CN107103976A - A kind of iron cobalt-based toughness nano-crystal soft magnetic alloy and preparation method thereof - Google Patents
A kind of iron cobalt-based toughness nano-crystal soft magnetic alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of iron cobalt-based toughness nano-crystal soft magnetic alloy and preparation method thereof, iron cobalt-based toughness nano-crystal soft magnetic alloy composition has following expression (Fe0.8Co0.2)aBbMc, wherein, M is Cr, Mo or Nb, and a, b and c represent the atomic percent of each component respectively, and a, b, c meet following condition:84≤a≤87,12≤b≤16,0≤c≤2, a+b+c=100, iron cobalt-based toughness nano-crystal soft magnetic alloy of the invention nano-crystal soft magnetic alloy different from the past, i.e., although iron cobalt-based toughness nano-crystal soft magnetic alloy of the invention is amorphous/nanocomposite structure, but bending toughness can be presented, doubling constantly, solves the bending brittleness problems of nano-crystal soft magnetic alloy.Meanwhile, the alloy have higher saturation induction density and superior soft magnet performance, and excellent mechanical performance and machinability, available for various iron core soft magnetic materials.
Description
Technical field
The invention belongs to magnetic functional material field, relate in particular to a kind of iron cobalt-based toughness nano-crystal soft magnetic alloy and its
Preparation method.
Background technology
Iron-base amorphous alloy material is a kind of new soft magnetic materials, by rapid solidification in atomic layer secondary control liquid gold
The arrangement of category, makes atomic arrangement keep the longrange disorder state of liquid metal.Because atomic arrangement is irregular, longrange disorder,
There is no a presence of crystal particle crystal boundary, thus amorphous soft magnetic material has low-loss, splendid mechanical performance, magnetic property and anti-corruption
The advantages of corrosion.
Nanocrystalline controllability is developed by non-crystaline amorphous metal, the more excellent amorphous/nanocrystalline composite construction of performance has been obtained soft
Magnetic material.For example, by the annealing to Fe-Si-B-Nb-Cu non-crystaline amorphous metals suitably, Yoshizawa has obtained amorphous
/ nanocomposite structure, i.e., be uniform-distribution with the crystal grain of about 10 nanometers of average grain diameter in the matrix of amorphous.They
It was found that, the alloy system can show excellent soft magnet performance.With Fe73.5Si13.5B9Nb3Cu1Exemplified by alloy, its coercivity
As little as 0.53A/m, magnetic conductivity is up to 100000, core loss as little as 280kW/m3.The alloy system is due to excellent soft
Magnetic property was named as FINEMET (Y.Yoshizawa, S.Oguma, K.Yamauchi. in successful commercialization in 1988
New Fe-based soft magnetic alloys composed of ultrafine grain structure.J.Appl.Phys.,64
(1988)6044-6046.)。
After this, large quantities of nano-crystal soft magnetic alloys come out one after another again.For example, Fe-M-B-Cu alloys and
Fe-Co-M-B-Cu alloys (M=Zr, Hf, Nb, Ta) were commercially used respectively in 1991 and 1999, were named as
NANOPERM(K.Suzuki,M.Kikuchi,A.Makino,A.Inoue,T.Masumoto,Changesin
Microstructure and Soft Magnetic-Properties of an Fe86Zr7B6Cu1Amorphous Alloy Upon
Crystallization, Mater.Trans., JIM, 32 (1991) 961-968.) and HITPERM (M.A.Willard, M.Q.
Huang,D.E.Laughlin,M.E.McHenry,J.O.Cross,V.G.Harris,C.Franchetti,Magnetic
properties of HITPERM(Fe,Co)88Zr7B4Cu1magnets,J.Appl.Phys.,85(1999)4421-4423.)。
NANOPERM has higher saturation induction density compared with FINEMET, and HITPERM is improved because of Co addition
Curie temperature, is more suitable for the application scenario of high temperature.
In the last few years, in order to meet the requirement that device is integrated, people, which are directed to exploitation, has more high saturated magnetic induction
Modern Nanocrystalline alloying component.For example, 2007, Ohta et al. is obtained in Fe-Si-B-Cu nanometer crystal alloys system
High saturated magnetic induction (M.Ohta, Y.Yoshizawa, Magnetic properties of more than 1.8T
nanocrystalline Fe82.65Cu1.35SixB16-xAlloys (x=0-7), Appl.Phys.Lett., 91 (2007) 062517.), and
Subsequent 2009, the Fe of Makino et al. exploitations81.7Si9B7P2Cu0.3Nanometer crystal alloy saturation induction density reaches 1.9
T(A.Makino,H.Men,T.Kubota,K.Yubuta,A.Inoue,New ExcellentSoft Magnetic
FeSiBPCu Nanocrystallized Alloys With High Bs of 1.9TFrom Nanohetero-Amorphous Phase,
IEEE T.Magn., 45 (2009) 4302-4305.), it is the peak of all nanometer crystal alloy reports at present.
But, different from non-crystaline amorphous metal, bending fragility (being broken after doubling) is presented in iron-base nanometer crystal alloy band, and this is
The problem of most serious that nanocrystalline material is faced.All the time, it is desirable to find to overcome the approach of this problem, but
Related achievement is but rarely reported.
