CN107910155A - A kind of high saturation and magnetic intensity Fe B Si P Zr amorphous and nanocrystalline soft magnetic alloys - Google Patents

A kind of high saturation and magnetic intensity Fe B Si P Zr amorphous and nanocrystalline soft magnetic alloys Download PDF

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Publication number
CN107910155A
CN107910155A CN201711344036.1A CN201711344036A CN107910155A CN 107910155 A CN107910155 A CN 107910155A CN 201711344036 A CN201711344036 A CN 201711344036A CN 107910155 A CN107910155 A CN 107910155A
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alloy
amorphous
saturation magnetization
magnetic
alloys
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惠希东
李高峰
吕旷
王拓
张利伟
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Luoyang Cohim Amorphous Technology Co Ltd
University of Science and Technology Beijing USTB
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Luoyang Cohim Amorphous Technology Co Ltd
University of Science and Technology Beijing USTB
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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
    • C—CHEMISTRY; METALLURGY
    • 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
    • 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
    • H01F1/15341—Preparation processes therefor

Abstract

The invention belongs to amorphous nano-crystalline alloy field, and in particular to a kind of series bulk amorphous alloys of Fe B Si P Zr with high saturation and magnetic intensity and higher amorphous formation ability.The chemical composition expression formula of alloy is FeaBbSicPdZre, composition characteristics are：80≤a≤85,5≤b≤15,1≤c≤11,0.5≤d≤5,0.1≤e≤3, a+b+c+d+e=100.Further optimize by component, Fe80B13Si3P3Zr1The critical dimension of non-crystaline amorphous metal is 40 μm, saturation magnetization 1.68T, more than the level of business amorphous soft-magnetic alloy.Meanwhile the addition of a small amount of amorphous formation element Zr and P ensure that the alloy of the present invention has higher amorphous formation ability, expand the preparation process window of the alloy system significantly.The amorphous nano peritectic alloy is suitable for the motor of power industry transformer core, electric automobile, unmanned plane and automatic field, mutual inductor etc., it may also be used for electromagnetic shielding material of communication field etc..

