CN116144937A - Electroslag mixing method for inhibiting boron element burning loss in boron-containing nitrogen-containing heat-resistant steel - Google Patents
Electroslag mixing method for inhibiting boron element burning loss in boron-containing nitrogen-containing heat-resistant steel Download PDFInfo
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- 239000010959 steel Substances 0.000 title claims abstract description 96
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 80
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- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000002156 mixing Methods 0.000 title claims abstract description 34
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 230000002401 inhibitory effect Effects 0.000 title claims abstract description 21
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/18—Electroslag remelting
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Abstract
The invention discloses an electroslag mixing method for inhibiting boron element burning loss in boron-containing nitrogen-containing heat-resistant steel, which comprises the steps of adding electroslag mixing slag into a heat-resistant steel ingot, wherein the electroslag mixing slag comprises boron nitride and carbon powder; electroslag remelting is carried out in a protective atmosphere, and the filling ratio d= (0.6-0.8) D is the diameter of the crystallizer; the melting speed of the electroslag is controlled to be 7-11 kg/min. The invention optimizes the electroslag remelting voltage, current and melting speed setting according to the steel grade characteristics, the steel billet specification and the filling ratio. For large size, the melting speed of the billet is appropriately reduced with a large filling ratio to suppress the segregation of components. Aiming at the B element burning loss, the full-flow process optimization is carried out, and the method starts from the aspects of component optimization, billet solidification (including heat treatment) and electroslag remelting process, truly stabilizes and improves the yield of B, and realizes the component stability control of the boron-containing nitrogen-containing heat-resistant steel in smelting.
Description
Technical Field
The invention relates to the technical field of ferrous metallurgy, in particular to an electroslag mixing method for inhibiting boron element burning loss in boron-containing nitrogen-containing heat-resistant steel.
Background
The loss of a large amount of easily burnt element B in the electroslag remelting process of the boron-containing and nitrogen-containing martensitic heat-resistant steel for the turbine blade is a key common problem affecting component control in the smelting process. In the production practice of heat-resistant steel, the content of part B is relatively high, particularly the B content of the heat-resistant steel containing boron and nitrogen is easy to have large fluctuation in the smelting process, and the yield of the B is extremely unstable in several key technical links (such as external refining, electroslag remelting and the like). The fluctuation between the upper limit and the lower limit of the possible control range of the B content in the steel billet is difficult to realize stable control of the B element by only reserving the burning loss allowance in the ingredients (the condition that the B content exceeds the upper limit or is lower than the lower limit is easy to occur), and the receiving rate of the practical stable relation B is an effective way for realizing stable control of the components.
Firstly, key nodes for component control are found out through field investigation, and secondly, a burning loss mechanism of B element in the smelting is combed, so that a B stable control process scheme is formulated on the basis.
1. Key process node
The whole-course follow-up production is carried out on the boron-containing and nitrogen-containing heat-resistant steel 10Cr11Co3W3NiMoVNbNB (vacuum induction furnace+ESR (electro slag remelting)) and the composition change condition of the elements easy to burn and damage in each process link is recorded (as shown in figure 1). Fig. 1 shows the content change conditions of the elements easy to burn (ingredients-induction furnace tapping ingredients-electrode bar ingredients-electroslag ingot ingredients) at each stage of vacuum induction + ESR smelting (unregulated process) of the boron-containing nitrogen-containing heat-resistant steel. In the figure, the composition is greatly reduced after the ESR treatment; obvious Si increasing phenomenon occurs; increasing Al after ESR; the Nb content remained relatively stable.
The B element remains relatively stable during the external refining process, but is greatly reduced after the electroslag remelting treatment.
The investigation found that the B and N elements are often added in the form of alloys at the late stage of external refining (LF or VD) or before tapping, at which time the composition can be fine-tuned. At this time, the relative content of B is relatively stable, and the N content changes with time (N increase phenomenon may occur when the N content is low, and gradually decreases with time when the N content is too high).
The content of B is obviously reduced after electroslag remelting treatment, the B receiving rate generally fluctuates between 40 and 70 percent, and the B is not burnt at all under individual conditions. The key process node that can affect the final yield of B element is electroslag remelting.
