ 1580 DEG C, and supercharging and pouring time are 8 ~ 15min altogether.
2. method according to claim 1, is characterized in that the target component of described high nitrogen stainless steel steel grade is by weight percentage: be no more than the C of 0.2%, 12 ~ 23% Mn, 15 ~ 24% Cr, be no more than 1% Si, be no more than 4.5% Mo, 0.7 ~ 2% N, be no more than the Ni of 4.5%, the Fe of surplus.
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| CN106011371A (en) * | 2016-06-24 | 2016-10-12 | 东北大学 | Pressurizing induction and pressurizing electroslag remelting duplex high-nitrogen steel smelting method |
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| CN106513619A (en) * | 2016-12-02 | 2017-03-22 | 机械科学研究总院青岛分院 | Process for centrifugally casting high-nitrogen austenitic stainless steel pipe at normal pressure |
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| CN111850422A (en) * | 2020-04-30 | 2020-10-30 | 中科益安医疗科技（北京）股份有限公司 | High-nitrogen nickel-free austenitic stainless steel seamless thin-walled tube and preparation method thereof |
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| CN112281049A (en) * | 2020-11-23 | 2021-01-29 | 浙江宝武钢铁有限公司 | Preparation method of non-magnetic high-nitrogen stainless steel |
| CN112695151A (en) * | 2020-12-18 | 2021-04-23 | 东北大学 | Method for obtaining solidification pressure required by preparing high-nitrogen austenitic stainless steel through pressure induction and preparation method |
| CN112733465A (en) * | 2020-12-18 | 2021-04-30 | 东北大学 | Method for acquiring solidification pressure required by pressurized electroslag remelting high-nitrogen austenitic stainless steel and preparation method |
| CN112695151B (en) * | 2020-12-18 | 2022-01-25 | 东北大学 | Method for obtaining solidification pressure required by preparing high-nitrogen austenitic stainless steel through pressure induction and preparation method |
| CN112733465B (en) * | 2020-12-18 | 2023-06-02 | 东北大学 | Method for acquiring solidification pressure required by pressurizing electroslag remelting high-nitrogen austenitic stainless steel and preparation method |
| CN113388709A (en) * | 2021-06-11 | 2021-09-14 | 东北大学 | Method for accurately controlling nitrogen content in high-nitrogen stainless steel |
| CN116024398A (en) * | 2023-02-24 | 2023-04-28 | 东北大学 | Determination method for minimum value of solidification pressure for inhibiting nitrogen pores, application of determination method and preparation method of high-nitrogen stainless steel cast ingot |
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