CN107393673A - 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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- H—ELECTRICITY
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- 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
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Abstract
The invention provides a kind of iron-based amorphous and nanocrystalline soft magnetic alloy, has the formula shown in Formulas I, FexSiyBzPwCumCnI；Wherein, 85.5≤x≤86.0,0≤y≤2,8≤z≤10,2≤w≤6,0.5≤m≤0.8,0≤n≤0.5, and x+y+z+n+m+w=100.The present invention is arranged in pairs or groups by specific element, propose the new Fe-based amorphous Nanocrystalline soft magnetic alloy with high saturated magnetic induction, Fe content more greatly improved, bring up to more than 85.5, adjust the ratio of each element again, the interaction between further Refining Elements so that saturation magnetization further improves, and coercivity declines to a great extent so that the overall performance of Fe-based amorphous Nanocrystalline soft magnetic alloy is obviously improved.The alloy has the excellent soft magnet performance such as higher saturation induction density, lower coercivity, and does not include expensive metallic element Nb, and 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 alloy
And preparation method thereof.
Background technology
With the continuous progress of society, due to computer network, high density recording technology, power system and the micro- chinaware of high frequency
The development in the fields such as part and needs, increasingly require that various components used possess 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 improves constantly 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 combinations thereof), for producing
Magnetisation；The latter is vitrifying element, and its main function is the critical cooling rate for reducing Formation of Amorphous Alloy state, readily available
Amorphous state.Magnesium-yttrium-transition metal (zirconium, hafnium, niobium etc.) and rare earth metal also easily form amorphous alloy with iron, cobalt, nickel, can replace
For nonmetalloid.The Fe-based amorphous alloy developed since late 1960s and the later stage eighties are again Fe-based amorphous
Since developing Fe-based amorphous nanocrystalline alloy on the basis of alloy, as in electric power and electronic communication industry magnetic elements
The study hotspot of soft magnetic materials used.
Fe-based amorphous/nano-crystal soft magnetic alloy has excellent soft magnet performance, such as high saturated magnetic induction, low coercive
Power, high magnetic permeability, the features such as low-loss, recent decades are the study hotspot in material and Condensed Matter Physics field all the time.Moreover,
The preparation technology of Fe-based amorphous/nano-crystal soft magnetic alloy is simple, cost is cheap, is widely used in transformer, inductor, biography
The fields such as sensor all have a good application prospect.Japanese Yoshizawa in 1988 et al. has found Fe-Si-B-Cu-Nb first
Alloy system.Develop by 20 years of researches, main development turns into 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 alloys are wherein primarily now applied, with its preferable soft magnet performance and relatively low cost in many necks
Domain has obtained extensive popularization.But with the development and requirement in downstream application field, because its saturation induction density is relatively low
(only 1.25T or so), compared with the silicon steel of high saturated magnetic induction, under equal conditions application needs larger volume, no
Lightweight, the demand for development of miniaturization are adapted to, serious limits its application.For Fe-based amorphous/nanometer crystal alloy, especially
It is Finemet (Fe73.5Si13.5B9Cu1Nb3) be alloy for, to improve saturation induction density, raising iron that need to be contains as far as possible
Amount, but because the increase of iron content consequently reduces the content of metalloid, the reduction of these metalloids will cause nanometer
The amorphous formation ability of brilliant presoma (amorphous) declines, even if so it is also extremely difficult that the content of iron, which improves 0.1%,.
2014, A.Inoue etc. existed《Journal of alloys and componds》On " Fe-based
amorphous soft magnetic alloys with high saturation magnetization and good
It is few in the magnetic report related higher than 82at.% that bending ductility " article middle fingers go out iron content, most of
The all middle iron content of Fe base noncrystal alloys is all in below 80at.%.2015, K.Takenaka existed《Journal of
magnetism and magnetic materials》On " Industrialization of nanocrystalline
Itd is proposed in Fe-Si-B-P-Cu alloys for high magnetic flux density cores " articles due in alloy
High Fe content is in 83~85at.%, result in relatively low amorphous formation ability, and the production of alloy receives serious limitation.
Thus, although the lifting of the content of iron suffered from for the amorphous formation ability and saturation induction density of alloy it is vital
Influence, but think that lifting iron content is extremely difficult.And contain noble metal Nb in alloy, and the cost of material is also increased, it is unfavorable
In the development of society, but the amorphous formation ability decline that Nb elements will also result in the alloy is added or not added less, these are not
Beneficial to preparing amorphous band, and cause the deterioration of magnetic property.
Therefore, how iron content is further improved, obtains a kind of coercive lower with higher saturation induction density
Power, meet lightweight, the demand for development of miniaturization, the magnetically soft alloy material with relatively low production cost, it has also become industry
The focus of many researcher's extensive concerns.
The content of the invention
In view of this, the technical problem to be solved in the present invention be to 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, have it is more high Fe contained, higher saturation induction is strong
Degree and lower coercivity, and noble metal Nb is free of, cost of material is reduced, in addition, preparation technology is simple, is suitable for scale
Chemical industry produces.
