CN101509109B - FeNbBDy metallic glass magnetic materials and method of producing the same - Google Patents

FeNbBDy metallic glass magnetic materials and method of producing the same Download PDF

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CN101509109B
CN101509109B CN2009100963516A CN200910096351A CN101509109B CN 101509109 B CN101509109 B CN 101509109B CN 2009100963516 A CN2009100963516 A CN 2009100963516A CN 200910096351 A CN200910096351 A CN 200910096351A CN 101509109 B CN101509109 B CN 101509109B
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alloy
fenbbdy
magnetic material
metallic glass
glass magnetic
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CN101509109A (en
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严密
陶姗
马天宇
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Zhejiang University ZJU
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Abstract

The invention discloses a FeNbBDy serial metal glass magnetic material and a preparation method thereof. The metal glass alloy of the invention has the following chemical formula: (FeaNbbBc) 1-x Dyx, wherein, a is more than or equal to 65 and less than or equal to 75, b is more than or equal to 2 and less than or equal to 8, c is more than or equal to 20 and less than or equal to 25, x is more than or equal to 1 and less than or equal to 10, and a plus b plus c equals 100. The preparation method of the FeNbBDy metal glass magnetic material of the invention has the following steps: pure metal Fe, Nb and FeB alloy are mixed according to a general formula; FeaNbbBc is smelted into master alloy by induction melting; then a FeaNbbBc master alloy spindle is ground to small pieces; according to atomic ratio of (FeaNbbBc) 1-x Dyx, Dy metal is added; a bar-shaped alloy sample is obtained by putting the raw materials to a silica tube of an induction furnace for smelting and then carrying out direct spray casting; as a result, volatilization of rare earth element Dy can be reduced. The FeNbBDy metal glass magnetic material of the invention has wide supercooling liquid phase region. Moreover,the glass transition temperature and crystallization temperature thereof are relatively high, thus demonstrating high thermal stability and fine amorphous forming capacity of the alloy. Meanwhile, soft magnetic performance of the alloy is good, therefore, the metal glass magnetic material enjoys potential application prospect.

Description

FeNbBDy is metallic glass magnetic material and preparation method thereof
Technical field
The present invention relates to the metallic glass magnetic material field, particularly a kind of FeNbBDy is a metallic glass magnetic material.
Background technology
Natural material is pressed textural classification, roughly can be divided into two big classes: crystalline state and non-crystalline state.The chaotic arranging situation of non-crystaline amorphous metal atom is similar to glass, so be also referred to as metallic glass (Bulk Metal Glass).Because amorphous metal and alloy have unique long-range disordered structure, so it has physics, chemistry and the mechanical property of the uniqueness that is different from the crystalline state metal.As high intensity and fracture toughness property, superior corrosion resistance, excellent magnetism energy, can obtain magnetostriction coefficient high, plus or minus.Based on the good characteristic of non-crystaline amorphous metal, it has all obtained to use widely in field such as Aeronautics and Astronautics, information and electronics, precision optical machinery and chemical industry and industry, also significant in scientific research and application facet, so the research of non-crystaline amorphous metal becomes one of advanced subject of material and physical field.
Non-crystaline amorphous metal comes across 1934 as novel material, and silent (Kramer) obtains amorphous alloy film with the hydatogenesis method by the Germany scientist Cray.Real amorphous history be from nineteen sixty California Inst Tech USA professor P.Duwez invention prepare amorphous alloy (Au with rapid quenching technique 75Si 25) beginning, make the range extension of synthetic glass arrive metal system, but its critical cooling rate (Rc) must be 10 6K/s is above could to form amorphous, and higher rate of cooling makes non-crystaline amorphous metal to occur with the low-dimensional size and dimension, as thin ribbon shaped, thread or powder.Pond in 1969 and Maddin successfully prepare the band of the continuous non-crystaline amorphous metal with certain-length with the roll method, and this technology has been created condition for the scale operation non-crystaline amorphous metal.In the same year, Chen Heshou etc. adopt fast cold continuous casting roll method (speed of cooling＞10 5K/s) once made the amorphous thin ribbon that supplies experimental study, thick about 30 μ m, wide several millimeters, reach tens meters, for the scale operation of non-crystaline amorphous metal is laid a good foundation.Chen in 1974 etc. by quartz tube water quenching in conjunction with the method that suppresses heterogeneous nucleation 〉=10 3Prepared millimetre-sized non-crystaline amorphous metal under the speed of K/s.The generation of millimeter level non-crystaline amorphous metal is the important breakthrough of bulk-metallic glass research, but these millimeters level non-crystaline amorphous metal is confined to precious metals such as Pd, Pt, can't be widely used as engineering materials.