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 cobalt-based toughness nano-crystal soft magnetic alloy and its system
Preparation Method, iron cobalt base amorphous alloy band annealed by direct melting-get rid of band method and under proper condition and obtains amorphous
The alloy strip of/nanocomposite structure, the alloy strip possesses bending toughness, and doubling is continuous.
The purpose of the present invention is achieved by following technical proposals.
A kind of iron cobalt-based toughness nano-crystal soft magnetic alloy, its composition has following expression (Fe0.8Co0.2)aBbMc, wherein, M
For Cr, Mo or Nb, a, b and c represent the atomic percent of each component respectively, and a, b, c meet following condition:
84≤a≤87,12≤b≤16,0≤c≤2, a+b+c=100.
In the above-mentioned technical solutions, the expression formula is (Fe0.8Co0.2)87B13、(Fe0.8Co0.2)86B14、(Fe0.8Co0.2)85B15、
(Fe0.8Co0.2)86B13Mo1、(Fe0.8Co0.2)85B14Mo1、(Fe0.8Co0.2)84B14Mo2、(Fe0.8Co0.2)85B14Cr1With
(Fe0.8Co0.2)85B14Nb1。
In the above-mentioned technical solutions, the iron cobalt-based toughness nano-crystal soft magnetic alloy between Curie temperature and crystallization temperature certain
It is annealed at a temperature of one and obtains amorphous/nanocrystalline composite construction, the alloy strip of the amorphous/nanocrystalline composite construction possesses bending
Toughness, is not broken after doubling.
In the above-mentioned technical solutions, before the Vickers hardness after the iron cobalt-based toughness nano-crystal soft magnetic alloy annealing is less than annealing
The Vickers hardness of single noncrystalline structure.
In the above-mentioned technical solutions, the saturation induction density (Bs) of annealed state alloy is 1.5-1.95T, coercivity (Hc)
Less than or equal to 25A/m.
In the above-mentioned technical solutions, the nano-crystalline granule that the iron cobalt-based toughness nano-crystal soft-magnetic is closed is evenly distributed on amorphous base
In body, the average grain diameter of the nano-crystalline granule is less than or equal to 5nm.
In the above-mentioned technical solutions, the average grain diameter of the nano-crystalline granule is 2-5nm.
The preparation method of above-mentioned iron cobalt-based toughness nano-crystal soft magnetic alloy, is prepared as steps described below:
Step 1, raw material is configured according to the composition expression formula of above-mentioned iron cobalt-based toughness nano-crystal soft magnetic alloy;
Step 2, vacuum is evacuated to less than or equal to 9.5 × 10-3Pa, under the protection of inert gas, step 1 is configured
Raw material be heated to being completely melt it is uniform after, be cooled to 20-25 DEG C of room temperature, master alloy ingot be made;
In step 2, raw material step 1 configured is heated to after being completely melt uniformly, is cooled to through 3~5 meltings
20-25 DEG C of room temperature, is made master alloy ingot.
In step 2, the master alloy ingot that step 2 is made is crushed to after 0.1-0.6mm, be cleaned by ultrasonic in alcohol
30-60min。
In step 2, the raw material configured using arc-melting furnace to step 1 is heated.
In step 2, vacuum is 6 × 10-3-8×10-3Pa。
Step 3, the master alloy ingot obtained by step 2 is melted again, at room temperature, using single roller under the protection of inert gas
Chilling method prepares alloy strip sample;
In step 3, the technological parameter that single roller chilling method prepares alloy strip sample is:Spraying pressure is
0.02-0.04Mpa, 800-1200 DEG C of injection temperation, copper roller rotating speed linear resonance surface velocity is 20-50m/s.
In step 3, the technological parameter that single roller chilling method prepares alloy strip sample is preferably:Spraying pressure is
0.02-0.03Mpa, 900-1100 DEG C of injection temperation, copper roller rotating speed linear resonance surface velocity is 30-40m/s.
In step 3, in single roller chilling method of alloy strip sample is prepared, master alloy ingot is placed in quartz ampoule
Row melts again.
In step 3, the mouth of pipe of the quartz ampoule is polishing to a diameter of 0.7-0.8mm with 1200-2000 sand paper.
In step 1,3, the inert gas is argon gas.
In step 3, the alloy strip sample thickness that prepared by the step 3 is 0.01-0.03mm.
Step 4, the alloy strip that step 3 is obtained is made annealing treatment, is placed in 20-30 DEG C of water and cools down rapidly after annealing
To generate the iron cobalt-based toughness nano-crystal soft magnetic alloy of the present invention, wherein, annealing temperature be Curie temperature and crystallization temperature it
Between.
In step 4, annealing temperature is 25K below crystallization temperature, either 50K below crystallization temperature or crystallization temperature
100K below 75K, or crystallization temperature below degree.
In step 4, it is less than or equal to 9.5 × 10 in vacuum-3Annealed under Pa.
In step 4, the time of annealing is 0.5-20 minutes.
In step 4, the annealing time is preferably 10-20 minutes.
Compared to prior art, iron cobalt-based toughness nano-crystal soft magnetic alloy of the invention nano-crystal soft-magnetic different from the past is closed
Gold, i.e., although iron cobalt-based toughness nano-crystal soft magnetic alloy of the invention is amorphous/nanocomposite structure, but can be presented curved
Toughness is rolled over, doubling constantly, solves the bending brittleness problems of nano-crystal soft magnetic alloy.Meanwhile, the alloy is satisfied with higher
With magnetic induction intensity and superior soft magnet performance, it is and excellent mechanical performance and machinability, soft available for various iron cores
Magnetic material.
