CN111020098A - Preparation method of high-purity electromagnetic pure iron - Google Patents

Preparation method of high-purity electromagnetic pure iron Download PDF

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CN111020098A
CN111020098A CN201911302388.XA CN201911302388A CN111020098A CN 111020098 A CN111020098 A CN 111020098A CN 201911302388 A CN201911302388 A CN 201911302388A CN 111020098 A CN111020098 A CN 111020098A
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pure iron
vacuum
temperature
electromagnetic
purity
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CN111020098B (en
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陈梅
杨平
侯蕊
王小明
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Shaanxi Sirui Advanced Materials Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21CPROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C3/00Manufacture of wrought-iron or wrought-steel
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21CPROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C7/00Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/10Handling in a vacuum
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216Modifying 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
    • C21D8/1222Hot rolling
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244Modifying 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
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
    • C21D8/1283Application of a separating or insulating coating

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Electromagnetism (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a preparation method of high-purity electromagnetic pure iron, and belongs to the technical field of pure iron preparation. Comprises the steps of vacuum induction melting, vacuum consumable remelting, cogging rolling and aging treatment; the invention selects the industrial pure iron with the purity higher than 99 percent as the raw material, adopts a double-vacuum smelting mode in the production process, fully expounds the capability of a vacuum induction furnace for smelting and removing gas, non-metal isomerate and harmful elements, and simultaneously obtains the electromagnetic pure iron with high purity, good density and average chemical composition and microstructure through vacuum consumable remelting secondary purification; the surface hardness, wear resistance and high temperature resistance of the electromagnetic pure iron can be effectively improved by carrying out vacuum magnetron sputtering and glow nitriding treatment on the rolled section.

Description

Preparation method of high-purity electromagnetic pure iron
Technical Field
The invention belongs to the technical field of pure iron preparation, and particularly relates to a preparation method of high-purity electromagnetic pure iron.
Background
The X-ray tube is generally applied to the X-ray imaging technology, and the common X-ray tubes on the market at present have two types, one is a fixed anode tube, and the other is a rotary anode tube for increasing the heat capacity. The rotating anode X-ray tube is a high vacuum electric vacuum device, and its working principle is that it is fixed on the bearing seat of one end placed in the vacuum glass tube by means of rotor, and can be driven to rotate by means of action of stator placed outside the vacuum glass tube, and the filament is fixed on the cathode placed at another end in the vacuum glass tube, and respectively applies negative voltage to the filament, and after the positive voltage is applied to the anode, the electron emitted from filament can be impacted on the anode, so that the X-ray can be produced.
At present, the rotating speed of a rotating anode bulb rotor is more than 3000 revolutions per minute, the rotating speed of a high-speed rotating anode bulb can reach 7200 revolutions per minute, the rotating speed of an ultra-high-speed bulb can reach more than 1 ten thousand revolutions per minute at present, the rotating speed of the bulb anode rotor is designed according to the focus current density of the bulb, the focus of the bulb with the same current is smaller, the rotating speed of the bulb rotating anode rotor is required to be higher, if the rotating speed of the rotor is abnormal, the accuracy of kV and mA output by the bulb can be lowered when the bulb is ignited, the imaging quality can be reduced, the judgment of medical staff on the state of an illness can be influenced, and the importance of ensuring good heat dissipation of the bulb can be seen.
Because the rotor is difficult to bear the high temperature that the rotation produced when rotating, burn out easily, influence the normal use of rotary anode X-ray tube, so, the rotor that has high temperature resistance can avoid its high temperature to burn out when fast turn round, and the rotor waits for a long time, can produce wearing and tearing, make rotor and stator air gap increase, lead to the vortex to increase, make the operating current have the increase of certain degree, and the purity of preparation rotor part material also can influence the rotor performance, and current rotor still lacks in high purity, high temperature resistance and wear resistance, need improve.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of high-purity electromagnetic pure iron with high temperature resistance, good compactness and uniform chemical components.