2. Burning loss of B element
The action, the existence form and the main burning loss mechanism of B (including N) elements in the heat-resistant steel are clear:
(1) The B, N element in the heat-resistant steel has the main functions:
the solubility of B in Fe is low, and a small amount of B (less than or equal to 8 ppm) is dissolved in the matrix in a solid manner, so that the hardenability of the material can be improved. The B content in the boron-containing heat-resistant steel is relatively high (0.03 percent or more and 0.01 percent or more), and most of B can be biased to grain boundaries in a free state or a compound form. Wherein, the free B and the inter-crystal carbide are combined to form a boron carbon compound (such as M23 (C, B) 6 and the like), so that the Ostwald ripening of the inter-crystal carbide can be inhibited, and the high-temperature durability and the high-temperature creep property of the material can be obviously improved.
The N element can replace a part of noble metal to improve the yield strength of the steel, and meanwhile, the influence on plasticity and toughness is small under the cooperation of nitrogen fixation elements such as V, nb, al and the like. As an austenite forming element, the formation of detrimental phase delta ferrite can be suppressed, and the structural uniformity can be improved. Furthermore, the addition of N to the heat-resistant steel improves the corrosion resistance of the material.
The BN precipitation phase generated by the reaction of B and N in the steel has the characteristic similar to MnS, and has little influence on the performance of a steel billet when the content is lower and the size is smaller; and when the content is higher, the cutting performance of the material can be improved when the size is larger.
(2) B, N form of existence
The B existing form in the heat-resistant steel comprises solid solution form, free form or compound form which is biased to grain boundary. B has higher chemical activity at high temperature, can react with N and O in steel to generate nitride and oxide with stable structure. The oxidation activity of B in smelting is higher than Mn, si and lower than Ti and AI. B is preferentially reacted with Mn, si and O in the smelting process to produce oxides, and if the oxides of boron cannot be reduced in time, the oxides of boron are easily adsorbed by slag, so that boron element loss is caused. The oxidation reaction of B is directly influenced by the oxygen content in molten steel, and when the oxygen content exceeds a certain threshold value, the proportion of B oxide in the total boron content gradually increases as the oxygen content increases.
[Mn]+[O]＝[MnO] s ΔG θ ＝-244300+107.6T
1/2[Si]+[O]＝1/2[SiO 2 ] s ΔG θ ＝-288220+109.1T
2/3[Al]+[O]＝1/3[Al 2 O 3 ] s ΔG θ ＝-408333+131.3T
1/2[Ti]+[O]＝1/2[TiO 2 ] s ΔG θ ＝-330960+114T
2/3[B]+[O]＝1/3[B 2 O 3 ] s ΔG θ ＝-254806.5+95.5T
B reacts with N to form stable compound BN, and the binding capacity of B and N is higher than Al (opposite to 1700 ℃ C.) and lower than Ti and Zr at relatively low temperature (1700 ℃ C.) as shown below. BN is easily gradually precipitated along with grain boundary movement during unbalanced solidification of a steel billet, so that the content and the morphology size of BN are simultaneously affected by the content of B, N in the steel and the solidification rate of the steel billet. If a large number of large-size BN or BN cluster structures exist in the heat-resistant steel electrode rod, the precipitated structures are easily adsorbed by slag in the electroslag process, so that the total B content is greatly reduced.
[Ti]+[N]＝[TiN] s ΔG θ ＝-291000+107.9T
[B]+[N]＝[BN] s ΔG θ ＝-267486+100.3T
[Al]+[N]＝[AlN] s ΔG θ ＝-129626+19.72T
3. Inhibiting B burn-out
By analyzing the burning loss mechanism, the inhibition of the loss of B element in the smelting process is started from the aspects of oxygen control and nitrogen fixation, and the conventional treatment at present is often concentrated on optimizing the deoxidization system and strengthening the deoxidization. But the nitriding burn-out of B is not of sufficient concern. For heat resistant steels containing both boron and nitrogen, the B loss due to nitriding burn-out may be no worse than that due to oxidizing burn-out.
Disclosure of Invention
The invention aims to provide an electroslag mixing method for inhibiting boron element burning loss in boron-containing nitrogen-containing heat-resistant steel. In order to achieve the above purpose, the present invention provides the following technical solutions:
an electroslag slag mixing method for inhibiting boron burning loss in boron-containing nitrogen-containing heat-resistant steel, which comprises the following steps of,
adding electroslag slag mixture into the heat-resistant steel ingot, wherein the electroslag slag mixture comprises boron nitride and carbon powder;
electroslag remelting is carried out in a protective atmosphere, and the filling ratio d= (0.6-0.8) D is the diameter of the crystallizer; the melting speed of the electroslag is controlled to be 7-11 kg/min.