Brief description of the drawings
Fig. 1 is (Fe0.8Co0.2)100-xBx(x=13,14,15) alloy X-ray diffractogram;
Fig. 2 is (Fe0.8Co0.2)100-xBx(x=13,14,15) different annealing conditions obtain the tough fragility summary of nanometer Jin Jing;
Fig. 3 is the (Fe of different annealing conditions0.8Co0.2)86B14X-ray diffractogram.
Fig. 4 is (Fe0.8Co0.2)100-xBx(x=13,14,15) state of quenching alloy Kissinger schemes;
Fig. 5 is (Fe0.8Co0.2)100-xBx(x=13,14,15) nanometer crystal alloy BH curve;
Fig. 6 is (Fe0.8Co0.2)86B14Nanometer crystal alloy transmission electron microscope photo;
Fig. 7 is (Fe0.8Co0.2)99-xBxMo1(x=13,14) state of quenching alloy DSC curve;
Fig. 8 is (Fe0.8Co0.2)99-xBxMo1(x=13,14) alloy sample X-ray diffractogram;
Fig. 9 is (Fe0.8Co0.2)85B14Mo1The relation of nanometer crystal alloy crystal volume fraction and hardness;
Figure 10 is (Fe0.8Co0.2)85B14Mo1Alloy Vickers hardness impression (a) is quenched state (b) annealed state;
Figure 11 is (Fe0.8Co0.2)99-xBxMo1(x=13,14) nanometer crystal alloy BH curve;
Figure 12 is (Fe0.8Co0.2)84B14Mo2State of quenching alloy DSC curve;
Figure 13 is (Fe0.8Co0.2)84B14Mo2State of quenching alloy X-ray diffractogram;
Figure 14 is (Fe0.8Co0.2)84B14Mo2The saturation induction density of nanometer crystal alloy difference annealing conditions, coercivity;
Figure 15 is (Fe0.8Co0.2)84B14Mo2Nanometer crystal alloy transmission electron microscope photo;
Figure 16 is (Fe0.8Co0.2)85B14M1(x=Cr, Nb) quenches state alloy X-ray diffractogram;
Figure 17 is (Fe0.8Co0.2)85B14M1Pattern photo after the bending of (x=Cr, Nb) nanometer crystal alloy;
Figure 18 is (Fe0.8Co0.2)85B14Nb1Stereoscan photograph near nanometer crystal alloy band folding line.
Embodiment
In an embodiment of the present invention, used raw material such as table 1;Wherein, the mouth of pipe of quartz ampoule 1200-2000 sand
Paper is polishing to a diameter of 0.7-0.8mm.
The preparing raw material information of table 1
The structural characterization for any iron cobalt-based toughness nano-crystal soft magnetic alloy that the present invention is obtained and performance test:
(1) alloy structure is characterized.The structure of alloy strip sample is detected with X-ray diffractometer (XRD).Amorphous knot
Structure should be single disperse peak, and amorphous/nanocrystalline composite construction should be disperse peak and sharp peak (bcc-Fe diffraction maximum)
Superposition.
(2) thermal parameters are measured.About 10-20mg band samples are shredded, it is real as being flattened in alumina crucible, with difference
Scanning calorimeter instrument (DSC) records the heating curve of alloy.At least one exothermic peak of DSC heating curves.(the first)
The initial temperature of exothermic peak is defined as crystallization temperature Tx。TxThe corresponding initial temperature in minor endothermic peak is Curie on curve before
Temperature Tc。
(3) bending toughness is characterized.The state that will quench alloy strip is in TcAnd TxBetween arbitrary temp anneal 0.5-20 minutes.Will
Alloy strip 180 degree doubling, will not fragment into two-section after the doubling of this series alloy, i.e., with bending toughness.
(4) Vickers hardness is measured.Alloy strip is pasted onto with chemical glue on slide and measures alloy with Vickers hardness instrument
Vickers hardness, load-up condition:Test force 0.05kgf, retention time 10s.And available observation by light microscope hardness test
The pattern of impression afterwards.
(5) magnetic parameter is measured.The state that will quench alloy strip is in TcAnd TxBetween arbitrary temp anneal 0.5-20 minutes.With
Vibration magnetometer (VSM) measures the hysteresis curve of alloy to obtain its saturation induction density;Alloy is measured with B-H instrument
Coercivity.Experiment is obtained, annealed state alloy saturation induction density (Bs) it is not less than 1.5T, coercivity (Hc) no
Higher than 25A/m.Preferably, BsReach as high as 1.95T.
Iron cobalt-based toughness nano-crystal soft magnetic alloy of the present invention and preparation method thereof is carried out with reference to the accompanying drawings and examples detailed
Describe in detail bright.