The invention provides a kind of iron-based amorphous and nanocrystalline soft magnetic alloy, has the formula shown in Formulas I：
FexSiyBzPwCumCnI；
Wherein, 85.5≤x≤86.0,0≤y≤2,8≤z≤10,2≤w≤6,0.5≤m≤0.8,0≤n≤0.5, and x
+ y+z+n+m+w=100.
Preferably, 85.6≤x≤85.8；
0≤y≤0.5；
8.5≤z≤9.5
3≤w≤4
0.6≤m≤0.7；
0.1≤n≤0.3.
Preferably, 85.7≤x≤85.8；
9≤z≤9.3
3.5≤w≤3.9
0.61≤m≤0.69；
0.2≤n≤0.3.
Present invention also offers a kind of preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy, comprise the following steps：
A) alloy pig will be obtained after iron, carbon iron, boron source and copper carries out melting, or by iron, carbon iron, copper and other raw materials
After carrying out melting, alloy pig is obtained；
Other described raw materials include ferrophosphorus and/or silicon；
The boron source includes boron and/or ferro-boron；
B carry out getting rid of band after) alloy pig for obtaining above-mentioned steps is broken, obtain amorphous alloy strip；
C) under conditions of vacuum or protective atmosphere, after 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 is specially：
First ferrophosphorus is put into smelting apparatus, then iron, boron source, copper and carbon iron are put into smelting apparatus and carry out melting；
Or first ferrophosphorus is put into smelting apparatus, then iron, silicon, boron source, copper and carbon iron are put into smelting apparatus and carried out
Melting.
Preferably, the band that gets rid of gets rid of band for single roller chilling；
The chilling roller linear velocity for getting rid of band is 30~50m/s.
Preferably, the width of the amorphous alloy strip is 1~2mm；
The thickness of the amorphous alloy strip is 18~35 μm.
Preferably, the temperature of the heat treatment is 410~450 DEG C；
The time of the heat treatment is 10~60min；
The heating rate of the heat treatment is 10~20 DEG C/min.
Preferably, cleaning step is also included after the alloy pig is broken；
The cleaning agent of the cleaning includes ethanol and/or acetone.
The invention provides a kind of iron-based amorphous and nanocrystalline soft magnetic alloy, has the formula shown in Formulas I,
FexSiyBzPwCumCnI；Wherein, 85.5≤x≤86.0,0≤y≤2,8≤z≤10,2≤w≤6,0.5≤m≤0.8,0≤n
≤ 0.5, and x+y+z+n+m+w=100.Compared with prior art, the present invention is directed to existing Finemet alloys, saturation magnetic strength
Answer intensity relatively low, under equal conditions application needs larger volume, it is impossible to lightweight, the demand for development of miniaturization are adapted to, with
And containing noble metal Nb, the defects of increasing material cost.The present invention is arranged in pairs or groups by specific element, it is proposed that new has height
The Fe-based amorphous Nanocrystalline soft magnetic alloy of saturation induction density, the alloy have higher saturation induction density, and lower rectifys
The excellent soft magnet performance such as stupid power, and do not include expensive metallic element Nb, the cost of material greatly reduces, effectively
Solve in existing iron-based amorphous and nanocrystalline soft magnetic alloy, to improve saturation induction density, iron content need to be improved；Reduce into
This, few to add or do not add noble metal Nb, but the increase of iron content, the reduction of bullion content can all cause nanocrystalline forerunner
The Forming ability of body (amorphous) declines, and is also unfavorable for the preparation of amorphous band, ultimately results in the contradiction of the deterioration of magnetic property.This
Invention technical scheme more for before, overcomes the technique direction and prejudice of Fe contents fine setting in the prior art, greatly improved
Fe content, creative brings up to more than 85.5, then adjusts the ratio of each element, the phase interaction between further Refining Elements
With so that saturation magnetization further improves, and can approach limiting value, and coercivity declines to a great extent so that Fe-based amorphous
The overall performance of Nanocrystalline soft magnetic alloy is obviously improved.
Test result indicates that amorphous/nanocrystalline magnetically soft alloy prepared by the present invention, iron content is high, but saturation magnetization
1.99T can be reached, approach 2.0T limiting value substantially, coercivity only has 6.5A/m, effectively improves existing amorphous/nanocrystalline
The shortcomings that magnetically soft alloy low saturation induction density high-coercive force.
