CN104934179B - Fe-based nanocrystalline magnetically soft alloy of strong amorphous formation ability and preparation method thereof - Google Patents
Fe-based nanocrystalline magnetically soft alloy of strong amorphous formation ability and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of Fe-based nanocrystalline magnetically soft alloy of strong amorphous formation ability and preparation method thereof, and the expression formula of the alloy is FexSiaBbPcNbdCue, x, a, b, c, d and e represent the atom percentage content of each correspondence component respectively in the expression formula, and meet following condition:0.5≤a≤12,0.5≤b≤15,0.5≤c≤12,0.1≤d≤3,0.1≤e≤3,70≤x≤85, x+a+b+c+d+e=100%.It is the Fe-based amorphous alloy of 3.5mm that magnetically soft alloy of the invention uses common copper mold casting method to prepare critical dimension, and after annealing, saturation induction density is more than 1.5T, and coercivity value is in below 1A/m.
Description
Technical field
The present invention relates to magnetic functional material field, more particularly to a kind of iron based nano crystal soft magnetism of strong amorphous formation ability
Alloy and preparation method thereof, the alloy has strong amorphous formation ability, high thermal stability, excellent soft magnet performance concurrently.
Background technology
Fe nanometer crystal alloys have high resistivity, low-loss, high-strength tenacity, high magnetic permeability and saturated magnetization higher strong
The advantages of spending, while preparation flow is short, product energy-conserving and environment-protective, therefore is considered as to make Switching Power Supply, pulse transformer core,
The preferable material of the electric power such as transformer, magnetic amplifier, Spike-killers, differential mode inductance iron core and core of reactor and electronic equipment
Material.
But compared with commercialization silicon steel sheet, iron-base nanometer crystal alloy saturation induction density is relatively low.Crystalline state oriented silicon
The B of steelsValue is about in 2T, and typical nanometer crystal alloy Fe73.5Cu1Nb3Si13.5B9BsValue is only 1.24T.With magnetic unit device
The development of part efficient small, the soft magnet performance to iron based nano crystal material proposes requirement higher, such as transformer core, electricity
Motivation rotor and magnetic switch etc., it is often desired to which the saturation induction density of these devices is higher, as it means that device chi
Very little reduction or the reduction of exciting power.
Japan Patent JP1156451A discloses a kind of receiving for the high saturated magnetic induction that expression formula is FeCoCuSiBM '
Rice peritectic alloy, wherein, M ' represents one or more element in Nb, W, Ta, Zr, Hf, Ti, and by controlling heat treating regime,
Keep crystalline phase volume fraction more than 50% so that the saturation induction density of alloy 1.4T and more than.This is actually
It is control heat treatment mode, more obtains α-Fe crystal grain and separate out, with the B high of α-Fe itselfsTo improve the saturation magnetic strength of alloy
Answer intensity.But the limited potential of this method lifting, the highest B that it is enumeratedsOnly in 1.58T.
Chinese patent application CN1704498A discloses the composition model of a kind of ternary and polynary iron-based lumpy nanometer peritectic alloy
Enclose.Its atom ratio is with chemical general formula MaXbZcRepresent, ferromagnetic element of the M basidigitales based on iron and contain a small amount of other units
Element (one kind in Sc, Ti, V, Cr, Mn, Co, Ni, Cu, Ag, Au, Pd, Pt, Zr, Nb, Mo, Hf, Ta, W, Al, Ga, Sn, Bi or
It is several), X is selected from one or more elements (can Zr, Nb replace on a small quantity) in Sc, Y, La, Ce, Sm, Dy, Ho, Er, Yb, Z
It is that, selected from one or more elements in B, C, Si, N, P, Ge, S, concrete content (atomic percent) is a=53-62% or 65-
85%, b=1-15%, c=9-15% or 17-27% or 35-41%.The saturation induction density of resulting alloy bar material is most
1.8T high, but coercivity is larger, up to 100A/m.
Japan Patent JP2006040906 disclose it is a kind of when state is quenched i.e. containing average grain diameter below 50nm α-Fe
The amorphous alloy of crystal grain, band can carry out 180 ° of bendings, after being annealed through the proper temperature higher than crystallization temperature, its saturation magnetic strength
Answering intensity can bring up to 1.6T.But the amorphous formation ability of this composition is poor, and micro-crystallization is just had occurred and that in preparation process, its example
The highest B of actsOnly 1.6T.
United States Patent (USP) US005449419 discloses the nanometer crystal alloy that a kind of expression formula is Fe-Zr/Hf-B (Cu), and it is satisfied
1.7T can be reached with the intensity of magnetization, soft magnet performance is excellent, but due to substantial amounts of Zr or Hf elements in alloy, not only increase conjunction
The cost of gold, and it is harsh to preparation condition requirement.
Chinese patent CN101834046B discloses a kind of expression formula for FexSiyBzPaCubNanometer crystal alloy, its saturation magnetic
Induction is up to 1.9T, and soft magnet performance is excellent.But the composition amorphous formation ability is very poor, produced in preparation process high
Density nanocrystal, follow-up crystallization and thermal treatment must can just obtain the nanometer double structure of excellent performance using short annealing, because
This composition annealing process is difficult to control, it is difficult to industrialized production.