Embodiment 1
A kind of iron cobalt-based toughness nano-crystal soft magnetic alloy (Fe0.8Co0.2)100-xBxThe preparation method of (x=13,14,15), under
Step is stated to be prepared:
Step 1, according to composition the expression formula ((Fe of above-mentioned iron cobalt-based toughness nano-crystal soft magnetic alloy0.8Co0.2)87B13、
(Fe0.8Co0.2)86B14(Fe0.8Co0.2)85B15) atomic percent is converted into mass percent progress configuration raw material, weigh
High-purity Fe of respective quality, Co, B mix stand-by, Fe, and Co, B purity and manufacturer etc. are shown in Table 1.
Step 2, the raw material that step 1 is configured is placed in vacuum arc melting furnace, is evacuated to 9.5 × 10-3During Pa, it is filled with
Raw material, under the protection of argon gas, is heated to after dissolving completely uniformly, is cooled to 20-25 DEG C of room temperature by argon gas through 3 meltings,
Master alloy ingot is made;Master alloy ingot is crushed to 0.1-0.6mm, is put into alcohol and is cleaned by ultrasonic 45min.
Step 3, the master alloy ingot for fritter step 2 cleaned is placed in the stone with appropriately sized opening (0.7-0.8mm)
Ying Guanzhong, then the quartz ampoule is fixed in the induction coil of melting fast cooling device and (is used for heating), vacuum is evacuated to
9.5×10-3Argon gas is filled with during Pa as protective atmosphere, after master alloy ingot fusing, at room temperature, is prepared and closed using single roller chilling method
Gold bar band sample:It is sprayed onto what is rotated with linear resonance surface velocity 40m/s when about 1000 DEG C of temperature with 0.02MPa injection pressure
On copper roller, chilling prepares alloy strip (alloy strip thickness is 0.01~0.03mm).After usual after alloy strip cooling
To take out alloy strip sample after spray is completed 10 minutes.
Step 4, the alloy strip that step 3 is obtained is placed in quartz ampoule, vacuum is evacuated to 9.5 × 10-3Annealing furnace is put into during Pa
It is middle to be annealed, annealed between Curie temperature and crystallization temperature at a certain temperature, rapid take out is equipped with alloy bar after annealing
The quartz ampoule of band, and put into 20-30 DEG C of water and cool down rapidly.
The thermodynamic parameter of alloy is characterized with differential scanning calorimeter.Table 2 summarizes the crystalline substance of each two exothermic peaks of alloying component
Change temperature (Tx) and Curie temperature (Tc).According to the crystallization temperature and Curie temperature of each alloy in table 2, by step 4
In annealing conditions be set as each alloying component crystallization temperature (Tx1) following 75K, i.e., in the step 4 of embodiment 1,
A certain temperature is crystallization temperature (T between the Curie temperature and crystallization temperaturex1) following 75K, annealing time is 10min.
(the Fe of table 20.8Co0.2)100-xBx(x=13,14,15) the magnetics parameter after the thermal parameters and nano-crystallization of alloy
The phase structure of alloy strip is characterized with X-ray diffractometer.Fig. 1 is the X ray diffracting spectrum of sample, wherein
(Fe0.8Co0.2)86B14(Fe0.8Co0.2)85B15Alloy is not yet made annealing treatment, each only one of which disperse peak of its diffracting spectrum,
It is single amorphous phase to show its alloy structure;(Fe0.8Co0.2)87B13After the annealed processing of alloy, also detected on disperse peak
Crystallization peak, to illustrate its structure be amorphous/nanocomposite structure.(Fe0.8Co0.2)86B14(Fe0.8Co0.2)85B15Alloy exists
After annealing, diffracting spectrum is shown and (Fe0.8Co0.2)87B13The basically identical crystallization peak of alloy.
Fig. 2 summarizes (Fe0.8Co0.2)100-xBx(x=13,14,15) under different annealing temperature the architectural feature of each alloying component and
Tough fragility, specific data are shown in Table 3.Therefrom we are it can be found that non crystalline structure and partial nanocrystalline structure show bending
Toughness.Wherein, the structure (amorphous or nanocrystalline or crystal) of alloy is differentiated by XRD.As reference example,
Fig. 3 is illustrated on the premise of the 10min that anneals, (the Fe of different annealing conditions0.8Co0.2)86B14X-ray diffractogram.
Wherein, the diffraction maximum of non crystalline structure is single disperse peak, and the diffraction maximum of nanocrystalline structure occurs in that bcc-Fe on disperse peak
Crystallization peak.As seen from the figure, (Fe0.8Co0.2)86B14Annealing conditions are in 610K and 585K, and it is nanocrystalline structure,
In 560K, it is non crystalline structure.It can thus be concluded that, in the case where annealing time is certain, the temperature for improving annealing conditions can
So that non crystalline structure is transformed into nanocrystalline structure.
(the Fe of table 30.8Co0.2)100-xBx(x=13,14,15) different annealing conditions obtain the tough fragility summary of band
It can further be seen from figure 2 that with the increase of B content, the highest annealing temperature (T of toughness can be presented in nanometer crystal alloyd)
Also gradually increase, this is relevant with the heat endurance of different-alloy.Fig. 4 ties for the Kissinger figure fittings of each alloy of this example
Really, the crystallization activation energy (E obtainedk) it is listed in table 2.From table 2 it can be seen that increasing with B content, the crystallization of alloy
Temperature and crystallization activation energy are raised, and illustrate that the heat endurance of alloy is improved, and crystallization becomes difficult, TdAlso increase
It is big.