Brief description of the drawings
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 amorphous thin ribbon prepared by the embodiment of the present invention；
Fig. 3 is the Fe-based amorphous nanometer that the amorphous thin ribbon of the embodiment of the present invention 1 obtains at a temperature of different annealings
Peritectic alloy X-ray diffractogram；
Fig. 4 is the magnetization curve figure of Fe-based amorphous nanocrystalline alloy prepared by the embodiment of the present invention；
Fig. 5 is the different change of the coercivity heat treatment temperature of Fe-based amorphous nanocrystalline alloy prepared by the embodiment of the present invention
Change curve；
Fig. 6 is the Fe-based amorphous nanometer that the amorphous thin ribbon of the embodiment of the present invention 2 obtains at a temperature of different annealings
Peritectic alloy X-ray diffractogram；
Fig. 7 is the Fe-based amorphous nanometer that the amorphous thin ribbon of the embodiment of the present invention 3 obtains at a temperature of different annealings
Peritectic alloy X-ray diffractogram；
Fig. 8 is the Fe-based amorphous nanometer that the amorphous thin ribbon of the embodiment of the present invention 4 obtains at a temperature of different annealings
Peritectic alloy X-ray diffractogram.
Embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described 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, its source is not particularly limited, commercially buying or according to people in the art
Known to member prepared by conventional method.
All raw materials of the present invention, its purity is not particularly limited, and present invention preferably employs analyze in pure or field to use
Conventional purity.
The invention provides a kind of iron-based amorphous and nanocrystalline soft magnetic alloy, has the formula shown in Formulas I：
FexSiyBzPwCumCnI；
Wherein, 85.5≤x≤86.0,0≤y≤2,8≤z≤10,2≤w≤6,0.5≤m≤0.8,0≤n≤0.5, and x
+ y+z+n+m+w=100.
The concept of the formula is not particularly limited the present invention, and the concept with formula well known to those skilled in the art is
Can, formula can be regarded as, atomic ratio can also be regarded as.
X of the present invention meets following condition：85.5≤x≤86.0, more preferably meet following condition：85.55≤x≤
85.95, more preferably meet following condition：85.6≤x≤85.9, more preferably meet following condition：85.65≤x≤85.85, more
It is preferred that meet following condition：85.6≤x≤85.8, most preferably meet following condition：85.7≤x≤85.8.
Y of the present invention meets following condition：0≤y≤2, more preferably meet following condition：0≤y≤1.5, it is more preferably full
It is enough lower condition：0.1≤y≤2, more preferably meet following condition：0.5≤y≤1.5, more preferably meet following condition：0.8≤y
≤ 1.2, most preferably meet following condition：0≤y≤0.5.
Z of the present invention meets following condition：8≤z≤10, more preferably meet following condition：8.2≤z≤9.8, it is more excellent
It is full and is enough lower condition：8.5≤z≤9.5, more preferably meet following condition 8.8≤z≤9.3, most preferably meet following condition 9
≤z≤9.3。
W of the present invention meets following condition：2≤w≤6, more preferably meet following condition：2.2≤w≤5.8, more preferably
Meet following condition：2.5≤w≤5.5, more preferably meet following condition：3≤w≤5, more preferably meet following condition：3.5≤w
≤ 4.5, more preferably meet following condition 3≤w≤4, most preferably meet following condition 3.5≤w≤3.9.
M of the present invention meets following condition：0.5≤m≤0.8, more preferably meet following condition：0.52≤m≤0.78,
More preferably meet following condition：0.55≤m≤0.75, more preferably meet following condition：0.6≤m≤0.7, more preferably meet with
Lower condition：0.61≤m≤0.69, more preferably meet following condition：0.63≤m≤0.67, most preferably meet following condition：0.6
≤m≤0.7。
N of the present invention meets following condition：0≤n≤0.5, more preferably meet following condition 0.05≤n≤0.45, more
It is preferred that meet following condition：0.1≤n≤0.4, more preferably meet following condition：0.15≤n≤0.35, more preferably meet following
Condition：0.1≤n≤0.3, most preferably meet following condition：0.2≤n≤0.3.
Present invention also offers a kind of preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy, comprise the following steps：
A) alloy pig will be obtained after iron, carbon iron, boron source and copper carries out melting, or by iron, carbon iron, copper and other raw materials
After carrying out melting, alloy pig is obtained；
Other described raw materials include ferrophosphorus and/or silicon；
The boron source includes boron and/or ferro-boron；
B carry out getting rid of band after) alloy pig for obtaining above-mentioned steps is broken, obtain amorphous alloy strip；
C) under conditions of vacuum or protective atmosphere, after amorphous alloy strip that above-mentioned steps are obtained is heat-treated,
Obtain iron-based amorphous and nanocrystalline soft magnetic alloy.
The present invention will obtain alloy pig after iron, carbon iron, boron source and copper carries out melting first, or by iron, carbon iron, copper and
After other raw materials carry out melting, alloy pig is obtained；
Other described raw materials include ferrophosphorus and/or silicon；The boron source includes boron and/or ferro-boron.
The title and purity of above-mentioned raw materials are not particularly limited 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%, more preferably greater than equal to 99.5%, are most preferably more than
Equal to 99.9%.
