AU2019100683A4 - Iron-based amorphous nanocrystalline soft magnetic alloy ribbon and preparation method thereof - Google Patents

Iron-based amorphous nanocrystalline soft magnetic alloy ribbon and preparation method thereof Download PDF

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AU2019100683A4
AU2019100683A4 AU2019100683A AU2019100683A AU2019100683A4 AU 2019100683 A4 AU2019100683 A4 AU 2019100683A4 AU 2019100683 A AU2019100683 A AU 2019100683A AU 2019100683 A AU2019100683 A AU 2019100683A AU 2019100683 A4 AU2019100683 A4 AU 2019100683A4
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alloy ribbon
iron
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Chunyong Liang
Hongshui Wang
Kai Zhao
Shengli ZHU
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Wangwei New Materials (pizhou) Co Ltd
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • 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
    • 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
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • 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
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • 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
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2200/00—Crystalline structure
    • C22C2200/02—Amorphous
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C2200/04—Nanocrystalline

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Abstract

The disclosure provides an iron-based amorphous nanocrystalline soft magnetic alloy ribbon, comprising the components as shown in FeaSibBcPdCueMef, wherein, a, b, c, d, e and f respectively represent contents of Fe, Si, B, P, Cu and Me in the alloy ribbon in parts by atom mass, 80< a<90, 0.5< b<5, 5<c<12, 1< d<9, 0.3< e< 2, 0.3<f<3, and a+b+c+d+f=100. According to the disclosure, a high-Bs iron-based amorphous nanocrystalline soft magnetic alloy ribbon is obtained through addition of microelements without thermal treatment. This alloy ribbon is prepared in high vacuum or under the protection of argon, has excellent soft magnetic property and high thermal stability, and is applicable to a transformer, an engine, a motor, a generator, a magnetic sensor and the like. a-Fe hitensity/a.u. 30 40 50 60 70 80 90 20/degree -10000 -5000 5000 10000 -10000 -00

Description

IRON-BASED AMORPHOUS NANOCRYSTALLINE SOFT
MAGNETIC ALLOY RIBBON AND PREPARATION
METHOD THEREOF [0001] This paragraph has been intentionally deleted.
TECHNICAL FIELD [0002] The disclosure relates to the field of alloys, and particularly relates to a soft magnetic alloy ribbon having an amorphous nanocrystalline composite structure and high saturation magnetic flux density (Bs) and a preparation method thereof.
BACKGROUD OF THE PRESENT INVENTION [0003] Soft magnetic alloys are early developed magnetic function materials, which from an initial stage to now, experience electromagnetic pure iron, electrical steel, PERMALLOY, Fe~Co alloys, soft magnetic ferrite and amorphous alloys and other systems. The amorphous alloys have the high electric resistance, high permeability (μ) and low coercivity (//c). Compared with silicon steel, the amorphous alloys are easy to produce and do not need special machining. Hence they are regarded to ideal material for using in iron core.
[0004] However, compared with the traditional silicon steel used in iron core, the amorphous alloys still have some shortages, the biggest of which is its relative lower Bs. The Bs value of the traditional oriented silicon steel can reach 2.0 T, and the Bs value of the typical iron-based amorphous alloy Fe78Si9Bi3 is only about 1.5 T.
[0005] Many researchers tried to obtain an iron-based amorphous alloy with high Bs. Atypical example is a Metglass2605Co alloy, which has the Bs of 1.8 T. But its high cost due to a large amount of Co content limits the applications for large-scale industrial magnetic products.
[0006] US Patent US4226619 discloses an amorphous FeBC alloy with the Bs of about 1.7. However the large coercivity and high brittleness would limit its industry applications.
[0007] Chinese Patent CN1721563A discloses a FeSiBC alloy with Bs of about 1.64 T. But its preparation process is complex and its cost is high.
[0008] Chinese Patent CN102471856A discloses a FeBPCu series alloy which
2019100683 21 Jun 2019 composed of amorphous alloy matrix and as-precipitated BCC Fe phases with size of less than 25 nm. This iron-based amorphous/nano crystalline soft alloy have the Bs higher than 1.6 T. CN101595237A discloses a FeSiBPCu series amorphous alloy with/?, of 1.6T. CN1-2741437Adiscloses a FeSiBPCu series amorphous alloy, in which BCC iron phase with average size of 10-25 nm can precipitate after thermal treatment. Its Bs is 1.8-1.9 T. However, since thermal treatment is performed during the preparation, it is inevitable to increase production cost. A corresponding academic paper is Akihiro Makino, nanocrustalline soft magnetic Fe-Si-B-P-Cu alloys with high Bs of 1.8-1.9 T contributable to energy saving, IEEE Transactions on Magnetics,48(2012)1331-1335.