The technical scheme of the invention is as follows: a preparation method of high-purity electromagnetic pure iron mainly comprises the following steps:
(1) vacuum induction melting: loading industrial pure iron into vacuum induction furnace, vacuumizing until vacuum degree reaches 5 × 10- 1Heating the ceramic crucible when the pressure is less than Pa, and heating the crucible when the pressure is lower than PaGradually melting the inner industrial pure iron, closing a vacuum system, filling inert protective gas until the vacuum degree is-0.2-0.02 Mpa so as to melt the industrial pure iron, and then pouring to form a prefabricated casting;
(2) vacuum consumable remelting: welding the prefabricated casting with a false electrode of a vacuum consumable electrode furnace, then placing the prefabricated casting into the vacuum consumable electrode furnace, vacuumizing, smelting at the heating rate of 45-50 ℃/min, completing the smelting when the temperature reaches 1500-;
(3) cogging and rolling; cogging the remelted electromagnetic pure iron ingot in a hot forging mode, wherein cogging is required to ensure that the final heat deformation is more than 45%, manufacturing a plate blank, heating the plate blank to 980-1020 ℃, rolling at the temperature of below 900 ℃ to obtain a rolled section, and finally annealing;
(4) aging treatment: and (3) carrying out aging treatment on the rolled section obtained in the step (4) by using an electromagnetic vibration aging instrument at the temperature of 220-.
Furthermore, the purity of the industrial pure iron in the step (1) is more than 99.9%, the high-purity electromagnetic pure iron can be prepared from the industrial pure iron with the purity of more than 99%, and the electromagnetic pure iron has high compactness and uniform components and meets the use requirements.
Further, when smelting is carried out in the step (1), adding rare earth element La with the weight percentage of less than or equal to 0.035% and rare earth element Ce with the weight percentage of less than or equal to 0.025% into the molten liquid, and then carrying out electromagnetic stirring; the added rare earth elements can act with other elements in a synergistic way, so that the crystal grains of the cast structure of the electromagnetic pure iron are fully refined, and the generation of segregation is reduced.
Further, the surface of the rolled section obtained in the step (3) is polished before annealing, then is cleaned and dried, and an electromagnetic shielding solution with the conductivity of 5-35S/m is sputtered on the surface of the rolled section by using a vacuum magnetron sputtering device, wherein the vacuum magnetron sputtering time is 2-3h, and the electromagnetic shielding solution is sputtered on the surface of the electromagnetic pure iron rolled section, so that the surface hardness, the wear resistance and the high-temperature chemical stability resistance of the electromagnetic pure iron can be effectively improved.
Further, the electromagnetic shielding solution is prepared by mixing graphene conductive carbon paste and polymer fiber fused mass according to the mass ratio of 1:3, wherein the graphene conductive carbon paste is the graphene conductive carbon paste produced by Nicotiana Huaheng energy-saving technology Limited and the model number of the graphene conductive carbon paste is HNX5, and the polymer fiber fused mass is polymethyl methacrylate.
Further, the specific process of the vacuum magnetron sputtering treatment is as follows:
s1: fixing the rolled section after polishing on a sputtering platform of vacuum magnetron sputtering equipment, then putting an electromagnetic shielding solution into a magnetron sputtering chamber, and closing the magnetron sputtering chamber;
s2: vacuumizing the magnetron sputtering chamber to a vacuum degree of 5 multiplied by 10-5-3×10-4Pa, then introducing argon, and turning on a power supply when the air pressure in the magnetron sputtering chamber is 0.8-1.1 Pa;
s3: adjusting the air pressure in the magnetron sputtering chamber to be 0.3-0.5Pa, and carrying out magnetron sputtering for 3-5h to obtain a finished product.