The present invention is when not containing Si and P in iron-based amorphous and nanocrystalline soft magnetic alloy component, then above-mentioned in above-mentioned steps
Step is after iron, carbon iron, boron source and copper are carried out into melting, to obtain alloy pig；When in iron-based amorphous and nanocrystalline soft magnetic alloy component
Containing Si, when not containing P, after iron, carbon iron, boron source, copper and silicon are carried out into melting, alloy pig is obtained；Work as iron-based amorphous nanometer crystalline
Si is not contained in magnetically soft alloy component, during containing P, after iron, carbon iron, boron source, copper and ferrophosphorus are carried out into melting, obtains alloy pig；
When both containing Si in iron-based amorphous and nanocrystalline soft magnetic alloy component, when containing P again, iron, carbon iron, boron source, copper, ferrophosphorus and silicon are entered
After row melting, alloy pig is obtained.
The condition of the melting is not particularly limited the present invention, is with melting condition well known to those skilled in the art
Can, those skilled in the art can be selected and adjusted 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 improves the alloy pig uniformity, described is preferably multiple melting to improve the effect of melting.More suboptimums
Elect as more than or equal to 3 times, more preferably higher than equal to 4 times, most preferably more than or equal to 5 times.The present invention is to improve the effect of melting
Fruit, the alloy pig uniformity is improved, more prevents ferrophosphorus scaling loss, be particularly preferred as the step of the melting：
First ferrophosphorus is put into smelting apparatus, then iron, boron source, copper and carbon iron are put into smelting apparatus and carry out melting；
It is identical by afore-mentioned, or be preferably：
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 preferably also includes cleaning step to improve the integrality and operability of technique after the alloy pig is broken
Suddenly.The cleaning agent of the cleaning is not particularly limited the present invention, routinely clear with alloy pig well known to those skilled in the art
Lotion, those skilled in the art can be selected and adjusted according to practical condition, product requirement and quality requirement,
Cleaning agent of the present invention preferably includes ethanol and/or acetone, more preferably ethanol or acetone.
The alloy pig that the present invention obtains above-mentioned steps carries out getting rid of band after crushing, and obtains amorphous alloy strip.
The broken condition is not particularly limited the present invention, with alloy pig breaker bars well known to those skilled in the art
Part, those skilled in the art can be selected and adjusted according to practical condition, product requirement and quality requirement.
The mode for getting rid of band is not particularly limited the present invention, and non-crystaline amorphous metal is prepared with well known to those skilled in the art
Get rid of band mode, those skilled in the art can be selected according to practical condition, product requirement and quality requirement
And adjustment, the band preferably single roller chilling of the present invention that gets rid of get 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 the present invention, and amorphous is prepared with well known to those skilled in the art
Alloy gets rid of band parameter, and those skilled in the art can be carried 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 30~50m/s, more preferably 32~47m/s, most preferably
For 35~45m/s.
Above-mentioned steps of the present invention have obtained amorphous alloy strip.The present invention is not limited especially the parameter of the amorphous alloy strip
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 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
For 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 the present invention, with non-crystaline amorphous metal well known to those skilled in the art
Heat treatment, those skilled in the art can be selected and adjusted according to practical condition, product requirement and quality requirement
Whole, heat treatment of the present invention is preferably to make annealing treatment.
The temperature of the heat treatment is not particularly limited the present invention, with non-crystaline amorphous metal well known to those skilled in the art
Heat treatment temperature, those skilled in the art can be selected according to practical condition, product requirement and quality requirement
And adjustment, the temperature of heat treatment of the present invention is preferably 410~450 DEG C, more preferably 415~445 DEG C, more preferably 420
~440 DEG C, most preferably 425~435 DEG C.
The time of the heat treatment is not particularly limited the present invention, with non-crystaline amorphous metal well known to those skilled in the art
Heat treatment time, those skilled in the art can be selected according to practical condition, product requirement and quality requirement
And adjustment, the time of heat treatment of the present invention is preferably 10~60min, more preferably 20~50min, most preferably 30~
40min。
The heating rate of the heat treatment is not particularly limited the present invention, is closed with amorphous well known to those skilled in the art
The heat treatment heating rate of gold, those skilled in the art can be according to practical condition, product requirement and quality requirement
Being selected and 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 by specific
Element is arranged in pairs or groups, it is proposed that the new Fe-based amorphous Nanocrystalline soft magnetic alloy with high saturated magnetic induction, the alloy have more
The excellent soft magnet performance such as high saturation induction density, lower coercivity, and do not include expensive metallic element Nb, greatly
The big cost for reducing material, effectively solves in existing iron-based amorphous and nanocrystalline soft magnetic alloy, to improve saturation magnetic
Induction, iron content need to be improved；Cost is reduced, it is few to add or do not add noble metal Nb, but the increase of iron content, noble metal contain
The reduction of amount can all cause the Forming ability of nanocrystalline presoma (amorphous) to decline, and also be unfavorable for the preparation of amorphous band,
Ultimately result in the contradiction of the deterioration of magnetic property.Present invention technical scheme more for before, it is micro- to overcome Fe contents in the prior art
The technique direction and prejudice of tune, Fe content greatly improved, creative direct tripping is to more than 85.5, then adjusts each element
Ratio, the interaction between further Refining Elements so that saturation magnetization further improves, and can approach the limit
Value, and coercivity declines to a great extent so that the overall performance of Fe-based amorphous Nanocrystalline soft magnetic alloy is obviously improved.