Further, the electroslag mixing slag also comprises CaF 2 、Al 2 O 3 One or more of CaO.
Further, in the electroslag mixed slag, the content of boron nitride is 0.01-0.02%, and the content of carbon powder is 0.1-0.15%.
Further, the electroslag remelting is carried out by adopting a protective atmosphere, which comprises
In the process of electroslag remelting by adopting protective atmosphere, introducing the protective atmosphere into a crystallizer for 10-15 min at a high flow rate before arc striking, and gradually reducing the flow rate of inert gas after the electroslag remelting processing is stable;
o in electroslag remelting process after flow of inert gas is adjusted downwards 2 The content is less than or equal to 0.02 percent.
Further, the average voltage in the electroslag remelting stabilization stage is 45-46V.
Further, for the heat-resistant steel ingot with the total weight of less than or equal to 3t, the electroslag melting speed is controlled to be 7-9 kg/min, and for the heat-resistant steel ingot with the total weight of more than or equal to 3t, the electroslag melting speed is controlled to be 9-11 kg/min.
Further, the method further comprises the steps of,
and standing the electroslag ingot in a crystallizer for 1-2 h, tapping, cooling for 24-36 h, and then annealing at 750-800 ℃ for 24-30 h.
Further, the obtaining of the heat-resistant steel ingot comprises,
pretreatment of raw materials: performing shot blasting treatment on the alloy raw material, completely removing oxide skin, and weighing for later use;
charging and melting: loading alloy raw materials into a crucible in a loosening and tightening mode, vacuumizing a furnace, feeding power to start smelting after the vacuum degree of a smelting chamber is lower than 20Pa, sampling and analyzing after the alloy quantity is smelted, and performing fine adjustment on the components in the furnace;
vacuum carbon deoxidization refining: heating to refining temperature, refining for 50-80 min in vacuum environment, adding deoxidizer, melting, sampling and analyzing, adding Nb-Fe and V-Fe, and stirring;
adding ferroboron, tapping and pouring: adding N-Cr and sponge Ti, stirring, adding B-Fe and Mn after melting, charging inert gas to increase the pressure in the furnace, controlling the tapping temperature range at 1550-1650 ℃, and casting to obtain the heat-resistant steel ingot.
Further, the heat-resistant steel ingot comprises the following raw material components in percentage by mass: 0.09-0.11 part of C, 0.4-0.5 part of Mn, less than or equal to 0.1 part of Si, less than or equal to 0.015 part of P, less than or equal to 0.01 part of S, 11-11.5 parts of Cr, 0.3-0.7 part of Ni, 0.1-0.4 part of Mo, 2.5-3.5 parts of Co, 2.4-3 parts of W, 0.2-0.24 part of V, 0.08-0.14 part of Nb, 0.012-0.02 part of N, 0.015-0.02 part of B, 0.01-0.015 part of Al and 0.01-0.02 part of Ti, and the balance of Fe except a small amount of impurity elements.
Further, in the vacuum carbon deoxidation refining process, the oxygen content in the electrode parent metal is controlled to be less than or equal to 30ppm.
Further, after casting to obtain a heat-resistant steel ingot, when the content of B in the head and the tail of the electrode rod is at the lower control limit, homogenizing the electrode parent metal for at least 10 hours at 1050-1150 ℃;
and removing the riser and the water gap end of the electrode rod after heat treatment, and carrying out surface polishing or polishing treatment.
