CN102304669A - Iron-based nanocrystalline soft magnetic alloy with high saturation magnetic induction and low cost - Google Patents
Iron-based nanocrystalline soft magnetic alloy with high saturation magnetic induction and low cost Download PDFInfo
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Abstract
The invention relates to an iron-based nanocrystalline soft magnetic alloy. The alloy is characterized in that: the alloy meets the following relation in composition: FeaBbCcMdCue, wherein M represents one or more of Si, Al, Cr and Mn, the subscripts a, b, c, d and e represent the atom percents of the corresponding elements of the alloy respectively and meet the following conditions: 78<=a<=88, 4<=b<=16, 3<=c<=10, 0<=d<=8, 0.3<=e<=1.5 and a+b+c+d+e=100. The iron-based nanocrystalline alloy consists of an amorphous matrix phase and a nanocrystalline phase. The alloy is obviously characterized in that: the alloy has excellent soft magnetic performances such as high saturation magnetic induction, low coercivity, low loss and the like; and the alloy does not contain precious metal elements and volatile elements, thereby reducing the processing cost of the raw materials and bringing convenience to popularization and application. The invention also relates to a preparation method of the alloy.
Description
Technical field
The present invention relates to a kind of high saturated magnetic induction Fe-based nanocrystalline magnetically soft alloy cheaply that has.The invention still further relates to the preparation method of this Fe-based nanocrystalline magnetically soft alloy.
Background technology
Magneticsubstance has energy and information translation, transmission, storage or changes the function of energy and information state, is important functional material, and they are widely used in fields such as machinery, electronics, electric power, communication and instrument.Wherein, the magneticsubstance that coercive force is low, magnetic permeability is high is called soft magnetic materials, and it is the widely used one type of magneticsubstances of industry such as electric power, motor and electronics.The equipment great majority of considering the soft magnetic materials manufacturing are under the alternating magnetic field condition, to work, require usually that its volume is little, power is big, highly sensitive, thermal value is few, good stability.For this reason, soft magnetic materials itself should possess several pacing itemss such as high saturated magnetic induction, low-coercivity, high magnetic permeability, hang down magnetic loss, high stability and Tc etc.1885, Ewing delivered the result of study about pure iron magnetic, indicated the generation of soft magnetic materials.In the same year, Westinghouse has invented alternative electric generation and power transmission method.The 19th-century end, Hadfield successfully smelts the Fe-Si alloy, and development of electric power industry has been played critical promoter action.Up to the present; For the soft magnetic materials of widespread use on the engineering, because of it uses power, the demands of different of frequency and different metal soft magnetic material (like technically pure iron, silicon steel, permalloy), soft magnetic ferrite, amorphous and the nano crystal soft magnetic materials of being divided into of material magnetic properties.
Nano crystal soft magnetic material is one type of novel soft magnetic materials, and it is by noncrystal substrate and be distributed in the crystal grain that has nano-grade size on the matrix and form, and can obtain by non-crystaline amorphous metal is partially-crystallized.Its performance has had both the multiple advantages such as low-coercivity, high magnetic permeability and low-loss of the high saturated magnetic induction and the amorphous soft magnetic material of traditional crystalline state soft magnetic materials.Nano crystal soft magnetic material can satisfy the demand of each class of electronic devices to high-efficiency and high-energy saving, the development of integrated aspect, and preparation is simple, with low cost, is called as " third generation soft magnetism " material.Research starts from 1988 to nano crystal soft magnetic material; Research through two more than ten years; At present nano-crystal soft magnetic alloy mainly contain three individual system: Fe-Si-B-M-Cu (M=Nb, Mo, W, Ta etc.) be FINEMET alloy, Fe-M-B-(Cu) be (M=Zr, Hf, Nb etc.) NANOPERM alloy and (Fe, Co)-M-B-Cu is (M=Zr, Hf, Nb etc.) HITPERM alloy.
Wherein, the FINEMET alloy is owing to its high magnetic permeability, and characteristics such as low-loss have just begun to put in the industrial application since research and development.But its saturation induction density is lower, the Fe that over-all properties is best
73.5Cu
1Nb
3Si
13.5B
9The alloy saturation induction density is merely 1.24T, thereby has limited its range of application.NANOPERM alloy saturation induction density is higher, has reached 1.6T, and magnetostriction coefficient is extremely low, levels off to zero, greatly reduces its stress sensitivity.With FINEMET alloy phase ratio, the loss of NANOPERM alloy is bigger, is permalloy but be superior to Fe-Ni, can under high frequency, use.NANOPERM alloy disadvantage is that processibility is relatively poor, because Zr element chemistry character is active, and very easily oxidation in atmosphere under the high temperature.Therefore, when the preparation amorphous, vacuum tightness is had relatively high expectations, need argon shield, thereby the NANOPERM alloy does not obtain real applying so far as yet.The HITPERM alloy partly substitutes Fe with Co at first and obtains on the basis of NANOPERM alloy, its crystallization is the α-FeCo of body-centered cubic structure mutually.Because the existence of α-FeCo makes it to have the high-temperature magnetic ability more excellent than preceding two kinds of alloys.The HITPERM alloy system has high saturation induction density, and high frequency characteristics also is superior to the NANOPERM alloy, but its coercive force is up to 200A/m, and loss is also bigger.The same with the NONAPERM alloy simultaneously owing to contain the Zr element, processibility is relatively poor, thereby is also applied so far.
