CN106756643B - A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof - Google Patents
A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof Download PDFInfo
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- CN106756643B CN106756643B CN201611239483.6A CN201611239483A CN106756643B CN 106756643 B CN106756643 B CN 106756643B CN 201611239483 A CN201611239483 A CN 201611239483A CN 106756643 B CN106756643 B CN 106756643B
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- 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
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/00—Making ferrous alloys
- C22C33/003—Making ferrous alloys making amorphous alloys
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- 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
- H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
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Abstract
The present invention provides a kind of iron-based amorphous and nanocrystalline soft magnetic alloys, have general formula shown in Formulas I, FexSiyBzPnCumCwI；Wherein, 84.0≤x≤85.0,0≤y≤2,8.5≤z≤10.5,3≤n≤4,0.3≤m≤1,0≤w≤1, and x+y+z+n+m+w=100.The present invention is by being added specific element, it is aided with corresponding ratio, propose the novel Fe-based amorphous Nanocrystalline soft magnetic alloy with high saturated magnetic induction, the alloy has high saturated magnetic induction, the excellent soft magnet performance such as low-coercivity, and do not include expensive metallic element Nb, the cost of material greatly reduces.
Description
Technical field
The invention belongs to magnetically soft alloy technical field of function materials more particularly to a kind of iron-based amorphous and nanocrystalline soft magnetic alloys
And preparation method thereof.
Background technique
With being constantly progressive for society, due to computer network, high density recording technology, electric system and the micro- chinaware of high frequency
The development in the fields such as part and needs increasingly require various components used to have high-performance, high-quality, small-sized, light weight, this
Require that preparing the Metallic Functional Materials such as the magnetically soft alloy of these devices is continuously improved performance.Among these, amorphous soft-magnetic alloy is equal
By respective parent metal and it is nonmetallic form, the former is ferromagnetic element (iron, cobalt, nickel or their combination), they use
To generate magnetism；The latter is vitrifying element, and main function is the critical cooling rate for reducing Formation of Amorphous Alloy state, is easy to
Obtain amorphous state.Magnesium-yttrium-transition metal (zirconium, hafnium, niobium etc.) and rare earth metal are also easy to form amorphous alloy, energy with iron, cobalt, nickel
Enough substitute nonmetalloid.
The Fe-based amorphous alloy that developed since late 1960s and the later period eighties are again in Fe-based amorphous alloy
On the basis of develop Fe-based amorphous nanocrystalline alloy since, become in electric power and electronic communication industry magnetic elements used
The research hotspot of soft magnetic materials at present not only in material and process aspect, and all achieves huge progress in application aspect,
It is widely used in various power equipments and electronic device.
Fe-based amorphous/nano-crystal soft magnetic alloy has excellent soft magnet performance, such as high saturated magnetic induction, low coercive
The features such as power, high magnetic permeability, low-loss is the research hotspot in material and Condensed Matter Physics field always for decades.Moreover,
The preparation process of Fe-based amorphous/nano-crystal soft magnetic alloy is simple, low in cost, is widely used in transformer, inductor, biography
The fields such as sensor all have a good application prospect.Japanese Yoshizawa in 1988 et al. first discovery Fe-Si-B-Cu-Nb
Alloy system.Develop by 20 years of researches, main development becomes three substantially to current Fe-based amorphous/nanometer crystal alloy
System, i.e. Finemet (Fe73.5Si13.5B9Cu1Nb3) be alloy, Nanoperm (Fe-M-B, M=Zr, Hf, Nb etc.) be alloy and
HITPERM (Fe-Co-M-B, M=Zr, Hf, Nb etc.) is alloy.
Finemet alloy is wherein primarily now applied, with its preferable soft magnet performance and lower cost in many necks
Domain has obtained extensive popularization.But with the development and requirement in downstream application field, since its saturation induction density is lower
(only 1.25T or so), compared with the silicon steel of high saturated magnetic induction, under equal conditions application needs biggish volume, no
The demand for development of lightweight, miniaturization is adapted to, it is serious to limit its application；And since your gold it contains compared with silicon steel
Belong to Nb, also increase the cost of material, is unfavorable for the development of society.
Therefore, how to obtain one kind has higher saturation induction density, meets lightweight, the development of miniaturization is wanted
It asks, and the magnetically soft alloy material with lower production cost, it has also become the focus of many researcher's extensive concerns of industry.
