Fe-Co BASED AMORPHOUS SOFT MAGNETIC ALLOY AND PREPARATION METHOD THEREOF
20200335246 ยท 2020-10-22
Inventors
- Baolong Shen (Nanjing, CN)
- Donghui LI (Nanjing, CN)
- Xingdu Fan (Nanjing, CN)
- Qianqian Wang (Nanjing, CN)
- Mufeng Jiang (Nanjingsu, CN)
- Xiangrong Jiang (Nanjing, CN)
- Xiangyue Wang (Nanjing, Jiangsu, CN)
Cpc classification
International classification
C21D9/52
CHEMISTRY; METALLURGY
Abstract
The invention relates to the technical field of amorphous soft magnetic material, specifically relating to the field of FeCo based amorphous soft magnetic alloy and preparation method thereof. The FeCo based amorphous soft magnetic alloy provided in the invention has chemical composition of Fe.sub.aCo.sub.bSi.sub.cB.sub.dCu.sub.e, which possesses merits of highly-saturated magnetic induction, outstanding soft magnetic property and great amorphous forming ability at the same time; the embodiment of FeCo based amorphous soft magnetic alloy disclosed in the invention has indicated that its saturation magnetic induction is 1.791.86 T, coercivity 1.44.3 A/m, and permeability 800014000; the invention has advantages of easy treatment process, low annealing temperature, which reduces process cost remarkably and economizes energy, thus having great application prospect.
Claims
1. A FeCo based amorphous soft magnetic alloy with a chemical composition of Fe.sub.aCo.sub.bSi.sub.cB.sub.dCu.sub.e wherein a, b, c, d, and e respectively represent the atomic percentage of corresponding components; a=6085, b=120, d=1216, e=0.51.5, a+b+c+d+e=100.
2. The FeCo based amorphous soft magnetic alloy of claim 1, wherein a+b=8283, c=02, d=1214, a+b+c+d+e=100.
3. The FeCo based amorphous soft magnetic alloy of claim 1, wherein said FeCo based amorphous soft magnetic alloy comprises Fe.sub.78.65Co.sub.4Si.sub.2B.sub.14Cu.sub.1.35, Fe.sub.74.65Co.sub.8Si.sub.2B.sub.14Cu.sub.1.35, Fe.sub.70.65Co.sub.12Si.sub.2B.sub.14Cu.sub.1.35, Fe.sub.66.65Co.sub.16Si.sub.2B.sub.14Cu.sub.1.35 and Fe.sub.62.65Co.sub.20Si.sub.2B.sub.14Cu.sub.1.35.
4. The method for the preparation of the FeCo based amorphous soft magnetic alloy defined by claim 1, wherein it comprising following steps: Mixing raw materials of Fe, Co, Si, B and Cu according to the atomic percentage to obtain a mixture; smelting said mixture to obtain a master alloy ingot; preparing the master alloy ingot into an amorphous alloy ribbon via single roll cold method; annealing said amorphous alloy ribbon to obtain the FeCo based amorphous soft magnetic alloy.
5. The preparation method of claim 4 wherein said Fe, Co, Si, B and Cu raw materials have a purity of >99%.
6. The preparation method of claim 4 wherein the injection pressure of said single roll cold method is 0.01-0.03 MPa, the injection temperature is 1000-1050 C., and the linear velocity of the surface of the copper roll is 3050 m/s.
7. Tho preparation method of claim 4 wherein the width of said amorphous alloy ribbon is 1-1.5 mm, and the thickness thereof is 20-30 m.
8. The preparation method of claim 4 wherein said annealing treatment is carried out in a vacuum atmosphere or an inert atmosphere, and the vacuum degree of the vacuum atmosphere is (58)10.sup.3 Pa.
9. The preparation method of claim 4 wherein said annealing process is carried out under the action of an external magnetic field; the magnetic field strength of said external magnetic field is 200-1500 Oe.
10. The preparation method of claim 4 wherein said annealing temperature is 290-370 and the annealing time is 5-30 min.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0039] The invention provides a FeCo based amorphous soft magnetic alloy with a chemical composition of Fe.sub.aCo.sub.bSi.sub.cB.sub.dCu.sub.e wherein a, b, c, d, and e respectively represent the atomic percentage of corresponding components; a=6085, b=120, c=04, d=1216, e=0.51.5, a+b+c+d+e=100.
[0040] In the invention, as a preferred solution, said a+b=8283, c=02, d=1214, e=11.5, a+b+c+d+e=100.
[0041] In the invention, preferably, said FeCo based amorphous soft magnetic alloy comprises Fe.sub.78.65Co.sub.4Si.sub.2B.sub.14Cu.sub.1.35, Fe.sub.74.65Co.sub.8Si.sub.2B.sub.14Cu.sub.1.35, Fe.sub.70.65Co.sub.12Si.sub.2B.sub.14Cu.sub.1.35, Fe.sub.66.65Co.sub.16Si.sub.2B.sub.14Cu.sub.1.35 and Fe.sub.62.65Co.sub.20Si.sub.2B.sub.14Cu.sub.1.35.
