CN108461246B - A kind of iron base amorphous magnetically-soft alloy and preparation method thereof - Google Patents

A kind of iron base amorphous magnetically-soft alloy and preparation method thereof Download PDF

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CN108461246B
CN108461246B CN201810122791.3A CN201810122791A CN108461246B CN 108461246 B CN108461246 B CN 108461246B CN 201810122791 A CN201810122791 A CN 201810122791A CN 108461246 B CN108461246 B CN 108461246B
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melting
purity
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master alloy
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CN108461246A (en
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许晓飞
李福山
董晓源
贾晓东
魏然
陈辰
王坦
董晓磊
李希涛
李成华
牛鹏飞
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Central Mountain Henan Amorphous New Material Ltd Co
Zhengzhou University
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Central Mountain Henan Amorphous New Material Ltd Co
Zhengzhou University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/147Alloys characterised by their composition
    • H01F1/153Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15341Preparation processes therefor
    • H01F1/1535Preparation processes therefor by powder metallurgy, e.g. spark erosion
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • C22C45/02Amorphous alloys with iron as the major constituent
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/147Alloys characterised by their composition
    • H01F1/153Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15308Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets

Abstract

The present invention relates to a kind of novel iron base amorphous magnetically-soft alloy and preparation method thereof, the expression formula of the alloy is FeaSibBcPdCueNbfA, b, c, d, e and f respectively indicate the atom percentage content of each corresponding component in expression formula, and meet the following conditions: a is 75~85, it be 7.5~14, d is 0.2~1.5 that b, which is 0.02~4, c, e is 0.1~1.0, f is 0~1.50, a+b+c+d+e+f=100, with high saturation induction density Bs, high Effective permeability μe, low coercivity Hc, excellent high frequency stability, and its good moldability, preparation process condition are simple, low production cost.

Description

A kind of iron base amorphous magnetically-soft alloy and preparation method thereof
Technical field
The invention belongs to amorphous alloy technical fields, and in particular to a kind of iron base amorphous magnetically-soft alloy, it is to pass through addition The mode of microelement develops a kind of high μe, low Hc, high BsSoft magnetic amorphous alloy.
Background technique
Non-crystalline material has the distinguishing feature of green energy conservation.Especially iron-based non-crystalline alloy, high, magnetic conductance that there are resistivity Rate is high, and loss is very low, its loss just corresponds to the 1/3~1/5 of orientation silicon steel, in addition compared with silicon steel, simple process, It without special processing, therefore is considered as the ideal core material for making power transformer.But compared with silicon steel, it is Fe-based amorphous For alloy there are still its shortcoming, i.e. fill factor and saturation induction density is relatively low.Such as crystalline state orientation silicon steel BsValue is about in 2T, and typical Fe-based amorphous alloy Fe78Si9Bl3BsValue is 1.56T.Furthermore when preparing magnetic element, such as Transformer core, motor rotor and magnetic switch etc., it is often desired to the saturation induction density of these devices is higher, because this Mean the reduction of plant bulk or the reduction of exciting power.For fill factor, general method is to improve strip surface Quality, such as the uniformity of surface smoothness and thickness of strip.But since amorphous band itself is only tens microns, promotion is filled out The potentiality for filling coefficient are limited.People more research and develop the amorphous soft-magnetic alloy with high magnetic saturation intensity.
Northeastern Japan university discloses a kind of FeSiBPCu system nano-crystal alloy, the alloy in patent CN102741437A Have the advantages that high saturation magnetic induction, typical effective component Fe83.3-84.3Si4B8P3-4Cu0.7Saturation induction density reach More than 1.8T.The introducing of P can play the role of that large scale primary phase is inhibited to be precipitated in the alloy, and during nano-crystallization Refine crystal grain.However the large-scale production of the alloy still remains three critical issues: 1) due in order to by P to crystal grain refinement Effect, high P content is used when design, keeps the alloy extremely sensitive to impurity, can not be using industry under existing smelting technology Raw material preparation.2) a large amount of additions of P are substantially reduced the inoxidizability of the alloy and corrosion resistance.3) the alloy heat treatment condition It is required that it is harsh, equally fail the requirement for overcoming high heating rate in heat treatment process.