Test result indicates that amorphous/nanocrystalline magnetically soft alloy prepared by the present invention, iron content is high, but saturation magnetization
1.99T can be reached, approach 2.0T limiting value substantially, coercivity only has 6.5A/m, effectively improves existing amorphous/nanocrystalline
The shortcomings that magnetically soft alloy low saturation induction density high-coercive force.
It is soft to a kind of iron-based amorphous nanometer crystalline provided by the invention with reference to embodiments in order to further illustrate the present invention
Magnetic alloy and preparation method thereof is described in detail, but it is to be understood that these embodiments be using technical solution of the present invention as
Under the premise of implemented, give detailed embodiment and specific operating process, simply be further illustrate the present 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
Fe85.7Si0.5B9.3P3.5Cu0.7C0.3
Fe-based amorphous nanocrystalline alloy, the composition constitutional chemistry formula of alloy is Fe85.7Si0.5B9.3P3.5Cu0.7C0.3。
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 process：
(1) prepared by foundry alloy raw material：By Fe85.7Si0.5B9.3P3.5Cu0.7C0.3Atomic percent is converted to matter by chemical formula
Percentage is measured, Fe (99.9%), FeB (17.6%) alloy, FeP (25%) alloy, FeC (2.25%) is weighed respectively in proportion and closes
Gold or graphite (C), Si (99.9%) blocks and Cu blocks.
(2) foundry alloy melting：The raw material prepared is put into vacuum arc melting furnace, 5 × 10 are evacuated to body of heater-3Afterwards
Argon gas/nitrogen atmosphere protection is filled with, when air pressure superatmospheric 0.01Mpa in stove, closes charging valve.It is former to heat melting
Material, after raw material is completely melt, continues melting 3 minutes, be subsequently cooled to solidify, melting 3 times is repeated after quickly being overturn, is obtained
To the uniform alloy pig of composition.
(3) alloy pig cleans：Alloy pig is broken for fritter alloy, and is put into the beaker equipped with ethanol or acetone and carries out
Cleaning.
(4) prepared by amorphous thin ribbon：It is fitted into after fritter alloy is cleaned in the quartz ampoule of lower ending opening, is subsequently placed in and gets rid of band and set
In standby induction coil, 5 × 10 are evacuated to-3It is electric as protective gas, regulation that the high-purity argon gas that purity is 99.99% is filled with afterwards
Stream makes alloy melting, during which controls temperature at 1250 DEG C, control 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 rotating speed is 50m/s by pressure difference, and obtained width is about 2mm, and thickness is about 25 μ
M 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.Ginseng
It is the X-ray diffractogram of amorphous thin ribbon prepared by the embodiment of the present invention to see Fig. 2, Fig. 2.As shown in Figure 2, complete amorphous material
About there is the diffraction maximum of widthization disperse at 45 °, and in other scopes without obvious sharp crystallization peak.
(6) Crystallizing treatment：
The Fe-based amorphous nanometer that the amorphous thin ribbon prepared to the embodiment of the present invention 1 obtains at a temperature of different annealings
Peritectic alloy carries out X-ray diffraction analysis.
Referring to Fig. 3, Fig. 3 is the iron-based that the amorphous thin ribbon of the embodiment of the present invention 1 obtains at a temperature of different annealings
Amorphous nano peritectic alloy X-ray diffractogram.
From the figure 3, it may be seen that at 340 DEG C relatively low of temperature, the alloy moves back at a higher temperature still in noncrystalline state
Fire, the alloy nano crystallization have separated out the saturation induction intensity that α-Fe are advantageous to improve alloy.But when temperature reaches 500 DEG C
When, the alloy has separated out the serious magnetic property that have impact on alloy of Fe-B compounds.
Amorphous thin ribbon is put into heat-treatment furnace and made annealing treatment, 420 DEG C is warming up to stove, is incubated 10min, wherein with
Stove heating rate is 20 DEG C/min, takes out strip after then cooling to room temperature with the furnace, obtains Fe-based amorphous nanocrystalline alloy.
The Fe-based amorphous nanocrystalline alloy prepared to the embodiment of the present invention 1 detects.
The strip after annealing is entered respectively with magnetic detection equipment (vibrating specimen magnetometer VSM and soft magnetism DC test instrument)
Row saturation induction density (Ms) and coercivity (Hc) performance test.Gained performance parameter as shown in drawings, wherein Bs=4 π ×
(ρ×Ms)×10-4(T)。
Referring to Fig. 4, Fig. 4 is the magnetization curve figure of Fe-based amorphous nanocrystalline alloy prepared by the embodiment of the present invention.Referring to figure
The change that the coercivity heat treatment temperature of 5, Fig. 5 Fe-based amorphous nanocrystalline alloys prepared for the embodiment of the present invention is different is bent
Line.