The invention has the technical effects and advantages that:
(1) Component optimization
The alloy composition is first optimized, especially for B, N content and the content of various kinds of nitrogen fixing elements. B. The relation between N content refers to an empirical formula lg [ B ] = -2.45lg [ N ] -6.81, (wherein [ B ], [ N ] are mass percentages of B and N, as shown in figure 2), and figure 2 is the relation between B, N mass percent in heat-resistant steel and BN precipitation and morphology size (large frame: protocol range of B, N content in alloy; small frame: optimized B, N content). In the diagram, the formula corresponds to the B, N component range on the right upper part of the straight line, so that BN is easy to generate; and the corresponding component range at the lower right part of the formula is generally not easy to generate BN. When the logarithmic relation of N, B of the steel billet is close to an empirical formula at 1050-1150 ℃, BN in the steel is mainly dispersed and distributed small-size particles; when lg [ B ] > -2.45lg [ N ] -6.81, BN is a large-size cluster structure; when lg [ B ] < -2.45lg [ N ] -6.81, BN is hardly precipitated in the steel billet. It is considered to increase the nitrogen fixation element ratio in the steel, such as to appropriately increase the relative contents of V, nb, al (residual Al in the steel) in the heat-resistant steel.
(2) Increase the nitrogen-strengthening element
Increasing the content of certain strong nitrogen elements (Ti, zr). M. Kapania et Al propose an effective boron estimation formula (shown below) reflecting the relationship between nitrogen fixation element and effective boron (acid soluble boron) (wherein 0.002 is the weight of nitrogen fixation element such as Al, V, etc.).
Since Ti reacts with N to form cubic TiN, the structure is easy to form crack sources, has negative influence on the fatigue performance of materials, ti in heat-resistant steel is often used as an impurity element, but the content can be considered to be properly increased, and the content can be controlled according to the lower middle limit of the composition.
(3) Enhanced deoxygenation
The deoxidization process in the smelting process is enhanced, and the oxygen content in the molten steel before tapping is controlled below 30ppm. The impact performance of the heat-resistant steel is required to be inspected, high requirements are put on inclusion control, and meanwhile, the content of Al and Si is required to be strictly controlled. Al can reduce SiO in slag in smelting 2 The steel billet is increased in Si, so that C and Al are generally adopted as main deoxidizers, and the total amount of Al is strictly controlled. But moderately improves the content of residual Al in the steel billet so as to prevent oxygenation in the smelting process.
After deoxidization, the alloy containing B and N is added, and the alloy contains more impurities and impurities, and is preferably purified before use, so that the content of impurity elements is reduced.
(4) Solidification rate of billet
The shape and the size of BN are directly influenced by the solidification rate, and when the solidification rate is higher, the BN is in a small-size particle structure in dispersion distribution; and when the solidification rate is low, BN particles are easy to agglomerate to form a large-size cluster structure. And the solidification rate of the steel billet is improved (such as properly reducing the casting temperature, adopting auxiliary cooling means and the like), so that BN with a large-size cluster structure is avoided.
(5) Heat treatment of
For some large-sized heat-resistant steel billets, the composition segregation is serious, it is difficult to suppress the occurrence of a large amount of BN of a cluster structure by rapid solidification, and it is considered to reduce the relative content of BN by the homogenization heat treatment. The heat treatment temperature is controlled at 1050-1150 ℃, the diffusion rate of residual Al in steel is improved, and BN is reduced by Al.
(6) Electroslag mixing optimization scheme
The electroslag remelting process needs to start from the aspects of optimizing protective atmosphere, slag system and slag mixing raw materials and technological parameters, wherein the important point is the adjustment of the protective atmosphere and slag mixing components.
First of all it must be ensured that O in the crystallizer 2 、N 2 The content is low enough to avoid serious element burning loss of the steel billet in the electroslag remelting process. The air tightness of the equipment is detected before ESR treatment, so that air infiltration is avoided; ar with higher purity is used as a protective atmosphere; ar is introduced into the crystallizer at a large flow rate before arc introduction, and the flow lasts for more than 10 minutes, so that air in the crystallizer is discharged as much as possible; after arc striking, ar is continuously introduced at a large flow, so that the protective atmosphere is prevented from being heated and expanded to the greatest extent, convection is formed between the Ar and air in an exhaust pipeline, and impurity gas is involved; and gradually reducing the flow rate of Ar after the process is stable.
Optimizing electroslag mixing components: ternary slag systems (such as CaF) with good inclusion removal effect are adopted 2 :Al 2 O 3 Cao=60:20:20), small amounts of BN powder and carbon powder as deoxidizer were added to form a slag mix. BN can increase B in slag 3+ The ratio of ions inhibits oxidation or nitridation of free B between slag and gold during ESR. The carbon powder can inhibit oxidation burning loss of steel billet elements in the arc striking stage, and simultaneously reduce C element burning loss in steel billets.