Further, the annealing treatment in the step (3) is performed in a stress relief annealing manner, and the specific process is as follows: and (3) placing the rolled section in the step (4) in a vacuum furnace, raising the temperature at a heating rate of 15-25 ℃/min under a protective atmosphere, carrying out uniform temperature treatment for 20-30min when the temperature reaches 550-600 ℃, then raising the temperature at a heating rate of 35-45 ℃/min, preserving the temperature for 35-45min when the temperature reaches 750-850 ℃, and finally reducing the temperature to room temperature at a cooling rate of 15-20 ℃/h.
Further, the rolled section obtained in the step (3) is subjected to glow nitriding treatment between annealing, and the specific process is as follows: putting the obtained rolled section into a glow ion nitriding furnace, introducing argon into the glow ion nitriding furnace, heating at the speed of 15-25 ℃/min, introducing ammonia gas into the glow ion nitriding furnace for 35-45min when the temperature reaches 450-600 ℃ until the pressure is 150-250Pa, stopping introducing the ammonia gas and the argon gas, finally introducing air into the glow ion nitriding furnace for low-pressure oxidation treatment for 30-35min, and cooling; by performing glow nitriding treatment on the electromagnetic pure iron cast ingot, the hardness of the surface of the electromagnetic pure iron cast ingot material is obviously improved, and the surface wear resistance and high temperature resistance are improved, so that the service life of a rotor in an X-ray bulb tube is prolonged.
The invention has the beneficial effects that: the invention selects the industrial pure iron with the purity higher than 99 percent as the raw material, so that the prepared electromagnetic pure iron has less impurity content, high purity and uniform components, meets the use requirement, fully expounds the capability of a vacuum induction furnace for removing gas, non-metal assimilates and harmful elements by smelting in a double vacuum smelting mode in the production process, and obtains the electromagnetic pure iron with high purity, good density and average chemical components and microstructure by vacuum consumable remelting secondary purification; by adding rare earth elements into the molten liquid in the smelting process, the grains of the cast structure of the electromagnetic pure iron can be fully refined, and the generation of segregation is reduced; the surface hardness, wear resistance and high temperature resistance of the electromagnetic pure iron can be effectively improved by carrying out vacuum magnetron sputtering and glow nitriding treatment on the rolled section, so that the service life of a rotor in the X-ray bulb tube is prolonged.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following examples, but the scope of the present invention is not limited thereto.
Example 1
The method for preparing the high-purity electromagnetic pure iron mainly comprises the following steps:
(1) vacuum induction melting: loading industrial pure iron with purity of 99.9% into a vacuum induction furnace, vacuumizing until the vacuum degree reaches 5 × 10-1Heating the ceramic crucible when Pa is needed, gradually melting industrial pure iron in the crucible, and adding 0.035 wt% of rare earth element La and 0.025 wt% of rare earth element into the molten liquidCarrying out electromagnetic stirring on the element Ce; the added rare earth elements can act with other elements in a synergistic way, so that the crystal grains of the cast structure of the electromagnetic pure iron are fully refined, the generation of segregation is reduced, a vacuum system is closed, inert protective gas is filled until the vacuum degree is-0.2 Mpa, so that the industrial pure iron is melted, and then pouring is carried out, so as to form a prefabricated casting;
(2) vacuum consumable remelting: welding the prefabricated casting with a false electrode of a vacuum consumable electrode furnace, then placing the prefabricated casting into the vacuum consumable electrode furnace, vacuumizing, smelting at the heating rate of 45 ℃/min, finishing the smelting when the temperature reaches 1500 ℃, and pouring again to obtain an electromagnetic pure iron ingot with the required specification;
(3) cogging and rolling; cogging the remelted electromagnetic pure iron ingot in a hot forging mode, wherein cogging is required to ensure that the final heat deformation is 45%, manufacturing a plate blank, heating the plate blank to 980 ℃, rolling at the temperature of below 900 ℃ to obtain a rolled section, and finally annealing;
(4) aging treatment: and (3) carrying out aging treatment on the rolled section obtained in the step (4) by using an electromagnetic vibration aging instrument at the temperature of 220 ℃, and finally cooling to obtain a finished product, wherein the frequency of the electromagnetic vibration aging instrument is 3000Hz, and the aging treatment time is 15 h.
