CN112281060A - Tube sealing hydrogenation heat treatment annealing process - Google Patents
Tube sealing hydrogenation heat treatment annealing process Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
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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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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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
- 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
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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
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15333—Amorphous metallic alloys, e.g. glassy metals containing nanocrystallites, e.g. obtained by annealing
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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
- C21D2201/00—Treatment for obtaining particular effects
- C21D2201/03—Amorphous or microcrystalline structure
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Abstract
The invention relates to the technical field of metal materials, in particular to a tube-sealing hydrogenation heat treatment annealing process aiming at iron-based amorphous alloy; the heat treatment annealing process comprises the following steps: preparing materials; preparing a strip material; packaging the belt material: cutting a section of amorphous thin belt with a certain length, putting the amorphous thin belt into a quartz tube, putting the quartz tube on a tube sealing machine, vacuumizing, introducing protective gas and high-purity hydrogen, and heating the wall of the quartz tube to obtain a packaged quartz tube with two closed ends and a sample inside; heat treatment; the tube-sealing hydrogenation heat treatment annealing process is carried out in the quartz tube with the inner diameter of 8mm and the outer diameter of 10mm, so that the gas consumption is low, the gas proportion and the gas content can be randomly regulated and controlled, the vacuum degree is good, and the product performance is stable. Compared with the traditional annealing operation in the furnace body, the annealing operation in the furnace body can effectively avoid hydrogen from damaging the furnace body, and because the vacuum quartz tube is adopted for operation, compared with the vacuumizing operation of the furnace body, the annealing operation in the furnace body has shorter heat treatment time and high efficiency.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a tube-sealing hydrogenation heat treatment annealing process aiming at iron-based amorphous alloy.
Background
The iron-based nanocrystalline soft magnetic alloy has excellent soft magnetic properties due to its unique structure, and thus is widely used in energy equipment, communication equipment and automatic control equipment. In the recently emerging field of wireless charging, the finnment nanocrystalline alloy becomes a key material for improving wireless charging power because of its higher saturation magnetization, lower loss and controllable magnetic permeability. The heat treatment efficiency of the existing iron-based nanocrystalline magnetically soft alloy needs to be improved.
Disclosure of Invention
The purpose of the invention is: the defects in the prior art are overcome, the tube sealing hydrogenation heat treatment annealing process for the iron-based amorphous alloy is high in heat treatment efficiency, and the iron-based nanocrystalline soft magnetic alloy prepared by the heat treatment annealing process is stable in performance.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a tube sealing hydrogenation heat treatment annealing process comprises the following steps:
preparing materials: according to the chemical formula Fe73.5Si13.5B9Cu3Nb1Calculating the mass of the raw materials corresponding to the ratio of the elements and weighing;
smelting a master alloy;
preparing a strip material;
packaging the belt material: cutting a section of amorphous thin belt with a certain length, putting the amorphous thin belt into a quartz tube, putting the quartz tube on a tube sealing machine, vacuumizing, introducing protective gas and high-purity hydrogen, and heating the wall of the quartz tube to obtain a packaged quartz tube with two closed ends and a sample inside;
and (3) heat treatment: and (4) putting the packaged quartz tube into a muffle furnace, carrying out heat treatment, and taking out and cooling.
Further, the smelting master alloy specifically comprises: and putting the weighed raw materials into a vacuum smelting furnace, vacuumizing, filling protective gas, smelting, and cooling to obtain a master alloy ingot.
Further, the vacuum melting furnace is a vacuum induction melting furnace, and the vacuumizing comprises opening a mechanical pump to pump down to 3 × 10-1Pa, opening a diffusion pump to pump high vacuum to 5X 10-3Pa, and protective gas is filled to 0.05 Mpa. The protective atmosphere in the invention is inert gas, and specifically can be: nitrogen, argon, helium, and the like.
Further, the smelting mother alloy is repeatedly smelted for multiple times at the controlled temperature of 1000-1600 ℃, and the smelting temperature can be specifically as follows: 1000 deg.C, 1050 deg.C, 1100 deg.C, 1150 deg.C, 1200 deg.C, 1250 deg.C, 1300 deg.C, 1350 deg.C, 1400 deg.C, 1450 deg.C, 1500 deg.C, 1550 deg.C, 1600 deg.C; the single melting time is 5-15 min, and the word melting time can be specifically as follows: 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15 min.
