CN110144498B - Rare earth soft magnetic alloy directly deposited by laser and magnetic property regulation and control method thereof - Google Patents
Rare earth soft magnetic alloy directly deposited by laser and magnetic property regulation and control method thereof Download PDFInfo
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- 229910001004 magnetic alloy Inorganic materials 0.000 title claims abstract description 72
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 59
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000033228 biological regulation Effects 0.000 title abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 51
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- 230000008021 deposition Effects 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000011002 quantification Methods 0.000 claims abstract description 6
- 239000000956 alloy Substances 0.000 claims description 21
- 229910045601 alloy Inorganic materials 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000000151 deposition Methods 0.000 claims description 15
- 230000006698 induction Effects 0.000 claims description 14
- 238000005253 cladding Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000004372 laser cladding Methods 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 8
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- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000011261 inert gas Substances 0.000 description 10
- 238000000889 atomisation Methods 0.000 description 9
- 238000009689 gas atomisation Methods 0.000 description 9
- 239000000758 substrate Substances 0.000 description 6
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- 239000000284 extract Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 230000000007 visual effect Effects 0.000 description 5
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
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- 238000001291 vacuum drying Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
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- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
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- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0433—Nickel- or cobalt-based alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention discloses a laser direct deposition rare earth soft magnetic alloy and a magnetic property regulation and control method thereof, which comprises the following steps: the rare earth soft magnetic alloy powder comprises the following components in parts by weight: ni: 79.0-80.0 parts of Mo: 1.5-2.5 parts, Gd: 1.0-2.0 parts of Si: 0.5-1.0 part, and the balance of Fe. Preparing the rare earth soft magnetic alloy by adopting a laser direct deposition technology, and then carrying out heat treatment on the formed soft magnetic alloy. The invention adopts a defect quantification mode to regulate and control the magnetic performance of the novel rare earth soft magnetic alloy, establishes the digital relation between the defects and the soft magnetic performance, and finally obtains the high-performance and high-density rare earth soft magnetic alloy with the self-defined specification. The optimal process parameters are as follows: the laser power is 700-900W, the spot size is 3-6mm, the laser scanning speed is 4-15 mm/s, and the powder feeding rate is 25-30 g/min. The invention meets the customized requirements of precision devices such as aerospace, ship navigation and the like on the high-performance soft magnetic alloy, and has important application prospects in military and high-precision industries.
Description
Technical Field
The invention relates to the field of metallurgical technology of soft magnetic alloy materials, in particular to a laser direct deposition rare earth soft magnetic alloy and a magnetic property regulation and control method thereof.
Background
The iron-nickel soft magnetic alloy material is a soft magnetic material with high magnetic conductivity and low coercive force, is widely applied to electronic devices such as magnetic induction transformers, filter inductors and the like due to special magnetic, mechanical and electrical properties, and occupies an important position in the current magnetic material market. In order to adapt to the application in various fields, various soft magnetic alloys with different characteristics can be obtained by regulating the component content of the soft magnetic alloy and adding one or more rare earth alloy elements such as Gd, Nd, La and the like, and the soft magnetic alloy with excellent performance meeting the requirements of various application fields is obtained by combining various regulating and controlling methods.
The laser direct deposition technology has been greatly developed in recent years in the direction of preparing functional materials, and is rapidly developed into a feasible technology. The laser has the advantages of high energy density, good directivity, large light spot, high scanning speed and the like, so that the laser becomes an advanced technology for processing the soft magnetic iron-nickel alloy, the processing process is green and environment-friendly, and the high-efficiency, quick and complex forming can be realized by combining with scanning track programming.
Compared with the advantages of the laser direct deposition technology, the soft magnetic alloy prepared by the traditional methods of metal pouring, mechanical metallurgy, high-energy sintering, thermal spraying and the like can cause the reduction of magnetism due to excessive grain growth under the condition of large area and high temperature, and is limited in processing space. The innovative development of new soft magnetic alloys is subject to expensive production line adjustments, which adversely affect the development of soft magnetic alloys. The laser direct deposition forming preparation can obtain the characteristics of fine tissue, uniform components, forming complex structure and the like, and is one of the best methods for preparing the high-performance high-density soft magnetic alloy.
