CN113355587A - High-speed steel and method for comprehensively improving as-cast structure by microalloying magnesium and rare earth thereof and increasing solidification pressure - Google Patents
High-speed steel and method for comprehensively improving as-cast structure by microalloying magnesium and rare earth thereof and increasing solidification pressure Download PDFInfo
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Abstract
The invention belongs to the technical field of high-speed steel, and particularly relates to high-speed steel and a method for comprehensively improving an as-cast structure by microalloying magnesium and rare earth of the high-speed steel and increasing solidification pressure. The invention provides a method for improving a cast structure of high-speed steel, which comprises the following steps: smelting industrial pure iron, a chromium-containing raw material, a molybdenum-containing raw material, metal tungsten, metal cobalt, graphite, industrial silicon, a manganese-containing raw material and a vanadium-containing raw material to obtain molten steel; adding magnesium alloy and rare earth into the molten steel under the pressure of 1-2 MPa for microalloying to obtain microalloyed molten steel; casting the microalloyed molten steel to obtain a cast ingot; carrying out pressurized electroslag remelting on the cast ingot to obtain a high-speed steel electroslag ingot; and the solidification pressure in the pressurized electroslag remelting process is 1-2 MPa. The invention effectively refines the high-speed steel as-cast structure under the combined action of magnesium element, rare earth and high solidification pressure, reduces the size of eutectic carbide and improves the distribution uniformity of the eutectic carbide.
Description
Technical Field
The invention belongs to the technical field of high-speed steel, and particularly relates to high-speed steel and a method for comprehensively improving an as-cast structure by microalloying magnesium and rare earth of the high-speed steel and increasing solidification pressure.
Background
High-speed tool steel is called high-speed steel for short, and is widely used for manufacturing various cutting tools and also partially used for high-load dies, aviation high-temperature bearings, high-performance rollers, special heat-resistant and wear-resistant parts and the like due to the characteristics of high hardness, high red hardness, high wear resistance and the like. In particular, it is important to manufacture a complex thin edge, an impact resistant cutting tool, and a large-section cutting tool, and particularly, demand for high-performance high-speed steel represented by M42 is strong.
At present, the production process flow of induction furnace (or electric arc furnace) smelting → LF → VD → die casting → electroslag remelting is commonly adopted by domestic and foreign special steel enterprises for producing high-speed steel. In the process, electroslag remelting is a key link for quality control of high-quality high-speed steel production, and can improve the purity and the structure compactness of steel, improve the macrostructure of steel and refine the cast structure of cast ingots. However, due to the high content of alloying elements (Mo, W, Cr and V) in high-speed steel, complex chemical composition, large solidification temperature range, limited cooling capacity of traditional electroslag remelting and the like, when the high-speed steel is produced by adopting the process, serious segregation of carbon and the alloying elements is easily formed during solidification, so that a large amount of coarse reticular eutectic carbides are generated at the grain boundary of a solidification structure. The existence of the reticular eutectic carbide destroys the continuity of a metal matrix, easily causes crack sources and expands, leads to the reduction of the thermoplasticity of the high-speed steel, leads to the difficult processing of the high-speed steel, easily causes cracking in the forging process and has low yield. On the other hand, eutectic carbides are hardly broken during forging, and the high speed steel is liable to have a problem of structural quality characterized by coarse carbides and uneven distribution, deteriorating the high speed steel performance.
In order to obtain higher structure quality, the high-speed steel cast ingot must be subjected to repeated multi-pass forging and rolling to reduce the size of carbide and improve the distribution uniformity of the carbide. The refining of the as-cast structure, the reduction of the size of the eutectic carbides and the improvement of the distribution uniformity are key factors for improving the processing yield and the service performance of high-speed steel and are also difficult problems in the production of high-speed steel by a smelting method.
Disclosure of Invention
In view of the above, the present invention provides a high-speed steel and a method for improving the cast structure comprehensively by microalloying magnesium and rare earth and increasing the solidification pressure thereof. The invention utilizes the magnesium alloy and the rare earth to carry out microalloying on the molten steel, simultaneously improves the solidification pressure in the pressurized electroslag remelting process, refines the high-speed steel as-cast structure, reduces the size of eutectic carbide, improves the distribution uniformity of the eutectic carbide, and further improves the processing yield and the service performance of the high-speed steel.
In order to solve the technical problems, the invention provides a method for comprehensively improving an as-cast structure by microalloying magnesium and rare earth and increasing solidification pressure, which comprises the following steps:
smelting industrial pure iron, a chromium-containing raw material, a molybdenum-containing raw material, metal tungsten, metal cobalt, graphite, industrial silicon, a manganese-containing raw material and a vanadium-containing raw material to obtain molten steel;
sequentially adding magnesium alloy and rare earth into the molten steel under the pressure of 1-2 MPa for microalloying to obtain microalloyed molten steel;
casting the microalloyed molten steel to obtain a cast ingot;
carrying out pressurized electroslag remelting on the cast ingot to obtain a high-speed steel electroslag ingot; and the solidification pressure in the pressurized electroslag remelting process is 1-2 MPa.
Preferably, the mass percentage of magnesium in the magnesium alloy is 5-20%; the mass of magnesium in the magnesium alloy is 0.03-0.07% of the mass of the cast ingot.