Therefore, it is full to have gone out the height for having one kind of excellent soft magnet performance novel by simple process preparation for this process exploitation
With magnetic induction intensity it is Fe-based amorphous/Nanoalloy.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that provide a kind of iron-based amorphous and nanocrystalline soft magnetic alloy and its
Preparation method.Iron-based amorphous and nanocrystalline soft magnetic alloy prepared by the present invention has higher saturation induction density, and is free of
Noble metal Nb, reduces cost of material, in addition, preparation process is simple, is suitable for scale industrial production.
The present invention provides a kind of iron-based amorphous and nanocrystalline soft magnetic alloys, have general formula shown in Formulas I:
FexSiyBzPnCumCwI；
Wherein, 84.0≤x≤85.0,0≤y≤2,8.5≤z≤10.5,3≤n≤4,0.3≤m≤1,0≤w≤1, and x
+ y+z+n+m+w=100.
Preferably, 84.2≤x≤84.7；
0≤y≤1.5；
3.5≤n≤4；
0.5≤m≤0.7；
0≤w≤0.5.
Preferably, 9≤z≤10.5；
0≤w≤0.3.
The present invention provides a kind of preparation methods of iron-based amorphous and nanocrystalline soft magnetic alloy, comprising the following steps:
A after iron, silicon, boron source, ferrophosphorus, copper and carbon iron) are carried out melting, alloy pig is obtained；
The boron source includes boron and/or ferro-boron；
B it carries out getting rid of band after) being crushed the alloy pig that above-mentioned steps obtain, obtains amorphous alloy strip；
C) under conditions of vacuum or protective atmosphere, after the amorphous alloy strip that above-mentioned steps are obtained is heat-treated,
Obtain iron-based amorphous and nanocrystalline soft magnetic alloy.
Preferably, the temperature of the melting is 1100~1350 DEG C；The time of the melting is 1~5min；
The melting is multiple melting；Described is repeatedly more than or equal to 3 times.
Preferably, the step of melting specifically:
First ferrophosphorus is put into smelting apparatus, then iron, silicon, boron source, copper and carbon iron are put into smelting apparatus and carry out melting.
Preferably, the band that gets rid of is that single roller chilling gets rid of band；
The chilling roller linear velocity for getting rid of band is 45~55m/s.
Preferably, the width of the amorphous alloy strip is 1~2mm；
The amorphous alloy strip with a thickness of 18~35 μm.
Preferably, the temperature of the heat treatment is 430~450 DEG C；
The time of the heat treatment is 10~60min；
The heating rate of the heat treatment is 10~20 DEG C/min.
It preferably, further include cleaning step after the alloy pig is broken；
The cleaning agent of the cleaning includes ethyl alcohol and/or acetone.
The present invention provides a kind of iron-based amorphous and nanocrystalline soft magnetic alloys, have general formula shown in Formulas I,
FexSiyBzPnCumCwI；Wherein, 84.0≤x≤85.0,0≤y≤2,8.5≤z≤10.5,3≤n≤4,0.3≤m≤1,0≤
W≤1, and x+y+z+n+m+w=100.Compared with prior art, the present invention is directed to existing Finemet alloy, saturation induction
Intensity is lower, and under equal conditions application needs biggish volume, does not adapt to the demand for development of lightweight, miniaturization, and
Containing noble metal Nb, the defects of increasing material cost.The present invention is aided with corresponding ratio, proposes by the way that specific element is added
The novel Fe-based amorphous Nanocrystalline soft magnetic alloy with high saturated magnetic induction, the alloy have high-saturation magnetic induction strong
Degree, the excellent soft magnet performance such as low-coercivity, and do not include expensive metallic element Nb, greatly reduce material at
This, in the existing iron-based amorphous and nanocrystalline soft magnetic alloy of effective solution, Yao Tigao saturation induction density need to improve iron and contain
Amount；Cost is reduced, then need few addition as far as possible or does not add noble metal Nb, but the increase of iron content consequently reduces noble metal
Content can all cause the Forming ability of nanocrystalline presoma (amorphous) to decline, and be also unfavorable for along with the control of cost
The preparation of amorphous band eventually leads to the contradiction of the deterioration of magnetic property.
The experimental results showed that amorphous/nanocrystalline magnetically soft alloy prepared by the present invention, iron content is high, but saturation magnetization
1.95T can be reached, coercivity can reach 28A/m, effectively improve the low saturation induction of existing amorphous/nanocrystalline magnetically soft alloy
The shortcomings that intensity.