SUMMARY OF PRESENT INVENTION [0009] Aiming at the above problems, the disclosure provides an iron-based amorphous/nanocrystalline ribbon with good soft magnetic properties and its preparation method thereof. The iron-based amorphous/nanocrystalline soft magnetic alloy ribbon with Bs is obtained through addition of microelements and without any thermal treatment. A known preparation method in the prior art is as follows: First step, metal elements are molten into master alloy; Second step, the master alloy is re-molten, and ejected to a copper roller rotating at a high speed to obtain an amorphous alloy ribbon; Third step, the amorphous ribbon is annealed in a thermal treatment furnace to obtain precipitated nano crystallines in the amorphous substrate. The preparation method provided by the present disclosure only needs melting-spraying to directly obtain a structure of amorphous substrate + nanocrystalline, without any thermal treatment. The alloy ribbon obtained in the disclosure is prepared in a high vacuum or under the protection of argon, and the alloy ribbon exhibits excellent soft magnetic property and high thermal stability. The alloy ribbon can be applied in transformer, engine, motor, generator, and magnetic sensor, etc.
[0010] The technical solution for achieving the above object is as follows: [0011] The disclosure provides an iron-based amorphous nanocrystalline soft magnetic alloy ribbon, comprising the components as shown in FeaSibBcPdCueMef, wherein, the Me is selected from one of Ti, Zr, Nb or Ta, a, b, c, d, e and f respectively represent contents of Fe, Si, B, P, Cu and Me in the alloy ribbon in parts by atom mass, and 80<a<90, 0.5<b<5, 5<c<12, l<d<9, 0.3<e<2, 0.3<f<3, and
2019100683 21 Jun 2019 a+b+c+d+f=100.
[0012] The value range of the content a of the component Fe in parts by atom mass is 80<a<90, preferably, 83<a<87.
[0013] The value range of the content b of the component Si in parts by atom mass is 0.5<b<5, preferably, l<b<3.
[0014] The value range of the content c of the component B in parts by atom mass is 5<c<12, preferably, 6<c<10.
[0015] The value range of the content d of the component P in parts by atom mass is l<d<9, preferably, 2<d<6.
[0016] The value range of the content e of the component Cu in parts by atom mass is 0.3<e<2, preferably, 0.5<e<l.
[0017] The value range of the content f of the component Me (one of Ti, Zr, Nb and Ta) in parts by atom mass is 0.3<f<3, preferably, 0.5<f< 1.
[0018] The alloy ribbon of the disclosure is 15-40 pm in thickness and 1-5 mm in width.
[0019] Another aspect of the disclosure provides a preparation method of an iron-based nanocrystalline soft magnetic alloy ribbon, comprising the following steps:
[0020] (1) taking Fe, Si, B, P, Cu and Me in parts by atom mass;
[0021] (2) vacuumizing, and heating raw materials prepared in step (1) at a protective atmosphere to 1200-1400 °C to be molten; and [0022] (3) ejecting liquid alloy molten in step (2) to a copper roller at 1200-1400°C under a protective atmosphere to prepare an iron-based amorphous nano soft magnetic alloy ribbon.
[0023] In the step (2), the vacuuming is performed to <9 x 10' Pa.
[0024] Preferably, the protective gas in the step (2) and (3) is argon or nitrogen.
[0025] Preferably, the melting time in the step (2) is 5-30 min.
[0026] Preferably, the melting device in the step (2) is a high frequency induction furnace or an arc melting furnace.
[0027] Preferably, the linear speed of the surface of the copper roller in the step (3) is 20-60 m/s.
[0028] The disclosure also discloses use of the prepared iron-based amorphous
2019100683 21 Jun 2019 nanocrystalline alloy ribbon in preparation of an iron core of an electronic apparatus; the electronic [0029] apparatus is an engine, a transformer, an electric reactor or a mutual inductor.