Another drawback of above-mentioned nano-crystal soft magnetic alloy three individual system is all to contain precious metal element such as Nb, Zr and Hf etc. in the alloy system and tooling cost is high.For this reason, the scientific research personnel is on existing alloy system basis, and through optimal preparation technology, the adjustment alloying constituent is researched and developed new alloy system and improved nanocrystalline soft magnetic performance, cuts down finished cost simultaneously.
One Chinese patent application CN 101255506A discloses a kind of method of manufacture and nanometer crystal alloy of super-magnetic conducting nanocrystalline alloy.Chemical ingredients comprises Fe, Cu, Nb, Si, five kinds of elements of B, and concrete atom % content is: Fe=72.5-74.5%; Cu=0.5-1.5%; Nb=2.5-3.5%; Si=12.5-14.5%; B=8-10%.Its production technique reduces the content of alloy inclusions, oxygen and oxide compound for adding carbon and silicon calcium powder in the course of processing carry out deoxidation treatment, thereby has improved the magnetic permeability of nanometer crystal alloy effectively.But the saturation induction density of alloy is not high, and the course of processing is complicated, is difficult to control.
One Chinese patent application CN 101104907A discloses the nano-crystal soft-magnetic Fe with high-curie temperature
44Co
43-xZr
7B
5Al
1+xAlloy.The Al element replaces the Cu element and part replaces the Co element through adding, and the Tc of alloy has been brought up to more than 1000 ℃, and reduced coercive force.But good comprehensive properties Fe wherein
44Co
41Zr
7B
5Al
3The alloy saturation induction density is merely 163emu/g, and Fe
44Co
37Zr
7B
5Al
7Saturation induction density is higher, but coercive force is up to 70A/m.
One Chinese patent application CN 101834046A discloses high saturation magnetization intensity Fe-based nanocrystalline magnetically soft alloy material and preparation method thereof.The chemical ingredients of alloy is Fe
xSi
yB
zP
aCu
b, concrete atom % content is: Fe=70-90%; Si=1-15%; B=1-20%; P=1-20%; Cu=0.1-1%.This invention is added through the content of raising Fe element and the mixing of P element and Cu element; Through suitable crystallization and thermal treatment; The saturated magnetic induction of the nano-crystal soft magnetic alloy that obtains is up to 1.90T; Coercive force is lower than 9.4A/m, has abandoned precious metal element such as Nb, Zr simultaneously thereby has reduced the cost of alloy.But this alloy system contains a small amount of volatile element P, and alloying constituent is difficult to accurate control, thereby has limited its industrial application to a certain extent.
One Chinese patent application CN 101629265A discloses the Fe-based nanocrystalline magnetically soft alloy of a kind of low cost, high soft magnetic performance.The chemical ingredients of alloy is expressed as with atom %: Si=6-9%; B=4-7%; P=3-6%; Cu=0.5-1.5%; Nb=0.05-0.15%; All the other are Fe.Through reducing the consumption of precious metal element Nb, partly replace the cost that B reduces alloy with cheap P element simultaneously, obtain having the nano-crystal soft magnetic alloy of excellent soft magnetic performance after utilizing the acting in conjunction of P and Cu that non-crystaline amorphous metal is annealed.But this alloy system has also limited its industrial application because of containing volatile element phosphorus.
One Chinese patent application CN 101840763A discloses a kind of Fe-based nanocrystalline magnetically soft alloy of high saturated magnetic induction.Chemical ingredients is FeT
aB
bCu
cC
dM
e, concrete atom % content is: 0.002≤a≤5; 2≤b≤18; 0.02≤c≤5; 0.002≤d≤3; 0.02≤e≤20; All the other are Fe and unavoidable impurities.The non-retentive alloy amorphous formation ability of this invention is strong, and saturation induction density is higher than 1.5T, and soft magnetic performance is excellent.But this alloy system contains among small amount of precious metals element Zr, Ta, Hf, Nb, W, the Cr etc. one or more, or contains volatile element P, thereby is also applied.
Along with developing rapidly of modern communication, electron electric power industry, the high-tension transmission circuit increases day by day, to the also sharp increase day by day of demand of magnetic apparatuses such as high-frequency inductor, high frequency switch power, high-frequency transformer.And along with the raising that these magnetic device accuracy, safety coefficient and production cost etc. are required, traditional crystalline state soft magnetic materials such as ferrite, silicon steel, permalloy etc. can't meet the demands.
