CN105986202B - Fe-based amorphous material and preparation method thereof - Google Patents
Fe-based amorphous material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of Fe-based amorphous materials and preparation method thereof.The ingredient of the Fe-based amorphous material is Fe100‑a‑b‑cMcBbAa, any one of M Si, Zr, Nb, Cr, P, Al, Co, Ni, Ti or a variety of, A is N and/or C, 0.5≤a≤2at%, 9≤b≤14at%, 0≤c≤10at%；Non-crystalline material includes noncrystal substrate layer and the superficial layer on noncrystal substrate layer, and superficial layer is FeA enriched layers.Noncrystal substrate layer in the Fe-based amorphous material is used to provide the basic performance of Fe-based amorphous material, and it is cooperateed with by the auxiliary of superficial layer performance, it can make the performance of Fe-based amorphous material be enhanced, it improves saturation magnetization, reduce coercivity, so as to improve the overall performance of Fe-based amorphous material.
Description
Technical field
The present invention relates to non-crystalline material field, in particular to a kind of Fe-based amorphous material and preparation method thereof.
Background technology
Non-crystaline amorphous metal is also known as glassy metal, is a kind of metastable new metallic material, has shortrange order, longrange disorder
Structure feature and high magnetic induction, high resistivity, high intensity, high rigidity, high elastic modulus, high abrasion and corrosion resistance,
The excellent properties such as low-loss, some non-crystaline amorphous metals also have very excellent magnetic performance.As a kind of new functional material
With engineering material, non-crystaline amorphous metal is in fields such as aerospace, military project, automobile, electronics, instrument and meter, sports equipment, medical equipments
It has broad application prospects, is known as 21 century new green energy saving material.
Just because of these excellent specific properties that non-crystalline material possesses, it is considered as the ideal for making power transformer to make it
Core material.And use non-crystaline amorphous metal replace thin silicon steel be used as power transformer iron core research work almost with Fe-based amorphous band
Making simultaneously starting.Fe-based amorphous still to have shortcoming but compared with orientation silicon steel, crystalline state orientation silicon steel Bs values about exist
2T, and typical Fe-based amorphous alloy Fe78Si9B13Bs values be 1.56T.When preparing magnetic element, 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, it means that plant bulk
Reduction or the reduction of exciting power.
In order to improve non-crystalline material performance, constituent parts are studied in terms of ingredient with preparation process.For example, China is specially
Sharp CN104233121A discloses Fe83.5B15Cu1.5Ingredient can improve the saturation magnetization of non-crystalline material by the ingredient.
Chinese patent CN1166800C discloses Fe:81~86wt.%, Co:7~12wt.%, Si:1~3wt.%, B:3~
5wt.%, the ingredient can improve saturation magnetization.Chinese patent CN100442402C discloses (Fe1-xMx)100-a-b- cPaTbDc, wherein M is at least one of Co, Ni, and two or more and Al, D Sn, Cr, Zr in T C, B, Si etc., x is
0.01~0.16；A is 8~15；B is 10~25；C is 0.5~6, is closed by the ingredient to obtain the amorphous of high-frequency soft magnetic performance
Bronze end.Chinese patent CN101492794A discloses Fe-based amorphous, the ingredient Fe of one kind100-a-b-c-d-eNiaCrbPcTdDe,
Middle T is the one or more in B, C and Si, and five kinds or less in D Y, V, Zr, Mo, Nb, Al, Ga, which can be significantly
Improve the amorphous formation ability of material.Chinese patent CN 101805876B disclose a kind of Fe100-a-b-c-xCoaSibBcMxMaterial,
The material reduces the ingredient of non-crystalline material by adding in cheap M element, improves the saturation magnetization of material.Chinese patent
CN101787500B discloses a kind of Fe80Si9B9C1.5Al0.5The preparation method of material, saturation magnetization can reach 1.7T, lead to
Addition Al is crossed to reduce cost.