[0030] The iron-based amorphous soft magnetic alloy ribbon prepared by the above preparation method is 15-40 pm in thickness and 1-5 mm in width.
[0031] The component design principle of the above iron-based amorphous nanocrystalline soft magnetic alloy ribbon will be described below.
[0032] In the disclosure, the main effects of the Si element are to improve glass forming ability and properly improve the thermal stability and Curie temperature of alloy. If the content of the Si element is too low, it is difficult to play its role of improving the glass forming ability, and if the content of the Si element is too high, the contents of ferromagnetic elements may be reduced, thereby reducing the Bs of alloy.
[0033] In the disclosure, the main effects of the P element are to improve the glass forming ability and properly improve the thermal stability of alloy. If the content of the P element is too low, it is difficult to play its role of improving the glass forming ability, and if the content of the Si element is too high, the contents of ferromagnetic elements may be reduced, thereby reducing the Bs of alloy.
[0034] In the disclosure, the main effects of the B element are to improve the glass forming ability and properly improve the thermal stability and Curie temperature of alloy. If the content of the B element is too low, it is difficult to play its role of improving the glass forming ability, and if the content of the B element is too high, the contents of ferromagnetic elements may be reduced, thereby reducing the Bs of alloy.
[0035] In the disclosure, Fe is a magnetic element, the high-content Fe element can obtain high magnetic induction intensity, however, if the content of Fe is too high, for example, reduction of amorphous formation elements and decrease of glass forming ability can be caused, and optimal comprehensive property cannot be obtained.
[0036] In the disclosure, the Cu element is easily precipitated out during the initial heating stage to form Cu-rich clusters and then the Cu-rich clusters serve as core formation points when Fe-rich nanocrystallines are formed, so as to promote the formation of nanocrystallines. However, in the process of ejection, Cu can be firstly significantly precipitated out as the temperature rises, the Cu element can form
2019100683 21 Jun 2019 excessive clusters if the content of Cu is too high, and then a large amount of crystals are locally based on these clusters as crystal cores in the process of subsequent rapid solidification, thereby reducing its glass forming ability.
[0037] In the disclosure, addition of the Me (one of Ti, Zr, Nb and Ta) element can significantly improve a core formation rate in Fe-based alloy supercooled liquid, thereby promoting the direct precipitation of a BCC nano iron phase in the alloy under the condition of shock cooling. This nanocrystalline phase is capable of greatly reducing the saturation magnetostriction of the Fe-based amorphous nanocrystalline alloy and bringing high magnetic flux density and high magnetic permeability.
[0038] According to the disclosure, high-saturation-induction-intensity iron-based amorphous nanocrystalline soft magnetic alloy ribbon is obtained through addition of microelements without thermal treatment (step three in “melting-ejecting-thermal treatment”) that is not required in the above prior art. This alloy ribbon is prepared in a high vacuum or under the condition of protective gas, has excellent soft magnetic property and high thermal stability, and is applicable to a transformer, an engine, a motor, a generator, a magnetic sensor and the like. Compared with the prior art, since addition of the Me element in the method of the disclosure effectively improves the core formation rate of the supercooled liquid and promotes the precipitation of the BCC nanocrystalline iron phase, the Fe-based nano alloy is prepared, the magnetostriction coefficient of the material is reduced, the initial permeability (μ,·) is improved, and the Bs is significantly increased to 1.7T or above.