Preferably, the rare earth comprises cerium and/or lanthanum; the addition amount of the rare earth is 0.1-0.25% of the mass of the cast ingot.
Preferably, the microalloying temperature is 1430-1480 ℃ and the microalloying time is 1-3 min.
Preferably, the voltage of the pressurized electroslag remelting is 33-40V, the current is 2200-3000A, and the pressure is 1-2 MPa.
Preferably, the smelting comprises the following steps:
carrying out induction smelting on industrial pure iron, a chromium-containing raw material, a molybdenum-containing raw material, metal tungsten and metal cobalt to obtain base molten steel;
adding partial graphite into the basic molten steel for vacuum carbon deoxidation to obtain pre-deoxidized molten steel;
adding a manganese-containing raw material, a vanadium-containing raw material, industrial silicon and residual graphite into the pre-deoxidized molten steel for alloying to obtain molten steel.
Preferably, the temperature of the induction melting is 1480-1530 ℃.
Preferably, the vacuum degree of vacuum carbon deoxidation is below 30Pa, and the temperature is 1430-1480 ℃.
Preferably, the alloying temperature is 1430-1480 ℃ and the alloying time is 5-9 min.
The invention also provides the high-speed steel prepared by the preparation method of the technical scheme, which comprises the following chemical components in percentage by mass:
the invention provides a preparation method of high-speed steel, which comprises the following steps: smelting industrial pure iron, a chromium-containing raw material, a molybdenum-containing raw material, metal tungsten, metal cobalt, graphite, industrial silicon, a manganese-containing raw material and a vanadium-containing raw material to obtain molten steel; sequentially adding magnesium alloy and rare earth into the molten steel under the pressure of 1-2 MPa for microalloying to obtain microalloyed molten steel; casting the microalloyed molten steel to obtain a cast ingot; carrying out pressurized electroslag remelting on the cast ingot to obtain a high-speed steel electroslag ingot; and the solidification pressure in the pressurized electroslag remelting process is 1-2 MPa. The magnesium alloy is added into the molten steel under the pressurizing condition, so that the yield of magnesium can be obviously improved, the high-efficiency deep deoxidation and the desulphurization can be realized, and the solid solution content of magnesium in the steel can be increased; the molten steel has low oxygen and sulfur contents after being treated by magnesium, and can obviously improve the yield of the rare earth and increase the solid solution content of the rare earth in the steel. In the invention, the molten steel is microalloyed by using magnesium alloy and rare earth, and the segregation of solid-solution magnesium in a crystal boundary or a phase boundary can block the diffusion of elements such as carbon, chromium, molybdenum and the like in the solidification process, thereby refining eutectic carbide; the rare earth inclusion as a heterogeneous nucleation position can increase primary austenite nucleation and refine primary austenite; meanwhile, rare earth is enriched at the growth front of the dendrite, so that the austenite dendrite is promoted to branch for multiple times and the growth of the austenite dendrite is limited, and the as-cast structure of the high-speed steel is refined. The invention can effectively reduce the air gap between the ingot and the crystallizer by improving the solidification pressure in the pressurized electroslag remelting process, enhance the cooling effect of cooling water on the ingot, improve the cooling rate, and overcome the problem of limited cooling capacity in the traditional electroslag remelting high-speed steel preparation process, thereby refining the high-speed steel casting structure, improving the distribution of eutectic carbide and reducing element segregation.
Under the combined action of microalloying of magnesium element and rare earth and increasing the solidification pressure in pressurized electroslag smelting, the invention can effectively refine the as-cast structure of high-speed steel, reduce the size of eutectic carbide and improve the distribution uniformity of the eutectic carbide, thereby improving the processing yield and the service performance of the high-speed steel.
Drawings
FIG. 1 is a microstructure diagram of a high-speed steel electroslag ingot prepared in example 1;
FIG. 2 is a microstructure diagram of a high-speed steel electroslag ingot prepared in example 2;
FIG. 3 is a microstructure diagram of a high-speed steel electroslag ingot prepared in example 3;
FIG. 4 is a microstructure diagram of a high-speed steel electroslag ingot prepared in example 4;
FIG. 5 is a microstructure diagram of a high-speed steel electroslag ingot prepared in comparative example 1;
FIG. 6 is a microstructure diagram of a high-speed steel electroslag ingot prepared in comparative example 2;
FIG. 7 is a microstructure view of an electroslag ingot of high-speed steel prepared in comparative example 3.
Detailed Description
The invention provides a method for comprehensively improving an as-cast structure by microalloying magnesium and rare earth and increasing solidification pressure, which comprises the following steps of:
smelting industrial pure iron, a chromium-containing raw material, a molybdenum-containing raw material, metal tungsten, metal cobalt, graphite, industrial silicon, a manganese-containing raw material and a vanadium-containing raw material to obtain molten steel;
sequentially adding magnesium alloy and rare earth into the molten steel under the pressure of 1-2 MPa for microalloying to obtain microalloyed molten steel;
casting the microalloyed molten steel to obtain a cast ingot;
carrying out pressurized electroslag remelting on the cast ingot to obtain a high-speed steel electroslag ingot; and the solidification pressure in the pressurized electroslag remelting process is 1-2 MPa.