Further, the tape preparation comprises: crushing the mother alloy ingot, putting the crushed mother alloy ingot into an induction furnace, vacuumizing, introducing protective gas for protection, heating, melting the mother alloy ingot, and spraying the melted mother alloy ingot onto a copper wheel rotating at a high speed to prepare an amorphous thin strip.
Further, the vacuum pumping comprises turning on a mechanical pump to reduce the vacuum to 3 × 10-1Pa, opening a diffusion pump to pump high vacuum to 5X 10-3And Pa, introducing protective gas to 0.05MPa for protection. The protective atmosphere in the invention is inert gas, and specifically can be: nitrogen, argon, helium, and the like.
Further, the surface linear speed of the copper wheel is 30 m/s.
Further, the length of the amorphous thin strip is 3cm-10cm, specifically: 3cm, 4cm, 5cm, 6cm, 7cm, 8cm, 9cm, and 10cm, and the quartz tube has an inner diameter of 8mm and an outer diameter of 10 mm.
Further, the vacuumizing operation in the tape packaging comprises opening a mechanical pump to vacuumize to 3 x 10-1Pa。
Further, the heat treatment temperature in the muffle furnace is 550 ℃, the heat preservation time is 300min, and the heating rate is 10K/min.
The technical scheme adopted by the invention has the beneficial effects that:
according to the tube sealing hydrogenation heat treatment annealing process, high-purity hydrogen is added into the original protective atmosphere in a certain proportion, and then annealing heat treatment is carried out, so that the iron-based amorphous alloy can be induced to be nano-crystallized, and the soft magnetic property of the iron-based amorphous alloy can be improved. Preparing an amorphous strip in an argon protective atmosphere by using a solution spinning quenching method, sealing the tube, and then carrying out hydrogenation annealing in a vacuum heat treatment furnace. The experimental result shows that compared with vacuum heat treatment, the hydrogenation heat treatment can induce the strip crystallization and reduce the coercive force of the iron core, greatly improves the soft magnetic property of the FINMENT nanocrystalline alloy and widens the application prospect.
The tube-sealing hydrogenation heat treatment annealing process is carried out in the quartz tube with the inner diameter of 8mm and the outer diameter of 10mm, so that the gas consumption is low, the gas proportion and the gas content can be randomly regulated and controlled, the vacuum degree is good, and the product performance is stable. Compared with the traditional annealing operation in the furnace body, the annealing operation in the furnace body can effectively avoid hydrogen from damaging the furnace body, and because the vacuum quartz tube is adopted for operation, compared with the vacuumizing operation of the furnace body, the annealing operation in the furnace body has shorter heat treatment time and high efficiency.
Drawings
FIG. 1 is an X-ray diffraction pattern of a vacuum heat-treated sample.
FIG. 2 is an X-ray diffraction pattern of a hydrotreated sample.
FIG. 3 is a selected area electron diffraction pattern and high resolution spectrum of a vacuum heat treated sample.
FIG. 4 is a selected area electron diffraction pattern and high resolution spectrum of a hydro-thermally treated sample.
FIG. 5 is a differential scanning thermogram spectrum of a vacuum heat-treated sample.
FIG. 6 is a differential scanning thermogram spectrum of a hydro-thermally treated sample.
Fig. 7 is a magnetic domain image of a vacuum heat-treated sample.
Fig. 8 is a magnetic domain image of a hydro-thermally treated sample.
FIG. 9 is a comparison graph of coercivity performance tests, with the coercivity of the ribbons reduced by the hydrogenation heat treatment.
Detailed Description
The invention will now be described in further detail with reference to specific embodiments and the accompanying drawings. The following examples are intended to provide those skilled in the art with a more complete understanding of the present invention, and are not intended to limit the scope of the present invention. Reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic may be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
A tube sealing hydrogenation heat treatment annealing process comprises the following steps:
(1) preparing materials: according to Fe73.5Si13.5B9Cu3Nb1And calculating the mass of the corresponding raw material and weighing, wherein Si is added through the FeSi alloy, and the purities of other elements are all in industrial grade.
