CN113539653B - Preparation method of soft magnetic alloy bar - Google Patents

Preparation method of soft magnetic alloy bar Download PDF

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CN113539653B
CN113539653B CN202111083682.3A CN202111083682A CN113539653B CN 113539653 B CN113539653 B CN 113539653B CN 202111083682 A CN202111083682 A CN 202111083682A CN 113539653 B CN113539653 B CN 113539653B
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alloy
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CN113539653A (en
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刘杰
苏辉
李�柱
徐建斌
杨新刚
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Xi'an Gangyan Special Alloy Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
    • C21D8/1222—Hot rolling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1261—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest following hot rolling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/07—Alloys based on nickel or cobalt based on cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C22C33/06—Making ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
    • C22C38/105—Ferrous alloys, e.g. steel alloys containing cobalt containing Co and Ni
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition

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Abstract

The invention discloses a preparation method of a soft magnetic alloy bar, which is used for preparing a high-strength soft magnetic alloy by optimizing chemical components and a process, and comprises the following components in percentage by mass: less than or equal to 0.04 percent of C, less than or equal to 0.30 percent of Si, less than or equal to 0.30 percent of Mn, less than or equal to 0.020 percent of P, less than or equal to 0.020 percent of S, less than or equal to 0.20 percent of Cu, less than or equal to 0.50 percent of Ni, 48.0-51.0 percent of Co, 1.80-2.10 percent of V, 0.1-0.2 percent of Mo, and the balance of Fe; the preparation process comprises the following steps: vacuum smelting, alloy ingot casting, forging and cogging, hot rolling of finished products and solution treatment. The tensile strength of the high-strength soft magnetic alloy bar 1J22MV prepared by the invention is more than 500 MPa; the yield strength is more than or equal to 250 MPa; b800 is more than or equal to 1.8T, B2400, 2400 is more than or equal to 2.1T, B4000 is more than or equal to 2.15T, B8000, 8000 is more than or equal to 2.2T; the coercive force Hc is less than or equal to 144A/m; curie point 980 ℃; saturated hysteresis coefficient of expansion (10)‑6）60~100。

Description

Preparation method of soft magnetic alloy bar
Technical Field
The invention belongs to the technical field of special material smelting, relates to preparation of a soft magnetic alloy, and particularly relates to a preparation method of a soft magnetic alloy bar.
Background
1J22 is high saturation induction density Fe-Co-V soft magnetic alloy, which is the existing soft magnetic alloyThe saturation magnetic induction intensity in gold is the highest (Bs = 2.45T), and the saturation magnetostriction coefficient is the largest (60-100 x 10)-6) The Curie point is also very high (980 ℃ C.), and the alloy is the soft magnetic alloy with the highest Curie point. It is not suitable for use at high frequencies because of saturation induction (0.4. mu. omega. m). By adding 0.8-1.8% of V element, the cold processing plasticity of the alloy is greatly improved, but the magnetism is reduced by adding V.
Since the 1J22 alloy has the above characteristics, it is used for ferromagnetic elements that require high Bs (magnetic induction), high λ s (saturated magnetostriction coefficient), and low-frequency, high-temperature use; such as electromagnet pole heads, end weld tubes in magnetrons, eardrum diaphragms for telephone headsets, torque motor rotors, micro-electronics rotors, magnetostrictive transducer cores, power transformers, relays, transducers, etc.
The 1J22 Fe-Co-V soft magnetic alloy has stable performance, and the specification of the finished product is mainly hot rolled material, forged material, cold wire drawing or cold rolled strip. The 1J22 alloy has the disadvantages of high price, easy oxidation, poor processability, insufficient strength and the like, and limits the application range to a certain extent. However, the 1J22 alloy material is a special material, the market demand gap is large, and the recent years are met with the increase of high-speed release, especially the soft magnetic alloy with high strength.
Disclosure of Invention
The invention aims to provide a preparation method of a soft magnetic alloy bar so as to improve the yield strength, the coercive force and the stability of magnetic performance of the bar.