Description

A kind of high saturation and magnetic intensity Fe-B-Si-P-Zr amorphous and nanocrystalline soft magnetic alloys
Technical field
The invention belongs to amorphous nano-crystalline alloy field, and in particular to one kind has high saturation and magnetic intensity and preferable amorphous The series bulk amorphous alloys of Fe-B-Si-P-Zr of Forming ability.
Background technology
In life and production now, soft magnetic materials be it is a kind of it is particularly important, using quite varied energy electronic material Material.Fe-based amorphous alloy as a kind of novel energy-saving environment-friendly type soft magnetic materials, have low-coercivity, high magnetic permeability, high resistivity, The good characteristics such as low-loss, frequency characteristic be good.If utilize Fe-based amorphous and its nanometer crystal alloy replacement or part substituted for silicon Steel is applied to power transformer, motor and electronic information field and uses, and can promote device to energy-saving, miniaturization, high efficiency and height Stability develops, thus has highly important economic value and social benefit.
Since 1967, Duwez et al. prepared the Fe-P-C with soft magnetic characteristic using the method quickly solidified first Since non-crystaline amorphous metal, a series of Fe-based amorphous and its nano-crystal soft magnetic alloy system is found.At present, iron-base soft magnetic alloy system The systems such as mainly Fe-B, Fe-P-C, Fe-P-B, Fe (Co, Ni)-Si-B, are mainly developed and are promoted by the researcher of Japan. Wherein, Fe bases soft magnetic amorphous alloy component mainly has：Fe80B20, trade mark Metglas 2605, saturation magnetization 1.61T, Coercivity is 3.2A/m)；Fe78B13Si9, trade mark Metglas 2605S-2, saturation magnetization 1.56T, coercivity is 2.4A/m).Typical Fe base Sol-Gel alloys have：Fe90Zr7B3, trade mark Nanoperm, saturation magnetization 1.63T, Coercivity is 5.6A/m；Fe73.5Si13.5B9Nb3Cu1, trade mark Finemet, saturation magnetization 1.24T, coercivity is 0.53A/m。
Ternary Fe-B-Si non-crystaline amorphous metals are the commercialization amorphous soft-magnetic alloys of current mainstream, amorphous formation energy in the system The alloying component of power maximum is Fe75B15Si10, but the non-of about 250 μm of thickness can be formed by the belt-rejecting technology maximum of high cooling rate Brilliant strip.2002, bright nine et al. by adding Zr, Nb alloying element, to significantly improve the system non-on northeastern Japan university well The amorphous formation ability of peritectic alloy.Wherein, (the Fe of diameter 0.75mm can be prepared by copper mold casting0.75B0.15Si0.1)99Zr1Non-crystaline amorphous metal, the saturation magnetization of the alloy is 1.53T；In addition, (Fe0.75B0.15Si0.1)99Nb2Block amorphous alloy Critical dimension reach 1mm, saturation magnetization 1.49T.Due to the addition of non magnetic constituent element Zr and Nb, alloy it is amorphous It is improved into ability, but saturation magnetization decreases.2013, Geng of Dalian University of Technology et al. reported one Kind critical dimension reaches the Fe of 1.5mm73.5B17.6Si5.9Zr3.0Block amorphous alloy, its saturation magnetization are 1.4T.Obviously, Fe-B-Si-Zr systems non-crystaline amorphous metal can generally show preferable amorphous formation ability and higher saturation magnetization.But It is while it can be found that high alloying component its Fe content (atomic fraction) of amorphous alloy forming ability is below 75%, obtains The saturation magnetization of non-crystaline amorphous metal be respectively less than 1.5T.
The comprehensive amorphous soft-magnetic alloy component developed in recent years, it can be seen that 15%- is typically contained in Fe-based amorphous alloy 25% metalloid element is to ensure the amorphous formation ability of alloy, therefore magnetic atom content is substantially less than silicon steel, tool There is the inferior position that saturation magnetization is low.Therefore, in order to obtain the Fe-based amorphous alloy of saturation magnetization higher, it is necessary to appropriate sacrificial The amorphous formation ability of domestic animal alloy is to ensure the Fe contents of higher.
In the present invention, inventor ensure that non-on the basis of Fe-B-Si systems non-crystaline amorphous metal by following two measures Peritectic alloy had not only had high saturation and magnetic intensity but also had improved the amorphous formation ability of alloy at the same time：First, in order to make to contain in alloy Sufficiently high magnetic atom, alloy of the present invention improve the content of Fe to more than 80% (atomic fraction), second, in Fe-B-Si systems Alloy is added on the basis of amorphous formation ability element Zr, further adds metalloid element P.P is metalloid element, it and Fe There is larger negative heat of mixing, its atomic radius is bigger than Fe, and according to the principle of Inoue amorphous formation abilities, the addition of P can carry High amorphous formation ability, but since its thick atom radius, the mechanism of action of P will differ from traditional Fe-B-Si systems non-crystaline amorphous metal In Si and B.Because P prices are lower than B, cost of alloy can be reduced, and in preparation process, can be with since the fusing point of P is low Energy loss during reduction alloy melting.Make the content of Fe increase to improve magnetic induction intensity, Makino et al. is in Fe- P is added in Si-B alloys, studies into and is grouped into Fe76(SixByPz)24Alloy, wherein Fe76(Si0.375B0.416P0.208)24Close The saturation induction density of gold is 1.51T, and higher than the Fe based alloys being previously reported by, its coercivity is 0.8A/m.It is above-mentioned summarizing On the basis of research work, present invention obtains the Fe-B-Si-P-Zr systems amorphous soft-magnetic alloy body with high saturation and magnetic intensity System.
