CN105986202A - Iron base non-crystalline material and preparation method thereof - Google Patents
Iron base non-crystalline material and preparation method thereof Download PDFInfo
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Abstract
The invention provides an iron base non-crystalline material and a preparation method thereof. The iron base non-crystalline material has components of Fe100-a-b-cMcBbAa, wherein M is any one or more of Si, Zr, Nb, Cr, P, Al, Co, Ni and Ti, A is N and/or C, a is not less than 0.5 and not more than 2 at%, b is not less than 9 and not more than 14 at%, and c is not less than 0 and not more than 10 at%; the non-crystalline material comprises a non-crystalline basal body layer and a surface layer positioned on the non-crystalline basal body layer; and the surface layer is a FeA enriched layer. The non-crystalline basal body layer in the iron base non-crystalline material is used for providing basic performances of the iron base non-crystalline material; and through auxiliary cooperation of the performances of the surface layer, the performances of the iron base non-crystalline material can be enhanced, the saturation magnetization is improved, the coercive force is reduced, and the overall performances of the iron base non-crystalline material are improved.
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 metal glass, it it is a kind of metastable new metallic material, having shortrange order, the architectural feature of longrange disorder and high magnetic induction, high resistivity, high intensity, high rigidity, high elastic modulus, high abrasion and the excellent properties such as corrosion resistance, low-loss, some non-crystaline amorphous metal also has the most excellent magnetic performance.As a kind of novel functional material and engineering material, non-crystaline amorphous metal has broad application prospects in fields such as Aero-Space, military project, automobile, electronics, instrument and meter, sports equipment, medical devices, is described as 21 century novel green energy-saving material.
These excellent specific properties possessed just because of non-crystalline material so that it is be considered as the preferable core material making mains transformer.And what the research work almost making with Fe-based amorphous band using non-crystaline amorphous metal to replace thin silicon steel to be used as power transformer iron core started to walk simultaneously.But compared with orientation silicon steel, Fe-based amorphous still have weak point, crystalline state orientation silicon steel Bs value is about at 2T, and typical Fe-based amorphous alloy Fe78Si9B13Bs value be 1.56T.When preparing magnetics, such as transformer core, motor rotor and magnetic switch etc., it is often desired to the saturation induction density of these devices is higher, it means that the reduction of plant bulk or the reduction of exciting power.
In order to improve non-crystalline material performance, constituent parts is studied in terms of composition with preparation technology.Such as, Chinese patent CN104233121A discloses Fe83.5B15Cu1.5Composition, can improve the saturation magnetization of non-crystalline material by this composition.Chinese patent CN1166800C discloses Fe:81～86wt.%, Co:7～12wt.%, Si:1～3wt.%, B:3～5wt.%, and this composition can improve saturation magnetization.Chinese patent CN100442402C discloses (Fe1-xMx)100-a-b-cPaTbDc, during wherein M is Co, Ni at least one, T be the two or more and Al, D in C, B, Si be Sn, Cr, Zr etc., x is 0.01～0.16；A is 8～15；B is 10～25；C is 0.5～6, is obtained the amorphous powdered alloy of high-frequency soft magnetic performance by this composition.Chinese patent CN101492794A discloses a kind of Fe-based amorphous, and composition is Fe100-a-b-c-d-eNiaCrbPcTdDe, one or more during wherein T is B, C and Si, D is five kinds in Y, V, Zr, Mo, Nb, Al, Ga or less, and this composition can be greatly improved the amorphous formation ability of material.Chinese patent CN 101805876B discloses a kind of Fe100-a-b-c-xCoaSibBcMxMaterial, this material reduces the composition of non-crystalline material, improves the saturation magnetization of material by adding cheap M element.Chinese patent CN101787500B discloses a kind of Fe80Si9B9C1.5Al0.5The preparation method of material, saturation magnetization can reach 1.7T, reduces cost by adding Al.