As a result show, the iron-based amorphous and nanocrystalline soft magnetic alloy prepared by the embodiment of the present invention 1
Fe85.7Si0.5B9.3P3.5Cu0.7C0.3, its saturation magnetization is 1.98T, coercivity 8.4A/m.
Embodiment 2
Fe85.8Si0.5B9.3P3.5Cu0.7C0.2
Fe-based amorphous nanocrystalline alloy, the composition constitutional chemistry formula of alloy is Fe85.8Si0.5B9.3P3.5Cu0.7C0.2。
Preparation process：
(1) prepared by foundry alloy raw material：By Fe85.8Si0.5B9.3P3.5Cu0.7C0.2Atomic percent is converted to matter by chemical formula
Percentage is measured, Fe (99.9%), FeB (17.6%) alloy, FeP (25%) alloy, FeC (2.25%) is weighed respectively in proportion and closes
Gold or graphite (C), Si (99.9%) blocks and Cu blocks.
(2) foundry alloy melting：The raw material prepared is put into vacuum arc melting furnace, 5 × 10 are evacuated to body of heater-3Afterwards
Argon gas/nitrogen atmosphere protection is filled with, when air pressure superatmospheric 0.01Mpa in stove, closes charging valve.It is former to heat melting
Material, after raw material is completely melt, continues melting 3 minutes, be subsequently cooled to solidify, melting 3 times is repeated after quickly being overturn, is obtained
To the uniform alloy pig of composition.
(3) alloy pig cleans：Alloy pig is broken for fritter alloy, and is put into the beaker equipped with ethanol or acetone and carries out
Cleaning.
(4) prepared by amorphous thin ribbon：It is fitted into after fritter alloy is cleaned in the quartz ampoule of lower ending opening, is subsequently placed in and gets rid of band and set
In standby induction coil, 5 × 10 are evacuated to-3It is electric as protective gas, regulation that the high-purity argon gas that purity is 99.99% is filled with afterwards
Stream makes alloy melting, during which controls temperature at 1250 DEG C, control 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 rotating speed is 50m/s by pressure difference, and obtained width is about 1mm, and thickness is about 20 μ
M 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 maximum of widthization disperse at 45 °, and in other scopes without obvious sharp crystallization peak.
(6) Crystallizing treatment：
The Fe-based amorphous nanometer that the amorphous thin ribbon prepared to the embodiment of the present invention 2 obtains at a temperature of different annealings
Peritectic alloy carries out X-ray diffraction analysis.
Referring to Fig. 6, Fig. 6 is the iron-based that the amorphous thin ribbon of the embodiment of the present invention 2 obtains at a temperature of different annealings
Amorphous nano peritectic alloy X-ray diffractogram.
It will be appreciated from fig. 6 that at 340 DEG C relatively low of temperature, the alloy moves back at a higher temperature still in noncrystalline state
Fire, the alloy nano crystallization have separated out the saturation induction intensity that α-Fe are advantageous to improve alloy.But when temperature reaches 500 DEG C
When, the alloy has separated out the serious magnetic property that have impact on alloy of Fe-B compounds.
Strip is put into heat-treatment furnace and made annealing treatment, 420 DEG C is warming up to stove, 10min is incubated, wherein with stove liter
Warm speed is 20 DEG C/min, takes out strip after then cooling to room temperature with the furnace, obtains Fe-based amorphous nanocrystalline alloy.
The Fe-based amorphous nanocrystalline alloy prepared to the embodiment of the present invention 2 detects.
The strip after annealing is entered respectively with magnetic detection equipment (vibrating specimen magnetometer VSM and soft magnetism DC test instrument)
Row saturation induction density (Ms) and coercivity (Hc) performance test.Gained performance parameter as shown in drawings, wherein Bs=4 π ×
(ρ×Ms)×10-4(T)。
As a result show, the iron-based amorphous and nanocrystalline soft magnetic alloy prepared by the embodiment of the present invention 2
Fe85.8Si0.5B9.3P3.5Cu0.7C0.2, its saturation magnetization is 1.98T, coercivity 8.1A/m.
Embodiment 3
Fe85.7Si0.5B9.3P3.6Cu0.6C0.3
Fe-based amorphous nanocrystalline alloy, the composition constitutional chemistry formula of alloy is Fe85.7Si0.5B9.3P3.6Cu0.6C0.3。
Preparation process：
(1) prepared by foundry alloy raw material：By Fe85.7Si0.5B9.3P3.6Cu0.6C0.3Atomic percent is converted to matter by chemical formula
Percentage is measured, Fe (99.9%), FeB (17.6%) alloy, FeP (25%) alloy, FeC (2.25%) is weighed respectively in proportion and closes
Gold or graphite (C), Si (99.9%) blocks and Cu blocks.
(2) foundry alloy melting：The raw material prepared is put into vacuum arc melting furnace, 5 × 10 are evacuated to body of heater-3Afterwards
Argon gas/nitrogen atmosphere protection is filled with, when air pressure superatmospheric 0.01Mpa in stove, closes charging valve.It is former to heat melting
Material, after raw material is completely melt, continues melting 3 minutes, be subsequently cooled to solidify, melting 3 times is repeated after quickly being overturn, is obtained
To the uniform alloy pig of composition.