And (3) electroslag technological parameter adjustment: and optimizing electroslag remelting voltage, current and melting speed setting according to steel grade characteristics, steel billet specifications and filling ratios. For large size, the melting speed of the billet is appropriately reduced with a large filling ratio to suppress the segregation of components.
Aiming at the B element burning loss, the full-flow process optimization is carried out, and the method starts from the aspects of component optimization, billet solidification (including heat treatment) and electroslag remelting process, truly stabilizes and improves the yield of B, and realizes the component stability control of the boron-containing nitrogen-containing heat-resistant steel in smelting.
The invention starts from the two aspects of inhibiting the precipitation of B compound in steel and reducing the slag loss of B in smelting, improves the billet solidification rate by optimizing components, adding nitrogen fixation elements, properly reducing casting temperature, carrying out solution treatment on electrode bars, carrying out electroslag remelting in Ar atmosphere with low O2 environment, and particularly adopting CaF 2 /Al 2 O 3 Electricity of +BN +carbon powderAnd carrying out electroslag remelting treatment by a slag mixing scheme. The method has obvious effects of improving the yield of boron elements in the electroslag remelting process of the boron-containing and nitrogen-containing steel (particularly steel grade with relatively high boron content) and realizing the stable control of B elements.
According to the invention, a small amount of BN is added into the mixed slag, so that stable control of B element in the electroslag remelting process of boron-containing steel (B% is 0.01-0.03%) is realized. And the BN added in each furnace time occupies relatively low weight, and hardly influences the ESR smelting cost. The yield of B can be improved from 40-50% to 70-80%, the consumption of boron-containing alloy in smelting is reduced, and impurities introduced along with the alloy are reduced.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and drawings.
Drawings
FIG. 1 shows the variation of Al, si, B and Nb components in each process of smelting the boron-containing nitrogen-containing heat-resistant steel;
FIG. 2 is a graph showing the relationship between the content of heat-resistant steel B, N and BN precipitation (1050 to 1150 ℃ C.);
FIG. 3 is a flow chart of an electroslag mixing method for inhibiting boron burning loss in boron-containing nitrogen-containing heat-resistant steel.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to solve the defects in the prior art, the invention discloses an electroslag slag mixing method for inhibiting boron element burning loss in boron-containing nitrogen-containing heat-resistant steel, which is shown in figure 3 and comprises the following steps:
pretreatment of raw materials: performing shot blasting treatment on the alloy raw material, completely removing oxide skin, and weighing for later use;
charging and melting: loading alloy raw materials into a crucible in a loosening and tightening mode, vacuumizing a furnace, feeding power to start smelting after the vacuum degree of a smelting chamber is lower than 20Pa, sampling and analyzing after the alloy quantity is smelted, and performing fine adjustment on the components in the furnace;
vacuum carbon deoxidization refining: heating to refining temperature, refining for 50-80 min in vacuum environment, adding deoxidizer, melting, sampling and analyzing, adding Nb-Fe and V-Fe, and stirring;
adding ferroboron, tapping and pouring: adding N-Cr and sponge Ti, stirring, adding B-Fe and Mn after melting, charging inert gas to increase the pressure in the furnace, controlling the tapping temperature range at 1550-1600 ℃, and casting to obtain the heat-resistant steel ingot.
Electroslag remelting: caF is preferably adopted in the invention for mixing slag 2 :Al 2 O 3 Cao=60:20:20 ternary slag system (or CaF 2 :Al 2 O 3 =70:30 binary slag system), pre-melted slag is adopted as much as possible, the total slag amount depends on the specification of the crystallizer, and the middle lower limit of the allowable range of the equipment is determined; the content of boron nitride in the slag is 0.01-0.02%, and the content of carbon powder is 0.1-0.15%. In the invention, preferably, 0.02 percent of BN and 0.1 percent of carbon powder are added to form mixed slag, and the mixed slag system and BN are fully baked for 6 to 8 hours at 800+/-20 ℃ before being used. In the invention, the preferable slag mixing process parameters are as follows: filling ratio d= (0.6-0.8) D, D being the crystallizer diameter; in the electroslag process, high-purity Ar is adopted as protective atmosphere, the high-purity Ar is introduced into a crystallizer at a large flow rate (10-15 min) before arc striking, and the Ar flow rate is gradually reduced after ESR processing is stable, so that O in the electroslag process is ensured 2 The content is less than or equal to 0.02 percent; the average voltage in the ESR stabilization stage is 45-46V; for the electrode rod with the melting speed less than or equal to 3t, the electroslag melting speed is controlled to be 7-9 kg/min, and for the ingot with the melting speed more than or equal to 3t, the melting speed is controlled to be 9-11 kg/min; and standing the electroslag ingot in a crystallizer for 1-2 h, tapping, cooling for 24-36 h, and then annealing at 750-800 ℃ for 24-30 h.