The invention is realized by the following technical scheme:
a preparation method of a soft magnetic alloy bar comprises the following operations:
1) vacuum smelting:
preparing the following raw materials according to the smelting requirement of the magnetically soft alloy 1J22MV in percentage by mass: less than or equal to 0.04 percent of C, less than or equal to 0.30 percent of Si, less than or equal to 0.30 percent of Mn, less than or equal to 0.020 percent of P, less than or equal to 0.020 percent of S, less than or equal to 0.20 percent of Cu, less than or equal to 0.50 percent of Ni, 48.0-51.0 percent of Co, 1.50-2.10 percent of V, 0.1-0.2 percent of Mo, and the balance of Fe;
putting pure iron, cobalt sheets, ferrovanadium and molybdenum strips in raw materials into a medium-frequency vacuum induction furnace for smelting;
vacuumizing to less than or equal to 133Pa after the vacuum induction furnace is closed, and transmitting power for preheating at 50-70 kw; increasing the power to 120-160 kw for material melting when the vacuum degree is less than or equal to 0.66Pa, and reducing the power to 80-100 kw in time if splashing occurs in the material melting process; material melting time: 1.5-2 hours;
heating the material to a refining temperature after melting, and then adding carbon and deoxidizing for multiple times at intervals of 5-8 minutes each time; entering a refining period after the carbon reaction is finished;
refining temperature: 1540-1560 ℃, and refining time: 30-40 minutes;
after refining for 5-15 minutes, closing a valve connected between the smelting chamber and an evacuating unit, adding SiCa alloy, and vacuumizing again until the pressure is less than or equal to 133Pa after the reaction is finished;
adding metal Mn 10-12 minutes before tapping and stirring;
tapping at 1510-1530 ℃, and carrying out charged pouring;
2) pouring an alloy ingot:
pouring the refined alloy liquid into an alloy ingot mold in vacuum, and after the pouring is finished, quickly breaking the air and adding a heating agent for covering so as to supplement the heat loss of the alloy liquid of the riser;
demoulding to obtain an alloy ingot;
3) forging and cogging:
heating an alloy ingot by using a resistance furnace, raising the temperature to 800-850 ℃, preserving heat for 30-40 min, raising the temperature to 1150-1200 ℃ along with the furnace, and preserving heat for 30-50 min;
when in forging, the small end of the alloy ingot is forged first, then the large end of the alloy ingot is forged, and the forging terminal temperature is lower than 950 ℃, and the alloy ingot needs to be re-melted and heated for new forging; the specification of the forging stock is (50-60) × L in millimeters, L is the length, and the forging ratio is more than or equal to 9;
after forging, completely burying the forging stock in sand for cooling;
4) hot rolling:
heating the cooled forging stock in a gas furnace or a resistance furnace, wherein the charging temperature is less than or equal to 400 ℃; heating to 980-1010 ℃ along with the furnace, preserving heat for 25-30 min, heating to 1140-1160 ℃ again, preserving heat for 20-30 min, and then hot rolling;
the hot rolling is carried out by adopting a horizontal two-roller hot rolling mill for 6-10 times, and the deformation of each time is controlled to be 16-20%; the finishing temperature is not lower than 900 ℃; the specification of the hot-rolled finished product is phi (15-30) multiplied by L in millimeters, and L is the length;
air cooling after hot rolling is finished;
5) solution treatment:
carrying out solution treatment on a bar obtained by hot rolling in a protective atmosphere: the charging temperature is less than or equal to 100 ℃, the temperature is increased to 850-870 ℃, the temperature is kept for 4-6 h, then the temperature is reduced to 750-780 ℃, the temperature is reduced to less than or equal to 300 ℃, the temperature is kept for 20-30 min, and then the mixture is discharged; obtaining the high-strength soft magnetic alloy bar.
During vacuum melting, firstly, filling pure iron in raw materials into the bottom of a crucible to be flatly filled into a layer, and filling the rest pure iron into the periphery and the middle upper part of the crucible; then, putting a cobalt sheet into the middle upper part of the crucible; finally, loading the ferrovanadium and molybdenum bars into the upper part of the crucible;
adding the materials in three batches during carbon adding, wherein 1/3 is added in each batch;
the SiCa alloy was added in two batches, 1/2 each.
Pouring the refined alloy liquid in vacuum, and immediately breaking the space after pouring to add a heating agent;
the heating agent is formed by mixing 60-70% of aluminum powder and 30-40% of sodium nitrate;
the amount of the heat generating agent is 0.2-0.6% of the mass of the alloy liquid.
During forging and cogging, an alloy ingot is heated to 1170-1190 ℃ in a resistance furnace, an electro-hydraulic hammer is adopted for forging after heat preservation, the frequency of the forging hammer is controlled to be more than 15-25 times/min, the initial forging temperature is more than or equal to 1190 ℃, and the final forging temperature is more than or equal to 950 ℃.