(2) Smelting a master alloy: weighing the step onePutting the obtained raw materials into a vacuum induction melting furnace, starting a mechanical pump to pump down the vacuum to 3 multiplied by 10-1Pa, opening a diffusion pump to pump high vacuum to 5X 10-3Pa, and filling protective atmosphere argon to 0.05 MPa. The smelting temperature is 1000 ℃, the single smelting time is 15min, repeated smelting is carried out for multiple times to ensure uniform smelting, and the master alloy ingot is obtained after furnace cooling.
(3) Preparation of the strip: crushing the master alloy obtained in the step (2), putting the crushed master alloy into an induction furnace of a rapid solidification device, starting a mechanical pump to pump down the vacuum to 3 multiplied by 10-1Pa, opening a diffusion pump to pump high vacuum to 5X 10-3Pa, introducing argon to 0.05MPa for protection, opening induction current for heating, spraying the molten mother alloy on a copper wheel rotating at high speed under the action of pressure to prepare an amorphous thin strip, wherein the linear velocity of the surface of the copper wheel is 30m/s, and obtaining Fe73.5Si13.5B9Cu3Nb1And (3) amorphous alloy.
(4) Packaging the belt material: cutting the amorphous strip obtained in the step (3) to a certain length of 8cm, ensuring that the surface quality of the cut strip is good and the cut strip is not bent under stress, and placing the cut strip into a quartz tube with the inner diameter of 8mm and the outer diameter of 10 mm; then the quartz tube is loaded on a tube sealing machine, and the mechanical pump is opened to vacuumize to 3 x 10-1Pa, closing the mechanical pump, and introducing a protective atmosphere (nitrogen, argon, helium and the like) and high-purity hydrogen by using a three-way valve, wherein the volume ratio of the protective atmosphere to the hydrogen is 96: 4; and (3) slowly and uniformly heating the quartz tube wall by using a flame spray gun, and gradually softening and shrinking the heated part to finally obtain the packaged quartz tube with two closed ends and a sample inside.
(5) And (3) heat treatment: after checking that each component of the muffle furnace normally works, setting a temperature control program, such as a heating rate of 10K/min, a heat treatment temperature of 550 ℃ and a heat preservation time of 300 min. And (3) turning on a heating power supply, placing the packaged sample in the third step on a heat treatment tray and in the muffle furnace when the temperature in the muffle furnace is stabilized at the heat preservation temperature, taking out the sample after heat treatment for 10min, and cooling in the air, wherein the processes can be repeated until all samples are treated.
Example 2
A tube sealing hydrogenation heat treatment annealing process comprises the following steps:
(1) preparing materials: according to Fe73.5Si13.5B9Cu3Nb1And calculating the mass of the corresponding raw material and weighing, wherein Si is added through the FeSi alloy, and the purities of other elements are all in industrial grade.
(2) Smelting a master alloy: putting the raw materials weighed in the step one into a vacuum induction melting furnace, opening a mechanical pump to pump down the vacuum to 3 multiplied by 10-1Pa, opening a diffusion pump to pump high vacuum to 5X 10-3Pa, and filling protective atmosphere argon to 0.05 MPa. The smelting temperature is 1300 ℃, the single smelting time is 10min, repeated smelting is carried out for multiple times to ensure uniform smelting, and the master alloy ingot is obtained after furnace cooling.
(3) Preparation of the strip: crushing the master alloy obtained in the step (2), putting the crushed master alloy into an induction furnace of a rapid solidification device, starting a mechanical pump to pump down the vacuum to 3 multiplied by 10-1Pa, opening a diffusion pump to pump high vacuum to 5X 10-3Pa, introducing argon to 0.05MPa for protection, opening induction current for heating, spraying the molten mother alloy on a copper wheel rotating at high speed under the action of pressure to prepare an amorphous thin strip, wherein the linear velocity of the surface of the copper wheel is 30m/s, and obtaining Fe73.5Si13.5B9Cu3Nb1And (3) amorphous alloy.
(4) Packaging the belt material: cutting the amorphous strip obtained in the step (3) to a certain length of 8cm, ensuring that the surface quality of the cut strip is good and the cut strip is not bent under stress, and placing the cut strip into a quartz tube with the inner diameter of 8mm and the outer diameter of 10 mm; then the quartz tube is loaded on a tube sealing machine, and the mechanical pump is opened to vacuumize to 3 x 10-1Pa, closing the mechanical pump, and introducing a protective atmosphere (nitrogen, argon, helium and the like) and high-purity hydrogen by using a three-way valve, wherein the volume ratio of the protective atmosphere to the hydrogen is 96: 4; and (3) slowly and uniformly heating the quartz tube wall by using a flame spray gun, and gradually softening and shrinking the heated part to finally obtain the packaged quartz tube with two closed ends and a sample inside.