Detailed description of the invention
Fig. 1 is the process flow diagram that the present invention prepares iron-based amorphous and nanocrystalline soft magnetic alloy；
Fig. 2 is the X-ray diffractogram of the amorphous thin ribbon of preparation of the embodiment of the present invention；
Fig. 3 is the magnetization curve figure of the Fe-based amorphous nanocrystalline alloy of preparation of the embodiment of the present invention；
Fig. 4 is the different change of the coercivity heat treatment temperature of the Fe-based amorphous nanocrystalline alloy of preparation of the embodiment of the present invention
Change curve.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are intended merely to further illustrate the features and advantages of the present invention, rather than to invention claim
Limitation.
All raw materials of the present invention, are not particularly limited its source, buying on the market or according to those skilled in the art
The preparation of conventional method known to member.
All raw materials of the present invention, are not particularly limited its purity, and present invention preferably employs analyze in pure or field to use
Conventional purity.
The present invention provides a kind of iron-based amorphous and nanocrystalline soft magnetic alloys, have general formula shown in Formulas I:
FexSiyBzPnCumCwI；
Wherein, 84.0≤x≤85.0,0≤y≤2,8.5≤z≤10.5,3≤n≤4,0.3≤m≤1,0≤w≤1, and x
+ y+z+n+m+w=100.
The concept of the general formula is not particularly limited in the present invention, and the concept with general formula well known to those skilled in the art is
Can, general formula can be regarded as, atomic ratio can also be regarded as.
X of the present invention meets the following conditions: 84.0≤x≤85.0, more preferably meets the following conditions: 84.1≤x≤
84.9, more preferably meet the following conditions: 84.2≤x≤84.8, more preferably meets the following conditions: 84.3≤x≤84.7, most preferably
Meet the following conditions: 84.4≤x≤84.6.
Y of the present invention meets the following conditions: 0≤y≤2, more preferably meets the following conditions: 0≤y≤1.5, more preferably full
Sufficient the following conditions: 0.1≤y≤2 more preferably meet the following conditions: 0.5≤y≤1.5, most preferably meet the following conditions: 0.8≤y
≤1.2。
Z of the present invention meets the following conditions: 8.5≤z≤10.5, more preferably meets the following conditions: 8.7≤z≤10.3,
More preferably meet the following conditions: 9.0≤z≤10.0, most preferably meets the following conditions 9.3≤z≤9.8.
N of the present invention meets the following conditions: 3.5≤n≤4, more preferably meets the following conditions 3.6≤n≤3.9, optimal
Be full sufficient the following conditions: 3.7≤n≤3.8.
M of the present invention meets the following conditions: 0.5≤m≤0.7, more preferably meets the following conditions: 0.52≤m≤0.68,
More preferably meet the following conditions: 0.54≤m≤0.66, more preferably meet the following conditions: 0.56≤m≤0.64 most preferably meets
The following conditions: 0.58≤m≤0.62.
W of the present invention meets the following conditions: 0≤w≤1, more preferably meets the following conditions: 0≤w≤0.5, more preferably full
Sufficient the following conditions: 0≤w≤0.3 more preferably meets the following conditions: 0.1≤w≤0.4, most preferably meets the following conditions: 0.2≤w
≤0.3。
The present invention also provides a kind of preparation methods of iron-based amorphous and nanocrystalline soft magnetic alloy, comprising the following steps:
A after iron, silicon, boron source, ferrophosphorus, copper and carbon iron) are carried out melting, alloy pig is obtained；
The boron source includes boron and/or ferro-boron；
B it carries out getting rid of band after) being crushed the alloy pig that above-mentioned steps obtain, obtains amorphous alloy strip；
C) under conditions of vacuum or protective atmosphere, after the amorphous alloy strip that above-mentioned steps are obtained is heat-treated,
Obtain iron-based amorphous and nanocrystalline soft magnetic alloy.
After iron, silicon, boron source, ferrophosphorus, copper and carbon iron are carried out melting first by the present invention, alloy pig is obtained；The boron source packet
Include boron and/or ferro-boron.
The title and purity of above-mentioned raw materials is not particularly limited in the present invention, with conventional name well known to those skilled in the art
Claim and purity, those skilled in the art can be selected according to practical condition, product requirement and quality requirement and
Adjustment, the purity of raw material of the present invention are preferably greater than or equal to 99.0%, are more preferably greater than equal to 99.5%, are most preferably greater than
Equal to 99.9%.