During the solution treatment, the solution treatment is carried out in a hydrogen atmosphere, the temperature is increased to 870 ℃ within 2-3 h, the heat preservation is carried out for 4-6 h, then the temperature is reduced to 780 ℃ at the speed of 30 ℃/h, the temperature is reduced to be less than or equal to 300 ℃ at the speed of 200 ℃/h, and the temperature is preserved for half an hour and then the product is discharged.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the soft magnetic alloy bar, the high-strength soft magnetic alloy 1J22MV is prepared by optimizing the chemical components of 1J22 and the process in production; mainly optimizes the content of Co and V, and adds a small amount of Mo; wherein, Mo enhances the wear resistance and the yield strength, and enhances the strength of the soft magnetic alloy by optimizing the contents of Co, V and Mo; further smelting in a medium-frequency vacuum induction furnace, smoothly smelting according to the specific condition, and adding carbon and SiCa alloy in batches; the strict control on the chemical components of the alloy liquid is realized;
the process preparation of the invention is realized by cogging forging and multi-pass hot rolling with large deformation, and then solid solution treatment is combined to ensure the tensile strength, yield strength and crystallization homogenization of the alloy material; the method is characterized in that electro-hydraulic hammer forging and a horizontal two-roll hot rolling mill are adopted to optimize the blank-opening forging and hot rolling modes, and the strength of the soft magnetic alloy is enhanced in an optimal mode by combining the temperature and the hot rolling mode; the solid solution treatment adopts low solid solution temperature to dissolve carbides and gamma in the matrix to obtain uniform supersaturated solid solution, so that the carbides, gamma and other strengthening phases with fine particles and uniform distribution can be precipitated again during aging, and simultaneously, the stress generated by cold and hot processing is eliminated, so that the alloy can obtain smaller grain size during recrystallization, the grains are more homogenized, and higher yield strength is obtained.
The high-strength soft magnetic alloy (1J 22MV bar) prepared by the invention has the characteristics of high saturation magnetic induction intensity, high Curie point, high hysteresis expansion coefficient and the like; actual performance index: the tensile strength is more than 500 MPa; the yield strength is more than or equal to 250 MPa; b800 is more than or equal to 1.8T, B2400, 2400 is more than or equal to 2.1T, B4000 is more than or equal to 2.15T, B8000, 8000 is more than or equal to 2.2T; the coercive force Hc is less than or equal to 144A/m; curie point 980 ℃; saturated hysteresis coefficient of expansion (10)-6) 60-100 parts; the yield strength of the 1J22MV bar prepared by the invention in the low-temperature heat treatment state is about 40% higher than that of the domestic similar product 1J22 standard strength index; the coercive force is obviously superior to that of the similar products; the invention has the characteristics of relatively low preparation cost, good processability, stable magnetic property and the like.
The high-strength soft magnetic alloy (1J 22MV bar) prepared by the method can be used for manufacturing parts such as electromagnetic valve QDK-36 armature of an aeroengine, and the like, and improves the functions of the parts such as magnetic property, impact resistance, vibration resistance and the like of the products.
Detailed Description
The present invention will now be described in further detail with reference to the following examples, which are intended to be illustrative, but not limiting, of the invention.
A preparation method of a high-strength soft magnetic alloy bar comprises the following operations:
1) vacuum smelting:
preparing raw materials according to the smelting requirement of the magnetically soft alloy 1J22MV, wherein the raw materials comprise, by mass, less than or equal to 0.04% of C, less than or equal to 0.30% of Si, less than or equal to 0.30% of Mn, less than or equal to 0.020% of P, less than or equal to 0.020% of S, less than or equal to 0.20% of Cu, less than or equal to 0.50% of Ni, 48.0-51.0% of Co, 1.50-2.10% of V, 0.1-0.2% of Mo and the balance of Fe;
putting pure iron, cobalt sheets, ferrovanadium and molybdenum strips in raw materials into a medium-frequency vacuum induction furnace for smelting;
vacuumizing to less than or equal to 133Pa after the vacuum induction furnace is closed, and transmitting electricity for preheating at low power (50-70 kw); when the vacuum degree is less than or equal to 0.66Pa, increasing the power (120-160 kw) to rapidly melt the materials, and reducing the power (80-100 kw) in time when splashing occurs in the material melting process; material melting time: 1.5-2 hours;