Above patent, only improves the performance such as saturation magnetization of material in terms of composition and preparation technology etc., open is processed the technical scheme improving material overall performance by surface.Chinese patent CN102234797A, CN102268660A and CN102212815A individually disclose the preparation method using phosphatization, sol-gal process or high-temperature oxidation at iron-based amorphous nanometer crystalline material surface modifying, by one layer of phosphide thin film of amorphous & nanocrystalline surface-coated or TiO2Or ferroso-ferric oxide coating, improves the corrosion resistance of material.The method simply forms layer protecting film to improve non-oxidizability at surface physics, not improves material self magnetic property.Chinese patent CN102787282B discloses a kind of amorphous alloy, and this material occurs the enriched layer of O, C, Si, B from surface to inside in the range of 1～20nm, thus improves the saturation magnetization of material, reduces iron loss.The method is also by strictly controlling CO during preparing material2And CH4The concentration of mixed atmosphere reaches, and technology controlling and process aspect there is also bigger difficulty.
Summary of the invention
Present invention is primarily targeted at a kind of Fe-based amorphous material of offer and preparation method thereof, to improve the overall performance of Fe-based amorphous material.
To achieve these goals, according to an aspect of the invention, it is provided a kind of Fe-based amorphous material, the composition of this Fe-based amorphous material is Fe100-a-b-cMcBbAa, M is any one or more in Si, Zr, Nb, Cr, P, Al, Co, Ni, Ti, and A is N and/or C, 0.5≤a≤2at%, 9≤b≤14at%, 0≤c≤10at%；Fe-based amorphous material includes noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, and surface layer is FeA enriched layer.
Further, the thickness of surface layer is 5nm～5 μm.
Further, A is N, and the structure of surface layer includes α "-Fe16N2。
Further, when A is N, it is 50nm～FeN concentration at 5 μm is the highest along the direction upper surface layer away from noncrystal substrate layer at thickness.
Further, when A is C, along being that the FeC concentration at 5nm～50nm is the highest away from the direction upper surface layer of noncrystal substrate layer at thickness.
Further, the thickness of Fe-based amorphous material is 15～35 μm.
Present invention also offers the preparation method of a kind of above-mentioned Fe-based amorphous material, this preparation method comprises the following steps: prepare noncrystal substrate material, and the composition of noncrystal substrate material is Fe100-a-b-cMcBbAa, M is any one or more in Si, Zr, Nb, Cr, P, Al, Co, Ni, Ti, and A is N and/or C, 0.5≤a≤2at%, 9≤b≤14at%, 0≤c≤10at%；Noncrystal substrate material carries out surface process to form Fe-based amorphous material.
Further, the step that surface processes includes: using the ion beam containing A to carry out in ion implanting, and the step of ion implanting to noncrystal substrate material, the energy of ion beam is 50～500keV, and base reservoir temperature is 100～300 DEG C.
Further, the step that surface processes comprises determining that the crystallization temperature T1 of Fe-based amorphous material；Containing A atmosphere, (T1-100)～(T1+10) temperature range under noncrystal substrate material is carried out heat treatment；Fe-based amorphous material is obtained after being cooled to room temperature.
Further, the step of heat treatment includes: step S1, containing A atmosphere, (T1-100)～(T1-50) temperature range under carry out heat treatment 10～30min；Step S2, continue containing A atmosphere, (T1-20)～(T1+10) temperature range under carry out heat treatment 3～10min；Repeating step S1 and step S2N time, N is 5～10.
Application technical scheme, the Fe-based amorphous material that the present invention provides includes noncrystal substrate layer and surface layer, and noncrystal substrate layer is for providing the key property of Fe-based amorphous material, and worked in coordination with by the auxiliary of surface layer performance, the performance that can make Fe-based amorphous material is strengthened, improve saturation magnetization, reduce coercivity, thus improve the overall performance of Fe-based amorphous material.
Detailed description of the invention
It should be noted that in the case of not conflicting, the embodiment in the application and the feature in embodiment can be mutually combined.The application is described in detail below in conjunction with embodiment.
It should be noted that term used herein above merely to describe detailed description of the invention, and be not intended to the restricted root illustrative embodiments according to the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative is also intended to include plural form, in addition, it is to be further understood that, when using term " to comprise " in this manual and/or time " including ", it indicates existing characteristics, step, operation, device, assembly and/or combinations thereof.