(5) And (3) heat treatment: after checking that each component of the muffle furnace normally works, setting a temperature control program, such as a heating rate of 10K/min, a heat treatment temperature of 550 ℃ and a heat preservation time of 300 min. And (3) turning on a heating power supply, placing the packaged sample in the third step on a heat treatment tray and in the muffle furnace when the temperature in the muffle furnace is stabilized at the heat preservation temperature, taking out the sample after heat treatment for 20min, and cooling in the air, wherein the processes can be repeated until all samples are treated.
Example 3
A tube sealing hydrogenation heat treatment annealing process comprises the following steps:
(1) preparing materials: according to Fe73.5Si13.5B9Cu3Nb1And calculating the mass of the corresponding raw material and weighing, wherein Si is added through the FeSi alloy, and the purities of other elements are all in industrial grade.
(2) Smelting a master alloy: putting the raw materials weighed in the step one into a vacuum induction melting furnace, opening a mechanical pump to pump down the vacuum to 3 multiplied by 10-1Pa, opening a diffusion pump to pump high vacuum to 5X 10-3Pa, and filling protective atmosphere argon to 0.05 MPa. The smelting temperature is 1600 ℃, the single smelting time is 5min, repeated smelting is carried out for multiple times to ensure uniform smelting, and the master alloy ingot is obtained after furnace cooling.
(3) Preparation of the strip: crushing the master alloy obtained in the step (2), putting the crushed master alloy into an induction furnace of a rapid solidification device, starting a mechanical pump to pump down the vacuum to 3 multiplied by 10-1Pa, opening a diffusion pump to pump high vacuum to 5X 10-3Pa, introducing argon to 0.05MPa for protection, opening induction current for heating, spraying the molten mother alloy on a copper wheel rotating at high speed under the action of pressure to prepare an amorphous thin strip, wherein the linear velocity of the surface of the copper wheel is 30m/s, and obtaining Fe73.5Si13.5B9Cu3Nb1And (3) amorphous alloy.
(4) Packaging the belt material: cutting the amorphous strip obtained in the step (3) to a certain length of 8cm, ensuring that the surface quality of the cut strip is good and the cut strip is not bent under stress, and placing the cut strip into a quartz tube with the inner diameter of 8mm and the outer diameter of 10 mm; then the quartz tube is loaded on a tube sealing machine, and the mechanical pump is opened to vacuumize to 3 x 10-1Pa, closing the mechanical pump, and introducing protective atmosphere (nitrogen, argon, helium, etc.) through a three-way valveAnd high-purity hydrogen, wherein the volume ratio of the protective atmosphere to the hydrogen is 96: 4; and (3) slowly and uniformly heating the quartz tube wall by using a flame spray gun, and gradually softening and shrinking the heated part to finally obtain the packaged quartz tube with two closed ends and a sample inside.
(5) And (3) heat treatment: after checking that each component of the muffle furnace normally works, setting a temperature control program, such as a heating rate of 10K/min, a heat treatment temperature of 550 ℃ and a heat preservation time of 300 min. And (3) turning on a heating power supply, placing the packaged sample in the third step on a heat treatment tray and in the muffle furnace when the temperature in the muffle furnace is stable at the heat preservation temperature, taking out the sample after heat treatment for 30min, and cooling in the air, wherein the processes can be repeated until all samples are treated.
Comparative example
The comparative example was a vacuum heat treatment without hydrogen gas, and the other operation was the same as in example 2.
FIG. 1 is an X-ray diffraction pattern of a vacuum heat-treated sample.
FIG. 2 is an X-ray diffraction pattern of a hydrotreated sample.
As can be seen in fig. 1 and 2: FeB phase at 30 ℃ and alpha-Fe (Si) at 45 ℃. The FeB phase is a harmful phase and can improve the coercive force and loss of the alloy. The figure shows that the hydro-thermal treatment can promote the precipitation of alpha-Fe (Si) nanocrystals and inhibit the precipitation of harmful FeB phases.
FIG. 3 is a selected area electron diffraction pattern and high resolution spectrum of a vacuum heat treated sample.