The development and application of nano crystal soft magnetic material; Largely promoted the electron electric power industrial expansion; Yet development from present nano crystal soft magnetic material; It is not very high having some defectives such as saturation induction density generally, particularly can't realize high saturated magnetic induction, low-coercivity and low-loss simultaneously; In addition, all contain one or more of precious metal elements such as Nb, Zr, Hf, Co in the alloy system, or contain volatile element P, the higher or alloying constituent of the tooling cost of alloy is difficult to control, thereby has limited its industrial application.
Therefore, develop a kind of soft magnetic propertys such as high saturated magnetic induction, low-coercivity and low-loss that have concurrently, do not contain precious metal element and volatile element again simultaneously, cheap soft magnetic materials easy to utilize is most important.
Summary of the invention
Technical problem to be solved by this invention is to the above-mentioned state of the art, and a kind of Fe-based nanocrystalline magnetically soft alloy is provided, and this alloy can satisfy a kind of in the following requirement at least, and has preferably satisfied the multiple even whole requirements in the following requirement.Said requirement is a high saturated magnetic induction, low-coercivity, and low-loss does not contain precious metal element and volatile element, and cheap.
Another technical problem to be solved by this invention provides the preparation method of this Fe-based nanocrystalline magnetically soft alloy.
In one embodiment of the invention, a kind of Fe-based nanocrystalline magnetically soft alloy is provided, has it is characterized in that alloy composition satisfies relational expression: Fe
aB
bC
cM
dCu
e, M is selected among Si, A1, Cr and the Mn one or more in the formula, and subscript a, b, c, d, e represent the atomic percent of each corresponding alloying element respectively, and meet the following conditions: 78≤a≤88; 4≤b≤16; 3≤c≤10; 0≤d≤8; 0.3≤e≤1.5; A+b+c+d+e=100, said iron-base nanometer crystal alloy is by noncrystal substrate phase and nanocrystalline phase composite.
In another embodiment of the invention, the invention provides a kind of preparation method of high saturated magnetic induction low cost iron based nano crystal non-retentive alloy, this method comprises the steps:
(1) Fe in the alloy compositions, B, C, M and Cu element are pressed alloy composition relational expression Fe
aB
bC
cM
dCu
ePrepare burden, M is one or more among Si, Al, Cr, the Mn in the formula, and subscript a, b, c, d, e represent the atomic percent of each corresponding alloying element respectively, and meet the following conditions: 78≤a≤88; 4≤b≤16; 3≤c≤10; 0≤d≤8; 0.3≤e≤1.5; A+b+c+d+e=100; (2) said alloy raw material is placed melting in the smelting apparatus, obtain alloy pig thus;
(3) alloy pig that obtains is carried out fragmentation;
(4) with the alloy pig after the fragmentation pack into the bottom leave in the silica tube of nozzle, prepare the successive non-crystaline amorphous metal through single roller quench;
(5) said non-crystaline amorphous metal is packed into heat-treat in the heat treatment furnace, then quench cooled obtains said Fe-based nanocrystalline magnetically soft alloy to room temperature, and said iron-base nanometer crystal alloy by noncrystal substrate mutually and nanocrystalline phase composite.
Compared with prior art; The invention has the advantages that: the Fe-based nanocrystalline magnetically soft alloy with alloy composition of the present invention possesses high saturated magnetic induction simultaneously; Low-coercivity, the soft magnetic performance that low-loss etc. are excellent, and do not contain precious metal element and volatile element; Reduced raw-material tooling cost, easy to utilize.
Description of drawings
Fig. 1 is Fe in the embodiment of the invention 1
83B
10C
6Cu
1The X-ray diffraction pattern of amorphous and nanometer crystal alloy.
Fig. 2 is Fe in the embodiment of the invention 1
83B
10C
6Cu
1The DSC curve of non-crystaline amorphous metal.
Fig. 3 is Fe in the embodiment of the invention 1
83B
10C
6Cu
1The magnetic hysteresis loop of nanometer crystal alloy and coercive force.
Fig. 4 is Fe in the embodiment of the invention 2
82.7B
10C
6Cu
1.3The X-ray diffraction pattern of amorphous and nanometer crystal alloy.
Fig. 5 is the TEM bright field image and the SEAD style of nanometer crystal alloy in the embodiment of the invention 2.
Fig. 6 is Fe in the embodiment of the invention 3
83B
10C
4Si
2Cu
1The X-ray diffraction pattern of amorphous and nanometer crystal alloy.
Fig. 7 is Fe in the embodiment of the invention 3
83B
10C
4Si
2Cu
1The DSC curve of non-crystaline amorphous metal.
Fig. 8 is Fe in the embodiment of the invention 3
83B
10C
4Si
2Cu
1The magnetic hysteresis loop of nanometer crystal alloy and coercive force.