1988, the development work of block amorphous alloy obtained breakthrough.The Inoue of northeastern Japan university, people such as Zhang Tao are after accident has found to have the La-Al-Ni and La-Al-Cu amorphous alloys of glass forming ability, under lower rate of cooling, developed the Zr base successively by rational alloy designs and conventional castmethod, the Fe base, the Pd base, the Ti base, kind has the multicomponent system of strong amorphous formation ability surplus the Mg bases etc. ten, and formation ability, performance and the purposes of non-crystaline amorphous metal have been done a large amount of deep researchs, and the non-crystaline amorphous metal field has obtained developing swift and violently.The Fe base block amorphous alloy is because of its unique magnetic property, and strong amorphous formation ability receives publicity especially with relative cheap price, and the iron-base large-block amorphous alloy for preparing high glass forming ability and fine magnetic property will have practical significance and purposes widely.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, it is metallic glass magnetic material and preparation method thereof that a kind of FeNbBDy is provided.
FeNbBDy is that the chemical molecular formula of metallic glass magnetic material is (Fe aNb bB c) 1-xDy x, wherein 65≤a≤75,2≤b≤8,20≤c≤25,1≤x≤10, and a+b+c=100.
Described FeNbBDy is that the material purity of component Fe, Nb, B or the Dy of metallic glass magnetic material is 99.5%～99.9%.FeNbBDy is the wide supercooling liquid phase region that metallic glass magnetic material has 75K～94K.FeNbBDy is the saturation magnetization M of metallic glass magnetic material s=61.78～83.66emu/g, coercive force H Ci=4.10～5.12Oe.
FeNbBDy is that the preparation method of metallic glass magnetic material comprises following step:
Step 1: press atomic percent Fe aNb bB cWeighing purity is 99.6% Fe, and purity is 99.8% Nb and FeB alloy, with claim the target component raw material put into vacuum high-frequency induction smelting furnace, extracting vacuum to 4.0 * 10 -3Behind the Pa, charge into the high-purity argon gas protection, regulate electric current by little extremely big, induction heating melts until sample, and melt back 5-8 time is with the Fe that obtains to mix aNb bB cThe mother alloy spindle;
Step 2: the Fe of step 1 acquisition aNb bB cThe mother alloy spindle is broken into fritter Fe after removing zone of oxidation aNb bB cAlloy, and place the alcohol ultrasonic cleaning;
Step 3: the fritter Fe that obtains with step 2 aNb bB cAlloy and purity are that 99.9% Dy is by atomic percent (Fe aNb bB c) 1-xDy xWeighing, and be in the silica tube of 0.4mm～0.6mm with its pack into lower ending opening and aperture, extracting vacuum to 4.0 * 10 -3Behind the Pa; in the induction furnace cavity, charge into the high-purity argon gas protection; adopt the radio-frequency induction coil heating to make its fusing; the adjusting electric current is 15～35A; temperature sensor is 1100～1680 ℃; fused alloy liquid is sprayed and injects copper mold with high-purity argon gas behind melting 2～5min, and make (Fe with the copper mold cooling aNb bB c) 1-xDy xBlock amorphous alloy;
The step 4: (Fe that will obtain aNb bB c) 1-xDy xNon-crystaline amorphous metal after the Vacuum Package, is heated to 773～853K in box-annealing furnace in silica tube, temperature rise rate is 5～10 ℃/min, insulation 5～30min, furnace cooling.
Described FeNbBDy is that the minimum critical diameter of metallic glass non-crystaline amorphous metal is 2mm;
Cavity air pressure 0.05MPa, spraying pressure differs from 0.05～0.10MPa.
A kind of FeNbBDy of the present invention is that metallic glass magnetic material has following distinguishing feature: 1) glass forming ability is strong, and can make the minimum critical diameter is the non-crystaline amorphous metal bar of 2mm.Have the wide supercooling liquid phase region of 75K～94K, and have high glass transformation temperature and crystallization temperature.2) soft magnetic performance is good, saturation magnetization M s=61.78～83.66emu/g, coercive force H Ci=4.10～5.12Oe.In addition, metallic glass magnetic material of the present invention the preparation method simple, neither be very high to the purity requirement of raw material, material purity mostly is technical purity greatly.This FeNbBDy is that the superiority of metallic glass magnetic material means that it is a kind of functional materials with application prospect.