From background technology, the overall performance of existing Fe-based amorphous material is poor.The present inventor studies for this technical problem, it is proposed that a kind of Fe-based amorphous material.The composition of this Fe-based amorphous material is Fe100-a-b-cMcBbAa, M is any one or more in Si, Zr, Nb, Cr, P, Al, Co, Ni, Ti, and A is N and/or C, 0.5≤a≤2at%, 9≤b≤14at%, 0≤c≤10at%；Fe-based amorphous material includes noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, and surface layer is FeA enriched layer.
In above-mentioned Fe-based amorphous material, noncrystal substrate layer is for providing the key property of Fe-based amorphous material, and worked in coordination with by the auxiliary of surface layer performance, the performance that can make Fe-based amorphous material is strengthened, improve saturation magnetization, reduce coercivity, thus improve the overall performance of Fe-based amorphous material.
The illustrative embodiments of the Fe-based amorphous material provided according to the present invention is provided.But, these illustrative embodiments can be implemented by multiple different form, and should not be construed to be limited solely to embodiments set forth herein.It should be appreciated that these embodiments are provided so that disclosure herein is thorough and complete, and the design of these illustrative embodiments is fully conveyed to those of ordinary skill in the art.
The Fe-based amorphous material that the present invention provides is composition based on FeB, and add a certain amount of M element on this basis to improve amorphous formation ability, improve overall performance, wherein M is Si, Zr, Nb, Cr, P, Al, Co, Ni, one or more in Ti, and in these addition element, Si, the amorphous formation ability of non-crystalline material is played an important role by P, Nb, Cr, the Zr precipitation to suppression metastable phase, amorphous stability is kept to play an important role, Ni, Al, Co is to promoting overall non-crystalline material saturation magnetization, initial permeability plays an important role.The addition of these elements, plays obvious facilitation to ultimately forming base layer with surface layer double-layer structure.Meanwhile, A be the addition of N and/or C, N and/or C be one of key of the present invention, by N and/or C non-crystalline material surface formed enrichment, such that it is able to improve the overall performance of non-crystalline material.
The present invention also requiring, each element exists certain proportionate relationship, calculate with atomic ratio, wherein 0.5≤a≤2at.%, 9≤b≤14at.%, 0≤c≤10at.%, the value of a, b, c can ensure that Fe content is at more than 78at.%, so that non-crystalline material has higher Saturation magnetic sense intensity, in the present invention, the content of c can be zero, in this case, material basis is FeBA.
Above-mentioned Fe-based amorphous material, it is preferable that the thickness of surface layer is 5nm～5 μm, in this scope, A forms certain enrichment wherein, forms FeA compound, and the performance of this FeA compound directly affects the performance that material is overall.Preferably, when A is N, surface layer is 50nm at thickness～occurs FeN concentration peak at 5 μm, and now, N forms certain Gradient distribution at material surface, forms certain phase structure, defines the surface layer with certain performance.In the FeN compound on surface, a series of FeN structure can be formed, 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 impact on non-crystalline material overall performance is the most different, is wherein γ '-Fe when this structure4N、ζ-Fe2During N, the raising to material corrosion resistance has significantly effect.Preferably, the structure of surface layer mainly includes α "-Fe16N2, wherein α "-Fe16N2Saturation magnetization be up to 2.8T, this compound formed obvious to the raising effect of overall performance.
Preferably, when A is C, surface forms FeC rich region, and this FeC enrichment region structure includes Fe3C、Fe2C, FeC and FeMC etc., now the thickness of surface layer occurs concentration peak at 5nm～50nm, and the surface layer structure of formation has bigger facilitation to the corrosion resistance and mechanical property that promote entirety.Preferably, the thickness of Fe-based amorphous material is 15～35 μm.
Meanwhile, what the present invention provided states Fe-based amorphous material by a variety of preparation methoies.Specifically, the modes such as technical staff can use ion implanting, magnetron sputtering carry out surface process to form the Fe-based amorphous material including noncrystal substrate layer and surface layer to noncrystal substrate material.
The embodiment of the preparation method of above-mentioned Fe-based amorphous material will be specifically described below.The preparation method of this Fe-based amorphous material comprises the following steps: prepare noncrystal substrate material, and the composition of noncrystal substrate material is Fe100-a-b-cMcBbAa, M is any one or more in Si, Zr, Nb, Cr, P, Al, Co, Ni, Ti, and A is N and/or C, 0.5≤a≤2at%, 9≤b≤14at%, 0≤c≤10at%；Noncrystal substrate material carries out surface process to form Fe-based amorphous material.