(3) alloy pig cleans：Alloy pig is broken for fritter alloy, and is put into the beaker equipped with ethanol or acetone and carries out
Cleaning.
(4) prepared by amorphous thin ribbon：It is fitted into after fritter alloy is cleaned in the quartz ampoule of lower ending opening, is subsequently placed in and gets rid of band and set
In standby induction coil, 5 × 10 are evacuated to-3It is electric as protective gas, regulation that the high-purity argon gas that purity is 99.99% is filled with afterwards
Stream makes alloy melting, during which controls temperature at 1250 DEG C, control 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 rotating speed is 50m/s by pressure difference, and obtained width is about 1mm, and thickness is about 20 μ
M 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 maximum of widthization disperse at 45 °, and in other scopes without obvious sharp crystallization peak.
(6) Crystallizing treatment：
The Fe-based amorphous nanometer that the amorphous thin ribbon prepared to the embodiment of the present invention 3 obtains at a temperature of different annealings
Peritectic alloy carries out X-ray diffraction analysis.
Referring to Fig. 7, Fig. 7 is the iron-based that the amorphous thin ribbon of the embodiment of the present invention 3 obtains at a temperature of different annealings
Amorphous nano peritectic alloy X-ray diffractogram.
As shown in Figure 7, at 340 DEG C relatively low of temperature, the alloy moves back at a higher temperature still in noncrystalline state
Fire, the alloy nano crystallization have separated out the saturation induction intensity that α-Fe are advantageous to improve alloy.But when temperature reaches 500 DEG C
When, the alloy has separated out the serious magnetic property that have impact on alloy of Fe-B compounds.
Strip is put into heat-treatment furnace and made annealing treatment, 420 DEG C is warming up to stove, 10min is incubated, wherein with stove liter
Warm speed is 20 DEG C/min, takes out strip after then cooling to room temperature with the furnace, obtains Fe-based amorphous nanocrystalline alloy.
The Fe-based amorphous nanocrystalline alloy prepared to the embodiment of the present invention 3 detects.
The strip after annealing is entered respectively with magnetic detection equipment (vibrating specimen magnetometer VSM and soft magnetism DC test instrument)
Row saturation induction density (Ms) and coercivity (Hc) performance test.Gained performance parameter as shown in drawings, wherein Bs=4 π ×
(ρ×Ms)×10-4(T)。
As a result show, the iron-based amorphous and nanocrystalline soft magnetic alloy prepared by the embodiment of the present invention 3
Fe85.7Si0.5B9.3P3.6Cu0.6C0.3, its saturation magnetization is 1.99T, coercivity 6.5A/m.
Embodiment 4
Fe85.7Si0.5B9P3.9Cu0.6C0.3
Fe-based amorphous nanocrystalline alloy, the composition constitutional chemistry formula of alloy is Fe85.7Si0.5B9P3.9Cu0.6C0.3。
Preparation process：
(1) prepared by foundry alloy raw material：By Fe85.7Si0.5B9P3.9Cu0.6C0.3Atomic percent is converted to quality by chemical formula
Percentage, weigh Fe (99.9%), FeB (17.6%) alloy, FeP (25%) alloy, FeC (2.25%) alloy respectively in proportion
Or graphite (C), Si (99.9%) blocks and Cu blocks.
(2) foundry alloy melting：The raw material prepared is put into vacuum arc melting furnace, 5 × 10 are evacuated to body of heater-3Afterwards
Argon gas/nitrogen atmosphere protection is filled with, when air pressure superatmospheric 0.01Mpa in stove, closes charging valve.It is former to heat melting
Material, after raw material is completely melt, continues melting 3 minutes, be subsequently cooled to solidify, melting 3 times is repeated after quickly being overturn, is obtained
To the uniform alloy pig of composition.
(3) alloy pig cleans：Alloy pig is broken for fritter alloy, and is put into the beaker equipped with ethanol or acetone and carries out
Cleaning.
(4) prepared by amorphous thin ribbon：It is fitted into after fritter alloy is cleaned in the quartz ampoule of lower ending opening, is subsequently placed in and gets rid of band and set
In standby induction coil, 5 × 10 are evacuated to-3It is electric as protective gas, regulation that the high-purity argon gas that purity is 99.99% is filled with afterwards
Stream makes alloy melting, during which controls temperature at 1250 DEG C, control 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 rotating speed is 50m/s by pressure difference, and obtained width is about 1mm, and thickness is about 20 μ
M 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 maximum of widthization disperse at 45 °, and in other scopes without obvious sharp crystallization peak.
(6) Crystallizing treatment：
The Fe-based amorphous nanometer that the amorphous thin ribbon prepared to the embodiment of the present invention 4 obtains at a temperature of different annealings
Peritectic alloy carries out X-ray diffraction analysis.