The condition of the melting is not particularly limited in the present invention, is with melting condition well known to those skilled in the art
Can, those skilled in the art can select and adjust according to practical condition, product requirement and quality requirement, the present invention
The temperature of the melting is preferably 1100~1350 DEG C, more preferably 1150~1300 DEG C, most preferably 1200~1250 DEG C；Institute
The time for stating melting is preferably 1~5min, more preferably 2~4min, most preferably 3~4min.
The present invention is to improve the effect of melting, improves the alloy pig uniformity, the preferably multiple melting.It is described repeatedly excellent
It is selected as being more than or equal to 3 times, is more preferably higher than equal to 4 times, is most preferably more than or equal to 5 times.The present invention is to improve the effect of melting
The step of fruit improves the alloy pig uniformity, more prevents ferrophosphorus scaling loss, the melting is particularly preferred as:
First ferrophosphorus is put into smelting apparatus, then iron, silicon, boron source, copper and carbon iron are put into smelting apparatus and carry out melting.
The present invention is to improve the integrality and operability of technique, and it is also preferable to include cleanings to walk after the alloy pig is broken
Suddenly.The cleaning agent of the cleaning is not particularly limited in the present invention, routinely clear with alloy pig well known to those skilled in the art
Lotion, those skilled in the art can select and adjust according to practical condition, product requirement and quality requirement,
Cleaning agent of the present invention preferably includes ethyl alcohol and/or acetone, more preferably ethyl alcohol or acetone.
The present invention carries out getting rid of band after being crushed the alloy pig that above-mentioned steps obtain, and obtains amorphous alloy strip.
The broken condition is not particularly limited in the present invention, with alloy pig breaker bars well known to those skilled in the art
Part, those skilled in the art can select and adjust according to practical condition, product requirement and quality requirement.
The mode for getting rid of band is not particularly limited in the present invention, with preparation amorphous alloy well known to those skilled in the art
Get rid of band mode, those skilled in the art can select according to practical condition, product requirement and quality requirement
And adjustment, the band of the present invention that gets rid of is preferably that single roller chilling gets rid of band.The equipment of the present invention for getting rid of band is preferably that single roller chilling is got rid of
Band machine.
The design parameter for getting rid of band is not particularly limited in the present invention, prepares amorphous with well known to those skilled in the art
Alloy gets rid of band parameter, and those skilled in the art can carry out according to practical condition, product requirement and quality requirement
Selection and adjustment, the chilling roller linear velocity of the present invention for getting rid of band is preferably 45~55m/s, more preferably 47~53m/s, most preferably
For 49~51m/s.
Above-mentioned steps of the present invention have obtained amorphous alloy strip.The present invention does not limit the parameter of the amorphous alloy strip especially
System, with the parameter of conventional amorphous alloy strip well known to those skilled in the art, those skilled in the art can be according to reality
The condition of production, product requirement and quality requirement are selected and are adjusted, and the width of the amorphous alloy strip is preferably 1~2mm, more
Preferably 1.2~1.8mm, most preferably 1.4~1.6mm.The thickness of the amorphous alloy strip is preferably 18~35 μm, more preferably
It is 22~31 μm, most preferably 26~27 μm.
For the present invention finally under conditions of vacuum or protective atmosphere, the amorphous alloy strip that above-mentioned steps are obtained carries out heat
After processing, iron-based amorphous and nanocrystalline soft magnetic alloy is obtained.
The concept of the heat treatment is not particularly limited in the present invention, with amorphous alloy well known to those skilled in the art
Heat treatment, those skilled in the art can select and adjust according to practical condition, product requirement and quality requirement
Whole, heat treatment of the present invention preferably makes annealing treatment.
The temperature of the heat treatment is not particularly limited in the present invention, with amorphous alloy well known to those skilled in the art
Heat treatment temperature, those skilled in the art can select according to practical condition, product requirement and quality requirement
And adjustment, the temperature of heat treatment of the present invention are preferably 430~450 DEG C, more preferably 435~445 DEG C, most preferably 438
~442 DEG C.
The time of the heat treatment is not particularly limited in the present invention, with amorphous alloy well known to those skilled in the art
Heat treatment time, those skilled in the art can select according to practical condition, product requirement and quality requirement
And adjustment, the time of heat treatment of the present invention are preferably 10~60min, more preferably 20~50min, most preferably 30~
40min。
The heating rate of the heat treatment is not particularly limited in the present invention, with amorphous well known to those skilled in the art conjunction
The heat treatment heating rate of gold, those skilled in the art can be according to practical condition, product requirement and quality requirement
It being selected and is adjusted, the heating rate of heat treatment of the present invention is preferably 10~20 DEG C/min, more preferably 12~18 DEG C/
Min, most preferably 14~16 DEG C/min.