More than patent is only improved the performances such as the saturation magnetization of material from ingredient and preparation process etc., is not had
The open technical solution by being surface-treated to improve material overall performance.Chinese patent CN102234797A,
CN102268660A and CN102212815A is individually disclosed using phosphatization, sol-gal process or high-temperature oxidation Fe-based amorphous
Nanocrystalline material surface be modified preparation method, by amorphous ＆ nanocrystalline surface coat one layer of phosphide film or
TiO2Or ferroso-ferric oxide coating, to improve the corrosion resistance of material.This method simply forms one layer of guarantor in surface physics
Cuticula improves inoxidizability, and material itself magnetic property do not improved.Chinese patent CN102787282B discloses a kind of non-
There is the enriched layer of O, C, Si, B from surface to inside in the range of 1~20nm in crystal alloy, the material, so as to improve material
Saturation magnetization reduces iron loss.This method is also simply during material is prepared by strictly controlling CO2And CH4Gaseous mixture
The concentration of atmosphere reaches, and also there are larger difficulty in terms of technology controlling and process.
The content of the invention
It is a primary object of the present invention to provide a kind of Fe-based amorphous material and preparation method thereof, to improve Fe-based amorphous material
The overall performance of material.
To achieve these goals, according to an aspect of the invention, there is provided a kind of Fe-based amorphous material, the iron-based are non-
The ingredient of brilliant material is Fe100-a-b-cMcBbAa, any one of M Si, Zr, Nb, Cr, P, Al, Co, Ni, Ti or a variety of, A N
And/or C, 0.5≤a≤2at%, 9≤b≤14at%, 0≤c≤10at%；Fe-based amorphous material includes noncrystal substrate layer and position
Superficial layer on noncrystal substrate layer, superficial layer are FeA enriched layers.
Further, the thickness of superficial layer is 5nm~5 μm.
Further, A N, the structure of superficial layer include α "-Fe16N2。
Further, when A is N, along the direction upper surface layer away from noncrystal substrate layer at thickness is 50nm~5 μm
FeN concentration highests.
Further, when A is C, along the direction upper surface layer away from noncrystal substrate layer at thickness is 5nm~50nm
FeC concentration highests.
Further, the thickness of Fe-based amorphous material is 15~35 μm.
The present invention also provides a kind of preparation method of above-mentioned Fe-based amorphous material, which comprises the following steps：
Noncrystal substrate material is prepared, the ingredient of noncrystal substrate material is Fe100-a-b-cMcBbAa, M Si, Zr, Nb, Cr, P, Al, Co, Ni,
Any one of Ti or a variety of, A are N and/or C, 0.5≤a≤2at%, 9≤b≤14at%, 0≤c≤10at%；To amorphous
Basis material is surface-treated to form Fe-based amorphous material.
Further, the step of surface treatment includes：Ion note is carried out to noncrystal substrate material using the ion beam containing A
Enter, and in the step of ion implanting, the energy of ion beam is 50~500keV, and base reservoir temperature is 100~300 DEG C.
Further, the step of surface treatment includes：Determine the crystallization temperature T1 of Fe-based amorphous material；Atmosphere containing A,
(T1-100) noncrystal substrate material is heat-treated under the temperature range of~(T1+10)；It is non-that iron-based is obtained after being cooled to room temperature
Brilliant material.
Further, the step of heat treatment includes：Step S1, in atmosphere containing A, the temperature model of (T1-100)~(T1-50)
10~30min of heat treatment is carried out under enclosing；Step S2, continue to carry out under atmosphere containing A, the temperature range of (T1-20)~(T1+10)
It is heat-treated 3~10min；Step S1 and step S2N time are repeated, N is 5~10.
It applying the technical scheme of the present invention, Fe-based amorphous material provided by the invention includes noncrystal substrate layer and superficial layer,
And noncrystal substrate layer is used to provide the basic performance of Fe-based amorphous material, and cooperateed with by the auxiliary of superficial layer performance, it can make
The performance of Fe-based amorphous material is enhanced, and is improved saturation magnetization, is reduced coercivity, so as to improve Fe-based amorphous material
Overall performance.