DESCRIPTION OF THE DRAWINGS [0039] Fig.l is an XRD detection result diagram of an iron-based amorphous nanocrystalline soft magnetic alloy ribbon obtained according to example 1 of the disclosure;
[0040] Fig.2 is a VSM detection result diagram of an iron-based amorphous nanocrystalline soft magnetic alloy ribbon obtained according to example 1 of the disclosure;
[0041] Fig.3 is an XRD detection result diagram of an iron-based amorphous nanocrystalline soft magnetic alloy ribbon obtained according to example 2 of the disclosure;
[0042] Fig.4 is an XRD detection result diagram of an iron-based amorphous nanocrystalline soft magnetic alloy ribbon obtained according to example 3 of the
2019100683 21 Jun 2019 disclosure;
[0043] Fig.5 is an XRD detection result diagram of an iron-based amorphous nanocrystalline soft magnetic alloy ribbon obtained according to example 4 of the disclosure;
[0044] Fig.6 is an XRD detection result diagram of an iron-based amorphous nanocrystalline soft magnetic alloy ribbon obtained according to example 5 of the disclosure;
[0045] Fig.7 is an XRD detection result diagram of an iron-based amorphous nanocrystalline soft magnetic alloy ribbon obtained according to example 6 of the disclosure;
[0046] Fig.8 is an XRD detection result diagram of an iron-based amorphous nanocrystalline soft magnetic alloy ribbon obtained according to example 7 of the disclosure;
[0047] Fig.9 is an XRD detection result diagram of an iron-based amorphous nanocrystalline soft magnetic alloy ribbon obtained according to example 8 of the disclosure;
[0048] Fig. 10 is an XRD detection result diagram of an alloy ribbon obtained according to comparative example 1 of the disclosure;
[0049] Fig. 11 is an XRD detection result diagram of an alloy ribbon obtained according to comparative example 2 of the disclosure; and [0050] Fig. 12 is an XRD detection result diagram of an alloy ribbon obtained according to comparative example 3 of the disclosure.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS [0051] The disclosure will be described with reference to specific examples below. Those skilled in the art can understand that these examples are only for describing the disclosure, but not limiting the scope of the disclosure in any manners.
[0052] The experiment methods in the following examples, if no specifically stated, are all conventional methods. Raw materials, reagent materials and the like used in the following examples, if no specifically stated, are all commercially available products.
[0053] Example 1 [0054] (1) Pure iron, ferroboron or pure boron, ferrophosphorus, pure silicon, pure cupper and pure titanium were selected as raw materials, and various component
2019100683 21 Jun 2019 elements were prepared in parts by atom mass according to Fes5Si2B7P4CuiTii and then added into a high-frequency induction furnace;
[0055] (2) the high-frequency induction furnace was vacuumized to 5 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1300 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 10 min; and [0056] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1200 °C with argon, and the linear speed of the surface of the cupper roller was 50 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[0057] The crystal structure of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was detected via XRD. There were obviously widened α-Fe diffraction peaks on an XRD spectrogram, and in the meantime, there were diffusion scattering bags under the diffraction peaks, illustrating that the crystal structure of the alloy ribbon prepared in this example was coexistence of α-Fe and an amorphous structure, see Fig. 1. Via VSM detection, the obtained Bs was 2.03T, see Fig.2.
[0058] Example 2 [0059] (1) Pure iron, ferroboron or pure boron, ferrophosphorus, pure silicon, pure cupper and pure titanium were selected as raw materials, and various component elements were prepared in parts by atom mass according to Fe85Si2BeP4CuiTi2 and then added into a high-frequency induction furnace;
[0060] (2) the high-frequency induction furnace was vacuumized to 8 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1400 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 10 min; and [0061] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1200 °C with argon, and the linear speed of the surface of the cupper roller was 60 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[0062] The crystal structure of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was detected via XRD. There were obviously widened α-Fe diffraction peaks on an XRD spectrogram, and in the meantime, there were
2019100683 21 Jun 2019 diffusion scattering bags under the diffraction peaks, illustrating that the crystal structure of the ribbon was coexistence of α-Fe and an amorphous structure, see Fig.3. Via VSM detection, the obtained Bs was 1.92 T.
[0063] Example 3 [0064] (1) Pure iron, ferroboron or pure boron, ferrophosphorus, pure silicon, pure cupper and pure zirconium were selected as raw materials, and various component elements were prepared in parts by atom mass according to Fe85Si2B7P4CuiZri and then added into a high-frequency induction furnace;
[0065] (2) the high-frequency induction furnace was vacuumized to 8 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1300 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 10 min; and [0066] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1200 °C with argon, and the linear speed of the surface of the cupper roller was 40 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[0067] The crystal structure of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was detected via XRD. There were obviously widened α-Fe diffraction peaks on an XRD spectrogram, and in the meantime, there were diffusion scattering bags under the diffraction peaks, illustrating that the crystal structure of the ribbon was coexistence of α-Fe and an amorphous structure, see Fig.4. Via VSM detection, the obtained Bs was 1.88 T.