The present invention has obtained the double composite soft magnetic alloys of iron-based amorphous nanometer crystalline by above-mentioned steps, and the present invention is special by being added
Fixed element is aided with corresponding ratio, proposes the novel Fe-based amorphous nano soft magnetic with high saturated magnetic induction and closes
Gold, the alloy have high saturated magnetic induction, the excellent soft magnet performance such as low-coercivity, and do not include expensive metal member
Plain Nb, greatly reduce the cost of material, in the existing iron-based amorphous and nanocrystalline soft magnetic alloy of effective solution, Yao Tigao
Saturation induction density need to improve iron content；Cost is reduced, then need few addition as far as possible or does not add noble metal Nb, but iron contains
The increase of amount consequently reduces the content of noble metal, along with the control of cost, all nanocrystalline presoma can be caused (non-
It is brilliant) Forming ability decline, and be also unfavorable for the preparation of amorphous band, eventually lead to the contradiction of the deterioration of magnetic property.
The experimental results showed that amorphous/nanocrystalline magnetically soft alloy prepared by the present invention, iron content is high, but saturation magnetization
1.95T can be reached, coercivity can reach 28A/m, effectively improve the low saturation induction of existing amorphous/nanocrystalline magnetically soft alloy
The shortcomings that intensity.
In order to further illustrate the present invention, soft to a kind of iron-based amorphous nanometer crystalline provided by the invention with reference to embodiments
Magnetic alloy and preparation method thereof is described in detail, but it is to be understood that these embodiments are to be with technical solution of the present invention
Under the premise of implemented, the detailed implementation method and specific operation process are given, only for further illustrate it is of the invention
Feature and advantage, rather than limiting to the claimed invention, protection scope of the present invention are also not necessarily limited to following embodiments.
Embodiment 1
Fe84.7Si1.5B9P4Cu0.5C0.3
Fe-based amorphous nanocrystalline alloy, the ingredient constitutional chemistry formula of alloy are Fe84.7Si1.5B9P4Cu0.5C0.3。
Referring to Fig. 1, Fig. 1 is the process flow diagram that the present invention prepares iron-based amorphous and nanocrystalline soft magnetic alloy.
Preparation step:
(1) prepared by master alloy raw material: pressing Fe84.7Si1.5B9P4Cu0.5C0.3Atomic percent is converted to quality hundred by chemical formula
Point ratio, in proportion respectively weigh Fe (99.9%), FeB (17.6%) alloy, FeP (17%) alloy, FeC (2.25%) alloy,
Si (99.9%) block and Cu block.
(2) foundry alloy melting: the raw material prepared is put into vacuum arc melting furnace, is evacuated to 5 × 10 to furnace body-3Afterwards
It is filled with argon gas/nitrogen atmosphere protection and closes charging valve when air pressure in furnace is higher than atmospheric pressure 0.01Mpa.It is former to heat melting
Material continues melting 3 minutes, is subsequently cooled to solidify, repeat melting 3 times, obtain after quickly being overturn after raw material is completely melt
To the uniform alloy pig of ingredient.
(3) alloy pig cleans: alloy pig being broken for fritter alloy, and is put into the beaker equipped with ethyl alcohol or acetone and carries out
Cleaning.
(4) prepared by amorphous thin ribbon: will be fitted into the quartz ampoule of lower ending opening after the cleaning of fritter alloy, is subsequently placed in and gets rid of band and set
In standby induction coil, it is evacuated to 5 × 10-3Being filled with purity afterwards is 99.99% high-purity argon gas as protective gas, adjusts electricity
Stream makes alloy melting, during which controls temperature at 1250 DEG C, controls the time 2 minutes, when alloy melting and when there is white light, utilizes gas
Alloy under molten condition is ejected into the copper roller surface that revolving speed is 50m/s by pressure difference, and obtained width is about 1mm, and thickness is about 20 μ
The amorphous ribbon strip of m.
(5) structure detection is carried out to alloy strip steel rolled stock with X-ray diffractometer, so that it is determined that the amorphous formation ability of alloy.Ginseng
See that Fig. 2, Fig. 2 are the X-ray diffractogram of the amorphous thin ribbon of preparation of the embodiment of the present invention.As shown in Figure 2, complete amorphous material
About in 45 ° of diffraction maximums with widthization disperse, and in other ranges without obvious sharp crystallization peak.