The method comprises the steps of smelting industrial pure iron, a chromium-containing raw material, a molybdenum-containing raw material, metal tungsten, metal cobalt, graphite, industrial silicon, a manganese-containing raw material and a vanadium-containing raw material to obtain molten steel. In the present invention, the smelting preferably comprises the steps of:
carrying out induction smelting on industrial pure iron, a chromium-containing raw material, a molybdenum-containing raw material, metal tungsten and metal cobalt to obtain base molten steel;
adding part of graphite into the basic molten steel, and performing vacuum carbon deoxidation to obtain pre-deoxidized molten steel;
adding a manganese-containing raw material, a vanadium-containing raw material, industrial silicon and residual graphite into the pre-deoxidized molten steel for alloying to obtain molten steel.
The invention carries out induction melting on industrial pure iron, chromium-containing raw materials, molybdenum-containing raw materials, metal tungsten and metal cobalt to obtain the basic molten steel. In the present invention, the chromium-containing raw material preferably includes metallic chromium. In the present invention, the molybdenum-containing raw material preferably includes metallic molybdenum or ferromolybdenum, and more preferably ferromolybdenum. The invention has no special requirements on the mass ratio of the industrial pure iron to the chromium-containing raw material to the molybdenum-containing raw material to the metal tungsten to the metal cobalt, and the industrial pure iron and the chromium-containing raw material are prepared according to the content of the chemical components of the required high-speed steel.
In the invention, the induction melting is preferably vacuum induction melting; the vacuum degree of the vacuum induction melting is preferably less than 10Pa, and more preferably 5-8 Pa; the temperature of the vacuum induction melting is preferably 1480-1530 ℃, and more preferably 1500-1510 ℃.
After the basic molten steel is obtained, partial graphite is added into the basic molten steel for vacuum carbon deoxidation to obtain pre-deoxidized molten steel. In the invention, the mass percentage of the partial carbon source in the total mass of the carbon source is preferably 40-80%, and more preferably 50-60%. The mass ratio of the total mass of the graphite to the carbon in the target high-speed steel is preferably 1.03-1.08: 1, and more preferably 1.06-1.07: 1. In the present invention, the carbon source is used for deoxidation in addition to carbon in the target high-speed steel.
In the invention, the process of adding the graphite to the basic molten steel is preferably carried out in a protective atmosphere, the protective atmosphere is preferably argon with the purity of more than or equal to 99.999%, and the pressure of the protective atmosphere is preferably 0.01-0.05 MPa, and more preferably 0.02-0.03 MPa. In the present invention, the degree of vacuum in the vacuum carbon deoxidation is preferably 30Pa or less, and more preferably 10 to 20 Pa. In the invention, the temperature of vacuum carbon deoxidation is preferably 1430-1480 ℃, and more preferably 1450-1470 ℃. In the invention, the time for vacuum carbon deoxidation is preferably 20-30 min, and more preferably 20-25 min.
According to the invention, part of graphite is added into the molten steel under a protective atmosphere, so that severe carbon-oxygen reaction can be avoided, and the molten steel is prevented from being seriously splashed.
In the invention, the vacuum carbon deoxidation can reduce the oxygen content in the molten steel to less than 25ppm, and is beneficial to improving the yield of magnesium and rare earth elements and the effect of purifying the molten steel in the subsequent microalloying process.
After the pre-deoxidized molten steel is obtained, the manganese-containing raw material, the vanadium-containing raw material, the industrial silicon and the residual graphite are added into the pre-deoxidized molten steel for alloying to obtain the molten steel. In the present invention, the manganese-containing raw material preferably includes metallic manganese. In the present invention, the vanadium-containing raw material preferably includes metal vanadium or ferrovanadium, more preferably metal vanadium. The invention has no special requirement on the mass ratio of the industrial silicon to the manganese-containing raw material to the vanadium-containing raw material, and the industrial silicon to the manganese-containing raw material is prepared according to the content of the chemical components of the required high-speed steel.
In the invention, the manganese-containing raw material, the vanadium-containing raw material, the industrial silicon and the residual graphite are added into the pre-deoxidized molten steel, preferably the manganese-containing raw material, the vanadium-containing raw material, the industrial silicon and the residual graphite are sequentially added into the pre-deoxidized molten steel; the time interval for adding the manganese-containing raw material, the vanadium-containing raw material, the industrial silicon and the residual graphite is preferably 1-3 min, and more preferably 2 min. The present invention preferably performs alloying during the addition process. In the invention, the alloying process is preferably carried out in a protective atmosphere, the protective atmosphere is preferably argon with the purity of more than or equal to 99.999%, and the pressure of the protective atmosphere is preferably 0.01-0.03 MPa, and more preferably 0.02-0.03 MPa. In the invention, the alloying temperature is preferably 1430-1480 ℃, and more preferably 1450-1480 ℃; the time is preferably 5 to 9min, and more preferably 6 to 8 min.