Fig. 9 is Fe in the embodiment of the invention 3
83B
10C
4Si
2Cu
1The nanometer crystal alloy loss is with the magnetic induction density change curve.
Embodiment
The invention provides following specific embodiments and all possible combination between them.From succinct purpose, the application does not put down in writing the various concrete array mode of embodiment one by one, but will be understood that the application specifically puts down in writing and disclose all possible array mode of said technical scheme.
In one embodiment of the invention, a kind of Fe-based nanocrystalline magnetically soft alloy is provided, has it is characterized in that alloy composition satisfies relational expression: Fe
aB
bC
cM
dCu
e, M is selected among Si, Al, Cr and the Mn one or more in the formula, and subscript a, b, c, d, e represent the atomic percent of each corresponding alloying element respectively, and meet the following conditions: 78≤a≤88; 4≤b≤16; 3≤c≤10; 0≤d≤8; 0.3≤e≤1.5; A+b+c+d+e=100, said iron-base nanometer crystal alloy is by noncrystal substrate phase and nanocrystalline phase composite.
In a preferred embodiment of the present invention, the invention provides a kind of Fe-based nanocrystalline magnetically soft alloy, it is characterized in that M is Si and be selected among Al, Cr and the Mn one or more, preferred L is Si.
In a preferred embodiment of the present invention, the invention provides a kind of Fe-based nanocrystalline magnetically soft alloy, wherein the atomic percent of Fe is preferably 80≤a≤87, more preferably 82≤a≤86.
In a preferred embodiment of the present invention, the invention provides a kind of Fe-based nanocrystalline magnetically soft alloy, wherein the atomic percent of B is preferably 6≤b≤12, more preferably 7≤b≤10.
In a preferred embodiment of the present invention, the invention provides a kind of Fe-based nanocrystalline magnetically soft alloy, wherein the atomic percent of C is preferably 2≤c≤8, more preferably 3≤c≤6.
In a preferred embodiment of the present invention, the invention provides a kind of Fe-based nanocrystalline magnetically soft alloy, wherein the atomic percent of M is preferably d≤5, more preferably d≤3.
In a preferred embodiment of the present invention, the invention provides a kind of Fe-based nanocrystalline magnetically soft alloy, wherein the atomic percent of Cu is preferably 0.3≤e≤1.3, more preferably 0.5≤e≤1.3.
In a preferred embodiment of the present invention, the invention provides a kind of Fe-based nanocrystalline magnetically soft alloy, the grain-size of wherein said nanometer crystalline phase is between 5-30nm.
In a preferred embodiment of the present invention, the invention provides a kind of Fe-based nanocrystalline magnetically soft alloy, wherein the saturation induction density of this alloy is 1.7-1.9T, is preferably 1.73-1.83T; Coercive force is 4-17A/m, is preferably 4.5-16.5A/m.
In a preferred embodiment of the present invention, the invention provides a kind of Fe-based nanocrystalline magnetically soft alloy, wherein this alloy is at 1.0T, and the loss under 50Hz, 400Hz and the 1kHz condition is respectively 0.27-0.51W/kg, 3.6-6.9W/kg and 11.3-20.3W/kg.
In another embodiment of the invention, the invention provides a kind of preparation method of high saturated magnetic induction low cost iron based nano crystal non-retentive alloy, this method comprises the steps:
(1) Fe in the alloy compositions, B, C, M and Cu element are pressed alloy composition relational expression Fe
aB
bC
cM
dCu
ePrepare burden, M is one or more among Si, Al, Cr, the Mn in the formula, and subscript a, b, c, d, e represent the atomic percent of each corresponding alloying element respectively, and meet the following conditions: 78≤a≤88; 4≤b≤16; 3≤c≤10; 0≤d≤8; 0.3≤e≤1.5; A+b+c+d+e=100;
(2) said alloy raw material is placed melting in the smelting apparatus, obtain alloy pig thus;
(3) alloy pig that obtains is carried out fragmentation;
(4) with the alloy pig after the fragmentation pack into the bottom leave in the silica tube of nozzle, prepare the successive non-crystaline amorphous metal through single roller quench;
(5) said non-crystaline amorphous metal is packed into heat-treat in the heat treatment furnace, then quench cooled obtains said Fe-based nanocrystalline magnetically soft alloy to room temperature, and said iron-base nanometer crystal alloy by noncrystal substrate mutually and nanocrystalline phase composite.
In a preferred embodiment of the present invention, the invention provides a kind of preparation method, wherein in step (1), the purity of each raw material is all greater than 99%, and C adds with the form of iron-carbon, and the quality percentage composition of C is 4.0-4.6% in this iron-carbon.
In a preferred embodiment of the present invention, the invention provides a kind of preparation method, wherein in step (2), melting is arc melting or the induction melting that under protection of inert gas atmosphere, carries out.