(6) Crystallizing treatment: amorphous thin ribbon being put into heat-treatment furnace and is made annealing treatment, and is warming up to 440 DEG C with furnace, heat preservation
Strip is taken out after then cooling to room temperature with the furnace, is obtained Fe-based amorphous wherein being 20 DEG C/min with furnace heating rate by 10min
Nanometer crystal alloy.
The Fe-based amorphous nanocrystalline alloy prepared to the embodiment of the present invention 1 detects.
With magnetic detection equipment (vibrating specimen magnetometer VSM and soft magnetism DC test instrument) to the strip after annealing respectively into
Row saturation induction density (Ms) and coercivity (Hc) performance test.Gained performance parameter is as shown in the picture, wherein Bs=4 π ×
(ρ×Ms)×10-4(T)。
Referring to the magnetization curve figure for the Fe-based amorphous nanocrystalline alloy that Fig. 3, Fig. 3 are preparation of the embodiment of the present invention.Referring to figure
4, Fig. 4 is bent for the different variation of the coercivity heat treatment temperature of the Fe-based amorphous nanocrystalline alloy of preparation of the embodiment of the present invention
Line.
The result shows that iron-based amorphous and nanocrystalline soft magnetic alloy prepared by the embodiment of the present invention 1
Fe84.7Si1.5B9P4Cu0.5C0.3, saturation magnetization 1.95T, coercivity 28A/m.
Embodiment 2
Fe84.2Si2B9P4Cu0.5C0.3
Fe-based amorphous nanocrystalline alloy, the ingredient constitutional chemistry formula of alloy are Fe84.2Si2B9P4Cu0.5C0.3。
Preparation step:
(1) prepared by master alloy raw material: pressing Fe84.2Si2B9P4Cu0.5C0.3Atomic percent is converted to quality hundred by chemical formula
Point ratio, in proportion respectively weigh Fe (99.9%), FeB (17.6%) alloy, FeP (17%) alloy, FeC (2.25%) alloy,
Si (99.9%) block and Cu block.
(2) foundry alloy melting: the raw material prepared is put into vacuum arc melting furnace, is evacuated to 5 × 10 to furnace body-3Afterwards
It is filled with argon gas/nitrogen atmosphere protection and closes charging valve when air pressure in furnace is higher than atmospheric pressure 0.01Mpa.It is former to heat melting
Material continues melting 3 minutes, is subsequently cooled to solidify, repeat melting 3 times, obtain after quickly being overturn after raw material is completely melt
To the uniform alloy pig of ingredient.
(3) alloy pig cleans: alloy pig being broken for fritter alloy, and is put into the beaker equipped with ethyl alcohol or acetone and carries out
Cleaning.
(4) prepared by amorphous thin ribbon: will be fitted into the quartz ampoule of lower ending opening after the cleaning of fritter alloy, is subsequently placed in and gets rid of band and set
In standby induction coil, it is evacuated to 5 × 10-3Being filled with purity afterwards is 99.99% high-purity argon gas as protective gas, adjusts electricity
Stream makes alloy melting, during which controls temperature at 1250 DEG C, controls the time 2 minutes, when alloy melting and when there is white light, utilizes gas
Alloy under molten condition is ejected into the copper roller surface that revolving speed is 50m/s by pressure difference, and obtained width is about 1.5mm, and thickness is about
34 μm of amorphous ribbon strip.
(5) structure detection is carried out to alloy strip steel rolled stock with X-ray diffractometer, so that it is determined that the amorphous formation ability of alloy.It is complete
Full amorphous material has the diffraction maximums of widthization disperse at 45 °, and in other ranges without obvious sharp crystallization peak.
(6) Crystallizing treatment: strip being put into heat-treatment furnace and is made annealing treatment, and is warming up to 450 DEG C with furnace, heat preservation
Strip is taken out after then cooling to room temperature with the furnace, is obtained Fe-based amorphous wherein being 20 DEG C/min with furnace heating rate by 10min
Nanometer crystal alloy.
The Fe-based amorphous nanocrystalline alloy prepared to the embodiment of the present invention 2 detects.
With magnetic detection equipment (vibrating specimen magnetometer VSM and soft magnetism DC test instrument) to the strip after annealing respectively into
Row saturation induction density (Ms) and coercivity (Hc) performance test.Gained performance parameter is as shown in the picture, wherein Bs=4 π ×
(ρ×Ms)×10-4(T)。
The result shows that iron-based amorphous and nanocrystalline soft magnetic alloy prepared by the embodiment of the present invention 2
Fe84.2Si2B9P4Cu0.5C0.3, saturation magnetization 1.81T, coercivity 17A/m.