Example 2
The method for preparing the high-purity electromagnetic pure iron mainly comprises the following steps:
(1) vacuum induction melting: loading industrial pure iron with purity of 99.9% into a vacuum induction furnace, vacuumizing until the vacuum degree reaches 4 × 10-1Heating the ceramic crucible when Pa is needed, gradually melting industrial pure iron in the crucible, adding 0.034 wt% of rare earth element La and 0.024 wt% of rare earth element Ce into the molten liquid, and then performing electromagnetic stirring; the added rare earth elements can act with other elements in a synergistic way, so that the crystal grains of the cast structure of the electromagnetic pure iron are fully refined, the generation of segregation is reduced, a vacuum system is closed, inert protective gas is filled until the vacuum degree is 0.01Mpa, so that the industrial pure iron is melted, and then pouring is carried out, so as to form a prefabricated casting;
(2) vacuum consumable remelting: welding the prefabricated casting with a false electrode of a vacuum consumable electrode furnace, then placing the prefabricated casting into the vacuum consumable electrode furnace, vacuumizing, smelting at the heating rate of 48 ℃/min, finishing the smelting when the temperature reaches 1700 ℃, and pouring again to obtain the electromagnetic pure iron ingot with the required specification;
(3) cogging and rolling; cogging the remelted electromagnetic pure iron ingot in a hot forging mode, wherein the cogging requirement ensures that the final heat deformation is 48%, manufacturing a plate blank, heating the plate blank to 1000 ℃, rolling at the temperature of below 900 ℃ to obtain a rolled section, and finally annealing;
(4) aging treatment: and (3) carrying out aging treatment on the rolled section obtained in the step (4) by using an electromagnetic vibration aging instrument at the temperature of 240 ℃, and finally cooling to obtain a finished product, wherein the frequency of the electromagnetic vibration aging instrument is 4000Hz, and the aging treatment time is 17 h.
Example 3
The method for preparing the high-purity electromagnetic pure iron mainly comprises the following steps:
(1) vacuum induction melting: loading industrial pure iron with purity of 99.9% into a vacuum induction furnace, vacuumizing until the vacuum degree reaches 3 × 10-1Heating the ceramic crucible when Pa is needed, gradually melting industrial pure iron in the crucible, adding 0.033 weight percent of rare earth element La and 0.023 weight percent of rare earth element Ce into the melt, and then electromagnetically stirring; the added rare earth elements can act with other elements in a synergistic way, so that the crystal grains of the cast structure of the electromagnetic pure iron are fully refined, the generation of segregation is reduced, a vacuum system is closed, inert protective gas is filled until the vacuum degree is 0.02Mpa, so that the industrial pure iron is melted, and then pouring is carried out, so as to form a prefabricated casting;
(2) vacuum consumable remelting: welding the prefabricated casting with a false electrode of a vacuum consumable electrode furnace, then placing the prefabricated casting into the vacuum consumable electrode furnace, vacuumizing, smelting at the heating rate of 50 ℃/min, finishing the smelting when the temperature reaches 1850 ℃, and pouring again to obtain an electromagnetic pure iron ingot with the required specification;
(3) cogging and rolling; cogging the remelted electromagnetic pure iron ingot in a hot forging mode, wherein the cogging requirement ensures that the final heat deformation is 50%, manufacturing a plate blank, heating the plate blank to 1020 ℃, rolling at the temperature of below 900 ℃ to obtain a rolled section, and finally annealing;
(4) aging treatment: and (3) carrying out aging treatment on the rolled section obtained in the step (4) by using an electromagnetic vibration aging instrument at the temperature of 250 ℃, and finally cooling to obtain a finished product, wherein the frequency of the electromagnetic vibration aging instrument is 5000Hz, and the aging treatment time is 18 h.