A kind of FeSiBPCu that ingredient is close nanometer is disclosed in patent CN101834046A where Chinese Academy of Sciences's Ningbo material Peritectic alloy, the typical composition Fe of the alloy82.7Si3.95B8.4P4.3Cu0.6Thermal stability it is poor, heat treatment time is extremely short, it is clear that no Meet industrialized requirement, while the alloy similarly fails to overcome the problems, such as the raw material of industry.
Net is that new material (Pizhou City) Co., Ltd discloses a kind of Fe in patent CN105261435AaSibBcPdCueMef Iron-based amorphous and nanocrystalline soft magnetic alloy.
CN102741437A disclose FeSiBCuP series non-crystalline state alloy it is thermally treated after can be precipitated average-size 10~ The BCC iron phase of 25nm, makes its saturation induction density reach 1.8~1.9T.However it have passed through heat treatment, gesture during the preparation process Process must be increased, improve production cost.
Nanjing Aero-Space University discloses a kind of FeSiBPCu of high Si content in patent CN200910184483.4 The metalloid element content design of nanometer crystal alloy, the alloy is unreasonable, and amorphous formation ability is low, and conventional belt making process is difficult to Prepare completely amorphous alloy strip steel rolled stock.
In conclusion lacking the stable iron-based amorphous nanometer crystalline and its system with good manufacture practice of performance currently on the market Product, need based on the raw material of industry develop have both high magnetic flux density, high amorphous formation ability amorphous soft-magnetic alloy and its match Cover preparation method.
Summary of the invention
In view of the above-mentioned problems, the present invention develops a kind of new iron-based amorphous soft-magnetic alloy, there is high μe, low Hc, it is high Bs, and its good moldability, preparation process condition are simple, low production cost.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme:
The present invention provides a kind of iron base amorphous magnetically-soft alloy, the expression formula of the alloy is FeaSibBcPdCueNbf, institute It states a, b, c, d, e and f in expression formula and respectively indicates the atom percentage content of each corresponding component, and meet the following conditions: a 75 It is c be 7.5~14, d be 0.2~1.5, e be 0.1~1.0, f is 0~1.50, a+b+c+d+e+f that~85, b, which are 0.02~4, c, =100.
According to above-mentioned iron base amorphous magnetically-soft alloy, it be 2~3, c is 9.5~12.50, d 1.0 that a, which is 80~84, b, ~1.30, e are that 0.2~0.7, f is 0~1.0.
According to above-mentioned iron base amorphous magnetically-soft alloy, a is 83.33, b 2.35, and c 12.17, d 1.25, e are 0.70, f 0.20.
According to above-mentioned iron base amorphous magnetically-soft alloy, a is 83.08, b 2.34, and c 12.14, d 1.24, e are 0.70, f 0.50.
According to above-mentioned iron base amorphous magnetically-soft alloy, a is 82.66, b 2.33, and c 12.08, d 1.24, e are 0.69, f 1.00.
According to the preparation method of above-mentioned iron base amorphous magnetically-soft alloy, it the following steps are included:
(1) ingredient: choose purity be 99.99wt% Fe, purity be 99.99wt% Si, B content 17.40wt% FeB, P content be 24.98wt% FeP, purity be 99.99wt% Cu and purity be 99.99wt% Nb as raw material, Ingredient is carried out according to above-mentioned alloy expression formula atomic percentage content;
(2) master alloy melting: the above-mentioned raw material prepared is put into vacuum high-frequency induction melting furnace, suction to 2~3 ×10-3Pa, charged pressure are 0.04~0.05MPa argon gas protective gas;Adjusting 15~25A of electric current, smelting temperature 1000~ 1600 DEG C, furnace cooling obtains master alloy ingot after 5~10min of melting;
(3) preparation of band: under the conditions of Discontinuous manufacture, the master alloy ingot refuse of above-mentioned preparation is injected in On high-speed rotating copper wheel, it is prepared into iron-based amorphous thin ribbon, copper wheel linear resonance surface velocity is 20~30m/s.
Ingredient is carried out according to above-mentioned atom percentage content in above-mentioned steps (2), the placement order of raw material is according to raw material The high low setting of the fusing point of ingredient, low-melting steel alloy or alloying element are placed on upper layer, fusing point in material composition in material composition High steel alloy or alloying element is placed on lower layer.