heating the material to a refining temperature after melting, and then adding carbon and deoxidizing for multiple times at intervals of 5-8 minutes each time; entering a refining period after the carbon reaction is finished;
refining temperature: 1540-1560 ℃, and refining time: 30-40 minutes;
after refining for 5-15 minutes, closing a vacuum electronic valve (a valve connected between a smelting chamber and an evacuating unit), adding SiCa alloy, and re-evacuating after the reaction is finished (after the chemical reaction is finished, a large amount of gas generates insufficient vacuum degree, and if necessary, re-evacuating is carried out, so that the requirement that the vacuum degree is less than or equal to 133Pa is met);
adding metal Mn 10-12 minutes before tapping and stirring;
tapping at 1510-1530 ℃, and carrying out charged pouring;
2) pouring an alloy ingot:
pouring the refined alloy liquid into an alloy ingot mold in vacuum, and after the pouring is finished, quickly breaking the air and adding a heating agent for covering so as to supplement the heat loss of the alloy liquid of the riser;
demoulding to obtain an alloy ingot;
specifically, the refined alloy liquid needs to be poured under vacuum, and after pouring, a heating agent needs to be added immediately after breaking the air; the heating agent is formed by mixing 60-70% of aluminum powder and 30-40% of sodium nitrate;
the using amount of the heat generating agent is 0.2-0.6% of the mass of the alloy liquid;
3) forging and cogging:
heating an alloy ingot by using a resistance furnace, raising the temperature to 800-850 ℃, preserving heat for 30-40 min, raising the temperature to 1150-1200 ℃ along with the furnace, and preserving heat for 30-50 min;
when in forging, the small end of the alloy ingot is forged first, then the large end of the alloy ingot is forged, and the forging terminal temperature is lower than 950 ℃, and the alloy ingot needs to be re-melted and heated for new forging; the specification of the forging stock is (50-60) × L in millimeters, L is the length, and the forging ratio is more than or equal to 9;
after forging, completely burying the forging stock in sand for cooling;
4) hot rolling:
heating the cooled forging stock in a gas furnace or a resistance furnace, wherein the charging temperature is less than or equal to 400 ℃; heating to 980-1010 ℃ along with the furnace, preserving heat for 25-30 min, heating to 1140-1160 ℃ again, preserving heat for 20-30 min, and then hot rolling;
the hot rolling is carried out by adopting a horizontal two-roller hot rolling mill for 6-10 times, and the deformation of each time is controlled to be 16-20%; the finishing temperature is not lower than 900 ℃; the specification of the hot-rolled finished product is phi (15-30) multiplied by L in millimeters, wherein phi 15-30 is the diameter requirement of the hot-rolled finished product, and L is the length;
air cooling after hot rolling is finished;
5) solution treatment:
carrying out solution treatment on a bar obtained by hot rolling in a protective atmosphere: the charging temperature is less than or equal to 100 ℃, the temperature is increased to 850-870 ℃, the temperature is kept for 4-6 h, then the temperature is reduced to 750-780 ℃, the temperature is reduced to less than or equal to 300 ℃, the temperature is kept for 20-30 min, and then the mixture is discharged; obtaining the high-strength soft magnetic alloy 1J22MV alloy bar.
Specifically, the solution treatment is carried out in a hydrogen atmosphere, the temperature is increased to 870 ℃ within 2-3 h, the temperature is kept for 4-6 h, then the temperature is reduced to 780 ℃ at the speed of 30 ℃/h, the temperature is reduced to be less than or equal to 300 ℃ at the speed of 200 ℃/h, the temperature is kept for half an hour and then the alloy is discharged out of the furnace, so that the stress generated by cold and hot processing is eliminated, and the alloy is recrystallized.
Further, in order to ensure the accuracy of the smelting components, when vacuum smelting is carried out, firstly, pure iron in the raw materials is filled into the bottom of the crucible to be flatly filled into a layer, and the rest pure iron is filled into the periphery and the middle upper part of the crucible; then, putting a cobalt sheet into the middle upper part of the crucible; finally, loading the ferrovanadium and molybdenum bars into the upper part of the crucible;
adding the materials in three batches during carbon adding, wherein 1/3 is added in each batch;
the SiCa alloy was added in two batches, 1/2 each.
The carbon and SiCa alloy is used as a deoxidizer, and the deoxidizer adopts a strong-first-weak deoxidation sequence, so that the absorption rate of the alloy is improved, and the consumption of the alloy is reduced; the manganese metal is a volatile element and needs to be added at last, and the manganese is volatilized in the early stage and the middle stage, so that the components are not available.
Specific examples are given below.
