CN114058810A - Heat treatment method of high-performance iron-based amorphous nanocrystalline alloy - Google Patents
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 238000010438 heat treatment Methods 0.000 title claims abstract description 86
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 72
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 53
- 239000000956 alloy Substances 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 32
- 229910000808 amorphous metal alloy Inorganic materials 0.000 claims abstract description 31
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000004804 winding Methods 0.000 claims abstract description 16
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 10
- 239000010431 corundum Substances 0.000 claims abstract description 10
- 230000001681 protective effect Effects 0.000 claims abstract description 10
- 238000004321 preservation Methods 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 11
- 230000002457 bidirectional effect Effects 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 230000006698 induction Effects 0.000 abstract description 6
- 230000001276 controlling effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001004 magnetic alloy Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 208000012868 Overgrowth Diseases 0.000 description 1
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- DWCZIOOZPIDHAB-UHFFFAOYSA-L methyl green Chemical compound [Cl-].[Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC(=CC=1)[N+](C)(C)C)=C1C=CC(=[N+](C)C)C=C1 DWCZIOOZPIDHAB-UHFFFAOYSA-L 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- 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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/008—Heat treatment of ferrous alloys containing Si
-
- 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
- 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
-
- 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
- C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
-
- 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
- C21D2201/00—Treatment for obtaining particular effects
- C21D2201/03—Amorphous or microcrystalline structure
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
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Abstract
The invention provides a heat treatment method of a high-performance iron-based amorphous nanocrystalline alloy, which relates to the technical field of iron-based amorphous nanocrystalline alloys and comprises the following steps: (1) putting the iron-based amorphous alloy into a hearth of a heat treatment furnace, applying 1-3MPa of compressive stress on the iron-based amorphous alloy, and bidirectionally winding electric furnace wires on a corundum tube in the hearth; (2) vacuumizing the heat treatment furnace, and introducing protective gas; (3) heating the iron-based amorphous alloy in the hearth, and quickly cooling after heat preservation; (4) performing magnetic field heat treatment on the product in the step (3), controlling the magnetic field intensity to be 800-; (5) cooling to room temperature along with the furnace to prepare the high-performance iron-based amorphous nanocrystalline alloy; the residual magnetic induction intensity of the iron-based amorphous nanocrystalline alloy reaches 0.10T, and the coercive force of the iron-based amorphous nanocrystalline alloy reaches 0.10TReaches 0.42 A.m‑1Dynamic hysteresis loss reaches 8.3 W.kg‑1And has better performance.
Description
Technical Field
The invention relates to the technical field of iron-based amorphous nanocrystalline alloys, in particular to a heat treatment method of a high-performance iron-based amorphous nanocrystalline alloy.
Background
The iron-based amorphous/nanocrystalline soft magnetic alloy is used as a new generation of 'double green' energy-saving material, and is widely applied to the power electronic fields of transformers, inductors, sensors and the like due to the characteristics of excellent soft magnetic properties such as high saturation magnetic induction intensity, low coercive force, high magnetic conductivity, low loss and the like. With the continuous progress of society, due to the development and requirements in the fields of computer networks, high-density recording technology, power systems, high-frequency micro-magnetic devices and the like, various components used are increasingly required to have high performance, high quality, small size and light weight, and the performance of metal functional materials such as soft magnetic alloys for preparing the devices is required to be continuously improved. Firstly, the alloy is usually made into an amorphous strip by a mother alloy through a rapid quenching process, and then the microstructure of the alloy is finely regulated and controlled through a heat treatment process, so that a single magnetic alpha-iron phase is separated out and converted into a nanocrystalline structure. Therefore, the heat treatment process plays an important role in obtaining the high-performance iron-based nanocrystalline alloy.
The traditional heat treatment process generally starts from room temperature, the temperature is raised according to preset heating rate, heat preservation time and atmosphere, and finally the temperature is cooled to the room temperature along with the furnace; however, during the heat treatment process, uneven precipitation of crystal grains, over-growth of crystal grains, high magnetocrystalline anisotropy, uneven surface hardness of strip materials, severe brittleness and the like are easily caused, so that the alloy has low saturation magnetic induction intensity, large coercive force and poor toughness and plasticity, and is not favorable for obtaining the high-performance iron-based amorphous nanocrystalline alloy. Therefore, a heat treatment method of the high-performance iron-based amorphous nanocrystalline alloy is provided to solve the problems.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a heat treatment method of a high-performance iron-based amorphous nanocrystalline alloy, so as to overcome the problems mentioned in the background technology.