In a specific embodiment of the invention, the raw material components of the boron-containing and nitrogen-containing heat-resistant steel are as follows in percentage by mass: 0.08 to 0.12 percent of C, 0.35 to 0.6 percent of Mn, less than or equal to 0.1 percent of Si, less than or equal to 0.015 percent of P, less than or equal to 0.01 percent of S, 10 to 12.5 percent of Cr, 0.3 to 0.7 percent of Ni, 0.1 to 0.4 percent of Mo, 2.5 to 3.5 percent of Co, 2.4 to 3 percent of W, 0.15 to 0.25 percent of V, 0.05 to 0.15 percent of Nb, 0.01 to 0.4 percent of N, less than or equal to 0.01 to 0.03 percent of B, less than or equal to 0.02 percent of Al, less than or equal to 0.04 percent of Ti, and the balance of Fe except a small amount of impurity elements. The component optimization scheme for inhibiting the B burning loss comprises the following steps of: n is taken as the middle and lower limit (0.012-0.02%), B is taken as the middle limit (0.015-0.02%), V is controlled according to the upper limit (0.2-0.24%), and Nb is controlled according to the upper limit (0.08-0.14%); cr and Mn are controlled according to the upper limit (respectively 11-11.5%, 0.4-0.5%); c is controlled according to the middle lower limit (0.09-0.11%); adding proper amount of Ti (0.01-0.02%) as strong nitrogen element, and controlling the residual Al in steel according to the upper limit (0.01-0.015%).
In a specific embodiment of the invention, al is used for deoxidization, so that the residual Al in molten steel before tapping casting is ensured to be in the range of 0.01-0.015%; the oxygen content in the electrode parent metal is controlled to be less than or equal to 30ppm.
In one specific embodiment of the invention, B is added before tapping in the form of Fe-B alloy, and remelting treatment is carried out before Fe-B is used, so that B in the alloy is homogenized, and impurity elements and impurities are removed as much as possible; n is added in a nitrogen-containing alloy mode, alloy raw materials with fewer impurities and more uniform components are selected as far as possible; B. n is added separately and it must be ensured that the added alloy is totally dissolved.
In a specific embodiment of the invention, the casting temperature is designed according to the charging amount, the tapping temperature of the steel grade is controlled within 1550-1600 ℃, and the casting temperature is reduced as much as possible under the condition of allowing (avoiding casting); if the B content of the head and the tail of the electrode rod is relatively low (the B content is at the control lower limit), the electrode parent metal is subjected to homogenization treatment for at least 10 hours at 1050-1150 ℃. And removing the riser and the water gap end of the electrode rod after heat treatment, and carrying out surface polishing or polishing treatment.
The following is a further illustration of the inventive arrangements, but is not intended to limit the invention.
Example 1
An electroslag slag mixing scheme for inhibiting boron burning loss in boron-containing nitrogen-containing heat-resistant steel, which comprises the following steps:
1) Pretreatment of raw materials: the alloy raw materials are shot-blasted, surface oxide skin is removed, the alloy raw materials are weighed according to the component ranges and then are respectively put into a vacuum induction furnace, the components are shown in the table (wherein V-Fe and B-Fe are remelted in the vacuum induction furnace before being used):
TABLE 1 boron-containing and Nitrogen-containing heat-resistant Steel composition control Range (wt%)
2) Firstly, loading Fe, fe-Ni, fe-Cr, co, mo-Fe and W-Fe alloy materials into a crucible; vacuumizing the furnace to below 20Pa, and starting power transmission;
3) Sampling and analyzing after melting the alloy, and fine-adjusting the components in the furnace to ensure that the main components are in a control range;
4) Refining in a vacuum environment for 50-60 min, adding deoxidizer after refining, sampling and analyzing after melting, adding Nb-Fe and V-Fe respectively, and stirring;
5) Adding N-Cr and sponge Ti, stirring, adding B-Fe and Mn after melting, and filling Ar gas to improve the pressure in the furnace and measure the temperature;
6) Controlling the tapping temperature range at 1550-1600 ℃ and casting a billet at about 3t; the billet is homogenized at 1050-1150 ℃ for 10h.