It when preparing master alloy using high-purity raw material, is successively vacuumized with mechanical pump and diffusion pump, when vacuum degree reaches 2.0 ~3.0 × 10-3Then the argon gas that the purity that 0.04~0.05MPa is filled with after Pa is 99.999% starts to melt as protective gas Refine master alloy;When preparing master alloy using industrial pure material, in step (2) after ingredient, the total matter of raw material is added in ingredient The impurity absorption agent of amount 1~2%, impurity absorption agent are the B after drying2O3, the induction that is then placed in vacuum induction founding cavity It in coil, is successively vacuumized with mechanical pump and diffusion pump, when vacuum degree reaches 2.0~3.0 × 10-3It is filled with 0.04 after Pa~ The purity of 0.05MPa be 99.999% argon gas as protective gas, then start master alloy melting, using impurity absorption agent into Row cladding after the completion of melting, carries out 20min cladding to aluminium alloy, powers off.
Being put into bottom to be provided with the diameter in circular hole and hole by melted master alloy in above-mentioned steps (3) is 0.6mm~0.7mm Quartz ampoule in, be then placed in the induction coil in vacuum chamber and be fixed on above copper wheel at 0.5~1.2mm height, according to It is secondary to be evacuated to 5.0~6.0 × 10 using mechanical pump and diffusion pump-3The purity that 0.04~0.05MPa is filled with after Pa is 99.999% argon gas is then turned on the copper wheel and induction heating power for being connected with cooling water as protective gas, adjust electric current 2~ 900~1100 DEG C, 2~5min of smelting time of 10A, temperature sensor, then using high-frequency induction heating under the protection of argon gas Mode melts the master alloy in quartz ampoule uniformly, then in the case where quartz ampoule inside and outside differential pressure is 0.05MPa that melting is uniform female Alloy is ejected on high-speed rotating copper wheel, prepares band.
The atom percentage content of Fe ensure that amorphous formation ability in 75~85 (at%) ranges in alloy of the present invention With high Bs
Cu element can promote forming core, but its effect has significant difference with the difference of the microstructure in state band of quenching. In the present invention, design alternative low content of Cu, so that the amorphous formation ability of alloy not be greatly reduced.For few additive Cu element The effect of promotion forming core, the present invention, which mainly passes through, improves Fe content, introduces P and C element to realize, existing big in the outstanding band that makes to quench Highdensity cluster is measured as nucleation point, and does not cause the formation of coarse primary phase.
Nb then effectively improves crystalline active energy, and furthermore Nb interacts in phase boundary and B atom, forms atom Group hinders growing up for mono- Fe solid solution of α, advantageously forms nanocrystalline.
P element content appropriate is conducive to improve the amorphous formation ability of alloy in alloy, and P exists for FeSiBP alloy The effect that amorphous phase is formed is greater than Si and B.
The main function of Si element is to improve amorphous formation energy, properly increases alloy thermal stability and Curie temperature, Si member Element is too low, it is difficult to play its improve amorphous formation can effect, and too high levels then may be decreased the content of ferromagnetic element, To drop low-alloyed saturation induction density.Thus the preferred scope of Si is 2~3 (at%) in the present invention.
B and Fe member are known as biggish atomic radius difference, meet the requirement in three principles on well with large atomic radius difference, Be conducive to the decrystallized of Fe based alloy.B content can significantly improve the amorphous formation ability of alloy and steady more than 9 (at%) Qualitative, when content is lower than 5 (at%), the thermal stability of amorphous soft magnetic material is deteriorated, but when B content is higher than 18 (at%) When, being further added by for content is substantially decrystallized to alloy without too big contribution, so in the present invention B content preferred scope For 9.5~12.5 (at%).
Compared with prior art, the present invention obtain the utility model has the advantages that
1. the alloying component that the present invention designs has very strong compatibility to impurity, can be produced using the raw material of industry.
2. alloy system of the present invention do not need nano-crystallization annealing it is nanocrystalline to obtain, just obtained under amorphous state excellent Soft magnet performance.
3. alloy strip of the present invention contains element micro or without precious metal, is obtaining high performance while reducing into This, is conducive to industrialized application.
To sum up, iron base amorphous magnetically-soft alloy of the present invention has excellent comprehensive performance, strong with high saturation induction Spend Bs(up to 1.58T), high Effective permeability μe(up to 12717 in 1kHz) and high frequency stability, low coercivity Hc(minimum 3.432A/m) and good amorphous formation ability.