In a preferred embodiment of the present invention, the invention provides a kind of preparation method, wherein when adopting arc melting, said alloy raw material is put into the water jacketed copper crucible of arc-melting furnace, be evacuated to and be lower than 1.0 * 10
-2Pa, charging into rare gas element to air pressure then is 200-800mbar, preferred 500-700mbar, fusing back insulation 1-2 minute cools to the furnace then and solidifies.
In a preferred embodiment of the present invention, the invention provides a kind of preparation method, wherein repeat arc melting step 3-5 time, obtain the uniform alloy pig of composition.
In a preferred embodiment of the present invention, the invention provides a kind of preparation method, wherein when adopting induction melting, said alloy raw material is put into crucible, place the ruhmkorff coil of induction melting furnace, be evacuated to and be lower than 1.0 * 10
-2Pa, charging into rare gas element to air pressure then is-0.05--0.01MPa (relative pressure) that fusing back insulation 20-40 minute was poured molten alloy into the cooling frame internal cooling 5-10 minute then.
In a preferred embodiment of the present invention, the invention provides a kind of preparation method, wherein use vacuum quick quenching equipment under the protection of inert gas atmosphere, to carry out step (4).
In a preferred embodiment of the present invention, the invention provides a kind of preparation method, it is characterized in that the said non-crystaline amorphous metal of step (4) is a ribbon, preferred strip width is 1-5mm, and thickness is 20-25 μ m, and density is 7.4-7.7kg/m
3
In a preferred embodiment of the present invention, the invention provides a kind of preparation method, wherein in step (5); Under the protection of inert gas atmosphere, with the temperature rise rate of 0.3-3 ℃/s temperature is risen to 410-470 ℃, preferred 430-450 ℃; Be incubated 2-4 minute, quench cooled is to room temperature then.
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Preparation Fe
83B
10C
6Cu
1The nanometer crystal alloy band.
Concrete preparation method is following:
Step 1: with purity greater than 99% raw material Fe, B, C and Cu by iron-base nanometer crystal alloy component relationship formula Fe of the present invention
83B
10C
6Cu
1Prepare burden, wherein C adds with the form of iron-carbon, and the quality percentage composition of C is 4.26% in this iron-carbon.；
Step 2: the raw material that proportioning is good is put into the water jacketed copper crucible of arc-melting furnace, is evacuated to 5.0 * 10
-3Pa, charging into argon gas to air pressure then is that 600mbar carries out melting, continues melting 2 minutes after the fusing again, let then alloy with copper crucible be cooled to solidify after, rapidly with its upset, melt back 5 times obtains the uniform alloy pig of composition;
Step 3: the bottom of packing into after the alloy pig fragmentation that step 2 is obtained is left in the silica tube of nozzle, adopts single roller chilling belt-rejecting technology, and the speed with 40m/s in argon atmosphere is got rid of band, makes the AMORPHOUS ALLOY RIBBONS of wide about 1mm, thick about 21 μ m;
Step 4: the AMORPHOUS ALLOY RIBBONS that step 3 is obtained places silica tube, is evacuated to 5 * 10
-3Pa charges into argon gas to a normal atmosphere, then closed quartz tube; Silica tube is placed heat treatment furnace, rise to 430 ℃, be incubated 3 minutes, rapidly silica tube is taken out then and place quenching-in water to room temperature with the temperature rise rate of about 2 ℃/s.
Shown in Figure 1 is the XRD figure spectrum of alloy strip after prepared alloy strip of step 3 and the thermal treatment of process step 4.XRD adopts D8 Advance type polycrystalline X-ray diffractometer to measure, and step display 3 prepared alloy strips have the disperse diffraction peak of wideization among the figure, explain that this alloy strip is an amorphous structure.The crystallization peak has appearred in the alloy strip after the crystallization and thermal treatment, is body-centered cubic structure Fe mutually through analyzing this crystallization, and promptly α-Fe estimates that through the Scherrer formula its grain-size is about 15nm.Can find out that the alloy strip structure after the crystallization and thermal treatment is made up of amorphous phase and the nanocrystal that is distributed in the noncrystal substrate.
Shown in Figure 2 is the DSC curve of the prepared alloy strip of step 3.Wherein, the DSC curve adopts NETZSCH DSC 404C DSC to measure, and the temperature rise rate of measurement is 0.67 ℃/s.Can find out the first initial crystallization temperature T of AMORPHOUS ALLOY RIBBONS
X1Be 405 ℃, the second initial crystallization temperature T
X2It is 501 ℃.
Magnetic hysteresis loop and coercive force for alloy strip after the thermal treatment of process step 4 shown in Figure 3, wherein, magnetic hysteresis loop adopts vibrating sample magnetometer (VSM; Lakeshore7410) measure, be used for the saturation induction density of beta alloy, the illustration among the figure is the coercive force curve; (B-H Curve Tracer EXPH-100) measures, and can find out to adopt the dc magnetizing characteristic analyser; The saturation induction density of alloy is 1.78T, and coercive force is 5.1A/m.