In order to achieve the above purpose, the technical scheme of the invention is realized by the following technical scheme:
a heat treatment method of a high-performance iron-based amorphous nanocrystalline alloy specifically comprises the following steps:
(1) putting the iron-based amorphous alloy into a hearth of a heat treatment furnace, applying 1-3MPa of compressive stress on the iron-based amorphous alloy, and bidirectionally winding electric furnace wires on a corundum tube in the hearth;
(2) vacuumizing the heat treatment furnace, and introducing protective gas;
(3) heating the iron-based amorphous alloy in the hearth, heating to 480-plus-520 ℃ for the first time, preserving heat for 50-60min, then heating to 540-plus-580 ℃ for the second time, continuing preserving heat for 20-40min, and quickly cooling to 460-plus-480 ℃ after heat preservation is finished;
(4) performing magnetic field heat treatment on the product in the step (3), controlling the magnetic field intensity to be 800-;
(5) and cooling the alloy to room temperature along with the furnace to obtain the high-performance iron-based amorphous nanocrystalline alloy.
Preferably, the composition of the iron-based amorphous alloy is Fe85.7Si0.5B9.3Cu0.7P3.5C0.3。
Preferably, in the step (1), the bidirectional winding is to wind the electric furnace wire in one direction and then reversely wind the electric furnace wire.
Preferably, in step (1), the compressive stress applied is 1 MPa.
Preferably, the protective gas is high-purity nitrogen with the purity of 99.99 percent, and the gas flow is controlled to be 1-5 mL/s.
Preferably, in the step (3), the temperature is raised to 500 ℃ for the first time and is kept for 60min, and the temperature is raised to 560 ℃ for the second time and is kept for 30 min.
Preferably, the first temperature rise rate and the second temperature rise rate are both 10 ℃/min.
Preferably, in the step (4), the magnetic field intensity is controlled to be 800 gauss, and the temperature is kept for 60 min.
The invention provides a heat treatment method of a high-performance iron-based amorphous nanocrystalline alloy, which has the following advantages compared with the prior art:
the electric furnace wire on the corundum tube is wound in two directions, and after the electric furnace wire is electrified, the currents in the two directions flow in opposite directions, so that the magnetic fields are just counteracted with each other, the surrounding magnetic field is zero, the influence of the magnetic field of the electric furnace wire on the product during magnetic field heat treatment is avoided, the quality of the magnetic field heat treatment is ensured, and the quality of the iron-based amorphous nanocrystalline alloy is ensured;
according to the invention, a certain compressive stress is applied, the temperature is raised twice and the temperature is kept for a period of time, then the magnetic field intensity is controlled to be 800 gauss, the saturation magnetic induction intensity of the alloy is improved through the action of the compressive stress, the toughness and plasticity are improved, the coercive force of the iron-based amorphous nanocrystalline alloy is further reduced through the action of the magnetic field, and the quality of the iron-based amorphous nanocrystalline alloy is improved;
the iron-based amorphous nanocrystalline alloy (Fe) of the invention85.7Si0.5B9.3Cu0.7P3.5C0.3) The residual magnetic induction of (A) is up to 0.10T, and the coercive force is up to 0.42 A.m-1Dynamic hysteresis loss reaches 8.3 W.kg-1And has better performance.
Drawings
FIG. 1 is a schematic diagram of the bidirectional winding of a corundum tube according to the present invention;
FIG. 2 is a graph showing the dynamic hysteresis loss of Fe-based amorphous nanocrystalline alloy according to example 3 of the present invention as a function of magnetic field strength;
fig. 3 is a graph showing the variation of coercive force and residual magnetic induction strength of the iron-based amorphous nanocrystalline alloy with magnetic field strength in example 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but 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.
Example 1
A heat treatment method of a high-performance iron-based amorphous nanocrystalline alloy specifically comprises the following steps:
(1) putting the iron-based amorphous alloy into a hearth of a heat treatment furnace, applying 1MPa of compressive stress on the iron-based amorphous alloy, and bidirectionally winding electric furnace wires on a corundum tube in the hearth; wherein, the bidirectional winding is to wind the electric furnace wire in one direction and then reversely wind the electric furnace wire;
(2) vacuumizing the heat treatment furnace, and introducing 99.99% high-purity nitrogen with the flow rate of 1mL/s as protective gas;
(3) heating the iron-based amorphous alloy in the hearth, heating to 480 ℃ for the first time, preserving heat for 50min, then heating to 540 ℃ for the second time, continuing preserving heat for 20min, and quickly cooling to 460 ℃ after heat preservation; wherein the first heating rate and the second heating rate are both 10 ℃/min;
(4) performing magnetic field heat treatment on the product in the step (3), controlling the magnetic field intensity to be 800 gauss, and preserving the temperature for 30 min;
(5) and cooling the alloy to room temperature along with the furnace to obtain the high-performance iron-based amorphous nanocrystalline alloy.