[0068] Example 4 [0069] (1) Pure iron, ferroboron or pure boron, ferrophosphorus, pure silicon, pure cupper and pure zirconium were selected as raw materials, and various component elements were prepared in parts by atom mass according to Fe8sSi2B6P4CuiZr2 and then added into a high-frequency induction furnace;
[0070] (2) the high-frequency induction furnace was vacuumized to 5 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1300 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 15 min; and [0071] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1200 °C with argon, and the linear speed of the surface of the cupper roller
2019100683 21 Jun 2019 was 40 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[0072] The crystal structure of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was detected via XRD. There were obviously widened α-Fe diffraction peaks on an XRD spectrogram, and in the meantime, there were diffusion scattering bags under the diffraction peaks, illustrating that the crystal structure of the ribbon was coexistence of α-Fe and an amorphous structure, see Fig.5. Via VSM detection, the obtained Bs was 1.75 T.
[0073] Example 5 [0074] (1) Pure iron, ferroboron or pure boron, ferrophosphorus, pure silicon, pure cupper and pure niobium were selected as raw materials, and various component elements were prepared in parts by atom mass according to Fes5Si2B7P4CuiNbi and then added into a high-frequency induction furnace;
[0075] (2) the high-frequency induction furnace was vacuumized to 5 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1400 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 15 min; and [0076] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1200 °C with argon, and the linear speed of the surface of the cupper roller was 20 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[0077] The crystal structure of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was detected via XRD. There were obviously widened α-Fe diffraction peaks on an XRD spectrogram, and in the meantime, there were diffusion scattering bags under the diffraction peaks, illustrating that the crystal structure of the ribbon was coexistence of α-Fe and an amorphous structure, see Fig.6. Via VSM detection, the obtained Bs was 1.77 T.
[0078] Example 6 [0079] (1) Pure iron, ferroboron or pure boron, ferrophosphorus, pure silicon, pure cupper and pure niobium are selected as raw materials, and various component elements are prepared in parts by atom mass according to Fes5Si2B6P4CuiNb2 and then added into a high-frequency induction furnace;
2019100683 21 Jun 2019 [0080] (2) the high-frequency induction furnace was vacuumized to 8 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1400 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 20 min; and [0081] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1200 °C with argon, and the linear speed of the surface of the cupper roller was 35 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[0082] The crystal structure of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was detected via XRD. There were obviously widened α-Fe diffraction peaks on an XRD spectrogram, and in the meantime, there were diffusion scattering bags under the diffraction peaks, illustrating that the crystal structure of the ribbon was coexistence of α-Fe and an amorphous structure, see Fig.7. Via VSM detection, the obtained Bs was 1.74 T.
[0083] Example 7 [0084] (1) Pure iron, ferroboron or pure boron, ferrophosphorus, pure silicon, pure cupper and pure tantalum were selected as raw materials, and various component elements were prepared in parts by atom mass according to Fes5Si2B7P4CuiTai and then added into a high-frequency induction furnace;
[0085] (2) the high-frequency induction furnace was vacuumized to 8 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1400 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 25 min; and [0086] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1400 °C with argon, and the linear speed of the surface of the cupper roller was 20 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[0087] The crystal structure of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was detected via XRD. There were obviously widened α-Fe diffraction peaks on an XRD spectrogram, and in the meantime, there were diffusion scattering bags under the diffraction peaks, illustrating that the crystal structure of the ribbon was coexistence of α-Fe and an amorphous structure, see Fig.8. Via VSM detection, the obtained Bs was 1.72 T.
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2019100683 21 Jun 2019 [0088] Example 8 [0089] (1) Pure iron, ferroboron or pure boron, ferrophosphorus, pure silicon, pure cupper and pure tantalum are selected as raw materials, and various component elements are prepared in parts by atom mass according to Fe85Si2BgP4CuiTa2 and then added into a high-frequency induction furnace;
[0090] (2) the high-frequency induction furnace was vacuumized to 5 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1400 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 30 min; and [0091] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1400 °C with argon, and the linear speed of the surface of the cupper roller was 35 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[0092] The crystal structure of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was detected via XRD. There were obviously widened α-Fe diffraction peaks on an XRD spectrogram, and in the meantime, there were diffusion scattering bags under the diffraction peaks, illustrating that the crystal structure of the ribbon was coexistence of α-Fe and an amorphous structure, see Fig.9. Via VSM detection, the obtained Bs was 1.73 T.