Embodiment 3
Fe85Si1.4B9P4Cu0.5C0.1
Fe-based amorphous nanocrystalline alloy, the ingredient constitutional chemistry formula of alloy are Fe85Si1.4B9P4Cu0.5C0.1。
Preparation step:
(1) prepared by master alloy raw material: pressing Fe85Si1.4B9P4Cu0.5C0.1Atomic percent is converted to quality hundred by chemical formula
Point ratio, in proportion respectively weigh Fe (99.9%), FeB (17.6%) alloy, FeP (17%) alloy, FeC (2.25%) alloy,
Si (99.9%) block and Cu block.
(2) foundry alloy melting: the raw material prepared is put into vacuum arc melting furnace, is evacuated to 5 × 10 to furnace body-3Afterwards
It is filled with argon gas/nitrogen atmosphere protection and closes charging valve when air pressure in furnace is higher than atmospheric pressure 0.01Mpa.It is former to heat melting
Material continues melting 3 minutes, is subsequently cooled to solidify, repeat melting 3 times, obtain after quickly being overturn after raw material is completely melt
To the uniform alloy pig of ingredient.
(3) alloy pig cleans: alloy pig being broken for fritter alloy, and is put into the beaker equipped with ethyl alcohol or acetone and carries out
Cleaning.
(4) prepared by amorphous thin ribbon: will be fitted into the quartz ampoule of lower ending opening after the cleaning of fritter alloy, is subsequently placed in and gets rid of band and set
In standby induction coil, it is evacuated to 5 × 10-3Being filled with purity afterwards is 99.99% high-purity argon gas as protective gas, adjusts electricity
Stream makes alloy melting, during which controls temperature at 1250 DEG C, controls the time 2 minutes, when alloy melting and when there is white light, utilizes gas
Alloy under molten condition is ejected into the copper roller surface that revolving speed is 50m/s by pressure difference, and obtained width is about 1mm, and thickness is about 23 μ
The amorphous ribbon strip of m.
(5) structure detection is carried out to alloy strip steel rolled stock with X-ray diffractometer, so that it is determined that the amorphous formation ability of alloy.It is complete
Full amorphous material has the diffraction maximums of widthization disperse at 45 °, and in other ranges without obvious sharp crystallization peak.
(6) Crystallizing treatment: strip being put into heat-treatment furnace and is made annealing treatment, and is warming up to 440 DEG C with furnace, heat preservation
Strip is taken out after then cooling to room temperature with the furnace, is obtained Fe-based amorphous wherein being 20 DEG C/min with furnace heating rate by 10min
Nanometer crystal alloy.
The Fe-based amorphous nanocrystalline alloy prepared to the embodiment of the present invention 3 detects.
With magnetic detection equipment (vibrating specimen magnetometer VSM and soft magnetism DC test instrument) to the strip after annealing respectively into
Row saturation induction density (Ms) and coercivity (Hc) performance test.Gained performance parameter is as shown in the picture, wherein Bs=4 π ×
(ρ×Ms)×10-4(T)。
The result shows that iron-based amorphous and nanocrystalline soft magnetic alloy prepared by the embodiment of the present invention 3
Fe85Si1.4B9P4Cu0.5C0.1, saturation magnetization 1.94T, coercivity 25A/m.
A kind of iron-based amorphous and nanocrystalline soft magnetic alloy provided by the invention and preparation method thereof is carried out above detailed
It introduces, used herein a specific example illustrates the principle and implementation of the invention, the explanation of above embodiments
Be merely used to help understand method and its core concept of the invention, including best mode, and but also this field it is any
Technical staff can practice the present invention, including any device or system of manufacture and use, and implement the method for any combination.It answers
It, for those skilled in the art, without departing from the principle of the present invention, can also be to this when pointing out
Some improvement and modification can also be carried out for invention, and these improvements and modifications also fall within the scope of protection of the claims of the present invention.The present invention
The range of patent protection is defined by the claims, and may include those skilled in the art it is conceivable that other embodiments.
If these other embodiments, which have, is not different from the structural element of claim character express, or if they include with
Equivalent structural elements of the character express of claim without essence difference, are wanted then these other embodiments should also be included in right
In the range of asking.