Disclosure of Invention
The invention provides a laser direct deposition method
Rare earth soft magnetic alloy and a magnetic property regulating method thereof. According to the self-invented component proportioning, a hot inert gas atomization method mode (or a rotary electrode atomization mode) is adopted to prepare NiFeGdMoSi rare earth magnetically soft alloy powder with good sphericity and uniform components.
The method comprehensively quantifies and extracts the defects in the rare earth soft magnetic alloy, and establishes the digital relation between the defects and the soft magnetic performance parameters, thereby realizing the optimization regulation and control of the soft magnetic performance by adopting a defect quantification means; and finally obtaining the high-performance high-density rare earth soft magnetic alloy through a heat treatment optimization process.
The technical scheme for realizing the invention is that the laser direct deposition rare earth soft magnetic alloy and the magnetic property regulation and control method thereof are characterized by comprising the following steps:
(1) preparing NiFeGdMoSi rare earth soft magnetic alloy powder by adopting a component ratio, wherein the components in parts by weight are as follows: ni: 79.0-80.0 parts of Mo: 1.5-2.5 parts, Gd: 1.0-2.0 parts of Si: 0.5-1.0 part, and the balance of Fe. Preparing powder by adopting a hot inert gas atomization mode (or a rotary electrode atomization mode), smelting the powder to an alloy solution by using a magnesium oxide crucible, pouring the alloy solution into a tundish, starting high-temperature supersonic inert gas atomization, and then sieving the powder to finally obtain the rare earth magnetically soft alloy powder with good sphericity and average particle size of 200-300 meshes. The high-temperature supersonic inert gas is utilized, so that the atomization efficiency can be improved, the aim of controlling the granularity is achieved by controlling the speed, and the oxidation process of the powder is effectively avoided;
(2) the laser direct deposition modeling is carried out, and comprises the following parts. Firstly, performing primary laser surface remelting after cladding the 1 st layer of rare earth soft magnetic alloy powder; after cladding of the 2 nd layer of rare earth soft magnetic alloy powder is completed on the basis, remelting the surface of the laser is needed again; then keeping the designed laser cladding process parameters for continuous laser direct deposition molding;
(3) adopting LEMO Export software to comprehensively and quantitatively extract defects such as air holes, cracks and the like in the rare earth soft magnetic alloy, controlling the error to be 0.1%, and establishing digital relation between the defects and soft magnetic performance parameters, thereby realizing regulation and control of the soft magnetic performance by adopting a defect quantification means;
(4) and (3) placing the sample in a heating furnace at 900-1180 ℃ for heat treatment for 2-3 hours. The heat treatment process improves the metallurgical quality of the soft magnetic alloy, removes factors such as internal stress and the like, and reduces the resistance of the soft magnetic alloy to the rotation of the alloy magnetic moment or magnetic domain under the action of an external magnetic field, thereby improving the soft magnetic performance, such as improving the saturation magnetic induction intensity and reducing the coercive force;
(5) the range for regulating and controlling the magnetic performance of the rare earth soft magnetic alloy by adopting a defect quantification mode comprises the following steps: the porosity is between 4.0 and 6.6 percent, the coercive force is regulated to be between 26.42 and 50.10A/m, and the saturation magnetic induction intensity is between 0.43 and 0.67T; the porosity is between 2.1 and 4.0 percent, the controlled coercive force is between 22.79 and 26.42A/m, and the saturated magnetic induction intensity is between 0.67 and 0.79T; the porosity is between 0.6 and 2.1 percent, the controlled coercive force is between 19.15 and 22.79A/m, and the saturated magnetic induction intensity is between 0.79 and 0.88T; the porosity is between 0.1 and 0.6 percent, the controlled coercive force is between 14.49 and 19.15A/m, and the saturated magnetic induction intensity is between 0.88 and 0.95T.
(6) Adopting laser processing technological parameters: the laser output power is 700W-900W, the size of a circular light spot is 3mm-6mm, the laser scanning speed is 7 mm/s-25 mm/s, the powder feeding speed is 25 g/min-30 g/min, the gas flow rate of powder feeding is 350L/h, and argon gas with the flow rate of 20L/min is adopted for protection in the laser cladding process;
(7) the real-time monitoring system performs closed-loop regulation and control, and comprises a charge coupled visual sensor (CCD) system and thermal infrared imager Systems (FLIR Systems). The forming quality of the soft magnetic alloy can be effectively monitored, and the laser processing technological parameters can be adjusted in real time according to the feedback data.