After molten steel is obtained, the magnesium alloy and the rare earth are sequentially added into the molten steel under the pressure of 1-2 MPa to carry out microalloying, so that microalloyed molten steel is obtained. In the present invention, the magnesium alloy preferably includes a nickel-magnesium alloy or an iron-magnesium alloy, and more preferably a nickel-magnesium alloy. In the invention, the mass percentage of magnesium in the magnesium alloy is preferably 5-20%. In the invention, the mass of magnesium in the magnesium alloy is preferably 0.03-0.07% of the mass of an ingot. In the present invention, the rare earth preferably comprises cerium and/or lanthanum, more preferably cerium. In the invention, when the rare earth is cerium and lanthanum, the invention has no special requirement on the mass ratio of the cerium to the lanthanum, and any ratio can be adopted. In the invention, the addition amount of the rare earth is preferably 0.1-0.25% of the mass of the ingot.
In the invention, the microalloying process is preferably carried out in a protective atmosphere, the protective atmosphere is preferably argon with the purity of more than or equal to 99.999%, and the pressure of the protective atmosphere is preferably 1.0-2.0 MPa, and more preferably 1.5-1.8 MPa. In the invention, the microalloying temperature is preferably 1430-1480 ℃, and more preferably 1450-1480 ℃; the time is preferably 1-3 min, and more preferably 2 min.
In the invention, the magnesium element and the rare earth have strong affinity with oxygen and sulfur impurity elements, and can effectively remove the oxygen and sulfur impurity elements in steel to purify molten steel, thereby playing the roles of deep deoxidation and desulfurization. Meanwhile, magnesium and rare earth elements which are dissolved in molten steel are easy to segregate in grain boundaries, so that impurity elements such as sulfur, phosphorus and the like can be prevented from segregating in the grain boundaries, and the grain boundaries are purified and strengthened. In addition, the magnesium can also inhibit rare earth inclusions as nucleation sites to promote the formation of fishbone-shaped M in the high-speed steel cast structure6C eutectic carbide (hard to decompose and break during heating). The invention can fully improve the cast structure of the high-speed steel under the combined action of magnesium and rare earth elements.
The magnesium-containing alloy is added into the molten steel under the pressure of 1-2 MPa, so that the yield of magnesium (more than 25%) can be remarkably improved, efficient deep deoxidation and desulfurization are realized, and the solid solution content of magnesium in the steel is increased. The molten steel has low oxygen and sulfur contents after vacuum carbon deoxidation and microalloying, can obviously improve the yield of rare earth (more than 40 percent) in the subsequent rare earth treatment process, and increases the solid solution content of the rare earth in the steel.
After the microalloyed molten steel is obtained, the microalloyed molten steel is cast to obtain a cast ingot. In the invention, the temperature of the microalloyed molten steel during casting is preferably 1430-1480 ℃, and more preferably 1450-1470 ℃. In the present invention, the casting method further preferably comprises: and preserving the heat of the microalloyed molten steel at the casting temperature. In the invention, the heat preservation time is preferably 2-4 min, and more preferably 3 min. The invention has no special requirements on the casting and can be carried out by adopting a conventional mode in the field.
After obtaining a cast ingot, carrying out pressurized electroslag remelting on the cast ingot to obtain a high-speed steel electroslag ingot; and the solidification pressure in the pressurized electroslag remelting process is 1-2 MPa. In the invention, the cooling mode of the pressurized electroslag remelting is cooling water cooling, and the solidification pressure refers to the gas pressure in the smelting chamber. The invention preferably fills argon into the melting chamber of the pressurized electroslag remelting furnace and simultaneously improves the pressure of the cooling water in the jacket of the crystallizer, so that the pressure of the cooling water is consistent with the pressure in the melting chamber.
In the present invention, the pressurized electroslag remelting is preferably performed in a pressurized electroslag remelting furnace. The invention preferably forges the cast ingot to obtain the consumable electrode which is suitable for the size of the pressurized electroslag remelting furnace crystallizer. The size of the consumable electrode is not specially limited, and the consumable electrode can be adapted to the size of the crystallizer of the pressurized electroslag remelting furnace. In an embodiment of the invention, the consumable electrode is a rod of 80mm diameter and length. In the present invention, the pressurized electroslag remelting process preferably further comprises: welding the consumable electrode to a dummy electrode and connecting the dummy electrode to an electrode holder; placing arc striking scraps in an arc striking ring at the center of a pressurized electroslag remelting furnace bottom water tank; and baking the pre-melted slag, and adding the baked pre-melted slag into a crystallizer of a pressurized electroslag remelting furnace for arc starting and slag making.
In the present invention, the material of the arc ignition scrap is preferably the same as that of the target high speed steel. In the invention, the amount of the arc striking dust is preferably 0.25-0.35 kg, and more preferably 0.28-0.32 kg. In the invention, a gasket is preferably arranged between the arc ignition ring and the pressurizing electroslag remelting furnace crystallizer, the gasket is preferably made of cast iron, and the diameter of the gasket is preferably 108-112 mm, and more preferably 110 mm; the thickness of the gasket is preferably 8-12 mm, and more preferably 10 mm. In the invention, the consumable electrode, the arc striking chips and the pressurized electroslag remelting furnace bottom water tank are in close contact, so that current can pass after the power is on.