Detailed description of the invention
Fig. 1 is the XRD diagram of Examples 1 to 3 iron base amorphous magnetically-soft alloy;Abscissa is scanning angle in figure, and ordinate is Intensity;
Fig. 2 is that the DSC of Examples 1 to 3 iron base amorphous magnetically-soft alloy schemes;Abscissa is temperature in figure, and ordinate is heat release Amount;
Fig. 3 is the VSM figure under the different externally-applied magnetic fields of Examples 1 to 3 iron base amorphous magnetically-soft alloy;Abscissa is magnetic in figure Field intensity, ordinate are the intensity of magnetization;
Fig. 4 is the magnetic conductivity figure under different impressed frequencies of Examples 1 to 3 iron base amorphous magnetically-soft alloy;Horizontal seat in figure It is designated as frequency, ordinate is Effective permeability;
Fig. 5 is that the coercive under the different externally-applied magnetic fields of Examples 1 to 3 iron base amorphous magnetically-soft alloy is tried hard to;Abscissa in figure For magnetic field strength, ordinate is the intensity of magnetization;
X1 is embodiment 1 in figure, and X2 is embodiment 2, and X3 is embodiment 3.
Specific embodiment
The present invention is described further combined with specific embodiments below, but protection scope of the present invention is not limited to This.
Embodiment 1
The present invention provides a kind of iron base amorphous magnetically-soft alloy Fe83.33Si2.35B12.17P1.25Cu0.70Nb0.20(at%), remember Make X1, preparation method includes the following steps:
1) ingredient: choose purity be 99.99wt% Fe, purity be 99.99wt% Si, B content be 17.40wt%'s The Nb that the Cu and purity that FeP that FeB, P content are 24.98wt%, purity are 99.99wt% are 99.99wt% is pressed as raw material Ingredient is carried out according to above-mentioned alloy expression formula atomic percentage content, the placement order of raw material is high according to the fusing point of material composition Low setting, low-melting steel alloy or alloying element are placed on upper layer in material composition, in material composition the high steel alloy of fusing point or Alloying element is placed on lower layer;
2) master alloy melting: first putting above-mentioned prepared master alloy ingredient in silica crucible into, then adds in ingredient B after entering the drying of total mass of raw material 1%2O3, it is then placed in the induction coil in vacuum induction founding cavity, successively uses machine Tool pump and diffusion pump vacuumize, when vacuum degree reaches 3.0 × 10-3The purity that 0.04~0.05MPa is filled with after Pa is 99.999% Argon gas as protective gas;1600 DEG C of electric current 15A, smelting temperature beginning master alloy meltings are adjusted, B is utilized2O3It is coated, After the completion of melting, 20min cladding is carried out to aluminium alloy, powers off, the master alloy ingot that uniform ingredient is finally is prepared;
3) preparation of band: after melted master alloy is cut, taking 7g to be put into, bottom is provided with circular hole and the diameter in hole is In the quartz ampoule of 0.6mm, it is then placed in the induction coil in vacuum chamber and is fixed on above copper wheel at 0.8mm height, according to It is secondary to be evacuated to 5.0 × 10 using mechanical pump and diffusion pump-3The argon gas that the purity of 0.04MPa is 99.999% is filled with after Pa, so The copper wheel and induction heating power for being connected with cooling water are opened afterwards, adjust electric current 5A, 950 DEG C of temperature sensor, smelting time 3min connects Melt master alloy in quartz ampoule uniformly, then in stone English pipe inside and outside differential pressure is that the 0.05MPa lower uniform master alloy of melting is ejected on high-speed rotating copper wheel, copper wheel surface linear speed Degree is 25m/s, prepares strip X1.