[0093] Comparative example 1 [0094] (1) Pure iron, ferroboron or pure boron, ferrophosphorus alloy, pure silicon and pure cupper were selected as raw materials, and various component elements were prepared in parts by atom mass according to Fe85Si2B7P4Cui and then added into a high-frequency induction furnace;
[0095] (2) the high-frequency induction furnace was vacuumized to 5 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1300 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 10 min; and [0096] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1200 °C with argon, and the linear speed of the surface of the cupper roller was 50 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
2019100683 21 Jun 2019 [0097] The crystal structure of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was detected via XRD. There were no obvious diffraction peaks on an XRD spectrogram, illustrating that the iron-based amorphous nanocrystalline soft magnetic alloy ribbon mainly has an amorphous structure, see Fig.10. Via VSM, the obtained Bs was 1.49 T.
[0098] Comparative example 2 [0099] (1) Pure iron, ferroboron or pure boron, ferrophosphorus alloy, pure silicon and pure cupper were selected as raw materials, and various component elements were prepared in parts by atom mass according to Fes5Si2BsP4Cui and then added into a high-frequency induction furnace;
[00100] (2) the high-frequency induction furnace was vacuumized to 8 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1400 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 30 min; and [00101] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1400 °C with argon, and the linear speed of the surface of the cupper roller was 50 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[00102] The crystal structure of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was detected via XRD. There were no obvious diffraction peaks on an XRD spectrogram, illustrating that the iron-based amorphous nanocrystalline soft magnetic alloy ribbon mainly has an amorphous structure, see Fig.l 1. Via VSM, the obtained Bs was 1.45 T.
[00103] Comparative example 3 [00104] (1) Pure iron, ferroboron or pure boron, ferrophosphorus alloy, pure silicon and pure cupper were selected as raw materials, and various component elements were prepared in parts by atom mass according to Fe85.5Si2B8P4Cuo.5 and then added into a high-frequency induction furnace;
[00105] (2) the high-frequency induction furnace was vacuumized to 8 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1400 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 20 min; and
2019100683 21 Jun 2019 [00106] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1200 °C with argon, and the linear speed of the surface of the cupper roller was 50 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[00107] The crystal structure of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was detected via XRD. There were no obvious diffraction peaks on an XRD spectrogram, illustrating that the iron-based amorphous nanocrystalline soft magnetic alloy ribbon mainly has an amorphous structure, see Fig. 12. Via VSM detection, the obtained Bs was 1.46 T.
[00108] Comparative example 4 [00109] (1) Pure iron, ferroboron or pure boron, ferrophosphorus alloy, pure silicon, pure cupper and pure aluminum were selected as raw materials, and various component elements were prepared in parts by atom mass according to Fe85Si2B7.5P4Cui AI0.5 and then added into a high-frequency induction furnace;
[00110] (2) the high-frequency induction furnace was vacuumized to 8 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1400 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 20 min; and [00111] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1200 °C with argon, and the linear speed of the surface of the cupper roller was 50m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[00112] Via XRD detection, the Bs of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was 1.58 T.
[00113] Comparative example 5 [00114] (1) Pure iron, ferroboron or pure boron, ferrophosphorus, pure silicon, pure cupper and pure aluminum are selected as raw materials, and various component elements are prepared in parts by atom mass according to Fe85Si2B7P4Cui Gai and then added into a high-frequency induction furnace;
[00115] (2) the high-frequency induction furnace was vacuumized to 8 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1400 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 20 min; and
2019100683 21 Jun 2019 [00116] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1200 °C with argon, and the linear speed of the surface of the cupper roller was 50 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[00117] Via XRD detection, the Bs of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was 1.60 T.
[00118] Comparative example 6 [00119] (1) Pure iron, ferroboron or pure boron, ferrophosphorus, pure silicon, pure cupper and pure aluminum were selected as raw materials, and various component elements are prepared in parts by atom mass according to Fes5Si2B6P4Cui Im and then added into a high-frequency induction furnace;
[00120] (2) the high-frequency induction furnace was vacuumized to 8 x 10' Pa, then argon was introduced, and the raw materials prepared in step (1) were heated to 1400 °C in a quartz tube of the high-frequency induction furnace so as to be molten, lasting for 20 min; and [00121] (3) the molten liquid alloy was ejected to a copper roller rotating at a high speed at 1200 °C with argon, and the linear speed of the surface of the cupper roller was 50 m/s, thereby preparing an iron-based amorphous nanocrystalline soft magnetic alloy ribbon.