In the invention, the pre-melted slag preferably comprises 50-58% of CaF in percentage by mass2，15～20％CaO，12～18％Al2O3，3～7％MgO，5～10％Ce2O30.5% or less of SiO2And unavoidable impurities; more preferably 53-55% CaF2，16～18％CaO，15～17％％Al2O3，4～6％MgO，6～8％Ce2O30.3% or less of SiO2And inevitable impurities. In the invention, the baking temperature is preferably 500-800 ℃, and more preferably 650-700 ℃; the time is preferably 6 to 10 hours, and more preferably 8 to 9 hours. The invention can fully remove the moisture in the premelting slag through baking.
In the invention, the magnesium and the rare earth elements in the consumable electrode are easy to react with the oxide in the pre-melted slag, so that a certain proportion of magnesium oxide and rare earth oxide is added into the pre-melted slag, the content of aluminum oxide in the slag is properly reduced, the content of silicon dioxide in the slag is strictly controlled, and the burning loss of the magnesium and the rare earth elements in the pressurizing electroslag remelting process can be effectively inhibited (the yield of the magnesium and the rare earth is more than 60 percent independently).
In the present invention, before the arc starting and slagging, the method further preferably comprises: argon is introduced into the smelting chamber of the pressurized electroslag remelting furnace. The purity of the argon is preferably more than or equal to 99.999%, the flow of the introduced argon is preferably 10-20 NL/min, more preferably 12-15 NL/min, and the time is preferably 4-10 min, more preferably 5-6 min. The invention removes the air in the melting chamber of the pressurized electroslag remelting furnace by introducing argon. In the invention, the voltage for arc starting and slagging is preferably 25-33V, and more preferably 28-30V; the current is preferably 1000-2100A, more preferably 1600-2000A; the time is preferably 7 to 15min, and more preferably 10 to 15 min.
In the invention, the voltage of the pressurized electroslag remelting is preferably 33-40V, and more preferably 35-40V; the current is preferably 2200 to 3000A, more preferably 2200 to 2500A. In the present invention, the fluctuation of the voltage and current is preferably less than 5%. In the present invention, the melting rate of the pressurized electroslag remelting is preferably determined according to formula 1:
v ═ 0.35 to 0.45 × Dkg/h formula 1;
wherein D is the size of the crystallizer of the pressurized electroslag remelting furnace and the unit is mm.
In the examples of the present invention, the melt rate was specifically 50 kg/h. In the present invention, the melting rate fluctuation is preferably less than 5%.
In the invention, the pressure of the pressurized electroslag remelting is preferably 1-2 MPa, and more preferably 1.5-1.8 MPa. In the present invention, the pressure is preferably formed by introducing argon gas into the melting chamber of the pressurized electroslag remelting furnace. The invention carries out the pressurized electroslag remelting under the pressure, can avoid oxygen absorption of a slag pool, and further reduces the burning loss of magnesium and rare earth elements. In the invention, the solidification pressure in the pressurized electroslag remelting process is 1-2 MPa, and preferably 1.5-1.8 MPa.
In the present invention, the pressurized electroslag remelting preferably further comprises: feeding and filling are carried out in a mode of gradually reducing current; and (5) closing the power supply, releasing pressure and taking out the electroslag ingot.
The invention adopts a mode of gradually reducing current to carry out feeding filling. In the invention, the current is reduced by 500-800A, preferably 600-800A, each time, so as to ensure that the feeding is fully filled and the feeding end face is flat. In the invention, the frequency of reducing the current is preferably 3-5 min/time, and more preferably 4 min/time.
After feeding and filling are finished, the electroslag ingot furnace closes a power supply, releases pressure and takes out the electroslag ingot. In the present invention, the pressure relief is preferably performed by reducing the pressure in the pressurized electroslag remelting furnace and in the crystallizer, and the pressure after the pressure relief is normal pressure. After the electroslag ingot is taken out, the electroslag ingot is preferably placed in a heat-insulating cover for slow cooling.
The invention also provides a high-speed steel prepared by the preparation method of the technical scheme, which comprises the following chemical components in percentage by mass:
in the invention, the high-speed steel preferably comprises the following chemical components in percentage by mass:
in the present invention, the rare earth element preferably includes cerium and/or lanthanum, and more preferably cerium.
In order to further illustrate the present invention, the following embodiments are described in detail, but they should not be construed as limiting the scope of the present invention.
In the embodiment of the invention, the induction melting is carried out in a 50kg pressure induction furnace, wherein the ultimate vacuum degree of the pressure induction furnace is 0.1Pa, the highest pressure is 7MPa, and the charging amount is 40-45 kg.
In the embodiment of the invention, the pressurized electroslag remelting is carried out in a 50kg pressurized electroslag remelting furnace, the highest pressure of the pressurized electroslag remelting furnace is 7MPa, the rated power of a power supply is 500kW, the inner diameter D of a crystallizer is 130mm, and the weight of a consumable electrode is 30-50 kg.