The invention has the beneficial effects that:
(1) the invention discloses a rare earth soft magnetic alloy material which comprises the following components in parts by weight: ni: 79.0-80.0 parts of Mo: 1.5-2.5 parts, Gd: 1.0-2.0 parts of Si: 0.5-1.0 part, and the balance of Fe. The application range of the soft magnetic alloy in high-end fields such as aerospace and the like is expanded, and the comprehensive application technical level of China in the field of the soft magnetic alloy is improved.
(2) The closed-loop feedback system comprises a charge coupled visual sensor (CCD) system and thermal infrared imager systems (FLIRSystems). The method can realize good molding and custom specification control of the soft magnetic alloy, avoids the adjustment of time consumption and investment of a production line in the original research and development and production processes, is suitable for special requirements on custom specification and real-time requirements in aerospace military and high-precision industries, and accelerates the technical change and industrial progress of high-end fields such as metallurgy enterprises and aerospace in China, so the method has obvious application prospect and development space.
(3) The defects such as air holes, cracks and the like in the soft magnetic alloy are comprehensively and quantitatively extracted, and the digital relation between the defects and soft magnetic performance parameters is established, so that the soft magnetic performance is regulated and controlled by adopting a defect quantification means; the novel regulation and control mode increases the mutual permeation and cross connection among the material science theory, the magnetic basic theory and the laser application technology. The method is an indispensable research content of modern high and new soft magnetic materials, and further promotes the technical progress of modern industry.
(4) The NiFeGdMoSi soft magnetic alloy prepared by the laser direct deposition forming preparation method has high density and good soft magnetic performance, such as the coercive force of 14.49A/m-50.10A/m and the saturation magnetic induction intensity of 0.43T-0.95T.
Drawings
FIG. 1 is a drawing of a laser direct deposition formed rare earth soft magnetic alloy substance
FIG. 2 is an optical microscope image and SEM image of a rare earth soft magnetic alloy
FIG. 3 is XRD spectrum line of rare earth soft magnetic alloy
FIG. 4 is a porosity distribution image of a rare earth soft magnetic alloy
FIG. 5 is a porosity curve of a rare earth soft magnetic alloy
FIG. 6 is a hysteresis loop of a rare earth soft magnetic alloy
FIG. 7 is a diagram showing a state of rapid flow of a molten pool
FIG. 8 is a graph of the real-time distribution of the temperature field
Detailed Description
Example 1
(1) Preparing raw materials of the rare earth soft magnetic alloy powder according to the component proportion, wherein the components are as follows by weight: ni: 80.0 parts, Mo: 2.5 parts, Gd: 2.0 part, Si: 1.0 part and the balance of Fe;
(2) preparing powder by adopting a hot inert gas atomization mode (or a rotary electrode atomization mode), smelting the powder to an alloy solution by using a magnesium oxide crucible, pouring the alloy solution into a tundish, starting high-temperature supersonic inert gas atomization, wherein an atomization medium is pure argon, and then sieving the powder to finally obtain rare earth magnetically soft alloy powder with good sphericity and 200 meshes of average particle size;
(3) placing the rare earth soft magnetic alloy powder in a vacuum drying oven for drying for 2 hours at the temperature of 80 ℃ and the vacuum degree of-0.06 MPa, and removing influence factors generated by water vapor on defects;
(4) selecting a Fe80NiSi cylinder with the inner diameter of 32mm as a carrier substrate, fixing the carrier substrate on a positioner, wherein a feedback system comprises a charge coupled visual sensor (CCD) system and thermal infrared imager Systems (FLIR Systems).