[0042] The invention provides the preparation method of said FeCo based amorphous soft magnetic alloy in the above technical plan comprising following steps:
[0043] Mixing raw materials of Fe, Co, Si, B and Cu according to the atomic percentage to obtain a mixture;
[0044] smelting said mixture to obtain a master alloy ingot;
[0045] preparing the master alloy ingot into an amorphous alloy ribbon via single roll cold method;
[0046] annealing said amorphous alloy ribbon to obtain the FeCo based amorphous soft magnetic alloy.
[0047] The invention mixes raw materials of Fe, Co, Si, B and Cu according to the atomic percentage to obtain a mixture wherein said Fe, Co, Si, B and Cu raw materials preferably have a purity of >99%.
[0048] The source of the raw materials of Fe, Co, Si, B and Cu is not particularly required in the invention, and those well known to those skilled in the art can be selected, such as raw materials available in the market.
[0049] After the mixture is obtained, the mixture will be smelted to obtain a master alloy ingot. In the invention, said smelting is preferably carried out in high-frequency induction melting furnace, the melting conditions of which are not particularly limited and may be carried out under conditions known to those skilled in the art.
[0050] After obtaining the master alloy ingot, the invention adopts single roll cold method to prepare said master alloy ingot into an amorphous alloy ribbon. In the invention, the single roll cold method is preferably carried out to prepare the amorphous alloy ribbon via VF-RQB20 type melt-spun apparatus produced by Japanese CompanyMakabe Giken Co., Ltd. In embodiments of the invention, preparing the amorphous alloy ribbon by the single roll cold method preferably includes following steps: adjusting the size of tube orifice of a quartz tube to be 0.81 mm by using sand paper; crushing the master alloy ingot, loading the crushed master alloy ingot into the quartz tube and fixing it in an induction coil; adjusting the upper position and the lower position of the quartz tube to control the distance between the tube orifice and roll surface to be about 0.25 mm; firstly evacuating to be below 5 Pa, secondly evacuating to 810.sup.3 Pa, then filling protective gas (high-purity argon) into the quartz tube; controlling pressure difference (0.0150.020 MPa) between the cavity of the melt-spun machine and the quartz tube, setting the surface linear velocity of a copper roll, switching on heating current, heating and melting the master alloy to injection temperature by using the solenoid, and pressing the injection button to inject to obtain amorphous alloy ribbon. In the invention, the injection pressure of the single roll cold method is preferably at 0.010.03 MPa, and more preferably at 0.0150.02 MPa; the injection temperature of said single roll cold method is preferably at 10001050 C., and more preferably at 10201040 C.; the surface linear velocity of the copper roll is preferably at 3050 m/s, and more preferably at 3545 m/s. In the invention, the bandwidth of the amorphous alloy ribbon is preferably 11.5 mm, and the thickness thereof is preferably 2030 m.
[0051] After obtaining amorphous alloy ribbon, the invention anneals said amorphous alloy ribbon to obtain the FeCo based amorphous soft magnetic alloy. The annealing process is preferably carried out in a vacuum atmosphere or an inert atmosphere, and the vacuum degree of the vacuum atmosphere is (58)10.sup.3 Pa, more preferably (67)10.sup.3 Pa. In the invention, said annealing process is carried out preferably under the action of external magnetic field; the magnetic field strength of said external magnetic field is 200-1500 Oe, more preferably 5001200 Oe and most preferably 1000 Oe. In the invention, said annealing temperature is preferably 290-370 C., and more preferably 350370 C.; said annealing time is 5-30 min, more preferably 1020 min and most preferably 15 min.
[0052] In embodiments of the invention, said annealing process includes following steps: Cutting the amorphous alloy ribbon into a 60-mm-long ribbon, placing the ribbon into the quartz tube matched with a tubular magnetic field annealing furnace; firstly evacuating to be below 5 Pa, secondly evacuating to (58)10.sup.3 Pa; when the temperature of the tubular furnace rises to 290370 C., pushing the quartz tube into the tubular furnace, simultaneously applying external magnetic field whose direction is parallel with that of ribbon, preserving heat, quenching the obtained product and cooling to room temperature to obtain the FeCo based amorphous ribbon, namely the FeCo based amorphous soft magnetic alloy.
[0053] The FeCo based amorphous soft magnetic alloy and preparation method thereof is further described in detail hereinafter with reference to the embodiments, but the protective scope of the invention is not limited thereto.