In the embodiment of the invention, the purity of industrial pure iron comprises 99.98 wt%, the purity of metal chromium is 99.17 wt%, the purity of metal molybdenum is 99.98 wt%, the purity of metal cobalt is 99.98 wt%, the purity of metal tungsten is 99.95 wt%, the purity of metal vanadium is more than or equal to 99.9 wt%, the purity of industrial silicon is 99.38 wt%, the purity of metal manganese is 97.92 wt%, the purity of graphite is more than or equal to 99.9 wt%, the purity of nickel-magnesium alloy contains 19.65 wt%, the purity of nickel is 79.27 wt%, the purity of rare earth cerium is more than or equal to 99.5 wt%, and the purity of argon in each step is more than or equal to 99.999%.
Example 1
29.738kg of industrial pure iron, 1.5kg of metal chromium, 3.8kg of metal molybdenum, 0.6kg of metal tungsten and 3.2kg of metal cobalt are placed in a crucible in an induction furnace, and induction melting is carried out under the condition that the temperature is 1510 ℃ and the vacuum degree is 5Pa to obtain base molten steel;
filling argon with the purity of more than or equal to 99.999 percent into a pressurized induction furnace to ensure that the pressure in the furnace is 0.025MPa, adding 0.232kg of graphite into the primary molten steel under the argon atmosphere, starting a vacuum pump after the graphite is melted down to perform vacuum carbon deoxidation, wherein the vacuum degree of the vacuum carbon deoxidation is 16Pa, the temperature is 1475 ℃, and the time is 24min to obtain pre-deoxidized molten steel;
argon with the purity of more than or equal to 99.999 percent is filled into the furnace to ensure that the pressure in the furnace is 0.013MPa, 0.12kg of metal manganese, 0.46kg of metal vanadium, 0.12kg of industrial silicon and the rest 0.23kg of graphite are sequentially added into the pre-deoxidized molten steel at intervals of 2min under the argon atmosphere for alloying, and the alloying temperature is 1480 ℃ to obtain molten steel;
filling argon with the purity of more than or equal to 99.999 percent into the furnace to ensure that the pressure in the furnace is 1.5MPa, sequentially adding 75g of nickel-magnesium alloy (the mass percentage of magnesium is 19.65 percent) and 92g of cerium into the molten steel under the argon atmosphere, and carrying out micro-alloying for 2min at 1460 ℃ to obtain micro-alloyed molten steel;
carrying out heat preservation on the microalloyed molten steel at 1460 ℃ for 3min, and then casting to obtain a cast ingot; forging the cast ingot to obtain a consumable electrode with the diameter phi of 80mm, welding the consumable electrode to a dummy electrode, and connecting the dummy electrode with an electrode holder;
placing 0.33kg of arc striking scraps (1.1% of C, 0.3% of Si, 0.3% of Mn, 3.75% of Cr, 9.5% of Mo, 8% of Co, 1.5% of W, 1.15% of V and the balance of Fe) in an arc striking ring at the center of a pressurized electroslag remelting furnace bottom water tank (a consumable electrode, the arc striking scraps and the pressurized electroslag remelting furnace bottom water tank are in close contact); wherein a gasket which has the diameter of 110mm and the thickness of 10mm and is made of cast iron is arranged between the arc ignition ring and the water tank;
3400g of CaF with a content of 55.5%2-17％CaO-15.5％Al2O3-5％MgO-7％Ce2O3-0.2％SiO2Baking the pre-melted slag at 650 ℃ for 8h, adding the pre-melted slag into a crystallizer of a pressurized electroslag remelting furnace, and then sealing the pressurized electroslag furnace; starting a water supply system to introduce normal-pressure cooling water into the crystallizer; introducing argon with the flow rate of 12NL/min into the pressurized electroslag remelting furnace for 8 min; carrying out arc starting and slagging for 12min under the conditions that the voltage is 27V and the current is 1650A;
after the arcing and slagging are finished, introducing argon into a smelting chamber of the pressurized electroslag remelting furnace to ensure that the gas pressure in the smelting chamber of the pressurized electroslag remelting furnace is 1.5MPa, and simultaneously ensure that the pressure of cooling water in a crystallizer jacket of the pressurized electroslag remelting furnace is 1.5MPa, and performing pressurized electroslag remelting (with the melting speed of 50kg/h) under the conditions that the voltage is 37V and the current is 2300A, wherein the voltage fluctuation is less than 3%, the current fluctuation is less than 5%, and the melting speed fluctuation is less than 5%;
after the consumable electrode is smelted, feeding and filling are carried out in a mode of gradually reducing current, the current is reduced once every 4min, and the current is reduced by 550A each time;
after the completion of the contraction, closing the alternating current power supply, opening a vent valve of the pressurized electroslag furnace to release pressure, and synchronously reducing the pressure of cooling water in a crystallizer of the pressurized electroslag furnace to normal pressure to obtain a high-speed steel electroslag ingot; and placing the high-speed steel in a heat-preserving cover for slow cooling.
Example 2
High speed steel was produced according to the method of example 1 except that the argon pressure in the pressure induction furnace at the microalloying stage was 2 MPa.
Example 3
High speed steel was manufactured according to the method of example 1 except that the amount of the nickel-magnesium alloy added in the micro-alloying stage was 93g and the amount of the cerium added was 79 g.
Example 4
High speed steel was manufactured according to the method of example 1, except that the amount of the nickel-magnesium alloy added in the micro-alloying stage was 125g and the amount of the cerium added was 41 g.