Example 1
A preparation method of a high-strength soft magnetic alloy bar comprises the following operations:
1) vacuum smelting:
the raw materials are proportioned according to the smelting requirement, and are weighed according to the requirement, and the raw materials comprise, by mass, not more than 0.04% of C, not more than 0.30% of Si, not more than 0.30% of Mn, not more than 0.020% of P, not more than 0.020% of S, not more than 0.20% of Cu, not more than 0.50% of Ni, 48.5-50.0% of Co, 1.90-2.10% of V, 0.1-0.15% of Mo and the balance of Fe;
firstly, filling pure iron into the bottom of a crucible and flatly filling 1 layer of the pure iron, and filling the rest pure iron into the periphery and the middle upper part of the crucible; then placing a Co sheet into the middle upper part of the crucible; finally, loading the high-vanadium iron and Mo bars into the upper part of the crucible; putting the mixture into a medium-frequency vacuum induction furnace for smelting;
vacuumizing to be less than or equal to 133Pa after furnace closing, then transmitting power at a low power (50-70 kw) for preheating, raising the power (120 kw) when the vacuum degree is less than or equal to 0.66Pa, transmitting power for rapid material melting, and reducing the power (80 kw) in time when splashing occurs in the material melting process; material melting time: 1.5 hours;
adding carbon for deoxidation every 5-8 minutes after the refining temperature is reached, and adding carbon in 3 batches (1/3 carbon in each batch); after the carbon reaction is finished, entering a refining period;
refining temperature: 1540-1560 ℃, and refining time: 40 minutes; tapping at 1510-1530 ℃, and carrying out charged 40kw pouring;
refining for 10 minutes, then closing a valve and adding SiCa alloy, adding the SiCa alloy in 2 batches at intervals of 1-2 min
After the reaction is finished, turning to vacuum;
adding metal Mn and stirring 10-12 minutes before tapping; finally obtaining alloy liquid;
2) pouring an alloy ingot:
pouring the refined alloy ingot into an alloy ingot mold in vacuum, and quickly breaking the air and adding a heating agent after pouring is finished;
the heat generating agent comprises the following components: 70% of aluminum powder and 30% of sodium nitrate; the using amount of the heating agent is 0.2-0.6% of the weight of the molten steel;
through high vacuum smelting, the components (mass percentage) of the alloy ingot meet the smelting requirement; if not, returning to the furnace and refiring;
3) forging and cogging:
heating with a resistance furnace, heating to 850 deg.C, maintaining for 40min, heating to 1180 deg.C with the furnace, and maintaining for 30-50 min; the specification of the forging stock is (50-60) × L, L is the length, and the forging ratio is more than or equal to 9;
when in forging, the small end of the alloy ingot is forged first, then the large end of the alloy ingot is forged, and the forging terminal temperature is lower than 950 ℃, and the alloy ingot needs to be re-melted and heated for new forging;
cooling after forging: sand cooling (complete embedding in sand);
4) hot rolling:
the charging temperature of the forging stock is less than or equal to 400 ℃; heating to 1000 deg.C with the furnace, maintaining for 30min, heating to 1150 deg.C, maintaining for 20min, and rolling; performing finished product hot rolling on a horizontal two-roller hot rolling mill (the deformation of each pass is controlled to be 16-20% after 8 passes), wherein the specification of the hot rolled finished product is as follows in terms of millimeter: phi (15-30) multiplied by L, wherein L is the length; the finishing temperature is not lower than 900 ℃; a cooling mode: air cooling;
5) solution treatment:
carrying out solution treatment in an atmosphere (hydrogen) protective furnace: the charging temperature is less than or equal to 100 ℃, the temperature is increased to 870 ℃ within 2h, the temperature is kept for 4h, the temperature is reduced to 780 ℃ at the speed of 30 ℃/h, then the temperature is reduced to less than or equal to 300 ℃ at the speed of 200 ℃/h, and the temperature is kept for half an hour and then the product is discharged.
The solid solution treatment can dissolve carbides and gamma in the matrix to obtain a uniform supersaturated solid solution, so that the carbides, gamma and other strengthening phases with fine particles and uniform distribution can be precipitated again during aging, and the stress generated by cold and hot processing is eliminated, so that the alloy is recrystallized.
The invention adopts lower solid solution temperature, can obtain smaller grain size, leads the grains to be more uniform and further obtains higher yield strength.