FIG. 4 is a selected area electron diffraction pattern and high resolution spectrum of a hydro-thermally treated sample.
As can be seen from fig. 3 and 4, the precipitation of the nanocrystals was promoted by the hydrogenation heat treatment, and the crystal grain size was about 10 nm.
FIG. 5 is a differential scanning thermogram spectrum of a vacuum heat-treated sample.
FIG. 6 is a differential scanning thermogram spectrum of a hydro-thermally treated sample.
In FIGS. 5 and 6, it can be seen that the crystallization is promoted by the hydrogenation heat treatment and the crystallization peak disappears.
Fig. 7 is a magnetic domain image of a vacuum heat-treated sample.
Fig. 8 is a magnetic domain image of a hydro-thermally treated sample.
As can be seen from fig. 7 and 8, the wider the magnetic domain, the lower the coercivity of the ribbon, and it can be seen from the figure that the coercivity is reduced after the hydrotreatment.
FIG. 9 is a comparison graph of coercivity performance tests, with the coercivity of the ribbons reduced by the hydrogenation heat treatment.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. A tube sealing hydrogenation heat treatment annealing process is characterized in that: the heat treatment annealing process comprises the following steps:
preparing materials: according to the chemical formula Fe73.5Si13.5B9Cu3Nb1Calculating the mass of the raw materials corresponding to the ratio of the elements and weighing;
smelting a master alloy;
preparing a strip material;
packaging the belt material: cutting a section of amorphous thin belt with a certain length, putting the amorphous thin belt into a quartz tube, putting the quartz tube on a tube sealing machine, vacuumizing, introducing protective gas and high-purity hydrogen, and heating the wall of the quartz tube to obtain a packaged quartz tube with two closed ends and a sample inside;
and (3) heat treatment: and (4) putting the packaged quartz tube into a muffle furnace, carrying out heat treatment, and taking out and cooling.
2. The tube-sealing hydrogenation heat treatment annealing process according to claim 1, characterized in that: the smelting master alloy specifically comprises: and putting the weighed raw materials into a vacuum smelting furnace, vacuumizing, filling protective gas, smelting, and cooling to obtain a master alloy ingot.
3. The tube-sealing hydrogenation heat treatment annealing process according to claim 2, characterized in that: the vacuum melting furnace is a vacuum induction melting furnace, and the vacuumizing comprises opening a mechanical pump to pump low vacuum to 3 multiplied by 10-1Pa, opening a diffusion pump to pump high vacuum to 5X 10-3Pa, and protective gas is filled to 0.05 Mpa.
4. The tube-sealing hydrogenation heat treatment annealing process according to claim 2, characterized in that: the smelting mother alloy is repeatedly smelted for multiple times at the controlled temperature of 1000-1600 ℃, and the single smelting time is 5-15 min.
5. The tube-sealing hydrogenation heat treatment annealing process according to claim 1, characterized in that: the strip preparation comprises the following steps: crushing the mother alloy ingot, putting the crushed mother alloy ingot into an induction furnace, vacuumizing, introducing protective gas for protection, heating, melting the mother alloy ingot, and spraying the melted mother alloy ingot onto a copper wheel rotating at a high speed to prepare an amorphous thin strip.
6. The tube-sealing hydrogenation heat treatment annealing process according to claim 5, characterized in that: the vacuum pumping comprises opening a mechanical pump to pump down to 3 × 10-1Pa, opening a diffusion pump to pump high vacuum to 5X 10-3And Pa, introducing protective gas to 0.05MPa for protection.
7. The tube-sealing hydrogenation heat treatment annealing process according to claim 5, characterized in that: the surface linear speed of the copper wheel is 30 m/s.
8. The tube-sealing hydrogenation heat treatment annealing process according to claim 1, characterized in that: the length of the amorphous thin strip is 3cm-10cm, the inner diameter of the quartz tube is 8mm, and the outer diameter of the quartz tube is 10 mm.
9. The tube-sealing hydrogenation heat treatment annealing process according to claim 1, characterized in that: the vacuumizing operation in the tape packaging comprises opening a mechanical pump to vacuumize to 3 x 10-1Pa。
10. The tube-sealing hydrogenation heat treatment annealing process according to claim 1, characterized in that: the heat treatment temperature in the muffle furnace is 550 ℃, the heat preservation time is 300min, and the heating rate is 10K/min.
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