The composition of the iron-based amorphous alloy is Fe85.7Si0.5B9.3Cu0.7P3.5C0.3。
Example 2
A heat treatment method of a high-performance iron-based amorphous nanocrystalline alloy specifically comprises the following steps:
(1) putting the iron-based amorphous alloy into a hearth of a heat treatment furnace, applying a compressive stress of 2MPa on the iron-based amorphous alloy, and bidirectionally winding electric furnace wires on a corundum tube in the hearth; wherein, the bidirectional winding is to wind the electric furnace wire in one direction and then reversely wind the electric furnace wire;
(2) vacuumizing the heat treatment furnace, and introducing 99.99% high-purity nitrogen with the flow rate of 2mL/s as protective gas;
(3) heating the iron-based amorphous alloy in the hearth, heating to 500 ℃ for the first time, preserving heat for 55min, then heating to 550 ℃ for the second time, continuing preserving heat for 25min, and quickly cooling to 470 ℃ after heat preservation; wherein the first heating rate and the second heating rate are both 10 ℃/min;
(4) performing magnetic field heat treatment on the product in the step (3), controlling the magnetic field intensity to be 900 gauss, and preserving the temperature for 40 min;
(5) and cooling the alloy to room temperature along with the furnace to obtain the high-performance iron-based amorphous nanocrystalline alloy.
The composition of the iron-based amorphous alloy is Fe85.7Si0.5B9.3Cu0.7P3.5C0.3。
Example 3
A heat treatment method of a high-performance iron-based amorphous nanocrystalline alloy specifically comprises the following steps:
(1) putting the iron-based amorphous alloy into a hearth of a heat treatment furnace, applying 1MPa of compressive stress on the iron-based amorphous alloy, and bidirectionally winding electric furnace wires on a corundum tube in the hearth; wherein, the bidirectional winding is to wind the electric furnace wire in one direction and then reversely wind the electric furnace wire;
(2) vacuumizing the heat treatment furnace, and introducing 99.99% high-purity nitrogen with the flow rate of 3mL/s as protective gas;
(3) heating the iron-based amorphous alloy in the hearth, heating to 500 ℃ for the first time, keeping the temperature for 60min, then heating to 560 ℃ for the second time, keeping the temperature for 30min, and quickly cooling to 480 ℃ after the heat preservation is finished; wherein the first heating rate and the second heating rate are both 10 ℃/min;
(4) performing magnetic field heat treatment on the product in the step (3), controlling the magnetic field intensity to be 800 gauss, and preserving the temperature for 60 min;
(5) and cooling the alloy to room temperature along with the furnace to obtain the high-performance iron-based amorphous nanocrystalline alloy.
The composition of the iron-based amorphous alloy is Fe85.7Si0.5B9.3Cu0.7P3.5C0.3。
Example 4
A heat treatment method of a high-performance iron-based amorphous nanocrystalline alloy specifically comprises the following steps:
(1) putting the iron-based amorphous alloy into a hearth of a heat treatment furnace, applying 3MPa of compressive stress on the iron-based amorphous alloy, and bidirectionally winding electric furnace wires on a corundum tube in the hearth; wherein, the bidirectional winding is to wind the electric furnace wire in one direction and then reversely wind the electric furnace wire;
(2) vacuumizing the heat treatment furnace, and introducing 99.99% high-purity nitrogen with the flow rate of 4mL/s as protective gas;
(3) heating the iron-based amorphous alloy in the hearth, heating to 500 ℃ for the first time, keeping the temperature for 60min, then heating to 580 ℃ for the second time, keeping the temperature for 30min, and quickly cooling to 460 ℃ after the heat preservation is finished; wherein the first heating rate and the second heating rate are both 10 ℃/min;
(4) performing magnetic field heat treatment on the product in the step (3), controlling the magnetic field intensity to be 1200 Gauss, and keeping the temperature for 30 min;
(5) and cooling the alloy to room temperature along with the furnace to obtain the high-performance iron-based amorphous nanocrystalline alloy.