Embodiment 2
The present invention provides a kind of new iron-based soft magnetic amorphous steel Fe83.08Si2.34B12.14P1.24Cu0.70Nb0.50
(at%), it is denoted as X2.Preparation method includes the following steps:
1) ingredient: choose purity be 99.99wt% Fe, purity be 99.99wt% Si, B content be 17.40wt%'s The Nb that the Cu and purity that FeP that FeB, P content are 24.98wt%, purity are 99.99wt% are 99.99wt% is pressed as raw material Ingredient is carried out according to above-mentioned alloy expression formula atomic percentage content, the placement order of raw material is high according to the fusing point of material composition Low setting, low-melting steel alloy or alloying element are placed on upper layer in material composition, in material composition the high steel alloy of fusing point or Alloying element is placed on lower layer;
2) master alloy melting: first putting above-mentioned prepared master alloy ingredient in silica crucible into, then adds in ingredient B after entering the drying of total mass of raw material 2%2O3, it is then placed in the induction coil in vacuum induction founding cavity, successively uses machine Tool pump and diffusion pump vacuumize, when vacuum degree reaches 2.0 × 10-3The argon gas that the purity of 0.05MPa is 99.999% is filled with after Pa As protective gas;1500 DEG C of electric current 25A, smelting temperature beginning master alloy meltings are adjusted, B is utilized2O3It is coated, melting is complete Cheng Hou carries out 20min cladding to aluminium alloy, powers off, the master alloy ingot that uniform ingredient is finally is prepared;
2) 3) preparation of band: after melted master alloy is cut, 8g is taken to be put into the diameter that bottom is provided with circular hole and hole In the quartz ampoule of 0.6mm, to be then placed in the induction coil in vacuum chamber and being fixed on above copper wheel at 1.2mm height, Successively 5.5 × 10 are evacuated to using mechanical pump and diffusion pump-3The argon gas that the purity of 0.05MPa is 99.999% is filled with after Pa, It is then turned on the copper wheel and induction heating power for being connected with cooling water, adjusts electric current 6A, 1100 DEG C of temperature sensor, smelting time 2min melts the master alloy in quartz ampoule uniformly, Then it is ejected on high-speed rotating copper wheel in the case where quartz ampoule inside and outside differential pressure is 0.05MPa uniform master alloy is melted, copper wheel Linear resonance surface velocity is 30m/s, prepares strip X2.
Embodiment 3
The present invention provides a kind of new iron-based soft magnetic amorphous steel Fe82.66Si2.33B12.08P1.24Cu0.69Nb1.0
(at%), it is denoted as X3.Preparation method includes the following steps:
1) ingredient: choose purity be 99.99wt% Fe, purity be 99.99wt% Si, B content be 17.40wt%'s The Nb that the Cu and purity that FeP that FeB, P content are 24.98wt%, purity are 99.99wt% are 99.99wt% is pressed as raw material Ingredient is carried out according to above-mentioned alloy expression formula atomic percentage content, the placement order of raw material is high according to the fusing point of material composition Low setting, low-melting steel alloy or alloying element are placed on upper layer in material composition, in material composition the high steel alloy of fusing point or Alloying element is placed on lower layer;
2) master alloy melting: first putting above-mentioned prepared master alloy ingredient in silica crucible into, then adds in ingredient B after entering the drying of total mass of raw material 2%2O3, it is then placed in the induction coil in vacuum induction founding cavity, successively uses machine Tool pump and diffusion pump vacuumize, when vacuum degree reaches 2.0 × 10-3The argon gas that the purity of 0.05MPa is 99.999% is filled with after Pa As protective gas;1000 DEG C of electric current 20A, smelting temperature beginning master alloy meltings are adjusted, B is utilized2O3It is coated, melting is complete Cheng Hou carries out 20min cladding to aluminium alloy, powers off, the master alloy ingot that uniform ingredient is finally is prepared;
3) preparation of band: after melted master alloy is cut, taking 8g to be put into, bottom is provided with circular hole and the diameter in hole is In the quartz ampoule of 0.6mm, it is then placed in the induction coil in vacuum chamber and is fixed on above copper wheel at 0.8mm height, according to It is secondary to be evacuated to 6.0 × 10 using mechanical pump and diffusion pump-3The argon gas that the purity of 0.05MPa is 99.999% is filled with after Pa, so It opens afterwards and is connected with the copper wheel and induction heating power of cooling water, adjust electric current 8A, 1000 DEG C of temperature sensor, smelting time 3min, Melt the master alloy in quartz ampoule uniformly, then exists Quartz ampoule inside and outside differential pressure is that the 0.05MPa lower uniform master alloy of melting is ejected on high-speed rotating copper wheel, copper wheel surface line Speed is 20~30m/s, prepares strip X3.