Specific embodiment
It should be noted that in the case where there is no conflict, the feature in embodiment and embodiment in the application can phase
Mutually combination.The application is described in detail below in conjunction with embodiment.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " bag
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
From background technology, the overall performance of existing Fe-based amorphous material is poor.The present inventor is directed to the skill
Art problem is studied, it is proposed that a kind of Fe-based amorphous material.The ingredient of the Fe-based amorphous material is Fe100-a-b-cMcBbAa, M is
Any one of Si, Zr, Nb, Cr, P, Al, Co, Ni, Ti or a variety of, A be N and/or C, 0.5≤a≤2at%, 9≤b≤
14at%, 0≤c≤10at%；Fe-based amorphous material includes noncrystal substrate layer and the superficial layer on noncrystal substrate layer, surface
Layer is FeA enriched layers.
In above-mentioned Fe-based amorphous material, noncrystal substrate layer is used to provide the basic performance of Fe-based amorphous material, and passes through table
The auxiliary collaboration of surface layer performance, can make the performance of Fe-based amorphous material be enhanced, and improve saturation magnetization, reduce coercive
Power, so as to improve the overall performance of Fe-based amorphous material.
The illustrative embodiments of the Fe-based amorphous material provided according to the present invention are provided.However,
These illustrative embodiments can be implemented by many different forms, and should not be construed to be limited solely to be explained here
The embodiment stated.It should be appreciated that these embodiments are provided so that disclosure herein is thoroughly and complete, and
And the design of these illustrative embodiments is fully conveyed to those of ordinary skill in the art.
Fe-based amorphous material provided by the invention is using FeB as basic ingredient, and adds a certain amount of M members on this basis
Usually improve amorphous formation ability, improve overall performance, wherein M be one kind in Si, Zr, Nb, Cr, P, Al, Co, Ni, Ti or
It is a variety of, and in these addition element, Si, P play an important role the amorphous formation ability of non-crystalline material, Nb, Cr, Zr couple
Inhibit the precipitation of metastable phase, amorphous stability is kept to play an important role, Ni, Al, Co satisfy to promoting whole non-crystalline material
And the intensity of magnetization, initial permeability play an important role.The addition of these elements, to ultimately forming base layer and two layers of knot of superficial layer
Structure plays apparent facilitation.Meanwhile the addition that A is N and/or C, N and/or C is the key that one of present invention, by N and/
Or C is formed on non-crystalline material surface and is enriched with, so as to improve the overall performance of non-crystalline material.
Each element is also required in the present invention there are certain proportionate relationship, calculated with atomic ratio, wherein 0.5≤a≤
The value of 2at.%, 9≤b≤14at.%, 0≤c≤10at.%, a, b, c can ensure Fe contents in more than 78at.%, thus
Make non-crystalline material that there is higher Saturation magnetic sense intensity, in of the invention, the content of c can be zero, in this case, material base
This ingredient is FeBA.
Above-mentioned Fe-based amorphous material, it is preferable that the thickness of superficial layer is 5nm~5 μm, in this scope, A shapes wherein
Into certain enrichment, FeA compounds are formed, the performance of the FeA compounds directly affects the performance of material entirety.Preferably, A is worked as
For N when, superficial layer in thickness to there are FeN concentration peaks at 50nm~5 μm, at this point, N forms certain ladder in material surface
Degree distribution, forms certain phase structure, forms the superficial layer with certain performance.In the FeN compounds on surface, it can be formed
A series of FeN structures, including α "-Fe16N2, γ '-Fe4N, ε-FexN(2<X≤3), ζ-Fe2N and a certain amount of amorphous and
α-Fe etc., the different properties of these nitride, the influence to non-crystalline material overall performance is also different, wherein when the structure for γ '-
Fe4N、ζ-Fe2During N, there is apparent effect to the raising of material corrosion resistance.Preferably, the structure of superficial layer mainly include α "-
Fe16N2, wherein α "-Fe16N2Saturation magnetization be up to 2.8T, the formation of the compound is bright to the raising effect of overall performance
It is aobvious.