7) After solidifying the billet, removing the riser end and the water gap end and processing the surface, welding a false electrode to prepare an electrode rod, and charging by an electroslag furnace;
8) Detecting the air tightness of equipment before electroslag remelting treatment, taking high-purity Ar as a protective atmosphere, continuously introducing the high-purity Ar into a crystallizer for 10min at a high flow rate before arc initiation, and ensuring O in the crystallizer under the Ar protective atmosphere 2 The content is less than 0.03%;
9) By CaF 2 :Al 2 O 3 CaO=60:20:20 ternary slag system, the total slag amount is 150kg, 0.02% BN and 0.1% carbon powder are added into slag to form mixed slag, wherein the mixed slag system and BN are baked for 6-8 hours at 800+/-20 ℃ before use; the mixed slag is temporarily stored in a 100 ℃ oven and is taken out quickly.
10 The steel material is used as a base cushion and an arc striking agent to carry out electroslag remelting treatment, the voltage in a stable stage is controlled to be 45-46V, and the average melting speed of electroslag is controlled to be 7-9 kg/min;
11 Steel billet is tapped after being cooled for 1 to 2 hours along with the furnace, is subjected to cover cooling for 24 to 36 hours, and is then subjected to annealing treatment for 24 to 30 hours at the temperature of 750 to 800 ℃.
Example 2
And carrying out an electroslag remelting test of a 150 kg-grade 10Cr11Co3W3NiMoVNbNB electrode rod in a laboratory, comparing the change conditions of the easily burnt elements in the billets before and after treatment, and calculating the element yield.
The diameter of the electrode rod is phi 150mm, and the inner diameter of the crystallizer is phi 220mm; the electroslag system is CaF 2 :Al 2 O 3 CaO=60:20:20 ternary slag system, total slag amount is 15kg; adding carbon powder and BN into slag to form mixed slag, and adopting two slag mixing schemes respectively: 0.1% carbon powder+0.02% BN,0.1% carbon powder+0.04% BN; the electroslag melting speed is 6-7 kg/min (for small ingot type, the melting speed is further adjusted downwards).
The composition comparison and element yield of the easy-to-burn elements before and after the electroslag of the steel billet are shown in the table 2, wherein the slag mixing scheme of adding 0.02% BN is adopted, the yield of B reaches 94.44%, and the yield of Nb approaches 100%; the 0.04% BN slag mixing scheme is adopted, the B yield is 77.27%, and the Nb yield is 92.23%. In both slag mixing schemes, the Si content in the steel billet is reduced to different degrees, and the phenomenon of Al increase exists.
TABLE 2 yield of 10Cr11Co3W3NiMoVNbNB billet B before and after electroslag remelting
Finally, it should be noted that: the foregoing description is only illustrative of the preferred embodiments of the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements or changes may be made without departing from the spirit and principles of the present invention.
Claims (11)
1. An electroslag mixing method for inhibiting boron element burning loss in boron-containing and nitrogen-containing heat-resistant steel is characterized by comprising the following steps of,
adding electroslag slag mixture into the heat-resistant steel ingot, wherein the electroslag slag mixture comprises boron nitride and carbon powder;
electroslag remelting is carried out in a protective atmosphere, and the filling ratio d= (0.6-0.8) D is the diameter of the crystallizer; the melting speed of the electroslag is controlled to be 7-11 kg/min.
2. The electroslag mixing method for inhibiting boron burning loss in boron-containing and nitrogen-containing heat-resistant steel as claimed in claim 1, wherein the electroslag mixing further comprises CaF 2 、Al 2 O 3 One or more of CaO.
3. The electroslag mixing method for inhibiting boron loss in boron-containing and nitrogen-containing heat-resistant steel according to claim 1 or 2, wherein the content of boron nitride in the electroslag mixing slag is 0.01-0.02%, and the content of carbon powder is 0.1-0.15%.