Claims (10)
1. a kind of iron-based amorphous and nanocrystalline soft magnetic alloy, which is characterized in that have general formula shown in Formulas I:
FexSiyBzPnCumCwI ；
Wherein, 84.0≤x≤85.0,02,8.5≤z≤10.5,3≤n≤4,0.3≤m≤1,0 < y < w≤1 <, and x+y+z
+n+m+w=100 。
2. iron-based amorphous and nanocrystalline soft magnetic alloy according to claim 1, which is characterized in that 84.2≤x≤84.7；
Y≤1.5 0 <；
3.5≤n≤4；
0.5≤m≤0.7；
W≤0.5 0 <.
3. iron-based amorphous and nanocrystalline soft magnetic alloy described in any one according to claim 1 ~ 2, which is characterized in that the 9≤z
≤10.5；
W≤0.3 0 <.
4. a kind of preparation method of the iron-based amorphous and nanocrystalline soft magnetic alloy as described in claim 1 ~ 3 any one, feature
It is, comprising the following steps:
A after iron, silicon, boron source, ferrophosphorus, copper and carbon iron) are carried out melting, alloy pig is obtained；
The boron source includes boron and/or ferro-boron；
B it carries out getting rid of band after) being crushed the alloy pig that above-mentioned steps obtain, obtains amorphous alloy strip；
C it) under conditions of vacuum or protective atmosphere, after the amorphous alloy strip that above-mentioned steps are obtained is heat-treated, obtains
Iron-based amorphous and nanocrystalline soft magnetic alloy.
5. the preparation method according to claim 4, which is characterized in that the temperature of the melting is 1100 ~ 1350 DEG C；It is described
The time of melting is 1 ~ 5min；
The melting is multiple melting；Described is repeatedly more than or equal to 3 times.
6. the preparation method according to claim 4, which is characterized in that the step of the melting specifically:
First ferrophosphorus is put into smelting apparatus, then iron, silicon, boron source, copper and carbon iron are put into smelting apparatus and carry out melting.
7. the preparation method according to claim 4, which is characterized in that the band that gets rid of is that single roller chilling gets rid of band；
The chilling roller linear velocity for getting rid of band is 45 ~ 55m/s.
8. the preparation method according to claim 4, which is characterized in that the width of the amorphous alloy strip is 1 ~ 2mm；
The amorphous alloy strip with a thickness of 18 ~ 35 μm.
9. according to preparation method described in claim 4 ~ 8 any one, which is characterized in that the temperature of the heat treatment be 430 ~
450℃；
The time of the heat treatment is 10 ~ 60min；
The heating rate of the heat treatment is 10 ~ 20 DEG C/min.
10. the preparation method according to claim 4, which is characterized in that further include cleaning step after the alloy pig is broken；
The cleaning agent of the cleaning includes ethyl alcohol and/or acetone.
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| CN107354400A (en) * | 2017-07-14 | 2017-11-17 | 广东工业大学 | A kind of Fe-based amorphous alloy and preparation method thereof |
| CN107369513B (en) * | 2017-07-17 | 2019-04-09 | 广东工业大学 | A kind of iron-base soft magnetic alloy and preparation method thereof of low cost high saturation and magnetic intensity |
| CN107393673B (en) * | 2017-07-31 | 2020-02-11 | 东莞美壹磁电科技有限公司 | Iron-based amorphous nanocrystalline magnetically soft alloy and preparation method thereof |
| JP6338001B1 (en) * | 2017-09-15 | 2018-06-06 | Tdk株式会社 | Soft magnetic alloys and magnetic parts |
| CN108220776B (en) * | 2018-01-16 | 2020-08-07 | 广东工业大学 | Iron-based nanocrystalline alloy and preparation method thereof |
| CN109440021A (en) * | 2018-11-13 | 2019-03-08 | 广东工业大学 | A kind of iron-based amorphous and nanocrystalline soft magnetic alloy and its preparation method and application |
| CN109112434A (en) * | 2018-11-14 | 2019-01-01 | 广东工业大学 | A kind of new iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof |
| CN110295322A (en) * | 2019-07-19 | 2019-10-01 | 广东工业大学 | A kind of new iron-based magnetically soft alloy of high saturated magnetic induction and preparation method thereof |
| CN114250426B (en) * | 2021-12-22 | 2022-10-11 | 青岛云路先进材料技术股份有限公司 | Iron-based amorphous nanocrystalline alloy and preparation method thereof |
| CN114381673B (en) * | 2022-01-14 | 2023-01-20 | 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 |
| CN115386811B (en) * | 2022-09-26 | 2023-11-17 | 安徽工业大学芜湖技术创新研究院 | High-saturation magnetic induction intensity toughness iron-based amorphous nanocrystalline strip |
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