Embodiment 2
Preparation Fe
82.7B
10C
6Cu
1.3The nanometer crystal alloy band.
Concrete preparation method is following:
Step 1: with purity greater than 99% raw material Fe, B, C and Cu by iron-base nanometer crystal alloy component relationship formula Fe of the present invention
82.7B
10C
6Cu
1.3Prepare burden, wherein C adds with the form of iron-carbon, and the quality percentage composition of C is 4.26% in this iron-carbon;
Step 2: the raw material that proportioning is good is put into the water jacketed copper crucible of arc-melting furnace, is evacuated to 5.0 * 10
-3Pa, charging into argon gas to air pressure then is that 600mbar carries out melting, continues melting 2 minutes after the fusing again, let then alloy with copper crucible be cooled to solidify after, rapidly with its upset, melt back 5 times obtains the uniform alloy pig of composition;
Step 3: the bottom of packing into after the alloy pig fragmentation that step 2 is obtained is left in the silica tube of nozzle, adopts single roller chilling belt-rejecting technology, and the speed with 40m/s in argon atmosphere is got rid of band, makes the AMORPHOUS ALLOY RIBBONS of wide about 1.2mm, thick about 21 μ m;
Step 4: the AMORPHOUS ALLOY RIBBONS that step 3 is obtained places silica tube, is evacuated to 5 * 10
-3Pa charges into argon gas to a normal atmosphere, then closed quartz tube; Silica tube is placed heat treatment furnace, rise to 430 ℃, be incubated 3 minutes, rapidly silica tube is taken out then and place quenching-in water to room temperature with the temperature rise rate of about 2 ℃/s.
Shown in Figure 4 is the XRD figure spectrum of alloy strip after prepared alloy strip of step 3 and the thermal treatment of process step 4.XRD adopts D8 Advance type polycrystalline X-ray diffractometer to measure, and step display 3 prepared alloy strips have the disperse diffraction peak of wideization among the figure, explain that this alloy strip is an amorphous structure.The crystallization peak has appearred in the alloy strip after the crystallization and thermal treatment, is body-centered cubic structure Fe mutually through analyzing this crystallization, and promptly α-Fe estimates that through the Scherrer formula its grain-size is about 25nm.Can find out that the alloy strip structure after the crystallization and thermal treatment is made up of amorphous phase and the nanocrystal that is distributed on the noncrystal substrate.
Shown in Figure 5 is alloy strip TEM bright field image and the SEAD styles of 430 ℃ of insulations after 3 minutes.Wherein, adopt Tecnai F20 type transmission electron microscope that the microtexture of sample is measured.Can find out that the structure of alloy is by noncrystal substrate and be distributed in the crystal grain that has nano-grade size on the matrix and form after the crystallization and thermal treatment, the size of this crystal grain is coincide with the X-ray diffraction analysis result about 20-25nm.
Embodiment 3
Preparation Fe
83B
10C
4Si
2Cu
1The nanometer crystal alloy band.
Concrete preparation method is following:
Step 1: with purity greater than 99% raw material Fe, B, C and Cu by iron-base nanometer crystal alloy component relationship formula Fe of the present invention
83B
10C
4Si
2Cu
1Prepare burden, wherein C adds with the form of iron-carbon, and the quality percentage composition of C is 4.26% in this iron-carbon;
Step 2: the raw material that proportioning is good is put into the water jacketed copper crucible of arc-melting furnace, is evacuated to 5.0 * 10
-3Pa, charging into argon gas to air pressure then is that 600mbar carries out melting, continues melting 2 minutes after the fusing again, let then alloy with copper crucible be cooled to solidify after, rapidly with its upset, melt back 4 times obtains the uniform alloy pig of composition;
Step 3: the bottom of packing into after the alloy pig fragmentation that step 2 is obtained is left in the silica tube of nozzle, adopts single roller chilling belt-rejecting technology, and the speed with 40m/s in argon atmosphere is got rid of band, makes the AMORPHOUS ALLOY RIBBONS of wide about 1.2mm, thick about 20 μ m;
Step 4: the AMORPHOUS ALLOY RIBBONS that step 3 is obtained places silica tube, is evacuated to 5 * 10
-3Pa charges into argon gas to a normal atmosphere, then closed quartz tube; Silica tube is placed heat treatment furnace, rise to 430 ℃, be incubated 3 minutes, rapidly silica tube is taken out then and place quenching-in water to room temperature with the temperature rise rate of about 2 ℃/s.
Shown in Figure 6 is the XRD figure spectrum of alloy strip after prepared alloy strip of step 3 and the thermal treatment of process step 4.XRD adopts D8 Advance type polycrystalline X-ray diffractometer to measure, and step display 3 prepared alloy strips have the disperse diffraction peak of wideization among the figure, explain that this alloy strip is an amorphous structure.The crystallization peak has appearred in the alloy strip after the crystallization and thermal treatment, and warp is analyzed this crystallization and is the solid molten body-centered cubic structure Fe that Si is arranged mutually, and promptly α-Fe (Si) estimates that through the Scherrer formula its grain-size is about 12nm.Can find out, form by amorphous phase and the nanocrystal that is distributed on the noncrystal substrate through the alloy strip structure after the crystallization and thermal treatment.