In sum, the high saturated magnetic induction nano-crystal soft magnetic alloy developed in the market is due to amorphous formation energy
Power is poor, required critical cooling rate it is very high (>106DEG C/s), or even amorphous precursor body occur controlled micro crystallization, this to producing equipment,
Technique and Technology for Heating Processing requirement are extremely harsh, are prepared to nanocrystalline production and bring great difficulty, while limit receiving
The application field of meter Jing.Therefore this area needs exploitation to have low critical cooling rate concurrently (for example<<103DEG C/s), strong amorphous formation
The high saturated magnetic induction Fe-based nanocrystalline magnetically soft alloy of the iron-base nanometer crystal alloy of ability, good Technology for Heating Processing, so that
Significantly break through limitation and the degree of difficulty of nanocrystalline production technology and annealing process.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of iron based nano crystal of strong amorphous formation ability
Magnetically soft alloy and preparation method thereof, the design of alloy is reasonable, amorphous formation ability is strong, heat endurance is good and soft magnet performance
It is excellent.
Inventor proposes this new iron-based nanometer crystal alloy according to weak point of the prior art.Its composition design
Thinking is, using alloy based on the FeSiBPNb systems alloy for possessing large-amorphous forming capacity, addition tool to be required according to designer
There is large-amorphous forming capacity ferromagnetic element and form nanocrystalline essential elements, composition and content are rationally designed,
Then the nano-crystal soft magnetic alloy of excellent performance is prepared by existing production technologies such as melting, fast quenching, copper mold castings.
To achieve these goals, present invention employs following technical scheme:
A kind of Fe-based nanocrystalline magnetically soft alloy of strong amorphous formation ability, the expression formula of the alloy is
FexSiaBbPcNbdCue, x, a, b, c, d and e represent the atom percentage content of each correspondence component respectively in the expression formula, and
Meet following condition:0.5≤a≤12,0.5≤b≤15,0.5≤c≤12,0.1≤d≤3,0.1≤e≤3,70≤x≤85, x
+ a+b+c+d+e=100%.
In above-mentioned Fe-based nanocrystalline magnetically soft alloy, as a kind of preferred embodiment, the atomic percent of the component Fe
Span than content x is 76≤x≤82.
In above-mentioned Fe-based nanocrystalline magnetically soft alloy, as a kind of preferred embodiment, the atomic percent of the component Si
Span than content a is 2≤a≤10.
In above-mentioned Fe-based nanocrystalline magnetically soft alloy, as a kind of preferred embodiment, the atomic percent of the component B
The span of content b is 2≤b≤10.
In above-mentioned Fe-based nanocrystalline magnetically soft alloy, as a kind of preferred embodiment, the atomic percent of the component P
The span of content c is 2≤b≤6.
In above-mentioned Fe-based nanocrystalline magnetically soft alloy, as a kind of preferred embodiment, the atomic percent of the component Nb
Span than content d is 0.5≤d≤2.5.
In above-mentioned Fe-based nanocrystalline magnetically soft alloy, as a kind of preferred embodiment, the atomic percent of the component Cu
Span than content e is 0.5≤e≤1.5.
The composition design principle to above-mentioned Fe-based nanocrystalline magnetically soft alloy is illustrated below:
In iron-base nanometer crystal alloy of the invention, the atom % of Si elements will meet:0.5≤a≤12, preferred scope
It is 2≤a≤10.Si elements are the common elements for constituting amorphous alloy, and the appropriate addition of Si elements can not only improve alloy
Heat endurance and Curie temperature, improve the amorphous formation ability of alloy, and can also improve the metalloid elements such as B and P in alloy
In solubility, expand alloy composition range;When Si Elements Atom % contents are less than 0.5, the promotion of Si elements forms non-
The effect of crystal alloy is difficult to give full play of, and when Si Elements Atom % contents are more than 12, then can reduce ferromagnetism unit
The content of element, it is impossible to obtain the magnetically soft alloy of high saturated magnetic induction.
In iron-base nanometer crystal alloy of the invention, the atom % of B element will meet 0.5≤b≤15, and preferred scope is
2≤b≤10.When B atoms % is less than 0.5, B element content is too low, then be difficult to form the presoma of nanometer crystal alloy, i.e. amorphous
State alloy.And when B atoms % is more than 15, then can reduce ferromagnetic element content in alloy and drop low-alloyed saturation induction
Intensity.
In iron-base nanometer crystal alloy of the invention, the atom % of P element will meet:0.5≤c≤12, preferred scope
It is 2≤c≤6.P element is the common element for constituting amorphous alloy, the appropriate addition of P element, the other elements in P and system
There is the larger negative heat of mixing, P's is added with beneficial to the stability for improving supercooling liquid phase region, can not only improve the non-of alloy
Brilliant Forming ability, and the heat endurance of alloy can be improved and expand the heat treatment warm area scope of non-crystaline amorphous metal.When P element is former
When sub- % contents are less than 0.5, the effect that the promotion of P element forms amorphous alloy is difficult to bring into play, and works as P element atom %
When content is more than 12, then the content of ferromagnetic element can be reduced, it is impossible to obtain the magnetically soft alloy of high saturated magnetic induction.
In iron-base nanometer crystal alloy of the invention, the atom % of Nb will meet 0.1≤d≤3, and preferred scope is 0.5
≤d≤2.5.Nb is thick atom element, while being also to suppress a-Fe nanograin growths, crystal grain thinning, lifting nano-crystal soft-magnetic
The effective element of performance.Because Nb elements are non-ferromagnetic elements, when content is more than 3 atom %, can reduce ferromagnetic in alloy
Property constituent content, so as to reduce saturation induction density.And Nb constituent contents be less than 0.1 atom % when, the raising of Nb elements is non-
Brilliant Forming ability, crystal grain thinning, the effect of improvement soft magnet performance are difficult to bring into play.