Example 4
This embodiment is substantially the same as embodiment 2 except that:
and (3) grinding and polishing the surface of the obtained rolled section before annealing, cleaning and drying, sputtering an electromagnetic shielding solution with the conductivity of 20S/m on the surface of the rolled section by using a vacuum magnetron sputtering device, wherein the time of the vacuum magnetron sputtering treatment is 2.5h, the electromagnetic shielding solution is prepared by mixing graphene conductive carbon slurry and polymer fiber melt according to the mass ratio of 1:3, the graphene conductive carbon slurry is graphene conductive carbon slurry with the model of HNX5 produced by Nicotiana Huaheng energy-saving technology Limited, the polymer fiber melt is polymethyl methacrylate, and the electromagnetic shielding solution is sputtered on the surface of the electromagnetic pure iron rolled section, so that the surface hardness, the wear resistance and the high-temperature chemical stability of the electromagnetic pure iron can be effectively improved.
The specific process of the vacuum magnetron sputtering treatment comprises the following steps:
s1: fixing the rolled section after polishing on a sputtering platform of vacuum magnetron sputtering equipment, then putting an electromagnetic shielding solution into a magnetron sputtering chamber, and closing the magnetron sputtering chamber;
s2: vacuumizing the magnetron sputtering chamber to a vacuum degree of 3 multiplied by 10-4Pa, then introducing argon, and turning on a power supply when the air pressure in the magnetron sputtering chamber is 1.1 Pa;
s3: and adjusting the air pressure in the magnetron sputtering chamber to be 0.5Pa, and performing magnetron sputtering for 5 hours to obtain a finished product.
Example 5
This example is substantially the same as example 4, except that:
the annealing treatment in the step (3) is carried out in a stress relief annealing mode, and the specific process is as follows: and (3) placing the rolled section in the step (3) into a vacuum furnace, heating at a heating rate of 25 ℃/min under a protective atmosphere, carrying out uniform temperature treatment for 30min when the temperature reaches 600 ℃, then heating at a heating rate of 45 ℃/min, keeping the temperature for 45min when the temperature reaches 850 ℃, finally, reducing the temperature to room temperature at a cooling rate of 20 ℃/h, and carrying out stress-relief annealing treatment on the rolled section, thereby effectively preventing the growth of crystal grains in the annealing process, effectively eliminating the residual stress inside a formed part, and not generating new cracks when the stress is eliminated.
Example 6
This example is substantially the same as example 5 except that:
the rolled section obtained in the step (3) is subjected to glow nitriding treatment between annealing, and the specific process is as follows: putting the obtained rolled section into a glow ion nitriding furnace, introducing argon into the glow ion nitriding furnace, heating at the speed of 25 ℃/min, introducing ammonia gas into the glow ion nitriding furnace for 45min when the temperature reaches 600 ℃ until the pressure is 250Pa, stopping introducing the ammonia gas and the argon gas, introducing air into the glow ion nitriding furnace for low-pressure oxidation treatment for 35min, and cooling; by performing glow nitriding treatment on the electromagnetic pure iron cast ingot, the hardness of the surface of the electromagnetic pure iron cast ingot material is obviously improved, and the surface wear resistance and high temperature resistance are improved, so that the service life of a rotor in an X-ray bulb tube is prolonged.
Test examples
The relevant performance parameters of the high purity electromagnetic pure iron materials prepared according to examples 1-6 of the present invention are shown in table 1:
table 1: high-purity electromagnetic pure iron material
Figure BDA0002322183860000081
And (4) conclusion: as can be seen from Table 1, the high-purity electromagnetic pure iron materials prepared by the preparation methods of the embodiments 1 to 6 of the present invention have an average conductivity of 3.16 × 106S/m, an average oxygen content of 375.2 or less, an average hardness of 77.8HB or more, and an average high temperature resistance of 730, so that the high-purity electromagnetic pure iron prepared by the present invention has high conductivity and hardness, and low oxygen content, and meanwhile, the surface working temperature of the anode rotor can reach 600-700 ℃, while the high temperature resistance of the high-purity electromagnetic pure iron materials prepared by the present invention has an average temperature of 730 which is higher than the surface working temperature of the anode rotor, so that the use requirements are met, and the preparation method of the embodiment 6 is the best.

