CN112522636A - Nb-doped Fe-Cr-Co permanent magnetic alloy and preparation method thereof - Google Patents
Nb-doped Fe-Cr-Co permanent magnetic alloy and preparation method thereof Download PDFInfo
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- CN112522636A CN112522636A CN202011271271.2A CN202011271271A CN112522636A CN 112522636 A CN112522636 A CN 112522636A CN 202011271271 A CN202011271271 A CN 202011271271A CN 112522636 A CN112522636 A CN 112522636A
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- C22C38/00—Ferrous alloys, e.g. steel alloys
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- 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/04—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering with simultaneous application of supersonic waves, magnetic or electric fields
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/005—Modifying the physical properties by deformation combined with, or followed by, heat treatment of ferrous alloys
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- 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
- H01F1/032—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 hard-magnetic materials
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Abstract
The invention discloses an Nb-doped iron-chromium-cobalt permanent magnetic alloy and a preparation method thereof, belonging to the technical field of magnetic material preparation. The alloy comprises the following chemical elements in percentage by mass: 42-55% of Fe, 25-27% of Cr, 14-16% of Co, 3-3.5% of Mo, 0.81-1.2% of Ti and 0.05-0.2% of Nb. The preparation method comprises a smelting process, a forging process, a hot rolling process, a solid solution treatment process, a magnetic field treatment process and a multi-stage tempering process, wherein the forging temperature is 1100-1200 ℃, the hot rolling temperature is 1100-1150 ℃, the solid solution heat treatment temperature is 1100-1300 ℃, and the isothermal magnetic field heat treatment temperature is 640-660 ℃. According to the invention, a small amount of Nb element is added on the basis of the traditional iron-chromium-cobalt permanent magnetic alloy, and the effects of grain refinement and grain boundary segregation of the element are utilized, so that the effects of improving the oxidation resistance and the coercive force of the alloy material are realized.
Description
Technical Field
The invention belongs to the technical field of magnetic material preparation, and particularly relates to an Nb-doped Fe-Cr-Co-based permanent magnetic alloy material and a preparation method thereof.
Background
The permanent-magnet Fe-Cr-Co alloy is a new type permanent-magnet alloy developed in the seventies of the last century because of its good machinability and its property of being compatible with AlNiCo5Compared with the magnetic property, the material has a good place in the permanent magnetic material. In recent decades, FeCrCo permanent magnetic alloy has been put into mass industrial production due to its advantages of low cobalt content and relatively high magnetic property, and has been developed greatly. With the increasing development of science and technology, new requirements are put forward for the magnetic material in various application fields. For example, the newly-appeared hysteresis motor, super-speed motor and some military instruments require isotropic FeCrCo alloy with higher magnetic performance. At present, a great deal of relevant reports are available for research on the influence of alloy components on the magnetic performance of isotropic FeCrCo alloy by properly changing the alloy components and adding alloying elements such as Si, V, Ti and the like on the basis of FeCrCo permanent magnetic alloy.
The traditional high-quality FeCrCo permanent magnet alloy comprises the following main components: 25-27% of Cr, 14-16% of Co, 3-3.5% of Mo, 0.5-0.8% of Ti and 42-55% of Fe. The permanent magnetic performance of the FeCrCo permanent magnetic alloy is obtained through instability decomposition, the coercive force can reach 650Oe, and the remanence is 1.2T. However, if the FeCrCo permanent magnetic alloy is used as a magnetic recording drum material, the coercive force is still low, and although the FeCrCo permanent magnetic alloy can still be applied, the FeCrCo permanent magnetic alloy has the problems of poor processability, such as easy surface deformation, scratches and non-uniformity of magnetization. In addition, the surface of the FeCrCo permanent magnetic alloy material can be oxidized after being placed for a period of time, so that the material is not favorable for continuous use.
Disclosure of Invention
Aiming at the problems of low coercive force, poor processing performance and easy oxidation of FeCrCo permanent magnetic alloy in practical application in the prior art, the invention provides an Nb-doped iron-chromium-cobalt permanent magnetic alloy material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the Nb-doped iron-chromium-cobalt permanent magnetic alloy comprises the following chemical elements in percentage by mass: 42-55% of Fe, 25-27% of Cr, 14-16% of Co, 3-3.5% of Mo, 0.81-1.2% of Ti and 0.05-0.2% of Nb.