In iron-base nanometer crystal alloy of the invention, it does not dissolve in Fe to Cu units procatarxis, in heat treatment, first from amorphous base
Uniformly separated out in body, promote α-Fe forming cores, be the general element for preparing nanometer crystal alloy.The atom % of Cu elements will meet:0.1
≤ e≤3, preferred scope is 0.5≤e≤1.5.When Cu atoms % is more than 3, the amorphous formation ability of alloy is deteriorated, it is difficult to
Prepare.And when Cu atoms % is less than 0.1, Cu is in annealing as α-Fe forming cores are promoted, the effect for forming nanometer crystal alloy is difficult
To bring into play.
In iron-base nanometer crystal alloy of the invention, in addition to above-mentioned element, surplus is made up of Fe, and Fe is magnetic element, is
Acquisition high saturated magnetic induction, it is necessary to assure alloy contains Fe contents higher.However, the rising of Fe contents, necessarily leads
The reduction of amorphous formation element is caused, amorphous formation ability declines, it is impossible to obtain optimal combination property.Fe contents are preferably 70≤x
≤ 85, and more preferably 76≤x≤82.
In above-mentioned Fe-based nanocrystalline magnetically soft alloy, as a kind of preferred embodiment, the component Nb can by Zr, Ti,
At least one element portions or replacing whole in Ta, Hf, V, W, Mo, Mn, Cr, Zn, wherein the element of the replacement Nb is in institute
It is less than 3% to state the atom percentage content in Fe-based nanocrystalline magnetically soft alloy.
In above-mentioned Fe-based nanocrystalline magnetically soft alloy, as a kind of preferred embodiment, the component B can by C, N, O, S,
At least one element portions or replacing whole in Sn, Ge, Ga, Al, wherein the element of the replacement B is in the iron based nano crystal
Atom percentage content in magnetically soft alloy is less than 5%.
In above-mentioned Fe-based nanocrystalline magnetically soft alloy, as a kind of preferred embodiment, the component Cu can by Au and/or
Ag is partly or entirely substituted, wherein atomic percent of the element of the replacement Cu in the Fe-based nanocrystalline magnetically soft alloy contains
Measure is less than 3%.
In above-mentioned Fe-based nanocrystalline magnetically soft alloy, also containing a small amount of inevitably impurity element, but may own
The total weight percent of impurity element is less than 0.5%.
A kind of preparation method of above-mentioned Fe-based nanocrystalline magnetically soft alloy, comprises the following steps:
Step one, dispensing is carried out by the atom percentage content of each component in above-mentioned alloy expression formula;
Step 2, being filled with after evacuation under the atmosphere of protective gas will be described using induction melting furnace or arc-melting furnace
The raw material melting that step one is prepared is uniform, and furnace cooling or injection mould are cooled to master alloy ingot;
Step 3, the master alloy ingot that the step 2 is obtained is crushed;
Step 4, the fritter master alloy ingot after crushing is fused into molten steel, then using single-roller method, casting or atomization
(respective shapes can be strip, block, powder or other are possible to prepare the Fe base noncrystal alloys material of respective shapes
Shape);
Step 5, the Fe base noncrystal alloys material is heat-treated in heat-treatment furnace, wherein, during the heat treatment
Between be 5-120min (such as 10min, 30min, 50min, 80min, 100min, 110min), the heat treatment temperature be 400-
600 DEG C (such as 410 DEG C, 430 DEG C, 460 DEG C, 490 DEG C, 520 DEG C, 550 DEG C, 590 DEG C).
In above-mentioned preparation method, as a kind of preferred embodiment, in the step one, original is used during the dispensing
Material purity is more than 99.5%.
In above-mentioned preparation method, as a kind of preferred embodiment, in the step 2, the vacuum for vacuumizing
Degree is less than 5 × 10-3Pa (such as 2 × 10-3Pa、1×10-3Pa、8×10-4Pa、3×10-4Pa、5×10-5Pa), the protection
The atmosphere of gas is nitrogen or argon gas atmosphere, and the smelting time is 30-40min, and is incubated 5-30min after being melted down so as to close
Golden raw material melting is uniform.
In above-mentioned preparation method, as a kind of preferred embodiment, in the step 4, will using the single-roller method
Molten steel quickly cooling with prepare thickness as 10~200 μm (such as 15 μm, 20 μm, 30 μm, 40 μm, 60 μm, 85 μm, 100 μm, 150
μm, 200 μm) Fe base noncrystal alloy bands;The casting is used quickly to cool down molten steel to prepare a diameter of 0.5-3.5mm
The Fe base noncrystal alloy bars of (such as 1mm, 1.5mm, 2mm, 2.5mm, 3mm, 3.5mm).It is highly preferred that prepared by the single-roller method
Atmosphere during band is nitrogen, argon gas or air, more preferably air.It is highly preferred that the atmosphere when casting prepares bar
It is nitrogen, argon gas or air, more preferably air.It is highly preferred that the rotating speed when single-roller method prepares band is 10-40m/s (ratios
Such as 10m/s, 15m/s, 20m/s, 25m/s, 30m/s, 35m/s, 40m/s), spray band temperature is 1100-1550 DEG C (such as 1110
℃、1150℃、1200℃、1240℃、1280℃、1320℃、1370℃、1410℃、1450℃、1480℃、1500℃、1520
DEG C, 1540 DEG C), spray band when surface tension more than 0.5N/m (such as 0.5N/m, 0.8N/m, 1.2N/m, 1.5N/m, 1.8N/m,
2N/m, 2.5N/m), viscosity is more than 0.5mPas (such as 0.5mPas, 1mPas, 1.5mPas, 2mPas, 2.5mPas) during spray band.