The composition of the iron-based amorphous alloy is Fe85.7Si0.5B9.3Cu0.7P3.5C0.3。
Example 5
A heat treatment method of a high-performance iron-based amorphous nanocrystalline alloy specifically comprises the following steps:
(1) putting the iron-based amorphous alloy into a hearth of a heat treatment furnace, applying 1MPa of compressive stress on the iron-based amorphous alloy, and bidirectionally winding electric furnace wires on a corundum tube in the hearth; wherein, the bidirectional winding is to wind the electric furnace wire in one direction and then reversely wind the electric furnace wire;
(2) vacuumizing the heat treatment furnace, and introducing 99.99% high-purity nitrogen with the flow rate of 2mL/s as protective gas;
(3) heating the iron-based amorphous alloy in the hearth, heating to 500 ℃ for the first time, keeping the temperature for 60min, then heating to 560 ℃ for the second time, keeping the temperature for 30min, and quickly cooling to 460 ℃ after the heat preservation is finished; wherein the first heating rate and the second heating rate are both 10 ℃/min;
(4) performing magnetic field heat treatment on the product in the step (3), controlling the magnetic field intensity to be 1600 gauss, and preserving the temperature for 30 min;
(5) and cooling the alloy to room temperature along with the furnace to obtain the high-performance iron-based amorphous nanocrystalline alloy.
The composition of the iron-based amorphous alloy is Fe85.7Si0.5B9.3Cu0.7P3.5C0.3。
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A heat treatment method of a high-performance iron-based amorphous nanocrystalline alloy is characterized by comprising the following steps:
(1) putting the iron-based amorphous alloy into a hearth of a heat treatment furnace, applying 1-3MPa of compressive stress on the iron-based amorphous alloy, and bidirectionally winding electric furnace wires on a corundum tube in the hearth;
(2) vacuumizing the heat treatment furnace, and introducing protective gas;
(3) heating the iron-based amorphous alloy in the hearth, heating to 480-plus-520 ℃ for the first time, preserving heat for 50-60min, then heating to 540-plus-580 ℃ for the second time, continuing preserving heat for 20-40min, and quickly cooling to 460-plus-480 ℃ after heat preservation is finished;
(4) performing magnetic field heat treatment on the product in the step (3), controlling the magnetic field intensity to be 800-;
(5) and cooling the alloy to room temperature along with the furnace to obtain the high-performance iron-based amorphous nanocrystalline alloy.
2. The heat treatment method of the high-performance iron-based amorphous nanocrystalline alloy according to claim 1, characterized in that: the iron-based amorphous alloy consists of Fe85.7Si0.5B9.3Cu0.7P3.5C0.3。
3. The heat treatment method of the high-performance iron-based amorphous nanocrystalline alloy according to claim 1, characterized in that: in the step (1), the bidirectional winding is to wind the electric furnace wire in one direction and then reversely wind the electric furnace wire.
4. The heat treatment method of the high-performance iron-based amorphous nanocrystalline alloy according to claim 1, characterized in that: in the step (1), the applied compressive stress is 1 MPa.
5. The heat treatment method of the high-performance iron-based amorphous nanocrystalline alloy according to claim 1, characterized in that: in the step (2), the protective gas is high-purity nitrogen with the purity of 99.99 percent, and the gas flow is controlled to be 1-5 mL/s.
6. The heat treatment method of the high-performance iron-based amorphous nanocrystalline alloy according to claim 1, characterized in that: in the step (3), the temperature is increased to 500 ℃ for the first time and is kept for 60min, and the temperature is increased to 560 ℃ for the second time and is kept for 30 min.
7. The heat treatment method of the high-performance iron-based amorphous nanocrystalline alloy according to claim 1, characterized in that: the first heating rate and the second heating rate are both 10 ℃/min.
8. The heat treatment method of the high-performance iron-based amorphous nanocrystalline alloy according to claim 1, characterized in that: in the step (4), the magnetic field intensity is controlled to be 800 gauss, and the temperature is kept for 60 min.
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Effective date of registration: 20240708 Address after: 237300 West of Meishanhu Road and North of Renmin Road, Jinzhai Economic Development Zone (Modern Industrial Park), Lu'an City, Anhui Province Patentee after: Anhui Zhonghuan Soft Magnetic Technology Co.,Ltd. Country or region after: China Address before: 237300 west of meishanhu road and north of Renmin Road, modern industrial park, Jinzhai County, Lu'an City, Anhui Province Patentee before: Anhui Zhonghuan Jingyan New Material Co.,Ltd. Country or region before: China |