We are to Tx1(the Fe of -75K annealing0.8Co0.2)87B13、(Fe0.8Co0.2)86B14(Fe0.8Co0.2)85B15Alloy nano
Crystalline substance carries out magnetic characterization.Fig. 5 is the hysteresis curve of three kinds of alloys of the present embodiment 1, shows typical soft magnetic materials special
Levy.The B of two alloyssAnd HcIt is shown in Table 2.
The architectural feature of nanometer crystal alloy is further characterized by transmission electron microscope.Fig. 6 is (Fe0.8Co0.2)86B14Nanocrystalline is saturating
Penetrate electromicroscopic photograph.Nano-crystalline granule is evenly distributed in noncrystal substrate, and its average grain diameter is 5nm.
Embodiment 2
A kind of iron cobalt-based toughness nano-crystal soft magnetic alloy (Fe0.8Co0.2)99-xBxMo1The preparation method of (x=13,14), according to following
It is prepared by step:
Step 1, according to composition the expression formula ((Fe of above-mentioned iron cobalt-based toughness nano-crystal soft magnetic alloy0.8Co0.2)86B13Mo1
(Fe0.8Co0.2)85B14Mo1) atomic percent is converted into mass percent progress configuration raw material, weigh respective quality
High-purity Fe, Co, B, Mo mix stand-by, Fe, and Co, B, Mo purity and manufacturer etc. are shown in Table 1.
Step 2, the raw material that step 1 is configured is placed in vacuum arc melting furnace, is evacuated to 9.5 × 10-3During Pa, it is filled with
Raw material, under the protection of argon gas, is heated to after dissolving completely uniformly, is cooled to 20-25 DEG C of room temperature by argon gas through 3 meltings,
Master alloy ingot is made;Master alloy ingot is crushed to 0.1-0.6mm, is put into alcohol and is cleaned by ultrasonic 45min.
Step 3, the master alloy ingot for fritter step 2 cleaned is placed in the stone with appropriately sized opening (0.7-0.8mm)
Ying Guanzhong, then the quartz ampoule is fixed in the induction coil of melting fast cooling device and (is used for heating), vacuum is evacuated to
9.5×10-3Argon gas is filled with during Pa as protective atmosphere, after master alloy ingot fusing, at room temperature, is prepared and closed using single roller chilling method
Gold bar band sample:It is sprayed onto what is rotated with linear resonance surface velocity 40m/s when about 1000 DEG C of temperature with 0.02MPa injection pressure
On copper roller, chilling prepares alloy strip (alloy strip thickness is 0.01~0.03mm).After usual after alloy strip cooling
To take out alloy strip sample after spray is completed 10 minutes.
Step 4, the alloy strip that step 3 is obtained is placed in quartz ampoule, vacuum is evacuated to 9.5 × 10-3Annealing furnace is put into during Pa
It is middle to be annealed, annealed between Curie temperature and crystallization temperature at a certain temperature, rapid take out is equipped with alloy bar after annealing
The quartz ampoule of band, and put into 20-30 DEG C of water and cool down rapidly.
The thermodynamic parameter of alloy is characterized with differential scanning calorimeter.Fig. 7 is the DSC heating curves of alloy strip, each song
Line has two exothermic peaks, and it is two-step reaction to show crystallization process.The thermal parameters obtained according to Fig. 7, by step 4
In annealing conditions be set as each alloying component crystallization temperature (Tx1) following 75K, annealing time is 20 minutes.
The phase structure of alloy strip is characterized with X-ray diffractometer.Fig. 8 is the X ray diffracting spectrum of alloy sample, its
In (Fe0.8Co0.2)85B14Mo1Not yet by annealing, the diffracting spectrum only one of which disperse peak that its alloy is shows it
Alloy structure is single amorphous phase;(Fe0.8Co0.2)86B13Mo1Alloy is after the annealing of step 4, at disperse peak
On also detected crystallization peak, illustrate its structure division crystallization.The result of comparison example 1 can be seen that the knot for state alloy of quenching
Structure is mainly influenceed by B content.
Fig. 9 summarizes (Fe0.8Co0.2)85B14Mo1Alloy is in the case where annealing conditions are 586K, after different annealing times
Vickers hardness (Hv) allomeric volume fraction (Vf) relation.It can be seen that, the scope within 20%, with Vf
The Vickers hardness of increase alloy is gradually reduced.I.e. alloy there occurs annealing softening phenomenon, can be maintained it is presumed that this is alloy
The reason for toughness being bent after annealing.
Further Figure 10 is shown in the observation to Vickers hardness impression.Wherein Figure 10 (a) is the state (Fe that quenches0.8Co0.2)85B14Mo1Close
The impression photo of gold, state of quenching alloy is to have obvious skid wire around non crystalline structure, impression, and this is typical toughness material
Feature;Figure 10 (b) is (Fe after 586K (below 661K 75K, see Fig. 8) anneals 3 minutes0.8Co0.2)85B14Mo1
The impression photo of alloy, vickers indentation then shows skid wire and hallrcuts simultaneously, and its area of indentation is slightly larger than the pressure for state of quenching
Trace, i.e. hardness are lower.It is presumed that, the reduction of hardness may be relevant with the generation of hallrcuts after alloy annealing.
Figure 11 is the hysteresis curve after two kinds of alloys annealing of the present embodiment 2, shows typical soft magnetic materials feature.