The content of the invention
Present disclosure is to have developed a kind of Fe-B-Si-P-Zr systems amorphous nano with high saturation and magnetic intensity Brilliant magnetically soft alloy.The cost of alloy is cheap, has preferable amorphous formation ability and high saturation and magnetic intensity.The Fe- of the present invention B-Si-P-Zr amorphous nanos peritectic alloy has a good application prospect in soft magnetic materials field.
The Fe-B-Si-P-Zr systems amorphous nano peritectic alloy of the present invention, it is characterised in that chemical composition expresses formula and is FeaBbSicPdZre, composition characteristics are：80≤a≤85,5≤b≤15,1≤c≤11,0.5≤d≤5,0.1≤e≤3, a+b+c+ D+e=100.
In above-mentioned alloy, its component can further be optimized to the alloy of the low Si of high B, its chemical composition expression formula is FeaBbSicPdZre, composition characteristics are：80≤a≤82,11≤b≤13,1≤c≤4,0.5≤d≤3,0.1≤e≤1.5.
Alloying component of the present invention can further be optimized to the alloy of low B high Si, its chemical composition expression formula is FeaBbSicPdZre, composition characteristics are：80≤a≤82,3≤b≤6,10≤c≤12,0.5≤d≤3,0.1≤e≤1.5.
In the alloy group of the low Si of high B, above-mentioned alloy can further optimize, and obtain a kind of chemical composition expression formula and be Fe80B13Si3P3Zr1, the critical dimension of the non-crystaline amorphous metal is 40 μm, saturation magnetization 1.68T.
In the alloy group of the low Si of high B, above-mentioned alloy can further optimize, and obtain a kind of chemical composition expression formula and be Fe81B13Si2P3Zr1, the critical dimension of the non-crystaline amorphous metal is 35 μm, saturation magnetization 1.66T.
In the alloy group of low B high Si, above-mentioned alloy can further optimize, and obtain a kind of chemical composition expression formula and be Fe80B5Si11P3Zr1Non-crystaline amorphous metal, the critical dimension of the non-crystaline amorphous metal is 35 μm, saturation magnetization 1.64T.
In the alloy group of low B high Si, above-mentioned alloy can further optimize, and obtain a kind of chemical composition expression formula and be Fe81B5Si10P3Zr1Amorphous nano peritectic alloy, the saturation magnetization of the non-crystaline amorphous metal is 1.64T.
The Fe base noncrystal alloys of the present invention have high Fe contents, and Fe atomic fractions are not less than 80%, and high Fe contents cause this Alloy has high saturation magnetization, and the saturation magnetization of alloy is up to 1.68T, more than the water of business amorphous soft-magnetic alloy It is flat.Meanwhile the addition of a small amount of amorphous formation element Zr and P ensure that the alloy of the present invention has higher amorphous formation ability, The preparation process window of the alloy system is expanded significantly.The amorphous nano peritectic alloy is suitable for power industry transformer core, electricity Electrical automobile, the motor of unmanned plane and automatic field, mutual inductor etc., it may also be used for electromagnetic shielding material of communication field etc..
Brief description of the drawings
Fig. 1 is Fe of the present invention80B16-xSixP3Zr1The X ray diffracting spectrum of (x=1~11) alloy thin band.
Fig. 2 is Fe of the present invention81B15-xSixP3Zr1(x=1,2,4,6,8,10) X ray diffracting spectrum of alloy thin band.
Fig. 3 is Fe of the present invention82B14-xSixP3Zr1The X ray diffracting spectrum of (x=1~10) alloy thin band.
Fig. 4 is Fe of the present invention80B16-xSixP3Zr1The differential scanning calorimetric curve of (x=1~11) alloy thin band.
Fig. 5 is Fe of the present invention81B15-xSixP3Zr1The differential scanning calorimetric curve of (x=1~10) alloy thin band.
Fig. 6 is Fe of the present invention82B14-xSixP3Zr1The differential scanning calorimetric curve of (x=1~10) alloy thin band.
Fig. 7 is Fe of the present invention80B16-xSixP3Zr1(x=1,2,3,5,7,9,11) hysteresis curve of alloy thin band.
Fig. 8 is Fe of the present invention81B15-xSixP3Zr1(x=1,2,4,6,8,10) hysteresis curve of alloy thin band.
Fig. 9 is Fe of the present invention82B14-xSixP3Zr1The hysteresis curve of (x=1~10) alloy thin band.
Table 1 is the high saturation magnetization intensity Fe-based alloy amorphous Forming ability of the present invention and saturation magnetization (Bs)
Embodiment
It is specific in terms of alloy is prepared with alloy property two below to introduce the present invention.
1. prepared by amorphous nano-crystalline alloy strip steel rolled stock
The detailed process for preparing amorphous alloy strips is as follows：
(1) dispensing.Required pure iron (purity is not less than 99.8%), silicon (purity is not less than 99.5%), work are chosen first Industry ferro-boron (impurity content is less than 0.7%), ferrophosphorus (impurity content is less than 0.9%) and metal zirconium (purity is not less than 99.8%), Then raw material are cleaned with alcohol, treat raw material to remove the oxide skin of material surface by mechanical grinding before dispensing Fully matched after drying using high-precision electronic analytical balance according to design of alloy and carry out dispensing.