Comparative example 1
High speed steel was prepared according to the method of example 1, except that microalloying of magnesium and rare earth was not performed after alloying, the pressure in the pressure induction furnace after alloying was increased to 0.1MPa, and then casting was performed; the pressure in the pressurized electroslag remelting furnace and the pressure of cooling water in the jacket of the crystallizer are 0.1MPa in the pressurized electroslag remelting process.
Comparative example 2
High-speed steel was prepared according to the method of example 1, except that the pressure of the protective atmosphere was 0.1MPa when the nickel-magnesium alloy and cerium were added at the microalloying stage; in the process of pressurizing electroslag remelting, the pre-melted slag has 60 +/-1 percent of CaF2-20±1％CaO-20±1％Al2O3Pressure in the melting chamber of the pressurized electroslag remelting furnace and cooling in the jacket of the crystallizerThe pressure of the water was 0.1 MPa.
Comparative example 3
High speed steel was manufactured according to the method of example 1, except that microalloying of magnesium and rare earth was not performed after alloying, and the pressure in the pressure induction furnace was 0.1MPa after alloying, followed by casting.
The chemical compositions of the ingots prepared by the pressure induction furnace smelting in examples 1 to 4 and comparative examples 1 to 3 are shown in table 1. Measuring the contents of Si, Mn, Cr, Mo, Co, W and V in the ingot by using a direct-reading spectrum; measuring the content of O in the ingot by using a nitrogen-oxygen analyzer; measuring the contents of C and S in the cast ingot by using a carbon-sulfur analyzer; and measuring the contents of Mg and Ce in the ingot by using an inductively coupled plasma mass spectrometer.
TABLE 1 chemical composition of ingots prepared in examples 1 to 4 and comparative examples 1 to 3 by pressure induction furnace
| Examples | C | Si | Mn | Cr | Mo | Co | W | V | Mg | Ce | O | S | Fe |
| Example 1 | 1.10 | 0.29 | 0.28 | 3.75 | 9.49 | 7.99 | 1.50 | 1.15 | 0.0094 | 0.112 | 0.0006 | 0.0019 | Balance of |
| Example 2 | 1.08 | 0.27 | 0.28 | 3.73 | 9.50 | 8.00 | 1.48 | 1.13 | 0.0103 | 0.120 | 0.0005 | 0.0017 | Balance of |
| Example 3 | 1.09 | 0.28 | 0.27 | 3.74 | 9.51 | 8.01 | 1.49 | 1.14 | 0.0143 | 0.089 | 0.0005 | 0.0018 | Balance of |
| Example 4 | 1.09 | 0.29 | 0.28 | 3.75 | 9.48 | 7.98 | 1.48 | 1.15 | 0.0206 | 0.044 | 0.0006 | 0.0020 | Balance of |
| Comparative example 1 | 1.12 | 0.29 | 0.28 | 3.73 | 9.48 | 7.99 | 1.49 | 1.14 | - | - | 0.0015 | 0.0035 | Balance of |
| Comparative example 2 | 1.11 | 0.29 | 0.27 | 3.74 | 9.47 | 7.97 | 1.49 | 1.15 | 0.0025 | 0.054 | 0.0008 | 0.0022 | Balance of |
| Comparative example 3 | 1.12 | 0.28 | 0.28 | 3.75 | 9.49 | 7.98 | 1.48 | 1.14 | - | - | 0.0016 | 0.0035 | Balance of |
As can be seen from the data in Table 1, the oxygen and sulfur contents in the ingot are reduced and the ultra-clean smelting is realized by adding magnesium alloy and rare earth elements for deep deoxidation and deep desulfurization in the ingot preparation process.
The chemical compositions of the high-speed steel electroslag ingots prepared by remelting the added slag in examples 1 to 4 and comparative examples 1 to 3 are shown in table 2. Measuring the contents of Si, Mn, Cr, Mo, Co, W and V in the high-speed steel electroslag ingot by using direct-reading spectrum; measuring the content of O in the high-speed steel electroslag ingot by using a nitrogen-oxygen analyzer; measuring the contents of C and S in the high-speed steel electroslag ingot by using a carbon-sulfur analyzer; and (3) measuring the contents of Mg and Ce in the high-speed steel electroslag ingot by using an inductively coupled plasma mass spectrometer.