(Fe0.8Co0.2)86B13Mo1Alloy and (Fe0.8Co0.2)85B14Mo1The B of alloysRespectively 1.93T and 1.88T, HcRespectively
For 20A/m and 23A/m.
Embodiment 3
A kind of iron cobalt-based toughness nano-crystal soft magnetic alloy (Fe0.8Co0.2)84B14Mo2Preparation method, give as steps described below
Prepare:
Step 1, according to the composition expression formula (Fe of above-mentioned iron cobalt-based toughness nano-crystal soft magnetic alloy0.8Co0.2)84B14Mo2By original
Sub- percentage is converted to mass percent and carries out configuration raw material, weighs high-purity Fe of respective quality, and Co, B, Mo mixing is treated
With Fe, Co, B, Mo purity and manufacturer etc. are shown in Table 1.
Step 2, the raw material that step 1 is configured is placed in vacuum arc melting furnace, is evacuated to 9.5 × 10-3During Pa, it is filled with
Raw material, under the protection of argon gas, is heated to after dissolving completely uniformly, is cooled to 20-25 DEG C of room temperature by argon gas through 3 meltings,
Master alloy ingot is made;Master alloy ingot is crushed to 0.1-0.6mm, is put into alcohol and is cleaned by ultrasonic 45min.
Step 3, the master alloy ingot for fritter step 2 cleaned is placed in the stone with appropriately sized opening (0.7-0.8mm)
Ying Guanzhong, then the quartz ampoule is fixed in the induction coil of melting fast cooling device and (is used for heating), vacuum is evacuated to
9.5×10-3Argon gas is filled with during Pa as protective atmosphere, after master alloy ingot fusing, at room temperature, is prepared and closed using single roller chilling method
Gold bar band sample:It is sprayed onto what is rotated with linear resonance surface velocity 40m/s when about 1000 DEG C of temperature with 0.02MPa injection pressure
On copper roller, chilling prepares alloy strip (alloy strip thickness is 0.01~0.03mm).After usual after alloy strip cooling
To take out alloy strip sample after spray is completed 10 minutes.
Step 4, the alloy strip that step 3 is obtained is placed in quartz ampoule, vacuum is evacuated to 9.5 × 10-3Annealing furnace is put into during Pa
It is middle to be annealed, annealed between Curie temperature and crystallization temperature at a certain temperature, rapid take out is equipped with alloy bar after annealing
The quartz ampoule of band, and put into 20-30 DEG C of water and cool down rapidly.The thermodynamic parameter of alloy is characterized with differential scanning calorimeter.
Figure 12 is the DSC heating curves of alloy strip, and curve has two exothermic peaks, and it is two-step reaction to show crystallization process.
Annealing conditions in step 4 are set as alloying component crystallization temperature (T by the thermal parameters obtained according to Figure 12x1) below
50K, annealing time is respectively 0.5,1,1.5 and 3 minutes.
The phase structure for state alloy strip of quenching, as shown in figure 13, the diffracting spectrum of state of quenching alloy are characterized with X-ray diffractometer
Mainly it is made up of a disperse peak, its alloy structure is mainly amorphous phase.Structure is amorphous/nanocrystalline composite junction after it is annealed
Structure (not shown).
Figure 14 is (Fe0.8Co0.2)84B14Mo2Saturation induction density (B after alloy difference annealing times), coercivity (Hc)
With the relation of annealing time.Obviously, increase with annealing time, alloy crystal volume fraction (Vf) it is also increased.I.e.
The B of alloysWith VfIncrease and increase.
Preferably, we observe (Fe0.8Co0.2)84B14Mo2The nanocrystalline structure that alloy is obtained after annealing half a minute
Feature.Figure 15 is its (Fe0.8Co0.2)86B14Nanocrystalline transmission electron microscope photo.Nano-crystalline granule is evenly distributed on amorphous base
In body, its average grain diameter is less than or equal to 5nm.
Embodiment 4
A kind of iron cobalt-based toughness nano-crystal soft magnetic alloy (Fe0.8Co0.2)85B14M1The preparation method of (M=Cr, Nb), under
Step is stated to be prepared:
Step 1, according to composition the expression formula ((Fe of above-mentioned iron cobalt-based toughness nano-crystal soft magnetic alloy0.8Co0.2)85B14Cr1With
(Fe0.8Co0.2)85B14Nb1) atomic percent is converted into mass percent progress configuration raw material, weigh the height of respective quality
Pure Fe, Co, B, Cr, Nb mix stand-by, Fe, and Co, B, Cr, Nb purity and manufacturer etc. are shown in Table 1.
Step 2, the raw material that step 1 is configured is placed in vacuum arc melting furnace, is evacuated to 9.5 × 10-3During Pa, it is filled with
Raw material, under the protection of argon gas, is heated to after dissolving completely uniformly, is cooled to 20-25 DEG C of room temperature by argon gas through 3 meltings,
Master alloy ingot is made;Master alloy ingot is crushed to 0.1-0.6mm, is put into alcohol and is cleaned by ultrasonic 45min.