Shown in Figure 7 is the DSC curve of the prepared alloy strip of step 3.Wherein, the DSC curve adopts NETZSCH DSC 404C DSC to measure, and the temperature rise rate of measurement is 0.67 ℃/s.Can find out the first initial crystallization temperature T of AMORPHOUS ALLOY RIBBONS
X1Be 409 ℃, the second initial crystallization temperature T
X2It is 535 ℃.The alloy that the difference of alloy two initial crystallization temperatures is not more added Si increases to some extent, this shows that the crystallization warm area has been widened in the interpolation of Si element, and this helps that it is carried out crystallization and thermal treatment and separates out monophasic α-Fe (Si).
Magnetic hysteresis loop and coercive force for alloy strip after the thermal treatment of process step 4 shown in Figure 8, wherein, magnetic hysteresis loop adopts vibrating sample magnetometer (VSM; Lakeshore7410) measure, be used for the saturation induction density of beta alloy, the illustration among the figure is the coercive force curve; (B-H Curve Tracer EXPH-100) measures, and can find out to adopt the dc magnetizing characteristic analyser; The saturation induction density of alloy is 1.78T, and coercive force is 4.5A/m.
Shown in Figure 9 is with the magnetic induction density change curve through alloy loss after step 4 thermal treatment.Ac magnetization specificity analysis appearance (B-H Curve Tracer is adopted in loss; AC BH-100k) measures; Be used for the loss of beta alloy under different magnetic induction density and different frequency, can find out, the loss of alloy under power frequency is lower than silicon steel; At magnetic strength 1.0T, the loss under the frequency 50Hz is 0.27W/kg.
Each item performance of embodiment 1 to embodiment 3 and the part nano-crystal soft magnetic alloy that the present invention relates to is as shown in the table, and we have also chosen 4 groups of existing non-retentive alloys example as a comparison simultaneously.Wherein, Sequence number 3,5,7 is the corresponding embodiment of the invention 1,2,3 respectively; Sequence number 1,2,4,6,8,9,10 corresponding nanometer crystal alloys all adopt the preparation technology's preparation described in the patented technology scheme of the present invention, and wherein the thermal treatment temp of sequence number 1,2,4,6,8 is 430 ℃, and soaking time is 3 minutes; Sequence number 9 and 10 thermal treatment temp are 450 ℃, and soaking time is 2 minutes.Sequence number 11-14 is a performance non-retentive alloy Comparative Examples preferably in the prior art of choosing.By finding out Fe of the present invention in the table
aB
bC
cSi
dCu
eNano-crystal soft magnetic alloy, the higher (B of saturation induction density
s=1.73-1.83T); FINEMET in Comparative Examples 11 (non-patent literature: J.Appl.Phys.64 (1988), 6044.) is an alloy, coercive force lower (Hc=4.5-16.5A/m); Loss also lower (P10/50=0.27-0.51W/kg); Be superior to the silicon steel in the Comparative Examples 12 and 13 (non-patent literature: IEEE Proc.Pt.C:Gen.Trans.Distrib.133 (1986), 451. and J.Mater.Eng.11 (1989), 109).And with the FINEMET alloy ratio; Alloy of the present invention does not contain precious metal element Nb, and all acquisitions easily of the starting material that adopted, thereby cheap; With Comparative Examples 14 (non-patent literature: IEEE Trans.Magn.45 (2009); 4302) the Fe83.3Si4B8P4Cu0.7 nanometer crystal alloy ratio that provides in, alloy of the present invention does not contain volatile element P, thereby alloying constituent can accurately be controlled.
Wherein, P
10/50, P
10/400And P
10/1kRepresent magnetic strength 1.0T respectively, the loss under frequency 50Hz, 400Hz and the 1kHz.
Claims (20)
1. a Fe-based nanocrystalline magnetically soft alloy is characterized in that alloy composition satisfies relational expression: Fe
aB
bC
cM
dCu
e, M is selected among Si, Al, Cr and the Mn one or more in the formula, and subscript a, b, c, d, e represent the atomic percent of each corresponding alloying element respectively, and meet the following conditions: 78≤a≤88; 4≤b≤16; 3≤c≤10; 0≤d≤8; 0.3≤e≤1.5; A+b+c+d+e=100, said iron-base nanometer crystal alloy is by noncrystal substrate phase and nanocrystalline phase composite.
2. Fe-based nanocrystalline magnetically soft alloy according to claim 1 is characterized in that M is Si and be selected among Al, Cr and the Mn one or more, and preferred L is Si.