Description of drawings
Fig. 1 is the DSC graphic representation of the metallic glass of the embodiment of the invention 2 preparations, and heating rate is 20K/min.
Fig. 2 is the magnetic hysteresis loop according to the metallic glass alloys of embodiment 1,2,3,4 preparations.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
Embodiment 1: preparation (Fe 72Nb 4B 24) 96Dy 4Metallic glass magnetic material
Press atomic percent Fe 72Nb 4B 24Accurately weighing purity is 99.6% Fe, and purity is 99.8% Nb and FeB alloy, with claim the target component raw material put into vacuum high-frequency induction smelting furnace, extracting vacuum to 4.0 * 10 -3Behind the Pa, charge into the high-purity argon gas protection, regulate electric current by little extremely big, induction heating melts until sample.Melt back 6 times is with the Fe that obtains to mix 72Nb 4B 24The mother alloy spindle.The Fe that obtains 72Nb 4B 24The mother alloy spindle is broken into fritter after removing zone of oxidation, and places the alcohol ultrasonic cleaning.With the Fe that obtains 72Nb 4B 24Fritter alloy and purity are that 99.9% Dy is by (Fe 72Nb 4B 24) 96Dy 4The atomic percent weighing, and be in the silica tube of 0.5mm with its pack into lower ending opening and aperture, extracting vacuum to 3.8 * 10 -3Behind the Pa; in the induction furnace cavity, charge into the high-purity argon gas protection; adopt the radio-frequency induction coil heating to make its fusing; the adjusting electric current is 35A; temperature sensor is 1680 ℃; with high-purity argon gas fused alloy liquid being sprayed and injects internal diameter behind the melting 2min is the copper mold of 2mm/3mm, makes (the Fe of diameter 2-3mm 72Nb 4B 24) 96Dy 4The block amorphous alloy rod.X ray diffracting spectrum (XRD) can prove that (Φ=2mm) is an amorphous alloy completely to this alloy.Obtain the thermodynamical coordinate of this block sample with dsc.Can get prepared (Fe 72Nb 4B 24) 96Dy 4Metallic glass glass transformation temperature T g=860K and initial crystallization temperature T x=935K, thus the supercooling liquid phase region Δ T of this alloy obtained x=75K illustrates that this alloy amorphous formation ability is strong, the thermostability height.Fig. 2 is the magnetic hysteresis loop of this metallic glass, (Fe 72Nb 4B 24) 96Dy 4The saturation magnetization M of metallic glass s=83.66emu/g, coercive force H Ci=5.12Oe.
Embodiment 2: preparation (Fe 72Nb 4B 24) 95Dy 5Metallic glass magnetic material
Press atomic percent Fe 72Nb 4B 24Accurately weighing purity is 99.6% Fe, and purity is 99.8% Nb and FeB alloy, with claim the target component raw material put into vacuum high-frequency induction smelting furnace, extracting vacuum to 4.0 * 10 -3Behind the Pa, charge into the high-purity argon gas protection, regulate electric current by little extremely big, induction heating melts until sample.Melt back 8 times is with the Fe that obtains to mix 72Nb 4B 24The mother alloy spindle.The Fe that obtains 72Nb 4B 24The mother alloy spindle is broken into fritter after removing zone of oxidation, and places the alcohol ultrasonic cleaning.With the Fe that obtains 72Nb 4B 24Fritter alloy and purity are that 99.9% Dy is by (Fe 72Nb 4B 24) 95Dy 5The atomic percent weighing, and be in the silica tube of 0.4mm with its pack into lower ending opening and aperture, extracting vacuum to 3.6 * 10 -3Behind the Pa; in the induction furnace cavity, charge into the high-purity argon gas protection; adopt the radio-frequency induction coil heating to make its fusing; the adjusting electric current is 15A; temperature sensor is 1100 ℃; with high-purity argon gas fused alloy liquid being sprayed and injects internal diameter behind the melting 5min is the copper mold of 2mm/3mm/4mm, makes (the Fe of diameter 2-3mm 72Nb 4B 24) 95Dy 5The block amorphous alloy rod.X ray diffracting spectrum (XRD) can prove that alloy is an amorphous alloy completely.Obtain the thermodynamical coordinate of this block sample with dsc.Fig. 1 is the DSC graphic representation of this embodiment.Can get prepared (Fe 72Nb 4B 24) 95Dy 5Metallic glass glass transformation temperature T g=876K and initial crystallization temperature T x=960K, thus the supercooling liquid phase region Δ T of this alloy obtained x=84K illustrates that this alloy amorphous formation ability is strong, the thermostability height.Fig. 2 is the magnetic hysteresis loop of this metallic glass, (Fe 72Nb 4B 24) 95Dy 5The saturation magnetization M of metallic glass s=78.71emu/g, coercive force H Ci=4.87Oe.