Example 2
A preparation method of a high-strength soft magnetic alloy bar comprises the following operations:
1) vacuum smelting:
the raw materials are proportioned according to the smelting requirement, and are weighed according to the requirement, and the raw materials comprise, by mass, not more than 0.04% of C, not more than 0.30% of Si, not more than 0.30% of Mn, not more than 0.020% of P, not more than 0.020% of S, not more than 0.20% of Cu, not more than 0.50% of Ni, 50.0-51.0% of Co, 2.00-2.10% of V, 0.15-0.2% of Mo and the balance of Fe;
firstly, filling pure iron into the bottom of a crucible and flatly filling 1 layer of the pure iron, and filling the rest pure iron into the periphery and the middle upper part of the crucible; then placing a Co sheet into the middle upper part of the crucible; finally, loading the high-vanadium iron and Mo bars into the upper part of the crucible; putting the mixture into a medium-frequency vacuum induction furnace for smelting;
vacuumizing to be less than or equal to 133Pa after furnace closing, then transmitting power (50 kw) for preheating, increasing power (160 kw) when the vacuum degree is less than or equal to 0.66Pa, transmitting power for rapid material melting, and reducing power (80-100 kw) in time when splashing occurs in the material melting process; material melting time: 1.5-2 hours;
adding carbon for deoxidation every 5-8 minutes after the refining temperature is reached, and adding carbon in 3 batches (1/3 carbon in each batch); after the carbon reaction is finished, entering a refining period;
refining temperature: 1540 ℃, refining time: 40 minutes; tapping temperature is 1510 ℃, and pouring is carried out under the condition of electrification at 40 kw;
refining for 10 minutes, then closing a valve and adding SiCa alloy, adding the SiCa alloy in 2 batches at intervals of 1-2 min
After the reaction is finished, turning to vacuum;
adding metal Mn and stirring 10-12 minutes before tapping; finally obtaining alloy liquid;
2) pouring an alloy ingot:
pouring the refined alloy ingot into an alloy ingot mold in vacuum, and quickly breaking the air and adding a heating agent after pouring is finished;
the heat generating agent comprises the following components: 70% of aluminum powder and 30% of sodium nitrate; the using amount of the heating agent is 0.2-0.6% of the weight of the molten steel;
through high vacuum smelting, the components (mass percentage) of the alloy ingot meet the smelting requirement;
3) forging and cogging:
heating with a resistance furnace, heating to 800 deg.C, maintaining the temperature for 30min, heating to 1150 deg.C, and maintaining the temperature for 30-50 min; the specification of the forging stock is (50-60) × L in millimeters, and L is the length; the forging ratio is more than or equal to 9;
when in forging, the small end of the alloy ingot is forged first, then the large end of the alloy ingot is forged, and the forging terminal temperature is lower than 950 ℃, and the alloy ingot needs to be re-melted and heated for new forging;
cooling after forging: sand cooling (complete embedding in sand);
4) hot rolling:
the charging temperature of the forging stock is less than or equal to 400 ℃; heating to 980 ℃ along with the furnace, preserving heat for 25min, heating to 1140 ℃, preserving heat for 20min, and then rolling; performing finished product hot rolling on a horizontal two-roller hot rolling mill (the deformation of each pass is controlled to be 16-20% after 6-10 passes), wherein the specification of the hot rolled finished product is phi (15-30) multiplied by L in mm, and L is the length;
the finishing temperature is not lower than 900 ℃; a cooling mode: air cooling;
5) solution treatment:
carrying out solution treatment in an atmosphere (hydrogen) protective furnace: the charging temperature is less than or equal to 100 ℃, the temperature is raised to 850 ℃ within 2h, the temperature is kept for 5h, the temperature is lowered to 750 ℃ at the speed of 30 ℃/h, the temperature is lowered to 200 ℃ at the speed of 200 ℃/h, and the temperature is kept for half an hour and then the product is discharged.
Example 3
A preparation method of a high-strength soft magnetic alloy bar comprises the following steps:
1) vacuum smelting:
proportioning according to smelting requirements, taking high-grade pure iron, metal cobalt and ferrovanadium as main raw materials, and taking the high-grade pure iron, the metal cobalt and the ferrovanadium as main raw materials, wherein the high-grade pure iron comprises, by mass, not more than 0.04% of C, not more than 0.30% of Si, not more than 0.30% of Mn, not more than 0.020% of P, not more than 0.020% of S, not more than 0.20% of Cu, not more than 0.50% of Ni, 48.5-50.5% of Co, 1.90-2.00% of V, 0.12-0.18% of Mo, and the balance Fe;
smelting in a vacuum induction furnace, vacuumizing to be less than or equal to 133Pa after furnace closing, transmitting power (50-70 kw) for preheating, extracting power (100 kw) when the vacuum degree is less than or equal to 0.66Pa, transmitting power for rapid material melting, and reducing power (80 kw) in time when splashing occurs in the material melting process; material melting time: 1.5-2 hours;