(2) Fe-Zr foundry alloys melting.Pure iron and metal zirconium are put into the copper crucible melting pond of vacuum arc furnace ignition, placed When should be smaller by density, raw material that are volatile or splashing are placed on copper crucible bottom during melting.After closed furnace body, use successively Mechanical pump and molecular pump are evacuated to 5 × 10-3Below Pa, it is (3~6) × 10 to pour vacuum in appropriate high-purity argon gas to stove4Pa, More argon gas should be suitably poured when containing volatile constituent element.Before molten alloy raw material, the high-purity Ti ingot first in smelting furnace To absorb oxygen remaining in stove, melting then is carried out to alloy raw material again.To ensure that master alloy ingot component is uniform, each melting After the completion of need to be overturn alloy pig to carry out next melting with stirring shovel, at least melt back more than 3 times of each alloy pig.Melting During plus electromagnetic agitation to alloy carry out melt back.Alloy pig after melting needs to be weighed, to ensure alloy molten Do not occur substantially to volatilize or splash loss during refining.
(3) band is sprayed.Fe-B-Si-P-Zr amorphous nano-crystalline alloy thin bands are made using amorphous alloy, that is, utilize high speed argon The alloy liquid melted in quartz ampoule is sprayed onto from the aperture of the mouth of pipe on high-speed rotating copper roller to obtain non-crystaline amorphous metal, copper by gas Roller roller speed is set as 35m/s, and the amorphous thin ribbon thickness of preparation is 30~50 μm, and width is 1~10mm.
2nd, the performance of non-crystaline amorphous metal
1) X-ray diffraction (XRD) is tested
Crystal species analysis is carried out to sample using X-ray diffractometer, sample uses Cu target X-ray diffraction device to test.Fig. 1 For Fe of the present invention80B16-xSixP3Zr1The XRD curves of (x=1~11) alloy thin band.It can be seen that from XRD curves when Si is 1% When~7%, the diffracting spectrum of alloy is a diffusion peak, and without any sharp crystallization peak, it is amorphous knot to show the strip Structure；When Si contents are more than 8%, there is obvious sharp crystallization peak, the amorphous formation ability of alloy reduces.So appropriate control Si contents processed can guarantee that the amorphous formation ability that alloy has had.
Fig. 2 is Fe of the present invention81B15-xSixP3Zr1(x=1,2,4,6,8,10) the XRD curves of strip.As it can be seen that Si contents exist When 1%~6%, alloy shows as non crystalline structure, occurs obvious crystallization peak more than 8%.Fig. 3 is Fe of the present invention82B14-xSixP3Zr1 The XRD curves of (x=1~10) strip.Only Si contents are can be seen that at 2% from XRD curves, and alloy does not occur obvious Crystallization peak, all there is obvious crystallization peak in remaining.
2) means of differential scanning calorimetry (DSC) is analyzed
Using differential scanning calorimeter to non-crystaline amorphous metal sample carry out Thermodynamic Analysis, heating rate 20K/min, Temperature elevating range is 300-1600K.Fig. 4-6 is Fe of the present invention80B16-xSixP3Zr1(x=1~11), Fe81B15-xSixP3Zr1(x=1 ~10) and Fe82B14-xSixP3Zr1The DSC curve of (x=1~10) alloy thin band.The crystallization temperature of alloy can be determined from figure Degree, the quantity at crystallization peak and peak-to-peak temperature difference, so that it is determined that go out the nano-crystallization heat treatment temperature of alloy, each alloy it is initial Crystallization temperature is included in table one.It can be seen from the figure that between the crystallization temperature of alloy and the amorphous formation ability of alloy not There is direct contact, but analysis is found, for the alloy system that Fe contents are 80% and 81%, when Si contents are low, it is brilliant Change peak and there was only a main peak, remaining equal unobvious.Then occur two obvious crystallization peaks when Si contents are high, two peaks it Between be clearly separated, this just for nano-crystallization processing create advantage.It also found from DSC figures, it is listed in present example Alloy, be cocrystallizing type alloy, but deviate eutectic composition to some extent.
3) soft magnet performance is tested
Use rotation method of quenching that alloy is prepared into thickness for 20-40 microns, width is the amorphous nano-crystalline strip of 1.5-2mm, Using the saturation magnetization of vibrating specimen magnetometer (VSM) beta alloy, using DC B-H hysteresiscope beta alloys Coercivity.
Fig. 7-9 is Fe of the present invention80B16-xSixP3Zr1(x=1~11), Fe81B15-xSixP3Zr1(x=1~10) and Fe82B14-xSixP3Zr1(x=1~10) alloy hysteresis curve.By constituent adjustment, with the change of Fe, Si, B content, saturation Also there occurs different changes for magnetization value.In low Si content alloys, Fe80Si3B13P3Zr1And Fe81B13Si2P3Zr1Alloy Saturation magnetization has respectively reached 1.68T and 1.66T, and in high Si content alloy, Fe80B5Si11P3Zr1With Fe81B5Si10P3Zr1The saturation magnetization of alloy has reached 1.64T.The saturation magnetization of these alloys has exceeded traditional non- Brilliant magnetically soft alloy, has good future in engineering applications
The high saturation magnetization intensity Fe-based alloy amorphous Forming ability of table 1 and saturation magnetization (Bs)