(5) The laser process parameters are as follows: the laser output power is 700W, the laser scanning speed is 17mm/s, the size of a circular light spot is 3.5mm, the powder feeding speed is 26.5g/min, the gas flow rate of powder feeding is 350L/h, and argon gas with the flow rate of 20L/min is adopted for protection in the laser cladding process. Firstly, performing laser surface remelting (the laser power is 700W, and the laser scanning speed is 17mm/s) once after cladding the 1 st layer of rare earth soft magnetic alloy powder; after the cladding of the 2 nd layer of rare earth soft magnetic alloy powder is finished on the basis, laser surface remelting (the laser power is 700W, the laser scanning speed is 17mm/s) needs to be carried out again, and then continuous laser direct deposition molding is carried out by keeping the designed optimal laser parameters and powder feeding amount;
(5) placing the sample in a heating furnace at 1180 ℃ for heat treatment for 2 hours;
(6) adopting LEMO Export software to comprehensively and quantitatively extract defects such as air holes, cracks and the like in the rare earth soft magnetic alloy to obtain the rare earth soft magnetic alloy with the average porosity of 0.38%;
(7) the obtained rare earth soft magnetic alloy is subjected to tissue structure analysis and magnetic property test, so that the coercive force of the rare earth soft magnetic alloy is 14.97A/m, and the saturation magnetic induction intensity is 0.92T.
Example 2
(1) Preparing raw materials of the rare earth soft magnetic alloy powder according to the component proportion, wherein the components are as follows by weight: ni: 80.0 parts, Mo: 2.5 parts, Gd: 2.0 part, Si: 1.0 part and the balance of Fe;
(2) preparing powder by adopting a hot inert gas atomization mode (or a rotary electrode atomization mode), smelting the powder to an alloy solution by using a magnesium oxide crucible, pouring the alloy solution into a tundish, starting high-temperature supersonic inert gas atomization, wherein an atomization medium is pure argon, and then sieving the powder to finally obtain rare earth magnetically soft alloy powder with good sphericity and 200 meshes of average particle size;
(3) placing the rare earth soft magnetic alloy powder in a vacuum drying oven for drying for 2 hours at the temperature of 80 ℃ and the vacuum degree of-0.06 MPa, and removing influence factors generated by water vapor on defects;
(4) selecting a Fe80NiSi cylinder with the inner diameter of 32mm as a carrier substrate, fixing the carrier substrate on a positioner, wherein a feedback system comprises a charge coupled visual sensor (CCD) system and thermal infrared imager Systems (FLIR Systems).
(5) The adopted process parameters are as follows: the laser output power is 700W, the laser scanning speed is 13.52mm/s, the circular light spot size is 3.5mm, the powder feeding speed is 26.5g/min, the powder feeding gas flow is 350L/h, and the argon protection with the flow of 20L/min is adopted in the laser cladding process. Firstly, after cladding the 1 st layer of rare earth soft magnetic alloy powder, carrying out laser surface remelting (the laser power is 700W, and the laser scanning speed is 13.52mm/s) once; after cladding of the 2 nd layer of rare earth soft magnetic alloy powder is completed on the basis, laser surface remelting (laser power 700W and laser scanning speed 13.52mm/s) needs to be carried out again, and then continuous laser direct deposition molding is carried out by keeping the designed optimal laser parameters and powder feeding amount;
(6) placing the sample in a heating furnace at 1000 ℃ for heat treatment for 2 hours;
(7) adopting LEMO Export software to comprehensively and quantitatively extract defects such as air holes, cracks and the like in the rare earth soft magnetic alloy to obtain the rare earth soft magnetic alloy with the average porosity of 1.455%;
(8) the obtained rare earth soft magnetic alloy is subjected to tissue structure analysis and magnetic performance test, the coercive force of the rare earth soft magnetic alloy is 19.78A/m, and the saturation magnetic induction intensity is 0.85T;
example 3
(1) Preparing raw materials of the rare earth soft magnetic alloy powder according to the component proportion, wherein the components are as follows by weight: ni: 80.0 parts, Mo: 2.5 parts, Gd: 2.0 part, Si: 1.0 part and the balance of Fe;
(2) preparing powder by adopting a hot inert gas atomization mode (or a rotary electrode atomization mode), smelting the powder to an alloy solution by using a magnesium oxide crucible, pouring the alloy solution into a tundish, starting high-temperature supersonic inert gas atomization, wherein an atomization medium is pure argon, and then sieving the powder to finally obtain rare earth magnetically soft alloy powder with good sphericity and 200 meshes of average particle size;
(3) placing the rare earth soft magnetic alloy powder in a vacuum drying oven for drying for 2 hours at the temperature of 80 ℃ and the vacuum degree of-0.06 MPa, and removing influence factors generated by water vapor on defects;
(4) selecting a Fe80NiSi cylinder with the inner diameter of 32mm as a carrier substrate, fixing the carrier substrate on a positioner, wherein a feedback system comprises a charge coupled visual sensor (CCD) system and thermal infrared imager Systems (FLIR Systems).