It is highly preferred that casting temperature when the casting prepares bar for 1250-1600 DEG C (such as 1260 DEG C, 1280 DEG C, 1300
℃、1340℃、1360℃、1380℃、1420℃、1460℃、1530℃、1570℃)。
In above-mentioned preparation method, as a kind of preferred embodiment, in the step 4, it is described it is broken after fritter
Master alloy ingot be fused into the fusion temperature of molten steel for 1000-1600 DEG C (such as 1010 DEG C, 1050 DEG C, 1080 DEG C, 1100 DEG C,
1140℃、1190℃、1250℃、1340℃、1430℃、1570℃)。
In above-mentioned preparation method, as a kind of preferred embodiment, in the step 4, the Fe bases amorphous is prepared
Required critical cooling rate is 10 when alloy strip steel rolled stock or the Fe base noncrystal alloys bar2-103DEG C/(i.e. described molten steel is fast for s
Quickly cooling but when cooldown rate be 102-103℃/s).That is, preparing Fe base noncrystal alloy materials using single-roller method or casting
Can be with extremely low cooldown rate 10 during material2-103DEG C/s completes.
In above-mentioned preparation method, used as a kind of preferred embodiment, in the step 5, the heat treatment temperature is
450 DEG C -550 DEG C, heat treatment time is 20-70min.
In above-mentioned preparation method, as a kind of preferred embodiment, the Fe base noncrystal alloy materials of the respective shapes
It is strip, block or powdered alloy material.
The alloy that above-mentioned preparation method is obtained, its saturation induction density be more than 1.5T, coercivity value in below 1A/m,
Effective permeability is more than 10K under 1kHz;The alloy has a strong amorphous formation ability, and single-roller method or casting can be with extremely low cold
But speed (critical cooling rate (<<103DEG C/s)) come prepare critical dimension be 3.5mm Fe-based amorphous alloy.
Application of the above-mentioned Fe-based nanocrystalline magnetically soft alloy in terms of electronic device iron core is prepared.
Present invention X-ray diffractometer (XRD) determines the non crystalline structure of amorphous alloy strips and bar.Completely amorphous state
The XRD of alloy has the disperse diffraction maximum of widthization, without the corresponding sharp diffraction peak of obvious crystal structure.
The present invention tests the crystallization behavior of non-crystaline amorphous metal with high temperature differential scanning calorimeter (DSC), and programming rate is 40K/
Min, analyzes the crystallization curve of non-crystaline amorphous metal, calculates heat treatment warm area Δ T (Δ T=Tx2-T x1)。
The present invention tests the magnetic property of alloy strip steel rolled stock of the present invention with Magnetic Test equipment, including with vibrating specimen magnetometer
(VSM) its saturation induction density B is testeds, coercivity H is tested with DC B-H loop testings instrumentc, magnetic conductance is surveyed with electric impedance analyzer
Rate μ.
Compared with prior art, compared with existing nanometer crystal alloy, its advantage exists the nanometer crystal alloy that the present invention is provided
In being provided simultaneously with following characteristics:
With saturation induction density higher, after optimizing components and annealing, the nanocrystalline saturated magnetization of gained is strong
Degree BsUp to more than 1.5T;
With low-coercivity, its HcBetween 0-1A/m;
With heat endurance very high, in Tx1-Tx2Between carry out Isothermal treatment, the time, band performance was still up to 2h
It is so excellent, greatly reduce follow-up iron core heat treatment difficulty.
With stronger amorphous formation ability, the alloy pig prepared with the raw material of industry is cast in atmosphere with copper mold casting method
Make amorphous bar, its diameter up to 3.5mm, sufficiently large amorphous formation ability and low critical cooling rate (<<103DEG C/s), pole
Big reduces requirement of the band preparation to production equipment and production technology, it is ensured that the stabilization of strip quality in production process
Property.
The present invention produces, low cost simple with annealing process, is easily achieved industrialization, and obtained product has excellent soft magnetism
Performance, can be applied to the fields such as electric power, electronics, information, communication as structure and function soft magnetic materials.
Brief description of the drawings
Fig. 1 is example Fe of the present inventionbal.Si9B10P5Nb1Cu0.75The full amorphous bar of alloy and its state XRD piece of quenching.
Fig. 2 is example of the present invention through 530 DEG C of Fe of annealing 10 minutesbal.Si6B6P3Nb1Au0.75The TEM pictures of alloy.