[00122] Via XRD detection, the Bs of the prepared iron-based amorphous nanocrystalline soft magnetic alloy ribbon was 1.62 T.
[00123] Crystal types, densities and saturation induction intensities in the above examples 1~8 and comparative examples 1~6 are seen in Table 1.
[00124] Table 1: Crystal types, densities and saturation induction intensities in the above examples 1~8 and comparative examples 1~6
Material number Components Crystal type Density (g/cm3) Bs(T)
Example 1 FeX5Si2B7P4Cu|Ti| A+C 7.35 2.03
Example 2 FeX5Si2B7P4Cu|Ti2 A+C 7.31 1.92
Example 3 Fe^SijB^CUjZrj A+C 7.46 1.88
Example 4 Fe^SijB^CUjZrj A+C 7.43 1.75
2019100683 21 Jun 2019
Example 5 Feg5 Si 2 B7P4Cu, Nb j A+C 7.49 1.77
Example 6 Fe85 Cu]Nb2 A+C 7.55 1.74
00125] The above description of the embodiments is not intended to limit the disclosure. Various variations or transformations can be made by those skilled in the art according to the disclosure, which are all included within the scope of the claims appended by the disclosure without departing from the spirit of the disclosure.
2019100683 21 Jun 2019

Claims (2)

  1. We claim:
    1. An iron-based amorphous nanocrystalline soft magnetic alloy ribbon, comprising the components as shown in FeaSibBcPdCueMef, wherein, the Me is selected from one of Ti, Zr, Nb or Ta, a, b, c, d, e and f respectively represent contents of Fe, Si, B, P, Cu and Me in the alloy ribbon in parts by atom mass, and 80 <a<90, 0.5<b<5, 5<c<12, l<d<9, 0.3<e<2, 0.3<f<3, and a+b+c+d+f=100.
    2. The alloy ribbon according to claim 1, wherein, 83^~a^~87.
    3. The alloy ribbon according to claim 1 or 2, wherein, 1 ^~b^~3.
    4. The alloy ribbon according to any one of claims 1-3, wherein, 6^~c^~ 10.
    5. The alloy ribbon according to any one of claims 1-4, wherein, 2^~d^~6.
    6. The alloy ribbon according to any one of claims 1-5, wherein, 0.5^~e^~ 1.
    7. The alloy ribbon according to any one of claims 1-6, wherein, 0.5^~f^~ 1.
    8. The alloy ribbon according to any one of claims 1-7, wherein, the alloy ribbon is
    15-40 pm in thickness and 1-5 mm in width.
    9. A preparation method of the alloy ribbon according to any one of claims 1-8, the preparation method comprising the following steps:
    (1) taking Fe, Si, B, P, Cu and Me in parts by atom mass;
  2. (2) vacuuming, and heating raw materials prepared in step (1) under a protective atmosphere to 1200-1400 °C to be molten; and (3) ejecting liquid alloy molten in step (2) to a copper roller at 1200-1400°C under a protective atmosphere to prepare an iron-based amorphous nano soft magnetic alloy ribbon.
    2019100683 21 Jun 2019
    10. The preparation method according to claim 9, wherein, in the step (2), the vacuuming is performed to <9 x 10'3 Pa;
    preferably, the protective gas is argon or nitrogen;
    preferably, the melting time is 5-30 min;
    preferably, the melting device is a high frequency induction furnace or an arc melting furnace;
    preferably, the linear speed of the surface of the copper roller is 20-60 m/s.
    11. Use of the alloy ribbon according to any one of claims 1-8 in preparation of an iron core of an electronic apparatus, wherein, preferably, the electronic apparatus is an engine, a transformer, an electric reactor or a mutual inductor.
    1/6
    2019100683 21 Jun 2019
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114381673A (en) * 2022-01-14 2022-04-22 青岛云路先进材料技术股份有限公司 Iron-based amorphous nanocrystalline strip and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114381673A (en) * 2022-01-14 2022-04-22 青岛云路先进材料技术股份有限公司 Iron-based amorphous nanocrystalline strip and preparation method thereof

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