Preferably, when A is C, surface forms FeC rich regions, and FeC enrichment plot structures include Fe3C、Fe2C, FeC with
And FeMC etc., at this time the thickness of superficial layer occur concentration peak at 5nm~50nm, the surface layer structure of formation is whole to being promoted
The corrosion resistance and mechanical property of body have larger facilitation.Preferably, the thickness of Fe-based amorphous material is 15~35 μm.
Meanwhile provided by the invention Fe-based amorphous material is stated by a variety of preparation methods.Specifically, technical staff can adopt
Noncrystal substrate material is surface-treated with modes such as ion implanting, magnetron sputterings includes noncrystal substrate layer and surface to be formed
The Fe-based amorphous material of layer.
The embodiment of the preparation method of above-mentioned Fe-based amorphous material will be specifically described below.The system of the Fe-based amorphous material
Preparation Method comprises the following steps：Noncrystal substrate material is prepared, the ingredient of noncrystal substrate material is Fe100-a-b-cMcBbAa, M Si,
Any one of Zr, Nb, Cr, P, Al, Co, Ni, Ti or a variety of, A be N and/or C, 0.5≤a≤2at%, 9≤b≤14at%,
0≤c≤10at%；Noncrystal substrate material is surface-treated to form Fe-based amorphous material.
In a kind of preferred embodiment of the present invention, Fe-based amorphous material is prepared using ion implantation technology.Ion implanting
Technology is a kind of material surface modifying technology to grow up in the past 30 years, and basic principle is：Energy is used under certain atmosphere
For 100keV magnitudes ion beam incidence into material, a series of physical will occur for atom or molecule in ion beam and material
And chemistry interaction, the gradual off-energy of incident ion finally rested in material, and cause material surface ingredient,
Structure and performance change, so as to optimize material surface performance or obtain some new excellent properties.Preferably, using containing A
Ion beam ion implanting is carried out to noncrystal substrate material, and in the step of ion implanting, the energy of ion beam for 50~
500keV, base reservoir temperature are 100~300 DEG C.
Specifically, in ion implantation process, non-crystalline material can be put into ion implantation device, the nitrogen of nitrogen containing atmosphere
(carbon) divides, the power of base reservoir temperature and ion implanting, to adjust the formation of each structures of superficial layer FeA.In order to reach this hair
Bright required effect.Particularly, when A be N when, ion implanting concrete technology selection be particularly important, by adjusting with
A series of variation can occur for upper technological parameter, the structure of corresponding FeA compounds, and in nitrogen containing atmosphere, nitrogen partial pressure carries
Height, the concentration of A is higher in superficial layer, so as to be more advantageous to being formed the FeN compounds of high N；Due to iron nitride magnetic moment and
Curie temperature is reduced with the increase of nitrogen content, the α "-Fe in the magnetic material having been found that16N2With highest saturation magnetic
Flux density (2.8~3.0T), and γ '-Fe4N, ε-FexN(2<X≤3) saturation flux density be respectively 1.7T and 1.4T, ζ-
Fe2N is at normal temperatures paramagnetism, from the aspect of magnetism, in order to prepare the FeN superficial layers with high saturation and magnetic intensity,
Key factor is to avoid the nitridation iron phase of the formation weak magnetic in sputtering process, the α "-Fe formed at this time16N2Superficial layer can be to whole
The magnetic property of body material plays facilitation, and Bs is more than 1.7T, and magnetostriction coefficient and coercivity also decrease, at this time nitrogen
Qi leel pressure is less than 10%, and base reservoir temperature is less than 150 DEG C.In addition, in order to improve the corrosion resistance of material and mechanical property, just need
The structure of high nitrogen-containing is obtained, it is 10~50% to require nitrogen partial pressure at this time, and base reservoir temperature is 150~300 DEG C.