Fig. 3 is example Fe of the present inventionbal.Si6B6P3Nb1Cu0.75Alloy Bs/HcWith annealing time variation diagram (soaking time t=
30min)。
Specific embodiment
Embodiment 1
The composition range of iron-base nanometer crystal alloy of the invention, we have done a series of experiments.According to of the invention
Composition carries out dispensing, and, referring to table 1 (sequence number 1-20), the raw material that will have been matched is put into sensing for specific composition and atom percentage content
Smelting furnace or arc-melting furnace, are evacuated to 5 × 10-3Below Pa, then applying argon gas atmosphere protection, is incubated again after being completely melt
30min makes alloy raw material be smelted into uniform molten steel, and injection mould cooling obtains the uniform master alloy ingot of composition;Again by foundry alloy
Ingot is crushed;Then fritter foundry alloy is loaded in quartz ampoule and be fused into molten steel, fusion temperature is 1300 DEG C or so, in air with
The speed of 35m/s gets rid of band, and spray band temperature is 1200 DEG C, and surface tension is 0.8N/m during spray band, and viscosity is 1mPas during spray band, cold
But speed is 102DEG C/s, 1mm wide, thick 20 μm AMORPHOUS ALLOY RIBBONS is obtained;Fritter foundry alloy is loaded and is fused into quartz ampoule
Molten steel, fusion temperature is 1300 DEG C or so, and molten steel quickly cools down with copper mold casting method (cooling velocity is 10 in air2℃/
S), casting temperature is 1250 DEG C, prepares the non-crystaline amorphous metal bar of a diameter of 0.5~3.5mm;Amorphous alloy strips or bar are put
Enter in heat-treatment furnace, 530 DEG C for the treatment of 10min.The non crystalline structure of amorphous bar is determined with X-ray diffractometer (XRD).Use magnetic
Test equipment tests the magnetic property of alloy strip steel rolled stock of the present invention, and its saturation induction density is tested with vibrating specimen magnetometer (VSM)
Bs, coercivity H is tested with DC B-H loop testings instrumentc, magnetic permeability μ is surveyed with electric impedance analyzer, measurement obtains the amorphous of alloy
Into ability, soft magnet performance is shown in Table 1.In order to contrast conveniently, we also enumerate the composition alloy of multigroup prior art simultaneously, specifically into
During the result of point contrast lists table 1 in.Sequence number 1-20 is the embodiment of the present invention, and sequence number 21-25 is to choose performance in the prior art
Preferable alloy system is as a comparison case.Expression formula of the invention can be seen that for Fe by the example in table 1xSiaBbPcNbdCue
Nanometer crystal alloy, its saturation magnetization is higher, concentrates on 1.5T~1.8T, and coercivity concentrates on below 0.8A/m, exchange
Magnetic conductivity concentrates on 1.5 ten thousand to 30,000.Saturation magnetization of the invention is handed over apparently higher than the FeCuNbSiB systems alloy of comparative example
Stream magnetic conductivity is higher than FeSiB systems, the silicon steel of comparative example, and cost of alloy is less than comparative example Fe/CoSiBNbCu systems.Integrated comparative
Embodiment and comparative example can be seen that the alloy of the combination property better than prior art of alloy of the present invention.This shows following four
Individual aspect:1. in terms of soft magnet performance, alloy of the invention possesses the saturation induction density and below 1A/m of more than 1.5T simultaneously
Coercivity, more than 1.5 ten thousand ac permeability, its property indices are all forward;2. in terms of cost of alloy, conjunction of the invention
The raw material major part that gold is used all is readily available, and price is relatively low, and the 21-23 comparative example Fe/CoCuNbSiB systems of comparative example close
Golden cost is greatly reduced.3. in terms of amorphous formation ability, alloy of the invention has compared with large-amorphous forming capacity, with No. 21-23
Comparative example is significantly improved compared to amorphous formation ability, and bar can be made substantially.4. in terms of heat treatment warm area, alloy of the invention
With wide up to 160 DEG C of heat treatment warm areas.
Embodiment and comparative example in Integrated comparative table 1 can be seen that alloy of the invention have concurrently strong amorphous formation ability,
Big heat treatment warm area, excellent soft magnet performance and the low cost of material of valency, can greatly reduce to production, annealing process and
The requirement of equipment, is a kind of iron-base nanometer crystal alloy for having very much an application prospect.
The alloying component of 1 embodiment of table 1 and performance
The comparative example of the present invention of (Continued) table 1
In table, subscript bal. represents surplus.
As seen from Figure 1, the alloying component of preparation is Febal.Si9B10P5Nb1Cu0.75Full glass bar surface it is smooth again
Metallic luster, the roomy steamed bun peak of XRD only one of which is typical non crystalline structure.
As seen from Figure 3, Febal.Si6B6P3Nb1Cu0.75Alloy after 450~550 DEG C of temperature range isothermal annealings, Bs
Between 1.7~1.8T, HcIn below 1A, illustrate that the alloy has excellent magnetic property and heat endurance.
Embodiment 2
The composition range of iron-base nanometer crystal alloy of the invention, we have done a series of experiments.It is of the invention high full
With the Fe of magnetic induction intensityxSiaBbPcNbdCueAlloy, its Cu is by least one element portions in Ag, Au of below 3 atom %
Or replacing whole.Table 2 is to carry out dispensing according to composition of the invention, and the raw material that will have been matched is put into induction melting furnace or electric arc melts
Furnace, is evacuated to 5 × 10-3Below Pa, then inflated with nitrogen atmosphere protection, 30min is incubated after fusing is smelted into alloy raw material
Uniform molten steel, injection mould cooling obtains the uniform alloy pig of composition;Master alloy ingot is crushed;Fritter foundry alloy is loaded into stone
Molten steel is fused into English pipe, fusion temperature is 1500 DEG C or so, band is got rid of with the speed of 30m/s in air, spray band temperature is 1400
DEG C, surface tension is 1.5N/m during spray band, and viscosity is 1.5mPas during spray band, and cooldown rate is 102DEG C/s, width 1mm, thickness is obtained
The AMORPHOUS ALLOY RIBBONS of 25um;Fritter foundry alloy is loaded molten steel is fused into quartz ampoule, fusion temperature is 1500 DEG C or so, empty
Molten steel quickly cools down with copper mold casting method (cooling velocity is 10 in gas2DEG C/s), casting temperature is 1400 DEG C, is prepared a diameter of
The non-crystaline amorphous metal bar of 0.5~3.5mm;Amorphous alloy strips or bar are placed in heat-treatment furnace, 530 DEG C for the treatment of 10min.