Claims (7)

1. The preparation method of the high-purity electromagnetic pure iron is characterized by mainly comprising the following steps of:
(1) vacuum induction melting: loading industrial pure iron into vacuum induction furnace, vacuumizing until vacuum degree reaches 5 × 10-1Heating the ceramic crucible when the pressure is lower than Pa, gradually melting the industrial pure iron in the crucible, closing a vacuum system, filling inert protective gas until the vacuum degree is-0.2-0.02 Mpa so as to melt the industrial pure iron, and then pouring to form a prefabricated casting;
(2) vacuum consumable remelting: welding the prefabricated casting with a false electrode of a vacuum consumable electrode furnace, then placing the prefabricated casting into the vacuum consumable electrode furnace, vacuumizing, smelting at the heating rate of 45-50 ℃/min, completing the smelting when the temperature reaches 1500-;
(3) cogging and rolling; cogging the remelted electromagnetic pure iron ingot in a hot forging mode, wherein cogging is required to ensure that the final heat deformation is more than 45%, manufacturing a plate blank, heating the plate blank to 980-1020 ℃, rolling at the temperature of below 900 ℃ to obtain a rolled section, and finally annealing;
(4) aging treatment: and (3) carrying out aging treatment on the rolled section obtained in the step (4) by using an electromagnetic vibration aging instrument at the temperature of 220-.
2. The method for preparing high-purity electromagnetic pure iron according to claim 1, wherein the purity of the industrial pure iron in the step (1) is more than 99.9%.
3. The method for preparing high-purity electromagnetic pure iron according to claim 1, wherein in the step (1), when smelting, the rare earth element La with the weight percentage less than or equal to 0.035% and the rare earth element Ce with the weight percentage less than or equal to 0.025% are added into the molten liquid, and then electromagnetic stirring is carried out.
4. The method for preparing high-purity electromagnetic pure iron according to claim 1, wherein the rolled section obtained in step (3) is subjected to grinding and polishing treatment on the surface of the obtained rolled section before annealing, then is cleaned and dried, and an electromagnetic shielding solution with the conductivity of 5-35S/m is sputtered on the surface of the rolled section by using a vacuum magnetron sputtering device, wherein the time of the vacuum magnetron sputtering treatment is 2-3 hours.
5. The method for preparing high-purity electromagnetic pure iron according to claim 4, wherein the electromagnetic shielding solution is prepared by mixing graphene conductive carbon paste and polymer fiber melt according to a mass ratio of 1: 3.
6. The method for preparing high-purity electromagnetic pure iron according to claim 4, wherein the vacuum magnetron sputtering treatment comprises the following specific steps:
s1: fixing the rolled section after polishing on a sputtering platform of vacuum magnetron sputtering equipment, then putting an electromagnetic shielding solution into a magnetron sputtering chamber, and closing the magnetron sputtering chamber;
s2: vacuumizing the magnetron sputtering chamber to a vacuum degree of 5 multiplied by 10-5-3×10-4Pa, then introducing argon, and turning on a power supply when the air pressure in the magnetron sputtering chamber is 0.8-1.1 Pa;
s3: adjusting the air pressure in the magnetron sputtering chamber to be 0.3-0.5Pa, and carrying out magnetron sputtering for 3-5h to obtain a finished product.