In another preferred embodiment of the invention, Fe-based amorphous material is prepared using heat treatment process.It is elected to be used in
The mode nitrogenized under nitrogen containing atmosphere come when preparing, it is necessary to consider that a key factor is that there is a situation where significantly change in matrix
The lower infiltration for carrying out A, particularly, it is impossible to noncrystal substrate be made to carry out crystallization, so as to influence whole performance.In the case, need
Entire nitridation schemes are optimized, in the present invention, the infiltration of surface carbon/nitrogen is realized by the way of multistep nitridation.
During nitrogen containing atmosphere nitrogen treatment, nitrogen containing atmosphere is preferably NH3, NH3+H2, N2+H2, N2.When atmosphere is NH3(N2)+H2
When, NH3(N2) and H2Ratio be less than 1:3.
Preferably, the step of being surface-treated using heat treatment process is included：Determine the crystallization temperature of Fe-based amorphous material
Spend T1；Noncrystal substrate material is heat-treated under atmosphere containing A, the temperature range of (T1-100)~(T1+10)；It is cooled to room
Fe-based amorphous material is obtained after temperature.It is further preferable that the step of heat treatment, includes：Step S1, atmosphere containing A, (T1-100)~
(T1-50) 10~30min of heat treatment is carried out under temperature range；Step S2, continue in atmosphere containing A, (T1-20)~(T1+10)
Temperature range under carry out 3~10min of heat treatment；Step S1 and step S2N time are repeated, N is 5~10.Pass through above segmentation
The step of heat treatment, can effectively enhance the activity of Nitrogen ion in atmosphere, so as to carry out nitriding when less than crystallization temperature
Operation, making base layer, recurring structure does not change, and keeps the stability of overall performance.
Fe-based amorphous material of offer and preparation method thereof is be provided below in conjunction with embodiment.
Embodiment 1
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe87.2B12.3N0.5, and the non-crystalline material includes thickness for noncrystal substrate layer and the superficial layer on noncrystal substrate layer, surface
The structure of layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 15 μm, and the thickness of superficial layer is 50nm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, using containing
The ion beam of nitrogen carries out noncrystal substrate material ion implanting to form Fe-based amorphous material, and the energy of wherein ion beam is
50keV, base reservoir temperature are 100 DEG C.
Embodiment 2
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe82.0P2.0Cr0.5B13.5N2.0, and it is noncrystal substrate layer and the surface on noncrystal substrate layer that the non-crystalline material, which includes thickness,
Layer, the structure of superficial layer include α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 35 μm, the thickness of superficial layer
For 5 μm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, using containing
The ion beam of nitrogen carries out noncrystal substrate material ion implanting to form Fe-based amorphous material, and the energy of wherein ion beam is
80keV, base reservoir temperature are 250 DEG C.
Embodiment 3
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe84.4Si1.5Zr1.9Co2.0B9.0N1.2, and the non-crystalline material includes thickness for noncrystal substrate layer and on noncrystal substrate layer
Superficial layer, the structure of superficial layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 19 μm, superficial layer
Thickness be 200nm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, using containing
The ion beam of nitrogen carries out noncrystal substrate material ion implanting to form Fe-based amorphous material, and the energy of wherein ion beam is
60keV, base reservoir temperature are 215 DEG C.
Embodiment 4
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe79.1P1.6Nb0.8Al1.9Ni2.5Ti1.2B11.1N1.8, and the non-crystalline material includes thickness for noncrystal substrate layer and positioned at amorphous base
Superficial layer on body layer, the structure of superficial layer include α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 26 μm,
The thickness of superficial layer is 800nm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, using containing
The ion beam of nitrogen carries out noncrystal substrate material ion implanting to form Fe-based amorphous material, and the energy of wherein ion beam is
70keV, base reservoir temperature are 300 DEG C.
Embodiment 5
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe82.3Si3.2B14.0N0.5, and the non-crystalline material includes thickness for noncrystal substrate layer and the superficial layer on noncrystal substrate layer,
The structure of superficial layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 15 μm, and the thickness of superficial layer is
500nm。
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, heat is carried out
Processing, wherein heat treatment temperature are 450 DEG C, and heat treatment time 30min obtains Fe-based amorphous material after being cooled to room temperature.