The non crystalline structure of amorphous bar is determined with X-ray diffractometer (XRD).The magnetic of alloy strip steel rolled stock of the present invention is tested with Magnetic Test equipment
Performance, its saturation induction density B is tested with vibrating specimen magnetometer (VSM)s, coercive is tested with DC B-H loop testings instrument
Power Hc, magnetic permeability μ is surveyed with electric impedance analyzer, measurement obtains the amorphous formation ability of alloy, and soft magnet performance is shown in Table 2.It is comprehensive to implement
Example is as can be seen that Ag/Au substitution Cu influence larger to material property.This shows following two aspects:1. in terms of soft magnet performance,
Alloy property indices of the invention are obviously improved, and particularly coercivity is down to below 1A/m, at the same possess 1.5T with
On saturation induction density and below 1A/m coercivity;2. in terms of amorphous formation ability, amorphous formation ability has larger carrying
Height, maximum amorphous formation ability is 3.5mm bars.But cost of alloy is substantially increased after Ag/Au substitutions Cu, therefore of the invention
Alloy has strong amorphous formation ability, greatly heat treatment warm area, excellent soft magnet performance concurrently, has as unique construction function soft magnetic materials
It is widely applied prospect.
The 2-in-1 golden composition of the embodiment of table 2 and performance
In table, subscript bal. represents surplus.
As seen from Figure 2, Febal.Si6B6P3Nb1Au0.75Alloy strip steel rolled stock shape after 530 DEG C of annealing, 30 minutes isothermal annealings
Into typical nanometer two-phase composite construction, the α-Fe nano-particles that a large amount of diameters are about 17nm are evenly distributed on noncrystal substrate.
Embodiment 3
The composition range of iron-base nanometer crystal alloy of the invention, we have done a series of experiments.It is of the invention high full
With the Fe of magnetic induction intensityxSiaBbPcNbdCueAlloy, its Nb by the Zr of below 3 atom %, Ti, Ta, Hf, V, W, Mo, Mn, Cr,
At least one element portions or replacing whole in Zn.Table 3 is to carry out dispensing according to composition of the invention, the raw material that will have been matched
Induction melting furnace or arc-melting furnace are put into, 5 × 10 are evacuated to-3Below Pa, then inflated with nitrogen atmosphere protection, is incubated after fusing
30min makes alloy raw material be smelted into uniform molten steel, and injection mould cooling obtains the uniform alloy pig of composition;Master alloy ingot is broken
It is broken;Fritter foundry alloy is loaded molten steel is fused into quartz ampoule, fusion temperature is 1550 DEG C or so, with the speed of 30m/s in air
Degree gets rid of band, and spray band temperature is 1500 DEG C, and surface tension is 2N/m during spray band, and viscosity is 2mPas during spray band, and cooldown rate is 102
DEG C/s, 10mm wide, thick 25 μm AMORPHOUS ALLOY RIBBONS is obtained;Fritter foundry alloy is loaded in quartz ampoule and is fused into molten steel, melted
Temperature is 1550 DEG C or so, and molten steel quickly cools down with copper mold casting method (cooling velocity is 10 in air2DEG C/s), casting temperature
It is 1500 DEG C, prepares the non-crystaline amorphous metal bar of a diameter of 0.5~3.5mm;Amorphous alloy strips or bar are placed in heat treatment
In stove, 530 DEG C for the treatment of 10min.The non crystalline structure of amorphous bar is determined with X-ray diffractometer (XRD).Surveyed with Magnetic Test equipment
The magnetic property of examination alloy strip steel rolled stock of the present invention, its saturation induction density B is tested with vibrating specimen magnetometer (VSM)s, with DC B-
H loop testings instrument test coercivity Hc, magnetic permeability μ is surveyed with electric impedance analyzer, measurement obtains the amorphous formation ability of alloy, soft magnetism
Performance is shown in Table 3.Integrated embodiment can be seen that Zr, Ti, Ta, Hf, V, W, Mo, Mn, Cr, Zn substitution Nb to be influenceed on material property
It is larger.This shows following two aspects:1. in terms of soft magnet performance, alloy property indices of the invention substantially do not become
Change, illustrate that such thick atom all has and stablize amorphous phase, suppress the effect of grain growth.2. in terms of amorphous formation ability, amorphous
Forming ability is declined slightly, and maximum amorphous formation ability is 3mm bars.Most elements remain to prepare more than 0.5mm after substituting
Bar.Test result indicate that Nb plays suppression a-Fe nanograin growths, crystal grain thinning, lifting nano-crystal soft-magnetic in the present invention
The effective element of performance, while the element can be substituted by Zr, Ti, Ta, Hf, V, W, Mo, Mn, Cr, Zn, illustrates that the alloy system can
The element of selection is a lot, and the kind requirement to raw material is not very strict, and this is just significant to industrialized production.