adding carbon for deoxidation every 5-8 minutes after the refining temperature is reached, and adding carbon in 3 batches (1/3 carbon in each batch); after the carbon reaction is finished, entering a refining period;
refining temperature: 1560 ℃, refining time: 36 minutes; tapping temperature is 1530 ℃, and pouring is carried out at charged 40 kw;
refining for 10 minutes, then closing a valve and adding SiCa alloy, wherein the SiCa alloy is added in 2 batches at intervals of 1-2 min;
after the reaction is finished, turning to vacuum;
adding metal Mn and stirring 10-12 minutes before tapping; finally obtaining alloy liquid;
controlling the chemical components of the alloy liquid in a required range;
2) pouring an alloy ingot:
and finishing the pouring work under vacuum, then quickly breaking the cavity, and adding a prepared heating agent into the cap opening to ensure that the alloy ingot is well fed. Then, peeling by using a common lathe to ensure that the surface of the alloy ingot has no defects of cracks, slag inclusion, air holes and the like;
3) forging and cogging:
heating the alloy ingot to 850 ℃ in a resistance furnace, and preserving heat for 36 min; then the temperature is raised to 1200 ℃ along with the furnace, and the temperature is kept for 45 min. After heat preservation, hot forging the blank into a square billet by adopting an electro-hydraulic hammer, wherein the forging ratio is more than or equal to 9; ensuring that the final forging temperature is more than or equal to 950 ℃, and cooling the sand to room temperature after forging; and after ultrasonic flaw detection, the tail part of the head of the forging stock is cut off, and then the surface is milled or polished to ensure that the surface of the stock has no defects such as cracks. Specifically, the alloy ingot is heated to 1180 +/-10 ℃ in a resistance furnace, and after heat preservation, an electro-hydraulic hammer is adopted to forge control parameters: the forging hammer frequency is controlled to be more than 15-25 times/min, the initial forging temperature is more than or equal to 1190 ℃, and the final forging temperature is more than or equal to 950 ℃. The electro-hydraulic hammer is characterized in that: energy conservation and environmental protection; the operation is convenient, labor is saved, and the action is flexible and reliable; the system works stably and is a safety device with complete design; the transmission efficiency of the hammer is as high as 65 percent, which is 30 times of that of a steam hammer and an air forging hammer; the energy utilization rate can be improved to 20-60%;
4) hot rolling:
heating the forging stock to 1150 +/-10 ℃ in a resistance furnace or a gas furnace, preserving heat for 20min, and then carrying out bar hot rolling on a transverse two-roller hot rolling mill, wherein the specification phi (15-30) xL is unit mm, L is the length, the deformation of each pass is controlled to be 16-20% after 6-10 passes, and the final rolling temperature is not lower than 900 ℃; after the completion, air cooling to room temperature, and removing oxide skin by polishing or acid washing;
5) solution treatment:
carrying out solution treatment on a hot-rolled finished product phi (15-30) multiplied by L and mm in an atmosphere (hydrogen) protective furnace, wherein the heat treatment system is as follows: the charging temperature is less than or equal to 100 ℃, the temperature is increased to 870 ℃ for 3h and is kept for 6h, the temperature is reduced to 780 ℃ at the speed of 30 ℃/h, then the temperature is reduced to less than or equal to 300 ℃ at the speed of 200 ℃/h, and the furnace is taken out after the temperature is kept for half an hour.
The high-strength soft magnetic alloy (1J 22MV bar) prepared by the invention has the characteristics of high saturation magnetic induction intensity, high Curie point, high hysteresis expansion coefficient and the like; actual performance index: the tensile strength is more than 500 MPa; the yield strength is more than or equal to 250 MPa; b800 is more than or equal to 1.8T, B2400, 2400 is more than or equal to 2.1T, B4000 is more than or equal to 2.15T, B8000, 8000 is more than or equal to 2.2T; the coercive force Hc is less than or equal to 144A/m; curie point 980 ℃; saturated hysteresis coefficient of expansion (10)-6) 60-100 parts; the average values of the composition index and the performance index of the multi-batch 1J22MV bar prepared by the invention are shown below.
1J22MV Bar Material composition index
Element(s) C Si Mn S Cu Ni Co Mo V Fe
Content% ≤0.04 ≤0.30 ≤0.30 ≤0.020 ≤0.20 ≤0.50 48.0~51.0 0.1~0.2 1.50~2.10 Balance of
1J22MV average value of mechanical property index of finished bar
Figure 899864DEST_PATH_IMAGE001
Average value of magnetic performance indexes of 1J22MV finished strip products
Hm（A/m） 400 800 1600 2400 4000 8000
Bs（T） 2.015 2.151 2.263 2.310 2.359 2.403
Br（T） 0.721 0.718 0.717 0.713 0.710 0.703
Hr（A/m） 46.76
The embodiments given above are preferable examples for implementing the present invention, and the present invention is not limited to the above-described embodiments. Any non-essential addition and replacement made by the technical characteristics of the technical scheme of the invention by a person skilled in the art belong to the protection scope of the invention.