In one preferred implementation of the present invention, ion implantation technology is used to prepare Fe-based amorphous material.Ion implantation technique is a kind of material surface modifying technology grown up over nearly 30 years, its ultimate principle is: with in the ion beam incidence that energy is 100keV magnitude to material under certain atmosphere, series of physical and chemical interaction will be there is in ion beam with the atom in material or molecule, incident ion gradually off-energy, finally rest in material, and cause material surface composition, structure and performance to change, thus optimize material surface performance, or obtain some new excellent properties.Preferably, using the ion beam containing A to carry out in ion implanting, and the step of ion implanting to noncrystal substrate material, the energy of ion beam is 50～500keV, and base reservoir temperature is 100～300 DEG C.
Specifically, in ion implantation process, can non-crystalline material be put in ion implantation device, nitrogen (carbon) dividing potential drop of nitrogen containing atmosphere, base reservoir temperature and the power of ion implanting, carry out the formation of the reconciliation statement each structure of surface layer FeA.In order to reach the effect required for the present invention.Particularly, when A is N, the concrete technology of ion implanting selects to be particularly important, by adjusting process above parameter, the structure of corresponding FeA compound can occur a series of change, along with the raising of nitrogen partial pressure in nitrogen containing atmosphere, in surface layer, the concentration of A is the highest, thus is more beneficial for being formed the FeN compound of high N；Owing to magnetic moment and the Curie temperature of iron nitride reduce along with the increase of nitrogen content, α "-Fe in the magnetic material having been found that16N2There is the highest saturation flux density (2.8～3.0T), and γ '-Fe4N, ε-FexThe saturation flux density of N (2 < x≤3) is respectively 1.7T and 1.4T, ζ-Fe2N is paramagnetism at normal temperatures, and from the standpoint of magnetic, in order to prepare the FeN surface layer with high saturation and magnetic intensity, key factor is to avoid being formed the nitrided iron phase of weak magnetic in sputter procedure, the α "-Fe now formed16N2The magnetic property of integral material can be played facilitation by surface layer, and Bs is more than 1.7T, and magnetostriction coefficient and coercivity also decrease, and now nitrogen partial pressure is less than 10%, and base reservoir temperature is less than 150 DEG C.It addition, for the corrosion resistance and the mechanical property that improve material, it is necessary to obtaining the structure of high nitrogen-containing, now require that nitrogen partial pressure is 10～50%, base reservoir temperature is 150～300 DEG C.
In another kind preferred implementation of the present invention, Technology for Heating Processing is used to prepare Fe-based amorphous material.When being elected to the mode being used under nitrogen containing atmosphere nitridation to prepare, need to consider that a key factor is to carry out the infiltration of A in the case of matrix does not occurs significantly to change, particularly, it is impossible to make noncrystal substrate carry out crystallization, thus affect the performance of entirety.In this case it is desirable to whole nitridation schemes is optimized, in the present invention, the mode of multistep nitridation is used to realize the infiltration of surface carbon/nitrogen.During using nitrogen containing atmosphere nitrogen treatment, nitrogen containing atmosphere is preferably NH3, NH3+H2, N2+H2, N2.When atmosphere is NH3(N2)+H2Time, NH3(N2) and H2Ratio less than 1:3.
Preferably, the step using Technology for Heating Processing to carry out surface process comprises determining that the crystallization temperature T1 of Fe-based amorphous material；Containing A atmosphere, (T1-100)～(T1+10) temperature range under noncrystal substrate material is carried out heat treatment；Fe-based amorphous material is obtained after being cooled to room temperature.It is further preferable that the step of heat treatment includes: step S1, containing A atmosphere, (T1-100)～(T1-50) temperature range under carry out heat treatment 10～30min；Step S2, continue containing A atmosphere, (T1-20)～(T1+10) temperature range under carry out heat treatment 3～10min；Repeating step S1 and step S2N time, N is 5～10.By the step of above Fractional Heat-treatment, can effectively strengthen the activity of Nitrogen ion in atmosphere, such that it is able to carry out nitriding operation when less than crystallization temperature, make base layer not recurring structure change, keep the stability of overall performance.