Embodiment 3: preparation (Fe 72Nb 4B 24) 94Dy 6Metallic glass magnetic material
Press atomic percent Fe 72Nb 4B 24Accurately weighing purity is 99.6% Fe, and purity is 99.8% Nb and FeB alloy, with claim the target component raw material put into vacuum high-frequency induction smelting furnace, extracting vacuum to 4.0 * 10 -3Behind the Pa, charge into the high-purity argon gas protection, regulate electric current by little extremely big, induction heating melts until sample.Melt back 5 times is with the Fe that obtains to mix 72Nb 4B 24The mother alloy spindle.The Fe that obtains 72Nb 4B 24The mother alloy spindle is broken into fritter after removing zone of oxidation, and places the alcohol ultrasonic cleaning.With the Fe that obtains 72Nb 4B 24Fritter alloy and purity are that 99.9% Dy is by (Fe 72Nb 4B 24) 94Dy 6The atomic percent weighing, and be in the silica tube of 0.5mm with its pack into lower ending opening and aperture, extracting vacuum to 3.6 * 10 -3Behind the Pa; in the induction furnace cavity, charge into the high-purity argon gas protection; adopt the radio-frequency induction coil heating to make its fusing; the adjusting electric current is 22A; temperature sensor is 13600 ℃; with high-purity argon gas fused alloy liquid being sprayed and injects internal diameter behind the melting 3min is the copper mold of 2mm/3mm/4mm, makes (the Fe of diameter 2-4mm 72Nb 4B 24) 94Dy 6The block amorphous alloy rod.X ray diffracting spectrum (XRD) can prove that alloy is an amorphous alloy completely.Obtain the thermodynamical coordinate of this block sample with dsc.Can get prepared (Fe 72Nb 4B 24) 94Dy 6Metallic glass glass transformation temperature T g=879K and initial crystallization temperature T x=973K, thus the supercooling liquid phase region Δ T of this alloy obtained x=94K illustrates that this alloy amorphous formation ability is strong, the thermostability height.Fig. 2 is the magnetic hysteresis loop of this metallic glass, (Fe 72Nb 4B 24) 94Dy 6The saturation magnetization M of metallic glass s=66.95emu/g, coercive force H Ci=4.64Oe.
Embodiment 4: preparation (Fe 72Nb 4B 24) 93Dy 7Metallic glass magnetic material
Press atomic percent Fe 72Nb 4B 24Accurately weighing purity is 99.6% Fe, and purity is 99.8% Nb and FeB alloy, with claim the target component raw material put into vacuum high-frequency induction smelting furnace, extracting vacuum to 4.0 * 10 -3Behind the Pa, charge into the high-purity argon gas protection, regulate electric current by little extremely big, induction heating melts until sample.Melt back 6 times is with the Fe that obtains to mix 72Nb 4B 24The mother alloy spindle.The Fe that obtains 72Nb 4B 24The mother alloy spindle is broken into fritter after removing zone of oxidation, and places the alcohol ultrasonic cleaning.With the Fe that obtains 72Nb 4B 24Fritter alloy and purity are that 99.9% Dy is by (Fe 72Nb 4B 24) 93Dy 7The atomic percent weighing, and be in the silica tube of 0.6mm with its pack into lower ending opening and aperture, extracting vacuum to 3.6 * 10 -3Behind the Pa; in the induction furnace cavity, charge into the high-purity argon gas protection; adopt the radio-frequency induction coil heating to make its fusing; the adjusting electric current is 25A; temperature sensor is 1600 ℃; with high-purity argon gas fused alloy liquid being sprayed and injects internal diameter behind the melting 3min is the copper mold of 2mm/3mm, makes (the Fe of diameter 2-3mm 72Nb 4B 24) 93Dy 7The block amorphous alloy rod.X ray diffracting spectrum (XRD) can prove that alloy is an amorphous alloy completely.Obtain the thermodynamical coordinate of this block sample with dsc.Can get prepared (Fe 72Nb 4B 24) 93Dy 7Metallic glass glass transformation temperature T g=893K and initial crystallization temperature T x=969K, thus the supercooling liquid phase region Δ T of this alloy obtained x=76K illustrates that this alloy amorphous formation ability is strong, the thermostability height.Fig. 2 is the magnetic hysteresis loop of this metallic glass, (Fe 72Nb 4B 24) 93Dy 7The saturation magnetization M of metallic glass s=61.78emu/g, coercive force H Ci=4.10Oe.