Alloy and its performance prepared by 3 embodiment of table 3
In table, subscript bal. represents surplus.
Embodiment 4
The composition range of iron-base nanometer crystal alloy of the invention, we have done a series of experiments.It is of the invention high full
With the Fe of magnetic induction intensityxSiaBbPcNbdCueAlloy, wherein B can be by C, N, O, S, Sn, Ge, Ga, Al of below 5at%
At least one element portions are substituted.Table 3 is to carry out dispensing according to composition of the invention, and the raw material that will have been matched is put into induction melting
Stove or arc-melting furnace, are evacuated to 5 × 10-3Below Pa, then applying argon gas atmosphere protection, 30min is incubated after fusing makes alloy
Raw material is smelted into uniform molten steel, and injection mould cooling obtains the uniform alloy pig of composition;Master alloy ingot is crushed;Fritter is female
Molten steel is fused into alloy loading quartz ampoule, fusion temperature is 1550 DEG C or so, and band is got rid of with the speed of 30m/s in air, sprays band
Temperature is 1500 DEG C, and surface tension is 2N/m during spray band, and viscosity is 2mPas during spray band, and cooldown rate is 102DEG C/s, width is obtained
The AMORPHOUS ALLOY RIBBONS of 5mm, thickness 25um;Fritter foundry alloy is loaded molten steel is fused into quartz ampoule, fusion temperature is 1550 DEG C
Left and right, molten steel quickly cools down with copper mold casting method (cooling velocity is 10 in air2DEG C/s), casting temperature is 1500 DEG C, system
The non-crystaline amorphous metal bar of standby a diameter of 0.5~3.5mm;Amorphous alloy strips or bar are placed in heat-treatment furnace, at 530 DEG C
Reason 10min.The non crystalline structure of amorphous bar is determined with X-ray diffractometer (XRD).Alloy of the present invention is tested with Magnetic Test equipment
The magnetic property of band, its saturation induction density B is tested with vibrating specimen magnetometer (VSM)s, with DC B-H loop testing instrument
Test coercivity Hc, magnetic permeability μ is surveyed with electric impedance analyzer, measurement obtains the amorphous formation ability of alloy, and soft magnet performance is shown in Table 4.
Integrated embodiment can be seen that C, N, O, S, Sn, Ge, Ga, Al substitution B influences larger to material property.This shows following two
Individual aspect:1. soft magnet performance aspect, alloy property indices of the invention have no significant change, and particularly the addition of C is somewhat
The amorphous formation ability of soft magnet performance 2. aspect is optimized, amorphous formation ability is not substantially reduced.Integrated embodiment can be seen that
C, N, O, S, Sn, Ge, Ga, Al do not have substantial effect to the system soft magnet performance and amorphous formation ability, and these elements are
The usual impurities element of industrial raw material, illustrates that the alloy system is very high to the degrees of tolerance of C, N, O, S, Sn, Ge, Ga, Al,
This substantially reduces the requirement to material purity and production technology, is very beneficial for industrialized production.
Alloy and its performance prepared by 4 embodiment of table 4
In table, subscript bal. represents surplus.
Embodiment 5
The present embodiment prepares the Fe of high saturated magnetic induction using single-roller methodbal.Si6B6P3Nb2Cu0.75Alloy, in difference
Viscosity, surface tension, spray tape speed carry out spray band, and design parameter is referring to table 5.Dispensing is carried out according to alloying component, will be matched
Raw material be put into induction melting furnace or arc-melting furnace, be evacuated to 5 × 10-3Below Pa, then applying argon gas atmosphere protection, melts
Insulation 30min makes alloy raw material be smelted into uniform molten steel afterwards, and injection mould cooling obtains the uniform alloy pig of composition;Mother is closed
Ingot is crushed;Fritter foundry alloy is loaded molten steel is fused into quartz ampoule, fusion temperature is 1550 DEG C or so, with 10- in air
The speed of 40m/s gets rid of band, and spray band temperature is 1400 DEG C, width 5mm, the AMORPHOUS ALLOY RIBBONS of different-thickness is obtained, by non-crystaline amorphous metal
Band is placed in heat-treatment furnace, 530 DEG C for the treatment of 10min.The non crystalline structure of amorphous bar is determined with X-ray diffractometer (XRD).
The magnetic property of alloy strip steel rolled stock of the present invention is tested with Magnetic Test equipment, its saturation magnetic strength is tested with vibrating specimen magnetometer (VSM)
Answer intensity Bs, coercivity H is tested with DC B-H loop testings instrumentc, magnetic permeability μ is surveyed with electric impedance analyzer, measurement obtains alloy
Amorphous formation ability, soft magnet performance is shown in Table 5.Integrated embodiment can be seen that surface tension, viscosity, spray tape speed to material
Can influence larger.This shows following two aspects:1. in terms of soft magnet performance, the non-crystal bar that low viscosity and spray tape speed high are formed
Carrying magnetic can be excellent;2. in terms of amorphous formation ability, high viscosity and low spray tape speed advantageously form amorphous thicker strip.It is comprehensive to implement
Example is it can be seen that spray band process must carry out Reasonable Regulation And Control to surface tension, viscosity, spray tape speed three.