TABLE 2 chemical compositions of high-speed steel electroslag ingots prepared in examples 1 to 4 and comparative examples 1 to 3 by pressurized electroslag remelting
| Examples | C | Si | Mn | Cr | Mo | Co | W | V | Mg | Ce | O | S | Fe |
| Example 1 | 1.08 | 0.27 | 0.24 | 3.74 | 9.49 | 7.98 | 1.50 | 1.13 | 0.0060 | 0.075 | 0.0007 | 0.0012 | Balance of |
| Example 2 | 1.08 | 0.26 | 0.24 | 3.73 | 9.50 | 8.00 | 1.49 | 1.12 | 0.0068 | 0.079 | 0.0006 | 0.0011 | Balance of |
| Example 3 | 1.07 | 0.28 | 0.25 | 3.75 | 9.47 | 7.97 | 1.47 | 1.13 | 0.0092 | 0.058 | 0.0007 | 0.0012 | Balance of |
| Example 4 | 1.08 | 0.28 | 0.27 | 3.73 | 9.47 | 7.97 | 1.48 | 1.14 | 0.0135 | 0.027 | 0.0006 | 0.0010 | Balance of |
| Comparative example 1 | 1.10 | 0.28 | 0.26 | 3.72 | 9.98 | 7.98 | 1.48 | 1.13 | - | - | 0.0012 | 0.0014 | Balance of |
| Comparative example 2 | 1.11 | 0.29 | 0.27 | 3.74 | 9.47 | 7.97 | 1.49 | 1.15 | 0.0004 | 0.010 | 0.0010 | 0.0012 | Balance of |
| Comparative example 3 | 1.09 | 0.27 | 0.25 | 3.72 | 9.47 | 7.97 | 1.47 | 1.13 | - | - | 0.0014 | 0.0013 | Balance of |
The data in table 2 show that the sulfur content in the high-speed steel electroslag ingot after the pressurized electroslag remelting is obviously reduced, and the cleanliness of the high-speed steel is further improved.
Table 3 summarizes the smelting process parameters, the addition amounts of magnesium and rare earth and the yield of the high-speed steel electroslag ingots prepared in the examples 1 to 4 and the comparative examples 1 to 3.
TABLE 3 smelting process parameters for preparing high speed steels in examples 1 to 4 and comparative examples 1 to 3, and addition amounts and yields of magnesium and rare earth
From the data in table 3, it can be seen that in the induction melting stage, the magnesium-containing intermediate alloy is added into the molten steel under the pressure of 1-2 MPa, so that the yield of magnesium (more than 25%) can be remarkably improved, and the yield of cerium (more than 40%) can be remarkably improved by efficient treatment of magnesium; the premelting slag can effectively inhibit the burning loss of magnesium and rare earth cerium in the electroslag remelting process, and the yield of the magnesium and the cerium is more than 60 percent.
Microstructure observation is carried out on the high-speed steel electroslag cast ingots prepared in the examples 1-4 and the comparative examples 1-3 by using a metallographic microscope, and microstructure diagrams are obtained and are shown in the figures 1-7. Wherein the observation sample is taken from the radius part of the high-speed steel electroslag 1/2 cast ingot prepared in the examples 1-4 and the comparative examples 1-3.
As can be seen from the combination of the figures 1-7, the high-speed steel prepared by the preparation method provided by the invention has smaller eutectic carbides, is uniformly distributed, refines the as-cast structure of the high-speed steel, is beneficial to reducing the cracking tendency in the hot processing process of the high-speed steel, and improves the processing yield and the service performance of the high-speed steel.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are within the scope of the present invention.
Claims (10)
1. A method for comprehensively improving an as-cast structure by microalloying magnesium and rare earth and increasing solidification pressure comprises the following steps:
smelting industrial pure iron, a chromium-containing raw material, a molybdenum-containing raw material, metal tungsten, metal cobalt, graphite, industrial silicon, a manganese-containing raw material and a vanadium-containing raw material to obtain molten steel;
sequentially adding magnesium alloy and rare earth into the molten steel under the pressure of 1-2 MPa for microalloying to obtain microalloyed molten steel;
casting the microalloyed molten steel to obtain a cast ingot;
carrying out pressurized electroslag remelting on the cast ingot to obtain a high-speed steel electroslag ingot; and the solidification pressure in the pressurized electroslag remelting process is 1-2 MPa.
2. The preparation method according to claim 1, wherein the mass percentage of magnesium in the magnesium alloy is 5-20%; the mass of magnesium in the magnesium alloy is 0.03-0.07% of the mass of the cast ingot.
3. The production method according to claim 1, wherein the rare earth includes cerium and/or lanthanum; the addition amount of the rare earth is 0.1-0.25% of the mass of the cast ingot.
4. The preparation method according to claim 1, wherein the microalloying temperature is 1430-1480 ℃ and the microalloying time is 1-3 min.
5. The method according to claim 1, wherein the pressure electroslag remelting is carried out at a voltage of 33 to 40V, a current of 2200 to 3000A, and a pressure of 1 to 2 MPa.
6. The method of claim 1, wherein the smelting comprises the steps of:
carrying out induction smelting on industrial pure iron, a chromium-containing raw material, a molybdenum-containing raw material, metal tungsten and metal cobalt to obtain base molten steel;
adding partial graphite into the basic molten steel for vacuum carbon deoxidation to obtain pre-deoxidized molten steel;
adding a manganese-containing raw material, a vanadium-containing raw material, industrial silicon and residual graphite into the pre-deoxidized molten steel for alloying to obtain molten steel.
7. The preparation method of claim 6, wherein the temperature of the induction melting is 1480-1530 ℃.
8. The method according to claim 6, wherein the vacuum carbon deoxidation is performed under a vacuum degree of 30Pa or less and at a temperature of 1430 to 1480 ℃.
9. The preparation method according to claim 6, wherein the alloying temperature is 1430-1480 ℃ and the alloying time is 5-9 min.
10. The high-speed steel prepared by the preparation method of any one of claims 1 to 9 comprises the following chemical components in percentage by mass:
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