A preparation method of Nb doped iron-chromium-cobalt permanent magnetic alloy comprises the following steps:
(1) smelting: smelting alloy raw materials according to chemical element composition, and casting into steel ingots;
(2) forging: the ingot is scalped and then forged to a proper size, and the forging heating temperature is 1100-1200 ℃;
(3) a hot rolling procedure: heating the hot rolled blank along with a furnace to 1100-1150 ℃, carrying out heat preservation for 30min, carrying out hot rolling forming according to the required specification, and cutting and processing into a sample with a preset specification;
(4) a solution treatment process: carrying out solution treatment on the sample at the temperature of 1100-1300 ℃ for 20-30 min, and carrying out water cooling to enable the alloy to form a single alpha phase;
(5) a magnetic field treatment process: carrying out isothermal magnetic field heat treatment on the sample subjected to the solution treatment at the temperature of 640-660 ℃, keeping the temperature for 30-100 min, keeping the magnetic field intensity to be more than 2500Oe, and cooling the sample to 500 ℃ along with a furnace in a magnetic field;
(6) a tempering procedure: and (4) performing multistage tempering on the sample subjected to the magnetic field treatment.
Further, in the smelting process in the step (1), a 25kg vacuum induction furnace is adopted to smelt the alloy, and after smelting, a vacuum water-cooling ingot casting mold is broken to cast a steel ingot, wherein the weight of the ingot is 20-25 kg.
Further, in the forging procedure in the step (2), the heating time is set according to the size of the steel ingot and the coefficient of 0.5min/mm, and the final forging temperature is not lower than 960 ℃.
Further, the multi-stage tempering system in the tempering process in the step (6) is as follows: and (3) performing step tempering at 610 deg.C for 30min-600 deg.C, 60min-580 deg.C for 120min-560 deg.C, 180min-540 deg.C for 240 min.
Compared with the prior art, the technical scheme of the invention has the following innovation points and beneficial effects:
(1) from the perspective of alloy design, the invention innovatively introduces trace alloy Nb, and widens the alloy design principle;
(2) according to the invention, a small amount of Nb is added into the FeCrCo permanent magnetic alloy, so that the processing performance of the FeCrCo permanent magnetic alloy is improved, meanwhile, the solid solution Nb is subjected to segregation at the grain boundary so as to increase the oxidation resistance of the FeCrCo permanent magnetic alloy, and the addition of Nb can effectively refine grains, so that the coercive force of the alloy material is increased to a certain extent.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 shows the hysteresis loops of the easy magnetization axis (Ea) and the hard magnetization axis (Ha) of FeCoCr permanent magnetic alloys not doped with Nb element (a) and doped with Nb element (b).
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
It should be understood that the described embodiments are only some embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention discloses an Nb-doped Fe-Cr-Co permanent magnetic alloy and a preparation method thereof.
Example 1:
the material comprises the following chemical elements in percentage by mass: 27% of Cr, 15% of Co, 3.5% of Mo, 1.1% of Ti, 53.3% of Fe and 0.1% of Nb, wherein the raw materials comprise industrial pure iron, metallic chromium, electrolytic cobalt and alloying elements Mo, Ti and Nb, the raw materials are smelted by adopting a 25kg vacuum induction furnace, and the smelted raw materials are broken into a vacuum water-cooled ingot casting mold and cast into an ingot with the weight of 20 kg. The ingot is scalped and then forged to a proper size, the forging heating temperature is 1100 ℃, the heating time is set according to the ingot size and the coefficient of 0.5min/mm, and the final forging temperature is 960 ℃. The hot rolled blank is heated up along with the furnace, heated to 1100 ℃, kept warm for 30 minutes, then hot rolled and formed according to the required specification, cut and processed into
The sample of (1). Carrying out heat treatment at 1100 ℃, carrying out solution treatment for 20min, and carrying out water cooling to enable the alloy to form a single alpha phase; then carrying out isothermal magnetic field heat treatment at 640 ℃, keeping the temperature for 30min, keeping the magnetic field intensity at 2600Oe, and cooling to 500 ℃ along with the furnace in a magnetic field; then, multi-stage tempering is carried out, and step tempering is carried out by keeping the temperature at 610 ℃ for 30min, keeping the temperature at 600 ℃ for 60min, keeping the temperature at 580 ℃ for 120min, keeping the temperature at 560 ℃ for 180min and keeping the temperature at 540 ℃ for 240 min.