Embodiment 6
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe83.3Nb1.3Cr2.0B12.9N0.5, and it is noncrystal substrate layer and the table on noncrystal substrate layer that the non-crystalline material, which includes thickness,
Surface layer, the structure of superficial layer include α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 22 μm, the thickness of superficial layer
It spends for 150nm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, heat is carried out
Processing, wherein heat treatment temperature are 410 DEG C, and heat treatment time 15min obtains Fe-based amorphous material after being cooled to room temperature.
Embodiment 7
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe82.1Co1.6Ni1.9B12.8N1.6, and it is noncrystal substrate layer and the table on noncrystal substrate layer that the non-crystalline material, which includes thickness,
Surface layer, the structure of superficial layer include α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 17 μm, the thickness of superficial layer
It spends for 80nm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, heat is carried out
Processing, wherein heat treatment temperature are 510 DEG C, and heat treatment time 29min obtains Fe-based amorphous material after being cooled to room temperature.
Embodiment 8
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe85.5Si2.1Zr0.9B9.7N1.8, and it is noncrystal substrate layer and the table on noncrystal substrate layer that the non-crystalline material, which includes thickness,
Surface layer, the structure of superficial layer include α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 25 μm, the thickness of superficial layer
It spends for 2 μm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, heat is carried out
Processing, wherein heat treatment includes：Step S1, heat treatment temperature is 400 DEG C, heat treatment time 10min；Step S2, it is heat-treated
Temperature is 480 DEG C, heat treatment time 3min；Step S1 and S25 times are repeated, Fe-based amorphous material is obtained after being cooled to room temperature
Material.
Embodiment 9
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe83.6Cr2.8Co1.5B10.2N1.9, and it is noncrystal substrate layer and the table on noncrystal substrate layer that the non-crystalline material, which includes thickness,
Surface layer, the structure of superficial layer include α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 31 μm, the thickness of superficial layer
It spends for 3 μm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, heat is carried out
Processing, wherein heat treatment includes：Step S1, heat treatment temperature is 460 DEG C, heat treatment time 20min；Step S2, it is heat-treated
Temperature is 510 DEG C, heat treatment time 10min；Step S1 and S210 times are repeated, is obtained after being cooled to room temperature Fe-based amorphous
Material.
Embodiment 10
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe83.4P1.8Ni1.3B13.4N0.1, and it is noncrystal substrate layer and the surface on noncrystal substrate layer that the non-crystalline material, which includes thickness,
Layer, the structure of superficial layer include α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 29 μm, the thickness of superficial layer
For 20nm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, heat is carried out
Processing, wherein heat treatment temperature are 500 DEG C, and heat treatment time 20min obtains Fe-based amorphous material after being cooled to room temperature.
Embodiment 11
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe84.8Zr1.2Al2.3B11.6N0.15, and it is noncrystal substrate layer and the table on noncrystal substrate layer that the non-crystalline material, which includes thickness,
Surface layer, the structure of superficial layer include γ '-Fe4N and ζ-Fe2N, the thickness of noncrystal substrate layer is 32 μm, and the thickness of superficial layer is
30nm。
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, using containing
The ion beam of nitrogen carries out noncrystal substrate material ion implanting to form Fe-based amorphous material, and the energy of wherein ion beam is
50keV, base reservoir temperature are 300 DEG C.
Embodiment 12
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe78.0Si4.5P2.6Nb1.4Co1.6B11.0C0.9, and the non-crystalline material includes thickness for noncrystal substrate layer and positioned at noncrystal substrate layer
On superficial layer, the structure of superficial layer includes Fe3C、Fe2C, FeC and FeMC etc., the thickness of noncrystal substrate layer is 22 μm, surface
The thickness of layer is 5nm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, using containing
The ion beam of nitrogen carries out noncrystal substrate material ion implanting to form Fe-based amorphous material, and the energy of wherein ion beam is
60keV, base reservoir temperature are 150 DEG C.