Referring to Fig. 8, Fig. 8 is the iron-based that the amorphous thin ribbon of the embodiment of the present invention 4 obtains at a temperature of different annealings
Amorphous nano peritectic alloy X-ray diffractogram.
As shown in Figure 8, at 340 DEG C relatively low of temperature, the alloy moves back at a higher temperature still in noncrystalline state
Fire, the alloy nano crystallization have separated out the saturation induction intensity that α-Fe are advantageous to improve alloy.But when temperature reaches 500 DEG C
When, the alloy has separated out the serious magnetic property that have impact on alloy of Fe-B compounds.
Strip is put into heat-treatment furnace and made annealing treatment, 420 DEG C is warming up to stove, 10min is incubated, wherein with stove liter
Warm speed is 20 DEG C/min, takes out strip after then cooling to room temperature with the furnace, obtains Fe-based amorphous nanocrystalline alloy.
The Fe-based amorphous nanocrystalline alloy prepared to the embodiment of the present invention 3 detects.
The strip after annealing is entered respectively with magnetic detection equipment (vibrating specimen magnetometer VSM and soft magnetism DC test instrument)
Row saturation induction density (Ms) and coercivity (Hc) performance test.Gained performance parameter as shown in drawings, wherein Bs=4 π ×
(ρ×Ms)×10-4(T)。
As a result show, the iron-based amorphous and nanocrystalline soft magnetic alloy prepared by the embodiment of the present invention 4
Fe85.7Si0.5B9P3.9Cu0.6C0.3, its saturation magnetization is 1.95T, coercivity 7.3A/m.
A kind of iron-based amorphous and nanocrystalline soft magnetic alloy provided by the invention and preparation method thereof is carried out above in detail
Introduce, specific case used herein is set forth to the principle and embodiment of the present invention, the explanation of above example
It is only intended to help the method and its core concept for understanding the present invention, including best mode, and also causes any of this area
Technical staff can put into practice the present invention, including manufacture and using any device or system, and implement the method for any combination.Should
, for those skilled in the art, under the premise without departing from the principles of the invention, can also be to this when pointing out
Invention carries out some improvement and modification, and these are improved and modification is also fallen into the protection domain of the claims in the present invention.The present invention
The scope of patent protection is defined by the claims, and may include those skilled in the art it is conceivable that other embodiment.
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, then these other embodiments should also be wanted included in right
In the range of asking.
Claims (10)
1. a kind of iron-based amorphous and nanocrystalline soft magnetic alloy, it is characterised in that there is the formula shown in Formulas I：
FexSiyBzPwCumCnI；
Wherein, 85.5≤x≤86.0,0≤y≤2,8≤z≤10,2≤w≤6,0.5≤m≤0.8,0≤n≤0.5, and x+y+z
+ n+m+w=100.
2. composite according to claim 1, it is characterised in that 85.6≤x≤85.8；
0≤y≤0.5；
8.5≤z≤9.5
3≤w≤4；
0.6≤m≤0.7；
0.1≤n≤0.3.
3. according to the composite described in claim 1~2 any one, it is characterised in that 85.7≤x≤85.8；
9≤z≤9.3
3.5≤w≤3.9
0.61≤m≤0.69；
0.2≤n≤0.3.
4. a kind of preparation method of iron-based amorphous and nanocrystalline soft magnetic alloy, it is characterised in that comprise the following steps：
A after iron, carbon iron, boron source and copper) are carried out into melting, alloy pig is obtained, or iron, carbon iron, copper and other raw materials are carried out
After melting, alloy pig is obtained；
Other described raw materials include ferrophosphorus and/or silicon；
The boron source includes boron and/or ferro-boron；
B carry out getting rid of band after) alloy pig for obtaining above-mentioned steps is broken, obtain amorphous alloy strip；
C) under conditions of vacuum or protective atmosphere, after amorphous alloy strip that above-mentioned steps are obtained is heat-treated, obtain
Iron-based amorphous and nanocrystalline soft magnetic alloy.
5. preparation method according to claim 4, it is characterised in that the temperature of the melting is 1100~1350 DEG C；Institute
The time for stating melting is 1~5min；
The melting is multiple melting；Described is repeatedly more than or equal to 3 times.
6. preparation method according to claim 4, it is characterised in that be specially the step of the melting：
First ferrophosphorus is put into smelting apparatus, then iron, boron source, copper and carbon iron are put into smelting apparatus and carry out melting；
Or 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. preparation method according to claim 4, it is characterised in that the band that gets rid of gets rid of band for single roller chilling；
The chilling roller linear velocity for getting rid of band is 30~50m/s.
8. preparation method according to claim 4, it is characterised in that the width of the amorphous alloy strip is 1~2mm；
The thickness of the amorphous alloy strip is 18~35 μm.
9. according to the preparation method described in claim 4~8 any one, it is characterised in that the temperature of the heat treatment is 410
~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.
10. preparation method according to claim 4, it is characterised in that also include cleaning step after the alloy pig is broken；
The cleaning agent of the cleaning includes ethanol and/or acetone.
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