(5) The adopted process parameters are as follows: the laser output power is 700W, the laser scanning speed is 8.1mm/s, the circular light spot size is 3.5mm, the powder feeding speed is 26.5g/min, the powder feeding gas flow is 350L/h, and the argon gas with the flow of 20L/min is adopted for protection in the laser cladding process. Firstly, performing laser surface remelting (the laser power is 700W, and the laser scanning speed is 8.1mm/s) once after cladding the 1 st layer of rare earth soft magnetic alloy powder; after the cladding of the 2 nd layer of rare earth soft magnetic alloy powder is finished on the basis, laser surface remelting (the laser power is 700W, and the laser scanning speed is 8.1mm/s) needs to be carried out again, and then continuous laser direct deposition molding is carried out by keeping the designed optimal laser parameters and powder feeding amount;
(5) placing the sample in a heating furnace at 900 ℃ for heat treatment for 3 hours;
(6) adopting LEMO Export software to comprehensively and quantitatively extract defects such as air holes, cracks and the like in the rare earth soft magnetic alloy to obtain the rare earth soft magnetic alloy with the average porosity of 4.838%;
(7) the rare earth soft magnetic alloy obtained in this example 3 was subjected to the tissue structure analysis and the magnetic property test, and the coercive force of the rare earth soft magnetic alloy was 32.73A/m, and the saturation magnetic induction was 0.59T.
The above-mentioned embodiments only express the embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (2)
1. A preparation method of a rare earth soft magnetic alloy directly deposited by laser comprises the following steps of 100 parts by weight: 79.0-80.0 parts of Mo: 1.5-2.5 parts, Gd: 1.0-2.0 parts of Si: 0.5-1.0 part, and the balance of Fe; the average grain size of the alloy powder is 200-300 meshes;
the method is characterized in that: firstly, performing primary laser surface remelting after cladding the 1 st layer of rare earth soft magnetic alloy powder; after cladding of the 2 nd layer of rare earth soft magnetic alloy powder is completed on the basis, remelting the surface of the laser is needed again; then carrying out continuous laser rapid deposition molding according to the following laser cladding process parameters; carrying out heat treatment for 2-3 hours at 900-1180 ℃ in an argon atmosphere to obtain the final state of the alloy; laser cladding process parameters: the laser output power is 700W-900W, the size of the circular light spot is 3mm-6mm, the laser scanning speed is 7 mm/s-25 mm/s, the powder feeding speed is 25 g/min-30 g/min, the gas flow for conveying the alloy powder is 150L/h-350L/h, and argon gas with the flow of 10-20L/min is adopted for protection in the laser cladding process.
2. The method for preparing the rare earth soft magnetic alloy by direct laser deposition according to claim 1, wherein the magnetic property of the rare earth soft magnetic alloy is regulated and controlled by a defect quantification mode, which comprises the following steps: the porosity is between 4.0 and 6.6 percent, the coercive force is regulated to be between 26.42 and 50.10A/m, and the saturation magnetic induction intensity is between 0.43 and 0.67T; the porosity is between 2.1 and 4.0 percent, the controlled coercive force is between 22.79 and 26.42A/m, and the saturated magnetic induction intensity is between 0.67 and 0.79T; the porosity is between 0.6 and 2.1 percent, the controlled coercive force is between 19.15 and 22.79A/m, and the saturated magnetic induction intensity is between 0.79 and 0.88T; the porosity is between 0.1 and 0.6 percent, the controlled coercive force is between 14.49 and 19.15A/m, and the saturated magnetic induction intensity is between 0.88 and 0.95T.
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| JPS5757854A (en) * | 1980-09-19 | 1982-04-07 | Hitachi Ltd | Metal-metal type ferromagnetic amorphous alloy and magnetic core using it |
| JPH01176050A (en) * | 1987-12-29 | 1989-07-12 | Nippon Steel Corp | Fe-ni magnetic alloy having excellent surface property |
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