Example 2:
according to the material components of 25 percent of Cr, 16 percent of Co, 3.5 percent of Mo, 1.0 percent of Ti, 54.3 percent of Fe and 0.2 percent of Nb, the industrial pure iron, the metallic chromium, the electrolytic cobalt and the alloying elements of Mo, Ti and Nb are taken as raw materials, a 25kg vacuum induction furnace is adopted to smelt the alloy, the ingot weight is 23kg, and the ingot mould is broken in vacuum and cooled by water after smelting to cast into steel ingots. The ingot is scalped and then forged to a proper size, the forging heating temperature is 1150 ℃, the heating time is set according to the ingot size and the coefficient of 0.5min/mm, and the final forging temperature is 1000 ℃. The hot rolled blank is heated up along with the furnace to 1120 ℃, is subjected to heat preservation for 30 minutes and then is subjected to hot rolling, forming and cutting according to the required specification to be processed into the finished product
The sample of (1). Carrying out solution treatment at 1200 ℃ for 25min, and carrying out water cooling to enable the alloy to form a single alpha phase; then carrying out isothermal magnetic field heat treatment at 650 ℃ for 60min at the magnetic field intensity of 2700Oe, and cooling to 500 ℃ along with the furnace in the magnetic field; then, multi-stage tempering is carried out, and the temperature is kept at 610 ℃ for 30min, 600 ℃ for 60min, 580 ℃ for 120min, 560 ℃ for 180min and 540 ℃ for 240min, so that step tempering is carried out.
Example 3:
the material comprises the following chemical elements in percentage by mass: cr 27%, Co 15%, Mo 3.5%, Ti 0.81%, Fe 53.64%, Nb 0.05%, using industrial pure iron, metallic chromium, electrolytic cobalt and alloying elements Mo, Ti and Nb as raw materials, adopting 25kg vacuum induction furnace to smelt alloy, breaking vacuum after smelting, water cooling ingot mould, and casting into ingot with weight of 25 kg. The ingot is scalped and then forged to a proper size, the forging heating temperature is 1200 ℃, the heating time is set according to the ingot size and the coefficient of 0.5min/mm, and the final forging temperature is 1100 ℃. The hot rolled blank is heated up along with the furnace to 1150 ℃, is subjected to heat preservation for 30 minutes, is hot rolled and formed according to the required specification, and is cut into
The sample of (1). Carrying out heat treatment at 1300 ℃, carrying out solution treatment for 100min, and carrying out water cooling to enable the alloy to form a single alpha phase; then carrying out isothermal magnetic field heat treatment at 660 ℃, keeping the temperature for 100min, keeping the magnetic field strength at 2650Oe, and cooling to 500 ℃ along with the furnace in a magnetic field; then, multi-stage tempering is carried out, and step tempering is carried out by keeping the temperature at 610 ℃ for 30min, keeping the temperature at 600 ℃ for 60min, keeping the temperature at 580 ℃ for 120min, keeping the temperature at 560 ℃ for 180min and keeping the temperature at 540 ℃ for 240 min.
The alloy materials obtained in examples 1 to 3 were subjected to machining tests, and the results showed that: the surface processing quality of the material is good, deformation or scratches are avoided, and the material still keeps metallic luster and is not oxidized after being placed in the air for one year.
FIG. 1 shows the hysteresis loops of the easy magnetization axis (Ea) and the hard magnetization axis (Ha) of FeCoCr permanent magnetic alloys doped with Nb (a) and Nb (b), respectively. The coercive force Hc of the easy magnetization axis (Ea) of the FeCoCr permanent magnetic alloy without Nb is 640Oe, and the coercive force Hc of the hard magnetization axis (Ha) is 500 Oe. The coercive force Hc of the easy magnetization axis (Ea) of the Nb-doped FeCoCr permanent magnetic alloy is improved to 700Oe, and the coercive force Hc of the hard magnetization axis (Ha) is 680 Oe. This shows that the coercivity of the FeCoCr permanent magnetic alloy is improved to a certain extent by doping Nb, the coercivity of the easy magnetization axis (Ea) is improved by 9%, and the coercivity of the hard magnetization axis (Ha) is improved by 36%.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. The Nb-doped iron-chromium-cobalt permanent magnet alloy is characterized by comprising the following chemical elements in percentage by mass: 42-55% of Fe, 25-27% of Cr, 14-16% of Co, 3-3.5% of Mo, 0.81-1.2% of Ti and 0.05-0.2% of Nb.