Embodiment 13
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe83.9Zr1.5Al1.2Ni2.0Ti0.9B9.0C1.5, and the non-crystalline material includes thickness for noncrystal substrate layer and positioned at noncrystal substrate
Superficial layer on layer, the structure of superficial layer include Fe3C、Fe2C, FeC and FeMC etc., the thickness of noncrystal substrate layer is 31 μm, table
The thickness of surface layer is 32nm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, using containing
The ion beam of nitrogen carries out noncrystal substrate material ion implanting to form Fe-based amorphous material, and the energy of wherein ion beam is
70keV, base reservoir temperature are 250 DEG C.
Embodiment 14
A kind of Fe-based amorphous material and preparation method thereof is present embodiments provided, wherein, the ingredient of the Fe-based amorphous material
For Fe85.0P2.0Cr1.0B10.0C2.0, and it is noncrystal substrate layer and the surface on noncrystal substrate layer that the non-crystalline material, which includes thickness,
Layer, the thickness of noncrystal substrate layer is 35 μm, and the thickness of superficial layer is 50nm.
The step of preparing the Fe-based amorphous material includes：First, noncrystal substrate material is prepared by proportioning；Then, using containing
The ion beam of nitrogen carries out noncrystal substrate material ion implanting to form Fe-based amorphous material, and the energy of wherein ion beam is
90keV, base reservoir temperature are 290 DEG C.
Comparative example 1
This comparative example provides a kind of Fe-based amorphous material, wherein, the ingredient of the Fe-based amorphous material is
Fe89.5Si1.5B9.0。
Comparative example 2
This comparative example provides a kind of Fe-based amorphous material, wherein, the ingredient of the Fe-based amorphous material is
Fe84.0P2.0B14.0。
Test：The Fe-based amorphous material obtained to embodiment 1 to 14 and comparative example 1 to 2 is tested for the property, test result
As shown in table 1.As it can be seen from table 1 the saturation magnetization Ms values for the Fe-based amorphous material that embodiment 1 to 14 obtains are 1.31
~2.35T, magnetostriction coefficient are 1.5~15；And the saturation magnetization Ms for the Fe-based amorphous material that comparative example 1 to 2 obtains
It is worth for 1.47~1.52T, magnetostriction coefficient is 26~23.As it can be seen that since the Fe-based amorphous material that comparative example 1 to 2 obtains does not have
There is superficial layer, make its coercivity larger.Meanwhile as it can be seen from table 1 embodiment 1 to 14 obtain Fe-based amorphous material it is resistance to
Corrosivity is better than the Fe-based amorphous material that comparative example 1 to 2 obtains.
Table 1
| Sequence number | Saturation magnetization | Magnetostriction coefficient | Corrosion resistance |
| Embodiment 1 | 2.1 | 3.6 | Micro point |
| Embodiment 2 | 1.98 | 2.7 | Micro point |
| Embodiment 3 | 2.35 | 5.3 | Micro point |
| Embodiment 4 | 1.86 | 1.5 | Micro point |
| Embodiment 5 | 1.93 | 4.9 | Micro point |
| Embodiment 6 | 1.88 | 3.7 | Micro point |
| Embodiment 7 | 1.74 | 3.9 | Micro point |
| Embodiment 8 | 2.09 | 3.5 | Micro point |
| Embodiment 9 | 2.28 | 2.9 | Micro point |
| Embodiment 10 | 1.65 | 15 | A large amount of points and white rust |
| Embodiment 11 | 1.53 | 13 | A large amount of points and white rust |
| Embodiment 12 | 1.31 | 11 | Without significant change |
| Embodiment 13 | 1.42 | 14 | Without significant change |
| Embodiment 14 | 1.27 | 16 | Without significant change |
| Comparative example 1 | 1.47 | 26 | A large amount of points and white rust |
| Comparative example 2 | 1.52 | 23 | A large amount of points and white rust |
As can be seen from the above embodiments, the above-mentioned example of the present invention realizes following technique effect：It is provided by the invention
Fe-based amorphous material includes noncrystal substrate layer and superficial layer, and noncrystal substrate layer is used to provide the basic nature of Fe-based amorphous material
Can, and cooperateed with by the auxiliary of superficial layer performance, the performance of Fe-based amorphous material can be made be enhanced, it is strong to improve saturated magnetization
Degree reduces coercivity, so as to improve the overall performance of Fe-based amorphous material.