3. Fe-based nanocrystalline magnetically soft alloy according to claim 1, wherein the atomic percent of Fe is preferably 80≤a≤87, more preferably 82≤a≤86.
4. Fe-based nanocrystalline magnetically soft alloy according to claim 1, wherein the atomic percent of B is preferably 6≤b≤12, more preferably 7≤b≤10.
5. Fe-based nanocrystalline magnetically soft alloy according to claim 1, wherein the atomic percent of C is preferably 2≤c≤8, more preferably 3≤c≤6.
6. Fe-based nanocrystalline magnetically soft alloy according to claim 1, wherein the atomic percent of M is preferably d≤5, more preferably d≤3.
7. Fe-based nanocrystalline magnetically soft alloy according to claim 1, wherein the atomic percent of Cu is preferably 0.3≤e≤1.3, more preferably 0.5≤e≤1.3.
8. Fe-based nanocrystalline magnetically soft alloy according to claim 1, α-Fe (Si) nanometer crystalline phase that wherein said nanometer crystalline phase is a body-centered cubic structure.
9. Fe-based nanocrystalline magnetically soft alloy according to claim 1, the grain-size of wherein said nanometer crystalline phase is between 5-30nm.
10. according to each described Fe-based nanocrystalline magnetically soft alloy of claim 1-9, wherein the saturation induction density of this alloy is 1.7-1.9T, is preferably 1.73-1.83T; Coercive force is 4-17A/m, is preferably 4.5-16.5A/m.
11. according to each described Fe-based nanocrystalline magnetically soft alloy of claim 1-10, wherein this alloy is at 1.0T, the loss under 50Hz, 400Hz and the 1kHz condition is respectively 0.27-0.51W/kg, 3.6-6.9W/kg and 11.3-20.3W/kg.
12. the preparation method of a high saturated magnetic induction low cost iron based nano crystal non-retentive alloy, this method comprises the steps:
(1) Fe in the alloy compositions, B, C, M and Cu element are pressed alloy composition relational expression Fe
aB
bC
cM
dCu
ePrepare burden, M is one or more among Si, Al, Cr, the Mn in the formula, and subscript a, b, c, d, e represent the atomic percent of each corresponding alloying element respectively, and meet the following conditions: 78≤a≤88; 4≤b≤16; 3≤c≤10; 0≤d≤8; 0.3≤e≤1.5; A+b+c+d+e=100;
(2) said alloy raw material is placed melting in the smelting apparatus, obtain alloy pig thus;
(3) alloy pig that obtains is carried out fragmentation;
(4) with the alloy pig after the fragmentation pack into the bottom leave in the silica tube of nozzle, prepare the successive non-crystaline amorphous metal through single roller quench;
(5) said non-crystaline amorphous metal is packed into heat-treat in the heat treatment furnace, then quench cooled obtains said Fe-based nanocrystalline magnetically soft alloy to room temperature, and said iron-base nanometer crystal alloy by noncrystal substrate mutually and nanocrystalline phase composite.
13. according to the preparation method of claim 12, wherein in step (1), the purity of each raw material is all greater than 99%, C adds with the form of iron-carbon, and the quality percentage composition of C is 4.0-4.6% in this iron-carbon.
14. according to the preparation method of claim 12, wherein in step (2), melting is arc melting or the induction melting that under protection of inert gas atmosphere, carries out.
15. according to the preparation method of claim 12, wherein when adopting arc melting, said alloy raw material is put into the water jacketed copper crucible of arc-melting furnace, is evacuated to and is lower than 1.0 * 10
-2Pa, charging into rare gas element to air pressure then is 200-800mbar, preferred 500-700mbar, fusing back insulation 1-2 minute cools to the furnace then and solidifies.
16. according to the preparation method of claim 15, wherein repeat arc melting step 3-5 time, obtain the uniform alloy pig of composition.
17., wherein when adopting induction melting, said alloy raw material is put into crucible according to the preparation method of claim 12, place the ruhmkorff coil of induction melting furnace, be evacuated to and be lower than 1.0 * 10
-2Pa, charging into rare gas element to air pressure then is-0.05--0.01MPa (relative pressure) that fusing back insulation 20-40 minute was poured molten alloy into the cooling frame internal cooling 5-10 minute then.
18., wherein use vacuum quick quenching equipment under the protection of inert gas atmosphere, to carry out step (4) according to the preparation method of claim 12.
19. according to the preparation of claim 12, it is characterized in that the said non-crystaline amorphous metal of step (4) is a ribbon, preferred strip width is 1-5mm, thickness is 20-25 μ m, and density is 7.4-7.7kg/m
3
20. according to the preparation method of claim 12, wherein in step (5), under the protection of inert gas atmosphere, temperature is risen to 410-470 ℃ with the temperature rise rate of 0.3-3 ℃/s, preferred 430-450 ℃, be incubated 2-4 minute, quench cooled is to room temperature then.
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