2. A method of making the Nb-doped ferrochromium-cobalt permanent magnet alloy as set forth in claim 1, comprising the steps of:
(1) smelting: smelting alloy raw materials according to chemical element composition, and casting into steel ingots;
(2) forging: the method comprises the following steps of (1) forging a steel ingot to a proper size after peeling, wherein the forging heating temperature is 1100-1200 ℃;
(3) a hot rolling procedure: heating the hot rolled blank along with a furnace to 1100-1150 ℃, keeping the temperature for 30min, then hot rolling and forming according to the required specification, and cutting and processing into a sample with a preset specification;
(4) a solution treatment process: carrying out solution treatment on the sample at the temperature of 1100-1300 ℃ for 20-30 min, and carrying out water cooling to enable the alloy to form a single alpha phase;
(5) a magnetic field treatment process: carrying out isothermal magnetic field heat treatment on the sample subjected to the solution treatment at the temperature of 640-660 ℃, keeping the temperature for 30-100 min, keeping the magnetic field intensity to be more than 2500Oe, and cooling the sample to 500 ℃ along with a furnace in a magnetic field;
(6) a tempering procedure: and (4) performing multistage tempering on the sample subjected to the magnetic field treatment.
3. The method for preparing the Nb-doped Fe-Cr-Co permanent magnetic alloy according to claim 2, wherein in the smelting process in the step (1), a 25kg vacuum induction furnace is adopted to smelt the alloy, a vacuum water-cooling ingot casting mold is broken after smelting, and a steel ingot is cast, wherein the weight of the ingot is 20-25 kg.
4. The method for preparing the Nb-doped ferrochrome-cobalt permanent magnet alloy according to claim 2, wherein the heating time is set by a factor of 0.5min/mm in the forging process in step (2) depending on the size of the steel ingot.
5. The method for preparing the Nb-doped ferrochromium-cobalt permanent magnet alloy according to claim 2, wherein the finish forging temperature in the forging step of step (2) is not lower than 960 ℃.
6. The method for preparing the Nb-doped ferrochromium-cobalt permanent magnet alloy according to claim 2, wherein the multi-stage tempering schedule in the tempering process in the step (6) is as follows: and (3) performing step tempering at 610 deg.C for 30min-600 deg.C, 60min-580 deg.C for 120min-560 deg.C, 180min-540 deg.C for 240 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114277322A (en) * | 2021-12-07 | 2022-04-05 | 王军 | Iron-cobalt-chromium-tungsten hysteresis alloy and deformation processing technology thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4174983A (en) * | 1978-07-13 | 1979-11-20 | Bell Telephone Laboratories, Incorporated | Fe-Cr-Co magnetic alloy processing |
| JPS5961004A (en) * | 1982-09-30 | 1984-04-07 | Toshiba Corp | Thin strip of permanent magnet and manufacture thereof |
| JPH06151136A (en) * | 1992-11-12 | 1994-05-31 | Kanegafuchi Chem Ind Co Ltd | Powder of metal-based permanent magnet material |
| US6001194A (en) * | 1997-04-30 | 1999-12-14 | Hitachi Metals, Ltd. | Bias material, magnetic marker and method of producing the bias material |
| CN101298647A (en) * | 2008-05-29 | 2008-11-05 | 天津冶金集团天材科技发展有限公司 | Iron-chromium-cobalt permanent magnetic alloy of composite microelements and deformation processing technique thereof |
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- 2020-11-13 CN CN202011271271.2A patent/CN112522636A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4174983A (en) * | 1978-07-13 | 1979-11-20 | Bell Telephone Laboratories, Incorporated | Fe-Cr-Co magnetic alloy processing |
| JPS5961004A (en) * | 1982-09-30 | 1984-04-07 | Toshiba Corp | Thin strip of permanent magnet and manufacture thereof |
| JPH06151136A (en) * | 1992-11-12 | 1994-05-31 | Kanegafuchi Chem Ind Co Ltd | Powder of metal-based permanent magnet material |
| US6001194A (en) * | 1997-04-30 | 1999-12-14 | Hitachi Metals, Ltd. | Bias material, magnetic marker and method of producing the bias material |
| CN101298647A (en) * | 2008-05-29 | 2008-11-05 | 天津冶金集团天材科技发展有限公司 | Iron-chromium-cobalt permanent magnetic alloy of composite microelements and deformation processing technique thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114277322A (en) * | 2021-12-07 | 2022-04-05 | 王军 | Iron-cobalt-chromium-tungsten hysteresis alloy and deformation processing technology thereof |
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