Fe-based amorphous material of present invention offer and preparation method thereof is be provided below in conjunction with embodiment.
Embodiment 1
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe87.2B12.3N0.5, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 15 μm, and the thickness of surface layer is 50nm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, using nitrogenous ion beam noncrystal substrate material to carry out ion implanting to form Fe-based amorphous material, wherein the energy of ion beam is 50keV, and base reservoir temperature is 100 DEG C.
Embodiment 2
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe82.0P2.0Cr0.5B13.5N2.0, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 35 μm, and the thickness of surface layer is 5 μm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, using nitrogenous ion beam noncrystal substrate material to carry out ion implanting to form Fe-based amorphous material, wherein the energy of ion beam is 80keV, and base reservoir temperature is 250 DEG C.
Embodiment 3
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe84.4Si1.5Zr1.9Co2.0B9.0N1.2, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 19 μm, and the thickness of surface layer is 200nm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, using nitrogenous ion beam noncrystal substrate material to carry out ion implanting to form Fe-based amorphous material, wherein the energy of ion beam is 60keV, and base reservoir temperature is 215 DEG C.
Embodiment 4
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe79.1P1.6Nb0.8Al1.9Ni2.5Ti1.2B11.1N1.8, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 26 μm, and the thickness of surface layer is 800nm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, using nitrogenous ion beam noncrystal substrate material to carry out ion implanting to form Fe-based amorphous material, wherein the energy of ion beam is 70keV, and base reservoir temperature is 300 DEG C.
Embodiment 5
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe82.3Si3.2B14.0N0.5, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 15 μm, and the thickness of surface layer is 500nm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, carrying out heat treatment, wherein heat treatment temperature is 450 DEG C, and heat treatment time is 30min, obtains Fe-based amorphous material after being cooled to room temperature.
Embodiment 6
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe83.3Nb1.3Cr2.0B12.9N0.5, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 22 μm, and the thickness of surface layer is 150nm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, carrying out heat treatment, wherein heat treatment temperature is 410 DEG C, and heat treatment time is 15min, obtains Fe-based amorphous material after being cooled to room temperature.
Embodiment 7
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe82.1Co1.6Ni1.9B12.8N1.6, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 17 μm, and the thickness of surface layer is 80nm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, carrying out heat treatment, wherein heat treatment temperature is 510 DEG C, and heat treatment time is 29min, obtains Fe-based amorphous material after being cooled to room temperature.
Embodiment 8
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe85.5Si2.1Zr0.9B9.7N1.8, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 25 μm, and the thickness of surface layer is 2 μm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, carrying out heat treatment, wherein heat treatment includes: step S1, heat treatment temperature are 400 DEG C, and heat treatment time is 10min；Step S2, heat treatment temperature are 480 DEG C, and heat treatment time is 3min；Repeated execution of steps S1 and S25 time, obtain Fe-based amorphous material after being cooled to room temperature.
Embodiment 9
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe83.6Cr2.8Co1.5B10.2N1.9, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 31 μm, and the thickness of surface layer is 3 μm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, carrying out heat treatment, wherein heat treatment includes: step S1, heat treatment temperature are 460 DEG C, and heat treatment time is 20min；Step S2, heat treatment temperature are 510 DEG C, and heat treatment time is 10min；Repeated execution of steps S1 and S210 time, obtain Fe-based amorphous material after being cooled to room temperature.
Embodiment 10
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe83.4P1.8Ni1.3B13.4N0.1, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes α "-Fe16N2, amorphous and α-Fe etc., the thickness of noncrystal substrate layer is 29 μm, and the thickness of surface layer is 20nm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, carrying out heat treatment, wherein heat treatment temperature is 500 DEG C, and heat treatment time is 20min, obtains Fe-based amorphous material after being cooled to room temperature.
Embodiment 11
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe84.8Zr1.2Al2.3B11.6N0.15, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes γ '-Fe4N and ζ-Fe2N, the thickness of noncrystal substrate layer is 32 μm, and the thickness of surface layer is 30nm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, using nitrogenous ion beam noncrystal substrate material to carry out ion implanting to form Fe-based amorphous material, wherein the energy of ion beam is 50keV, and base reservoir temperature is 300 DEG C.