Embodiment 1
[0054] Mixing raw materials of Fe, Co, Si, B and Cu whose purity exceed 99% according to the atomic percentage (molecular formula: Fe.sub.66.65Co.sub.16Si.sub.2B.sub.14Cu.sub.1.35) to obtain a mixture;
[0055] placing said mixture into crucible of the induction melting furnace and smelting to obtain a master alloy ingot;
[0056] the single roll cold method is adopted to prepare the amorphous alloy ribbon via VF-RQB20 type melt-spun apparatus produced by Japanese CompanyMakabe Giken Co., Ltd. Specifically, adjusting the sized of the tube orifice of a quartz tube to 0.8 mm by using sand paper; crushing said master alloy ingot, loading the crushed master alloy ingot into the quartz tube and fixing it in an induction coil; adjusting the upper position and the lower position of the quartz tube to control the distance between the tube orifice and roll surface to be about 0.25 mm; firstly evacuating to be below 5 Pa, secondly evacuating to 810.sup.3 Pa, then filling protective gas (high-purity argon) into the quartz tube; the pressure difference is 0.015 MPa; setting the surface linear velocity of a copper roll at about 45 m/s, switching on heating current, heating and melting the master alloy to 1050 C. by using the solenoid, then pressing the injection button, rapidly injecting melting alloy liquid onto the surface of a copper roll which is rotating at a high speed by utilizing the air pressure difference between internal quartz tube and the cavity, rapidly cooling to obtain the amorphous alloy ribbon with the width of 1.3 mm and the thickness of 30 m;
[0057] cutting said amorphous alloy ribbon into a 60-mm-long ribbon, placing the ribbon into the quartz tube matched with a tubular magnetic field annealing furnace; firstly evacuating to be below 5 Pa, secondly evacuating to 510.sup.3 Pa; when the temperature of the tubular furnace rises to 290370 C., pushing the quartz tube into the tubular furnace, simultaneously applying 1000 Oe external magnetic field whose direction is parallel with that of ribbon, preserving temperature for 15 min, quenching the obtained product and cooling to room temperature to obtain the FeCo based amorphous ribbon after stress-relief annealing in magnetic field, namely the FeCo based amorphous soft magnetic alloy.
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[0062] Besides, cutting said amorphous alloy ribbon into a 60-mm-long ribbon, placing the ribbon into the quartz tube matched with a tubular magnetic field annealing furnace; firstly evacuating to be below 5 Pa, secondly evacuating to 510.sup.3 Pa; when the temperature of the tubular furnace rises to 290370 C., pushing the quartz tube into the tubular furnace, preserving temperature for 15 min, quenching the obtained product and cooling to room temperature to obtain the FeCo based amorphous ribbon after going through common stress-relief annealing process.
[0063]
Embodiment 2
[0064] Mixing raw materials of Fe, Co, Si, B and Cu whose purity exceed 99% according to the atomic percentage (molecular formula: Fe.sub.62.65Co.sub.20Si.sub.2B.sub.14Cu.sub.1.35) to obtain a mixture;
[0065] placing said mixture into crucible of the induction melting furnace and smelting to obtain a master alloy ingot;
[0066] the single roll cold method is adopted to prepare the amorphous alloy ribbon via VF-RQB20 type melt-spun apparatus produced by Japanese CompanyMakabe Giken Co., Ltd. Specifically, adjusting the sized of the tube orifice of a quartz tube to 1 mm by using sand paper; crushing said master alloy ingot, loading the crushed master alloy ingot into the quartz tube and fixing it in an induction coil; adjusting the upper position and the lower position of the quartz tube to control the distance between the tube orifice and roll surface to be about 0.25 mm; firstly evacuating to be below 5 Pa, secondly evacuating to 810.sup.3 Pa, then filling protective gas (high-purity argon) into the quartz tube; the pressure difference is 0.015 MPa; setting the surface linear velocity of a copper roll at about 45 m/s, switching on heating current, heating and melting the master alloy to 1050 C. by using the solenoid, then pressing the injection button, rapidly injecting melting alloy liquid onto the surface of a copper roll which is rotating at a high speed by utilizing the air pressure difference between internal quartz tube and the cavity, rapidly cooling to obtain the amorphous alloy ribbon with the width of 1.3 mm and the thickness of 30 m;
[0067] cutting said amorphous alloy ribbon into a 60-mm-long ribbon, placing the ribbon into the quartz tube matched with a tubular magnetic field annealing furnace; firstly evacuating to be below 5 Pa, secondly evacuating to 510.sup.3 Pa; when the temperature of the tubular furnace rises to 290370 C., pushing the quartz tube into the tubular furnace, simultaneously applying 1000 Oe external magnetic field whose direction is parallel with that of ribbon, preserving temperature for 15 min, quenching the obtained product and cooling to room temperature to obtain the FeCo based amorphous ribbon after stress-relief annealing in magnetic field, namely the FeCo based amorphous soft magnetic alloy.