Step 3, the master alloy ingot for fritter step 2 cleaned is placed in the stone with appropriately sized opening (0.7-0.8mm)
Ying Guanzhong, then the quartz ampoule is fixed in the induction coil of melting fast cooling device and (is used for heating), vacuum is evacuated to
9.5×10-3Argon gas is filled with during Pa as protective atmosphere, after master alloy ingot fusing, at room temperature, is prepared and closed using single roller chilling method
Gold bar band sample:It is sprayed onto what is rotated with linear resonance surface velocity 40m/s when about 1000 DEG C of temperature with 0.02MPa injection pressure
On copper roller, chilling prepares alloy strip (alloy strip thickness is 0.01~0.03mm).After usual after alloy strip cooling
To take out alloy strip sample after spray is completed 10 minutes.
Step 4, the alloy strip that step 3 is obtained is placed in quartz ampoule, vacuum is evacuated to 9.5 × 10-3Annealing furnace is put into during Pa
It is middle to be annealed, annealed between Curie temperature and crystallization temperature at a certain temperature, rapid take out is equipped with alloy bar after annealing
The quartz ampoule of band, and put into 20-30 DEG C of water and cool down rapidly.The thermodynamic parameter of alloy is characterized with differential scanning calorimeter.
Table 4 summarizes the crystallization temperature (T of each two exothermic peaks of alloying componentx) and Curie temperature (Tc).According to each in table 4
Annealing conditions are set as each alloying component crystallization temperature (T by the crystallization temperature and Curie temperature of alloyx1) following 75K,
Annealing time 3 minutes.
The phase structure for state alloy strip of quenching is characterized with X-ray diffractometer.As shown in figure 16, the diffracting spectrum of state of quenching alloy
Only one of which disperse peak, its alloy structure is single amorphous phase.Structure is amorphous/nanocrystalline composite construction (figure after it is annealed
Not shown in).
Figure 17 is the result that alloy strip bending is tested after annealing, wherein (a) is (Fe0.8Co0.2)85B14Cr1, (b) is
(Fe0.8Co0.2)85B14Nb1, it can be seen that it is unbroken after band doubling, show bending toughness.
Figure 18 is (Fe0.8Co0.2)85B14Nb1Stereoscan photograph near nanometer crystal alloy band folding line.Wherein substantially can be with
It was observed that shear band, be the feature of toughness material.
Measure the B of nanometer crystal alloy respectively with vibration magnetometer and B-H instrumentsAnd Hc, it the results are shown in Table 4.
(the Fe of table 40.8Co0.2)85B14M1Magnetics parameter after the thermal parameters and nano-crystallization of (x=Cr, Nb) alloy
Exemplary description is done to the present invention above, it should explanation, in the case where not departing from the core of the present invention,
Any simple deformation, modification or other skilled in the art can not spend the equivalent substitution of creative work to fall
Enter protection scope of the present invention.
Claims (10)
1. a kind of iron cobalt-based toughness nano-crystal soft magnetic alloy, it is characterised in that its composition has following expression
(Fe0.8Co0.2)aBbMc, wherein, M is Cr, Mo or Nb, and a, b and c represent the atomic percent of each component respectively,
And a, b, c meet following condition:84≤a≤87,12≤b≤16,0≤c≤2, a+b+c=100;
The iron cobalt-based toughness nano-crystal soft magnetic alloy is prepared as steps described below:
Step 1, raw material is configured according to the composition expression formula of above-mentioned iron cobalt-based toughness nano-crystal soft magnetic alloy;
Step 2, vacuum is evacuated to less than or equal to 9.5 × 10-3Pa, under the protection of inert gas, step 1 is configured
Raw material be heated to being completely melt it is uniform after, be cooled to 20-25 DEG C of room temperature, master alloy ingot be made;
Step 3, the master alloy ingot obtained by step 2 is melted again, at room temperature, using single roller under the protection of inert gas
Chilling method prepares alloy strip sample;
Step 4, the alloy strip that step 3 is obtained is made annealing treatment, is placed in 20-30 DEG C of water and cools down rapidly after annealing
To generate the iron cobalt-based toughness nano-crystal soft magnetic alloy of the present invention, wherein, annealing temperature be Curie temperature and crystallization temperature it
Between.
2. iron cobalt-based toughness nano-crystal soft magnetic alloy according to claim 1, it is characterised in that in step 2,
The raw material that step 1 is configured is heated to after being completely melt uniformly through 3~5 meltings, is cooled to 20-25 DEG C of room temperature, is made
Master alloy ingot;In step 2, the master alloy ingot that step 2 is made is crushed to after 0.1-0.6mm, it is ultrasonic in alcohol
Clean 30-60min;In step 2, the raw material configured using arc-melting furnace to step 1 is heated;In step 2
In, vacuum is 6 × 10-3-8×10-3Pa。
3. iron cobalt-based toughness nano-crystal soft magnetic alloy according to claim 1, it is characterised in that in step 3,
The technological parameter that single roller chilling method prepares alloy strip sample is:Injection pressure is 0.02-0.04Mpa, injection temperation
800-1200 DEG C, copper roller rotating speed linear resonance surface velocity is 20-50m/s, is preferably:Injection pressure is 0.02-0.03Mpa, spray
900-1100 DEG C of temperature is penetrated, copper roller rotating speed linear resonance surface velocity is 30-40m/s;In step 3, alloy strip examination is being prepared
In single roller chilling method of sample, master alloy ingot is placed in quartz ampoule and melted again, the mouth of pipe of the quartz ampoule is used
1200-2000 sand paper is polishing to a diameter of 0.7-0.8mm;In step 1,3, the inert gas is argon gas;In step
In rapid 3, alloy strip sample thickness prepared by the step 3 is 0.01-0.03mm.