Claims (5)

1. A preparation method of a soft magnetic alloy bar is characterized by comprising the following operations:
1) vacuum smelting:
preparing the following raw materials according to the smelting requirement of the soft magnetic alloy in percentage by mass: less than or equal to 0.04 percent of C, less than or equal to 0.30 percent of Si, less than or equal to 0.30 percent of Mn, less than or equal to 0.020 percent of P, less than or equal to 0.020 percent of S, less than or equal to 0.20 percent of Cu, less than or equal to 0.50 percent of Ni, 48.0-51.0 percent of Co, 1.80-2.10 percent of V, 0.1-0.2 percent of Mo, and the balance of Fe;
putting pure iron, cobalt sheets, ferrovanadium and molybdenum strips in raw materials into a medium-frequency vacuum induction furnace for smelting;
vacuumizing to less than or equal to 133Pa after the vacuum induction furnace is closed, and transmitting power for preheating at 50-70 kw; increasing the power to 120-160 kw for material melting when the vacuum degree is less than or equal to 0.66Pa, and reducing the power to 80-100 kw in time if splashing occurs in the material melting process; material melting time: 1.5-2 hours;
heating the material to a refining temperature after melting, and then adding carbon and deoxidizing for multiple times at intervals of 5-8 minutes each time; entering a refining period after the carbon reaction is finished;
refining temperature: 1540-1560 ℃, and refining time: 30-40 minutes;
closing a valve connected between the smelting chamber and the evacuating unit after refining is completed for 5-15 minutes, adding SiCa alloy, and vacuumizing again until the pressure is less than or equal to 133Pa after the reaction is completed;
adding metal Mn 10-12 minutes before tapping and stirring;
tapping at 1510-1530 ℃, and carrying out charged pouring;
2) pouring an alloy ingot:
pouring the refined alloy liquid into an alloy ingot mold in vacuum, and after the pouring is finished, quickly breaking the air and adding a heating agent for covering so as to supplement the heat loss of the alloy liquid of the riser;
demoulding to obtain an alloy ingot;
3) forging and cogging:
heating an alloy ingot by using a resistance furnace, raising the temperature to 800-850 ℃, preserving heat for 30-40 min, raising the temperature to 1150-1200 ℃ along with the furnace, and preserving heat for 30-50 min;
when in forging, the small end of the alloy ingot is forged first, then the large end of the alloy ingot is forged, and the forging terminal temperature is lower than 950 ℃, and the alloy ingot needs to be re-melted and heated for new forging; the specification of the forging stock is (50-60) × L in millimeters, L is the length, and the forging ratio is more than or equal to 9;
after forging, completely burying the forging stock in sand for cooling;
4) hot rolling:
heating the cooled forging stock in a gas furnace or a resistance furnace, wherein the charging temperature is less than or equal to 400 ℃; heating to 980-1010 ℃ along with the furnace, preserving heat for 25-30 min, heating to 1140-1160 ℃ again, preserving heat for 20-30 min, and then hot rolling;
the hot rolling is carried out by adopting a horizontal two-roller hot rolling mill for 6-10 times, and the deformation of each time is controlled to be 16-20%; the finishing temperature is not lower than 900 ℃; the specification of the hot-rolled finished product is phi (15-30) multiplied by L in millimeters, and L is the length;
air cooling after hot rolling is finished;
5) solution treatment:
carrying out solution treatment on a bar obtained by hot rolling in a protective atmosphere: the charging temperature is less than or equal to 100 ℃, the temperature is increased to 850-870 ℃, the temperature is kept for 4-6 h, then the temperature is reduced to 750-780 ℃, the temperature is reduced to less than or equal to 300 ℃, the temperature is kept for 20-30 min, and then the mixture is discharged; obtaining the high-strength soft magnetic alloy bar.
2. The method for preparing a soft magnetic alloy bar according to claim 1, wherein, in the vacuum melting, pure iron in the raw materials is firstly filled into the bottom of the crucible to be flatly filled into a layer, and the rest pure iron is filled into the periphery and the middle upper part of the crucible; then, putting a cobalt sheet into the middle upper part of the crucible; finally, loading the ferrovanadium and molybdenum bars into the upper part of the crucible;
adding the materials in three batches during carbon adding, wherein 1/3 is added in each batch;
the SiCa alloy was added in two batches, 1/2 each.
3. The method for preparing the magnetically soft alloy bar according to claim 1, wherein the refined alloy liquid is poured under vacuum, and the heating agent is added after the refined alloy liquid is poured;
the heating agent is formed by mixing 60-70% of aluminum powder and 30-40% of sodium nitrate;
the amount of the heat generating agent is 0.2-0.6% of the mass of the alloy liquid.
4. The method for preparing a soft magnetic alloy bar according to claim 1, wherein during forging and cogging, an alloy ingot is heated to 1170-1190 ℃ in a resistance furnace, and is forged by an electro-hydraulic hammer after heat preservation, wherein the frequency of the forging hammer is controlled to be more than 15-25 times/min, the initial forging temperature is not less than 1190 ℃, and the final forging temperature is not less than 950 ℃.
5. The preparation method of the magnetically soft alloy bar according to claim 1, wherein the solution treatment is performed in a hydrogen atmosphere, the temperature is raised to 870 ℃ within 2-3 h, the temperature is kept for 4-6 h, then the temperature is lowered to 780 ℃ at a rate of 30 ℃/h, then the temperature is lowered to less than or equal to 300 ℃ at 200 ℃/h, and the temperature is kept for half an hour and then the bar is discharged.
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