By obtained X1, X2, X3 iron-based non-crystalline magnetically soft alloy using X-ray diffractometer (X-raydiffraction, XRD;UItima IV diffractometer, Japan;Cu-K α) test sample structure;Using differential scanning calorimetry (NETZSCH STA type Differential scanning calorimetry, DSC) is surveyed with the heating rate of 20 DEG C/min The initial crystallization temperature T of random sample productx, the XRD and DSC curve of iron-based non-crystalline alloy can be obtained, see Fig. 1 and Fig. 2, specific T respectivelyx Value is shown in Table 1.
Gained iron-based non-crystalline magnetically soft alloy is packed into quartz ampoule, is vacuumized, vacuum degree is 2.0 × 10-3When Pa, Tube sealing processing is carried out, stress relief annealing, annealing temperature T are then carried out in batch-type furnacex- 100 DEG C, soaking time 10min is left Then vibrating specimen magnetometer (vibrating sample magnetometer, VSM are used in the right side;7410, Lake Shore, beauty State) measurement annealed sample Bs, with the H of DC hysteresis loops measuring instrument (BHS-40, Riken, Japan) measurement annealed samplec, use Impedance analyzer (4294A, Agilent, the U.S.) measures stress relief annealing sample under the extrinsic motivated magnetic field of different frequency μe, the results are shown in Table 1, Fig. 3, Fig. 4, Fig. 5
The comprehensive performance table of 1 iron base amorphous magnetically-soft alloy X1~X3 of table

Claims (1)

1. a kind of iron base amorphous magnetically-soft alloy, which is characterized in that the expression formula of the alloy is Fe83.08Si2.34B12.14P1.24 Cu0.70Nb0.50, the preparation method of the iron base amorphous magnetically-soft alloy, comprising the following steps:
(1) ingredient: choose purity be 99.99wt% Fe, purity be 99.99wt% Si, B content be 17.40wt% FeB, P The Nb that the Cu and purity that FeP that content is 24.98wt%, purity are 99.99wt% are 99.99wt% is as raw material, according to above-mentioned conjunction Golden expression formula atomic percentage content carries out ingredient;
(2) master alloy melting: the above-mentioned raw material prepared is put into vacuum high-frequency induction melting furnace, and suction to 2~3 × 10-3Pa, charged pressure are 0.04~0.05MPa argon gas protective gas;Adjust 15~25A of electric current, smelting temperature 1000~1600 DEG C, furnace cooling obtains master alloy ingot after 5~10min of melting;
(3) preparation of band: under the conditions of Discontinuous manufacture, the master alloy ingot refuse of above-mentioned preparation is sprayed after melting On high-speed rotating copper wheel, it is prepared into iron-based amorphous thin ribbon, copper wheel linear resonance surface velocity is 20~30m/s;
Ingredient is carried out according to above-mentioned atom percentage content in step (1), the placement order of raw material is according to the molten of material composition High low setting is put, low-melting steel alloy or alloying element are placed on upper layer in material composition, the high alloy of fusing point in material composition Steel or alloying element are placed on lower layer;
In step (2) after ingredient, the impurity absorption agent of total mass of raw material 1 ~ 2% is added in ingredient, it is molten to be then placed in vacuum induction It in induction coil in mold cavity body, is successively vacuumized with mechanical pump and diffusion pump, when vacuum degree reaches 2.0~3.0 × 10-3 Pa Then the argon gas that the purity for being filled with 0.04~0.05 MPa afterwards is 99.999% starts master alloy melting as protective gas, utilize Impurity absorption agent is coated, and after the completion of melting, is carried out 20min cladding to aluminium alloy, is powered off;
Being put into bottom to be provided with the diameter in circular hole and hole by melted master alloy in step (3) is 0.6 mm~0.7mm quartz Guan Zhong is then placed in the induction coil in vacuum chamber and is fixed on above copper wheel at 0.5~1.2 mm height, successively uses Mechanical pump and diffusion pump are filled with the argon that the purity of 0.04~0.05MPa is 99.999% after being evacuated to 5.0~6.0 × 10-3Pa Gas is then turned on the copper wheel and induction heating power for being connected with cooling water as protective gas, adjusts 2~10A of electric current, temperature sensor 900~1100 DEG C, 2~5min of smelting time is made in quartz ampoule by the way of high-frequency induction heating under the protection of argon gas Master alloy melts uniformly, then the uniform master alloy of melting under conditions of quartz ampoule inside and outside differential pressure is 0.04~0.05MPa It is ejected on high-speed rotating copper wheel, prepares band;
Impurity absorption agent is the B after drying in step (2)2O3
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