4. iron cobalt-based toughness nano-crystal soft magnetic alloy according to claim 1, it is characterised in that in step 4,
Annealing temperature is 75K below 25K below crystallization temperature, either 50K below crystallization temperature or crystallization temperature, or
100K below crystallization temperature;In step 4, it is less than or equal to 9.5 × 10 in vacuum-3Annealed under Pa;In step 4
In, the time of annealing is 0.5-20 minutes, preferably 10-20 minutes.
5. iron cobalt-based toughness nano-crystal soft magnetic alloy according to claim 1, it is characterised in that the expression formula is
(Fe0.8Co0.2)87B13、(Fe0.8Co0.2)86B14、(Fe0.8Co0.2)85B15、(Fe0.8Co0.2)86B13Mo1、
(Fe0.8Co0.2)85B14Mo1、(Fe0.8Co0.2)84B14Mo2、(Fe0.8Co0.2)85B14Cr1(Fe0.8Co0.2)85B14Nb1。
6. iron cobalt-based toughness nano-crystal soft magnetic alloy according to claim 1, it is characterised in that the iron cobalt-based is tough
Property nano-crystal soft magnetic alloy be annealed between Curie temperature and crystallization temperature at a certain temperature obtain amorphous/nanocrystalline be combined
Structure, the alloy strip of the amorphous/nanocrystalline composite construction possesses bending toughness, is not broken after doubling;The iron cobalt
Vickers hardness of the Vickers hardness less than single noncrystalline structure before annealing after the annealing of base toughness nano-crystal soft magnetic alloy;Annealing
The saturation induction density (Bs) of state alloy is 1.5-1.95T, and coercivity (Hc) is less than or equal to 25A/m;The iron cobalt
The nano-crystalline granule that base toughness nano-crystal soft-magnetic is closed is evenly distributed in noncrystal substrate, the average grain diameter of the nano-crystalline granule
Less than or equal to 5nm, preferably 2-5nm.
7. a kind of preparation method of the iron cobalt-based toughness nano-crystal soft magnetic alloy in 1-6 such as claim as described in any one,
Characterized in that, being prepared as steps described below:
Step 1, raw material is configured according to the composition expression formula of above-mentioned iron cobalt-based toughness nano-crystal soft magnetic alloy;
Step 2, vacuum is evacuated to less than or equal to 9.5 × 10-3Pa, under the protection of inert gas, step 1 is configured
Raw material be heated to being completely melt it is uniform after, be cooled to 20-25 DEG C of room temperature, master alloy ingot be made;
Step 3, the master alloy ingot obtained by step 2 is melted again, at room temperature, using single roller under the protection of inert gas
Chilling method prepares alloy strip sample;
Step 4, the alloy strip that step 3 is obtained is made annealing treatment, is placed in 20-30 DEG C of water and cools down rapidly after annealing
To generate the iron cobalt-based toughness nano-crystal soft magnetic alloy of the present invention, wherein, annealing temperature be Curie temperature and crystallization temperature it
Between.
8. the preparation method of iron cobalt-based toughness nano-crystal soft magnetic alloy according to claim 7, it is characterised in that
In step 2, the raw material that step 1 is configured is heated to after being completely melt uniformly through 3~5 meltings, is cooled to room temperature
20-25 DEG C, master alloy ingot is made;In step 2, the master alloy ingot that step 2 is made is crushed to after 0.1-0.6mm,
It is cleaned by ultrasonic 30-60min in alcohol;In step 2, the raw material configured using arc-melting furnace to step 1 is added
Heat;In step 2, vacuum is 6 × 10-3-8×10-3Pa。
9. the preparation method of iron cobalt-based toughness nano-crystal soft magnetic alloy according to claim 7, it is characterised in that
In step 3, the technological parameter that single roller chilling method prepares alloy strip sample is:Injection pressure is 0.02-0.04Mpa,
800-1200 DEG C of injection temperation, copper roller rotating speed linear resonance surface velocity is 20-50m/s, is preferably:Spraying pressure is
0.02-0.03Mpa, 900-1100 DEG C of injection temperation, copper roller rotating speed linear resonance surface velocity is 30-40m/s;In step 3,
In single roller chilling method of alloy strip sample is prepared, master alloy ingot is placed in quartz ampoule and melted again, it is described
The mouth of pipe of quartz ampoule is polishing to a diameter of 0.7-0.8mm with 1200-2000 sand paper;In step 1,3, the inertia
Gas is argon gas;In step 3, the alloy strip sample thickness that prepared by the step 3 is 0.01-0.03mm.
10. the preparation method of iron cobalt-based toughness nano-crystal soft magnetic alloy according to claim 7, it is characterised in that
In step 4, annealing temperature is 25K below crystallization temperature, either 50K below crystallization temperature or crystallization temperature with
100K below lower 75K, or crystallization temperature;In step 4, it is less than or equal to 9.5 × 10 in vacuum-3Moved back under Pa
Fire;In step 4, the time of annealing is 0.5-20 minutes, preferably 10-20 minutes.
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