Alloy and its performance prepared by 5 embodiment of table 5
Claims (21)
1. a kind of Fe-based nanocrystalline magnetically soft alloy of strong amorphous formation ability, the expression formula of the alloy is FexSiaBbPcNbdCue,
X, a, b, c, d and e represent the atom percentage content of each correspondence component respectively in the expression formula, and meet following condition:0.5
≤ a≤12,0.5≤b < 5,0.5≤c≤12,0.1≤d≤3,0.1≤e≤3,70≤x≤85, x+a+b+c+d+e=
100%.
2. Fe-based nanocrystalline magnetically soft alloy according to claim 1, it is characterised in that the atomic percent of the component Fe
The span of content x is 76≤x≤82.
3. Fe-based nanocrystalline magnetically soft alloy according to claim 1, it is characterised in that the atomic percent of the component Si
The span of content a is 2≤a≤10.
4. Fe-based nanocrystalline magnetically soft alloy according to claim 1, it is characterised in that the atomic percent of the component B
The span of content b is 2≤b < 5.
5. Fe-based nanocrystalline magnetically soft alloy according to claim 1, it is characterised in that the atomic percent of the component P
The span of content c is 2≤c≤6.
6. Fe-based nanocrystalline magnetically soft alloy according to claim 1, it is characterised in that the atomic percent of the component Nb
The span of content d is 0.5≤d≤2.5.
7. Fe-based nanocrystalline magnetically soft alloy according to claim 1, it is characterised in that the atomic percent of the component Cu
The span of content e is 0.5≤e≤1.5.
8. Fe-based nanocrystalline magnetically soft alloy according to claim 1, it is characterised in that the component Nb by Zr, Ti, Ta,
At least one element portions or replacing whole in Hf, V, W, Mo, Mn, Cr, Zn, wherein the element of the replacement Nb is in the iron
Atom percentage content in base nanometer crystal magnetically soft alloy is less than 3%.
9. Fe-based nanocrystalline magnetically soft alloy according to claim 1, it is characterised in that the component B by C, N, O, S, Sn,
At least one element portions or replacing whole in Ge, Ga, Al, wherein the element of the replacement B is soft in the iron based nano crystal
Atom percentage content in magnetic alloy is less than 5%.
10. Fe-based nanocrystalline magnetically soft alloy according to claim 1, it is characterised in that the component Cu can by Au and/or
Ag is partly or entirely substituted, wherein atomic percent of the element of the replacement Cu in the Fe-based nanocrystalline magnetically soft alloy contains
Measure is less than 3%.
A kind of preparation method of any described Fe-based nanocrystalline magnetically soft alloys of 11. claim 1-10, it is characterised in that including
Following steps:
Step one, is matched somebody with somebody by the atom percentage content of each component in any described alloy expression formulas of claim 1-10
Material;
Step 2, is filled with the step under the atmosphere of protective gas using induction melting furnace or arc-melting furnace after evacuation
The one raw material melting for preparing is uniform, and furnace cooling or injection mould are cooled to master alloy ingot;
Step 3, the master alloy ingot that the step 2 is obtained is crushed;
Step 4, the fritter master alloy ingot after crushing is fused into molten steel, is then prepared using single-roller method, casting or atomization
Go out the Fe base noncrystal alloy materials of respective shapes;
Step 5, the Fe base noncrystal alloys material is heat-treated in heat-treatment furnace, wherein, the heat treatment time is
5-120min, the heat treatment temperature is 400-600 DEG C.
12. preparation methods according to claim 11, it is characterised in that in the step one, used during the dispensing
Material purity is more than 99.5%.
13. preparation methods according to claim 11, it is characterised in that in the step 2, it is described vacuumize it is true
Reciprocal of duty cycle is less than 5 × 10-3Pa, the atmosphere of the protective gas is nitrogen or argon gas atmosphere, and the smelting time is 30-40min,
And 5-30min is incubated after being melted down so that alloy raw material melting is uniform.
14. preparation methods according to claim 11, it is characterised in that in the step 4, using the single-roller method
Molten steel is quickly cooled down to prepare the Fe base noncrystal alloy bands that thickness is as 10-200 μm;It is using the casting that molten steel is quick
Cool down to prepare the Fe base noncrystal alloy bars of a diameter of 0.5-3.5mm.
15. preparation methods according to claim 14, it is characterised in that the atmosphere when single-roller method prepares band is nitrogen
Gas, argon gas or air;The atmosphere when casting prepares bar is nitrogen, argon gas or air.
16. preparation methods according to claim 14, it is characterised in that the rotating speed when single-roller method prepares band is
10-40m/s, spray band temperature is 1100-1550 DEG C, and surface tension is more than 0.5N/m during spray band, and viscosity is more than during spray band
0.5mPas;The casting temperature when casting prepares bar is 1250-1600 DEG C.
17. preparation method according to any one of claim 14-16, it is characterised in that described in the step 4
The fusion temperature that fritter master alloy ingot after broken is fused into molten steel is 1000-1600 DEG C.
18. preparation methods according to claim 11, it is characterised in that in the step 4, prepare the Fe bases non-
Required critical cooling rate 10 when peritectic alloy band or the Fe base noncrystal alloys bar2-103℃/s。
19. preparation methods according to claim 11, it is characterised in that in the step 5, the heat treatment temperature
It it is 450 DEG C -550 DEG C, heat treatment time is 20-70min.
20. preparation methods according to claim 11, it is characterised in that the Fe base noncrystal alloy materials of the respective shapes
It is strip, block or powdered alloy material.
21. Fe-based nanocrystalline magnetically soft alloys prepared using any described methods of claim 11-20 are preparing electronic device
Application in terms of iron core.
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