7. The method for preparing high-purity electromagnetic pure iron according to claim 1, wherein the annealing treatment in the step (3) is performed by stress relief annealing, and the specific process is as follows: and (4) placing the rolled section in the step (4) into a vacuum furnace, raising the temperature at a temperature raising rate of 15-25 ℃/min under a protective atmosphere, carrying out uniform temperature treatment for 20-30min when the temperature reaches 550-600 ℃, then raising the temperature at a temperature raising rate of 35-45 ℃/min, preserving the temperature for 35-45min when the temperature reaches 750-850 ℃, and finally lowering the temperature to the room temperature at a temperature lowering rate of 15-20 ℃/h.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112359186A (en) * 2020-11-13 2021-02-12 沈阳航天新光集团有限公司 Vacuum annealing method for magnetic material
CN115418579A (en) * 2022-08-02 2022-12-02 邢台钢铁有限责任公司 Production method of super electromagnetic pure iron DT4C high-speed wire

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103205548A (en) * 2013-04-16 2013-07-17 山西太钢不锈钢股份有限公司 Manufacturing method of low-coercive force electromagnetic pure ion cold-rolled sheet
CN103789609A (en) * 2014-02-13 2014-05-14 山西太钢不锈钢股份有限公司 Method for manufacturing electromagnetic pure iron
CN104232856A (en) * 2014-08-19 2014-12-24 西安三威安防科技有限公司 Annealing method for electromagnetic pure iron
CN107541591A (en) * 2017-08-29 2018-01-05 西安汇丰精密合金制造有限公司 A kind of manufacture method of super electromagnetic pure iron DT4C bars
CN107706386A (en) * 2017-09-30 2018-02-16 山西沃特海默新材料科技股份有限公司 A kind of copper alusil alloy nanometer anode material of lithium battery and preparation method thereof
CN107779544A (en) * 2017-09-14 2018-03-09 唐山钢铁集团有限责任公司 A kind of smelting process for producing electromagnetic pure iron
EP3321012A1 (en) * 2016-11-11 2018-05-16 United Technologies Corporation Additive manufacturing process with metal chips produced by machining processes as feedstock
CN110484762A (en) * 2019-09-04 2019-11-22 陕西斯瑞新材料股份有限公司 A kind of method of novel motor rotor Copper-iron alloy material

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103205548A (en) * 2013-04-16 2013-07-17 山西太钢不锈钢股份有限公司 Manufacturing method of low-coercive force electromagnetic pure ion cold-rolled sheet
CN103789609A (en) * 2014-02-13 2014-05-14 山西太钢不锈钢股份有限公司 Method for manufacturing electromagnetic pure iron
CN104232856A (en) * 2014-08-19 2014-12-24 西安三威安防科技有限公司 Annealing method for electromagnetic pure iron
EP3321012A1 (en) * 2016-11-11 2018-05-16 United Technologies Corporation Additive manufacturing process with metal chips produced by machining processes as feedstock
CN107541591A (en) * 2017-08-29 2018-01-05 西安汇丰精密合金制造有限公司 A kind of manufacture method of super electromagnetic pure iron DT4C bars
CN107779544A (en) * 2017-09-14 2018-03-09 唐山钢铁集团有限责任公司 A kind of smelting process for producing electromagnetic pure iron
CN107706386A (en) * 2017-09-30 2018-02-16 山西沃特海默新材料科技股份有限公司 A kind of copper alusil alloy nanometer anode material of lithium battery and preparation method thereof
CN110484762A (en) * 2019-09-04 2019-11-22 陕西斯瑞新材料股份有限公司 A kind of method of novel motor rotor Copper-iron alloy material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
常启兵: "《复合材料:案例式》", 30 September 2018, 江苏凤凰美术出版社 *
张定华 等: "《蜗轮叶片精密铸造模具技术》", 30 April 2014, 国防工业出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112359186A (en) * 2020-11-13 2021-02-12 沈阳航天新光集团有限公司 Vacuum annealing method for magnetic material
CN115418579A (en) * 2022-08-02 2022-12-02 邢台钢铁有限责任公司 Production method of super electromagnetic pure iron DT4C high-speed wire

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