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[0072] Besides, cutting said amorphous alloy ribbon into a 60-mm-long ribbon, placing the ribbon into the quartz tube matched with a tubular magnetic field annealing furnace; firstly evacuating to be below 5 Pa, secondly evacuating to 510.sup.3 Pa; when the temperature of the tubular furnace rises to 290370 C., pushing the quartz tube into the tubular furnace, preserving temperature for 15 min, quenching the obtained product and cooling to room temperature to obtain the FeCo based amorphous ribbon after going through common stress-relief annealing process.
[0073]
COMPARATIVE EXAMPLE 1
[0074] Mixing raw materials of Fe, Co, Si, B and Cu whose purity exceed 99% according to the atomic percentage (molecular formula: Fe.sub.82.65Si.sub.2B.sub.14Cu.sub.1.35) to obtain a mixture;
[0075] placing said mixture into crucible of the induction melting furnace and smelting to obtain a master alloy ingot;
[0076] the single roll cold method is adopted to prepare the amorphous alloy ribbon via VF-RQB20 type melt-spun apparatus produced by Japanese CompanyMakabe Giken Co., Ltd. Specifically, adjusting the sized of the tube orifice of a quartz tube to 0.8 mm by using sand paper; crushing said master alloy ingot, loading the crushed master alloy ingot into the quartz tube and fixing it in an induction coil; adjusting the upper position and the lower position of the quartz tube to control the distance between the tube orifice and roll surface to be about 0.25 mm; firstly evacuating to be below 5 Pa, secondly evacuating to 810.sup.3 Pa, then filling protective gas (high-purity argon) into the quartz tube; the pressure difference is 0.015 MPa; setting the surface linear velocity of a copper roll at about 45 m/s, switching on heating current, heating and melting the master alloy to 1050 C. by using the solenoid, then pressing the injection button, rapidly injecting melting alloy liquid onto the surface of a copper roll which is rotating at a high speed by utilizing the air pressure difference between internal quartz tube and the cavity, rapidly cooling to obtain the amorphous alloy ribbon with the width of 1 mm and the thickness of 20 m;
[0077] cutting said amorphous alloy ribbon into a 60-mm-long ribbon, placing the ribbon into the quartz tube matched with a tubular magnetic field annealing furnace; firstly evacuating to be below 5 Pa, secondly evacuating to 510.sup.3 Pa; when the temperature of the tubular furnace rises to 270350 C., pushing the quartz tube into the tubular furnace, simultaneously applying 1000 Oe external magnetic field whose direction is parallel with that of ribbon, preserving temperature for 15 min, quenching the obtained product and cooling to room temperature to obtain the FeCo based amorphous ribbon after stress-relief annealing in magnetic field.
[0078]
[0079]
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[0081]
[0082] Besides, cutting said amorphous alloy ribbon into a 60-mm-long ribbon, placing the ribbon into the quartz tube matched with a tubular magnetic field annealing furnace; firstly evacuating to be below 5 Pa, secondly evacuating to 510.sup.3 Pa; when the temperature of the tubular furnace rises to 270350 C., pushing the quartz tube into the tubular furnace, preserving temperature for 15 min, quenching the obtained product and cooling to room temperature to obtain the FeCo based amorphous ribbon after going through common stress-relief annealing process.
[0083]
[0084] According to the embodiments 1-2 and the comparative example 1, the invention obtains amorphous soft magnetic alloy with highly-saturated magnetic induction, outstanding soft magnetic property and great amorphous forming ability by adding Co element into the Fe-based amorphous alloy and combining annealing in the magnetic field; compared with current Fe-based amorphous magnetic alloy, in the FeCo based amorphous soft magnetic alloy prepared in the invention, its saturation magnetic induction can reach 1.86 T, coercivity can reach 4.3 A/m, and permeability can be up to 14000, improved the performance of the Fe-based amorphous magnetic alloy remarkably.
[0085] As can be seen from above embodiments, the invention provides a FeCo based amorphous soft magnetic alloy which possesses merits of highly-saturated magnetic induction, outstanding soft magnetic property and great amorphous forming ability at the same time; the embodiment of FeCo based amorphous soft magnetic alloy disclosed in the invention has indicated that its saturation magnetic induction is 1.791.86 T, coercivity 1.44.3 A/m, and permeability 800014000; the invention has advantages of easy treatment process, low annealing temperature, which reduces process cost remarkably and economizes energy, thus having great application prospect.
[0086] The invention and its embodiment have been described above, but the description is not limited thereto; In general, it is to be understood by those skilled in the art that equivalent structures or equivalent process transformations or use in other related technical fields directly or indirectly by taking advantage of the description of the specification and drawings in the invention shall all fall within the protective scope of the invention.