Every performance of the iron based metallic glass that the foregoing description obtains is shown in table 1 summary.
Table 1 (Fe aNb bB c) 1-xDy xIt is the performance of metallic glass magnetic material
Figure G2009100963516D00051

Claims (7)

1. a FeNbBDy is a metallic glass magnetic material, it is characterized in that: its chemical molecular formula is (Fe aNb bB c) 100-xDy x, wherein 65≤a≤75,2≤b≤8,20≤c≤25,1≤x≤10, and a+b+c=100.
2. a kind of FeNbBDy according to claim 1 is a metallic glass magnetic material, it is characterized in that: described FeNbBDy is that the material purity of component Fe, Nb, B or the Dy of metallic glass magnetic material is 99.5%～99.9%.
3. a kind of FeNbBDy according to claim 1 is a metallic glass magnetic material, it is characterized in that: described FeNbBDy is the wide supercooling liquid phase region that metallic glass magnetic material has 75K～94K.
4. a kind of FeNbBDy according to claim 1 is a metallic glass magnetic material, it is characterized in that: described FeNbBDy is the saturation magnetization M of metallic glass magnetic material S=61.78～83.66emu/g, coercive force H Ci=4.10～5.12Oe.
5. preparation method that FeNbBDy as claimed in claim 1 is a metallic glass magnetic material is characterized in that comprising following step:
Step 1: press atomic percent Fe aNb bB cWeighing purity is 99.6% Fe, and purity is 99.8% Nb and FeB alloy, with claim the target component raw material put into vacuum high-frequency induction smelting furnace, extracting vacuum to 4.0 * 10 -3Behind the Pa, charge into the high-purity argon gas protection, regulate electric current by little extremely big, induction heating melts until sample, and melt back 5-8 time is with the Fe that obtains to mix aNb bB cThe mother alloy spindle;
Step 2: the Fe of step 1 acquisition aNb bB cThe mother alloy spindle is broken into fritter Fe after removing zone of oxidation aNb bB cAlloy, and place the alcohol ultrasonic cleaning;
Step 3: the fritter Fe that obtains with step 2 aNb bB cAlloy and purity are that 99.9% Dy is by atomic percent (Fe aNb bB c) 100-xDy xWeighing, and be in the silica tube of 0.4mm～0.6mm with its pack into lower ending opening and aperture, extracting vacuum to 4.0 * 10 -3Behind the Pa; in the induction furnace cavity, charge into the high-purity argon gas protection; adopt the radio-frequency induction coil heating to make its fusing; the adjusting electric current is 15～35A; temperature sensor is 1100～1680 ℃; fused alloy liquid is sprayed and injects copper mold with high-purity argon gas behind melting 2～5min, and make (Fe with the copper mold cooling aNb bB c) 100-xDy xBlock amorphous alloy;
The step 4: (Fe that will obtain aNb bB c) 100-xDy xNon-crystaline amorphous metal after the Vacuum Package, is heated to 773～853K in box-annealing furnace in silica tube, temperature rise rate is 5～10 ℃/min, insulation 5～30min, furnace cooling.
6. a kind of FeNbBDy according to claim 5 is the preparation method of metallic glass magnetic material, it is characterized in that: described FeNbBDy is that the minimum critical diameter of metallic glass non-crystaline amorphous metal is 2mm;
7. a kind of FeNbBDy according to claim 5 is the preparation method of metallic glass magnetic material, it is characterized in that: described cavity air pressure 0.05MPa, spraying pressure differs from 0.05～0.10MPa.
CN2009100963516A 2009-02-23 2009-02-23 FeNbBDy metallic glass magnetic materials and method of producing the same Expired - Fee Related CN101509109B (en)

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