4. The method for suppressing burning loss of boron element in heat resistant steel containing boron and nitrogen as claimed in claim 1, wherein the electroslag remelting is carried out in a protective atmosphere comprising
In the process of electroslag remelting by adopting protective atmosphere, introducing the protective atmosphere into a crystallizer for 10-15 min at a high flow rate before arc striking, and gradually reducing the flow rate of inert gas after the electroslag remelting processing is stable;
o in electroslag remelting process after flow of inert gas is adjusted downwards 2 The content is less than or equal to0.02％。
5. The electroslag mixing method for inhibiting boron burning loss in boron-containing and nitrogen-containing heat-resistant steel of claim 4, wherein,
the average voltage of the electroslag remelting stabilization stage is 45-46V.
6. The electroslag mixing method for inhibiting boron burning loss in boron-containing and nitrogen-containing heat-resistant steel of claim 4, wherein,
for the heat-resistant steel ingot with the total weight of less than or equal to 3t, the electroslag melting speed is controlled to be 7-9 kg/min, and for the heat-resistant steel ingot with the total weight of more than or equal to 3t, the electroslag melting speed is controlled to be 9-11 kg/min.
7. The method for suppressing burning loss of boron element in boron-containing and nitrogen-containing heat-resistant steel according to claim 1, further comprising,
and standing the electroslag ingot in a crystallizer for 1-2 h, tapping, cooling for 24-36 h, and then annealing at 750-800 ℃ for 24-30 h.
8. The electroslag mixing method for inhibiting boron loss in boron-containing and nitrogen-containing heat-resistant steel as claimed in claim 1, wherein the obtaining of the heat-resistant steel ingot comprises,
pretreatment of raw materials: performing shot blasting treatment on the alloy raw material, completely removing oxide skin, and weighing for later use;
charging and melting: loading alloy raw materials into a crucible in a loosening and tightening mode, vacuumizing a furnace, feeding power to start smelting after the vacuum degree of a smelting chamber is lower than 20Pa, sampling and analyzing after the alloy quantity is smelted, and performing fine adjustment on the components in the furnace;
vacuum carbon deoxidization refining: heating to refining temperature, refining for 50-80 min in vacuum environment, adding deoxidizer, melting, sampling and analyzing, adding Nb-Fe and V-Fe, and stirring;
adding ferroboron, tapping and pouring: adding N-Cr and sponge Ti, stirring, adding B-Fe and Mn after melting, charging inert gas to increase the pressure in the furnace, controlling the tapping temperature range at 1550-1650 ℃, and casting to obtain the heat-resistant steel ingot.
9. The electroslag mixing method for inhibiting boron loss in boron-containing and nitrogen-containing heat-resistant steel according to claim 1 or 8, wherein,
the heat-resistant steel ingot comprises the following raw material components in percentage by mass: 0.09-0.11 part of C, 0.4-0.5 part of Mn, less than or equal to 0.1 part of Si, less than or equal to 0.015 part of P, less than or equal to 0.01 part of S, 11-11.5 parts of Cr, 0.3-0.7 part of Ni, 0.1-0.4 part of Mo, 2.5-3.5 parts of Co, 2.4-3 parts of W, 0.2-0.24 part of V, 0.08-0.14 part of Nb, 0.012-0.02 part of N, 0.015-0.02 part of B, 0.01-0.015 part of Al and 0.01-0.02 part of Ti, and the balance of Fe except a small amount of impurity elements.
10. The electroslag mixing method for inhibiting boron burning loss in boron-containing and nitrogen-containing heat-resistant steel as claimed in claim 8, wherein,
in the vacuum carbon deoxidizing refining process, the oxygen content in the electrode parent metal is controlled to be less than or equal to 30ppm.
11. The electroslag mixing method for inhibiting boron burning loss in boron-containing and nitrogen-containing heat-resistant steel as claimed in claim 8, wherein,
after casting to obtain a heat-resistant steel ingot, when the content of B at the head and the tail of the electrode rod is in the lower control limit, carrying out homogenization treatment on the electrode parent metal for at least 10 hours at 1050-1150 ℃;
and removing the riser and the water gap end of the electrode rod after heat treatment, and carrying out surface polishing or polishing treatment.
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