It these are only the preferred embodiment of the present invention, be not intended to limit the invention, for those skilled in the art
For member, the invention may be variously modified and varied.Any modification within the spirit and principles of the invention, being made,
Equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of Fe-based amorphous material, which is characterized in that the ingredient of the Fe-based amorphous material is Fe100-a-b-cMcBbAa, M is
Any one of Si, Zr, Nb, Cr, P, Al, Co, Ni, Ti or a variety of, A be N and/or C, 0.5≤a≤2at%, 9≤b≤
14at%, 0≤c≤10at%；The Fe-based amorphous material includes noncrystal substrate layer and the table on the noncrystal substrate layer
Surface layer, the superficial layer are FeA enriched layers.
2. Fe-based amorphous material according to claim 1, which is characterized in that the thickness of the superficial layer is 5nm~5 μm.
3. Fe-based amorphous material according to claim 1, which is characterized in that A N, the structure of the superficial layer include α "-
Fe16N2。
4. Fe-based amorphous material according to claim 1, which is characterized in that when A is N, along away from the noncrystal substrate
The superficial layer is the FeN concentration highests at 50nm~5 μm in thickness on the direction of layer.
5. Fe-based amorphous material according to claim 1, which is characterized in that when A is C, along away from the noncrystal substrate
The superficial layer is the FeC concentration highests at 5nm~50nm in thickness on the direction of layer.
6. Fe-based amorphous material according to any one of claim 1 to 5, which is characterized in that the Fe-based amorphous material
Thickness be 15~35 μm.
A kind of 7. preparation method of Fe-based amorphous material according to any one of claims 1 to 6, which is characterized in that the system
Preparation Method comprises the following steps：
Noncrystal substrate material is prepared, the ingredient of the noncrystal substrate material is Fe100-a-b-cMcBbAa, M Si, Zr, Nb, Cr, P,
Any one of Al, Co, Ni, Ti or a variety of, A be N and/or C, 0.5≤a≤2at%, 9≤b≤14at%, 0≤c≤
10at%；
The noncrystal substrate material is surface-treated to form the Fe-based amorphous material.
8. preparation method according to claim 7, which is characterized in that the step of surface treatment includes：Using containing A's
Ion beam carries out ion implanting to the noncrystal substrate material, and in the step of ion implanting, the energy of the ion beam
For 50~500keV, base reservoir temperature is 100~300 DEG C.
9. preparation method according to claim 7, which is characterized in that the step of surface treatment includes：
Determine the crystallization temperature T1 of the Fe-based amorphous material；
The noncrystal substrate material is heat-treated under atmosphere containing A, the temperature range of (T1-100)~(T1+10)；
The Fe-based amorphous material is obtained after being cooled to room temperature.
10. preparation method according to claim 9, which is characterized in that the step of heat treatment includes：
Step S1,10~30min of heat treatment is carried out under atmosphere containing A, the temperature range of (T1-100)~(T1-50)；
Step S2, continue to carry out 3~10min of heat treatment under atmosphere containing A, the temperature range of (T1-20)~(T1+10)；
Repeating said steps S1 and step S2N times, N are 5~10.
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| CN109852919A (en) * | 2019-02-20 | 2019-06-07 | 王静然 | A kind of non-crystalline material and nanocrystalline processing method |
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| CN109440023B (en) * | 2018-12-26 | 2019-10-18 | 中国科学院宁波材料技术与工程研究所 | A kind of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy and preparation method thereof |
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| CN110747411B (en) * | 2019-11-25 | 2024-02-13 | 佛山市中研非晶科技股份有限公司 | Master alloy for iron-based amorphous alloy |
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