Claims (7)

1. a kind of Fe-B-Si-P-Zr systems amorphous nano peritectic alloy, it is characterised in that chemical composition expression formula is FeaBbSicPdZre, Composition characteristics are：80≤a≤85,5≤b≤15,1≤c≤11,0.5≤d≤5,0.1≤e≤3, a+b+c+d+e=100.
A kind of 2. Fe-B-Si-P-Zr systems amorphous nano peritectic alloy according to claim 1, it is characterised in that composition characteristics For：80≤a≤82,11≤b≤13,1≤c≤4,0.5≤d≤3,0.1≤e≤1.5.
A kind of 3. Fe-B-Si-P-Zr systems amorphous nano peritectic alloy according to claim 1, it is characterised in that composition characteristics For：80≤a≤82,3≤b≤6,10≤c≤12,0.5≤d≤3,0.1≤e≤1.5.
A kind of 4. Fe-B-Si-P-Zr systems amorphous nano peritectic alloy according to claim 2, it is characterised in that chemical composition Expression formula is Fe80B13Si3P3Zr1, the critical dimension of the non-crystaline amorphous metal is 40 μm, saturation magnetization 1.68T.
A kind of 5. Fe-B-Si-P-Zr systems amorphous nano peritectic alloy according to claim 2, it is characterised in that chemical composition Expression formula is Fe81B13Si2P3Zr1, the critical dimension of the non-crystaline amorphous metal is 35 μm, saturation magnetization 1.66T.
A kind of 6. Fe-B-Si-P-Zr systems amorphous nano peritectic alloy according to claim 3, it is characterised in that chemical composition Expression formula is Fe80B5Si11P3Zr1, the critical dimension of the non-crystaline amorphous metal is 35 μm, saturation magnetization 1.64T.
A kind of 7. Fe-B-Si-P-Zr systems amorphous nano peritectic alloy according to claim 3, it is characterised in that chemical composition Expression formula is Fe81B5Si10P3Zr1, the saturation magnetization of the non-crystaline amorphous metal is 1.64T.
CN201711344036.1A 2017-12-15 2017-12-15 A kind of high saturation and magnetic intensity Fe B Si P Zr amorphous and nanocrystalline soft magnetic alloys Pending CN107910155A (en)

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CN111276311A (en) * 2020-02-18 2020-06-12 北京科技大学 Fe-B-P-C-Cu-N-Cr amorphous nanocrystalline magnetically soft alloy and preparation method thereof
CN114318178A (en) * 2021-12-29 2022-04-12 江西大有科技有限公司 Amorphous strip and preparation method thereof, and preparation method of amorphous motor iron core

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CN1787125A (en) * 2005-11-16 2006-06-14 安泰科技股份有限公司 Iron-base non-crystal alloy powder, magnetic powder core with excellent high frequency performance and preparation process thereof
CN102268617A (en) * 2011-08-19 2011-12-07 中国科学院宁波材料技术与工程研究所 Fe-based bulk amorphous alloy with high glass forming ability and excellent magnetic property and preparation method thereof
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111276311A (en) * 2020-02-18 2020-06-12 北京科技大学 Fe-B-P-C-Cu-N-Cr amorphous nanocrystalline magnetically soft alloy and preparation method thereof
CN114318178A (en) * 2021-12-29 2022-04-12 江西大有科技有限公司 Amorphous strip and preparation method thereof, and preparation method of amorphous motor iron core

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Application publication date: 20180413