Embodiment 12
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe78.0Si4.5P2.6Nb1.4Co1.6B11.0C0.9, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes Fe3C、Fe2C, FeC and FeMC etc., the thickness of noncrystal substrate layer is 22 μm, and the thickness of surface layer is 5nm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, using nitrogenous ion beam noncrystal substrate material to carry out ion implanting to form Fe-based amorphous material, wherein the energy of ion beam is 60keV, and base reservoir temperature is 150 DEG C.
Embodiment 13
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe83.9Zr1.5Al1.2Ni2.0Ti0.9B9.0C1.5, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the structure of surface layer includes Fe3C、Fe2C, FeC and FeMC etc., the thickness of noncrystal substrate layer is 31 μm, and the thickness of surface layer is 32nm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, using nitrogenous ion beam noncrystal substrate material to carry out ion implanting to form Fe-based amorphous material, wherein the energy of ion beam is 70keV, and base reservoir temperature is 250 DEG C.
Embodiment 14
Present embodiments providing a kind of Fe-based amorphous material and preparation method thereof, wherein, the composition of this Fe-based amorphous material is Fe85.0P2.0Cr1.0B10.0C2.0, and this non-crystalline material includes that thickness is noncrystal substrate layer and the surface layer being positioned on noncrystal substrate layer, the thickness of noncrystal substrate layer is 35 μm, and the thickness of surface layer is 50nm.
The step preparing this Fe-based amorphous material includes: first, prepares noncrystal substrate material by proportioning；Then, using nitrogenous ion beam noncrystal substrate material to carry out ion implanting to form Fe-based amorphous material, wherein the energy of ion beam is 90keV, and base reservoir temperature is 290 DEG C.
Comparative example 1
This comparative example provides a kind of Fe-based amorphous material, and wherein, the composition of this Fe-based amorphous material is Fe89.5Si1.5B9.0。
Comparative example 2
This comparative example provides a kind of Fe-based amorphous material, and wherein, the composition of this Fe-based amorphous material is Fe84.0P2.0B14.0。
Test: the Fe-based amorphous material obtaining embodiment 1 to 14 and comparative example 1 to 2 carries out performance test, and test result is as shown in table 1.As it can be seen from table 1 the saturation magnetization Ms value of the Fe-based amorphous material of embodiment 1 to 14 acquisition is 1.31～2.35T, magnetostriction coefficient is 1.5～15；And the saturation magnetization Ms value of the Fe-based amorphous material that comparative example 1 to 2 obtains is 1.47～1.52T, magnetostriction coefficient is 26～23.Visible, the Fe-based amorphous material obtained due to comparative example 1 to 2 does not has surface layer so that it is coercivity is bigger.Meanwhile, as it can be seen from table 1 the corrosion resistance of the Fe-based amorphous material of embodiment 1 to 14 acquisition 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 | Trace pit |
| Embodiment 2 | 1.98 | 2.7 | Trace pit |
| Embodiment 3 | 2.35 | 5.3 | Trace pit |
| Embodiment 4 | 1.86 | 1.5 | Trace pit |
| Embodiment 5 | 1.93 | 4.9 | Trace pit |
| Embodiment 6 | 1.88 | 3.7 | Trace pit |
| Embodiment 7 | 1.74 | 3.9 | Trace pit |
| Embodiment 8 | 2.09 | 3.5 | Trace pit |
| Embodiment 9 | 2.28 | 2.9 | Trace pit |
| Embodiment 10 | 1.65 | 15 | A large amount of pits and white rust |
| Embodiment 11 | 1.53 | 13 | A large amount of pits 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 pits and white rust |
| Comparative example 2 | 1.52 | 23 | A large amount of pits and white rust |
As can be seen from the above embodiments, the above-mentioned example of the present invention achieves following technique effect: the Fe-based amorphous material that the present invention provides includes noncrystal substrate layer and surface layer, and noncrystal substrate layer is for providing the key property of Fe-based amorphous material, and worked in coordination with by the auxiliary of surface layer performance, the performance that can make Fe-based amorphous material is strengthened, improve saturation magnetization, reduce coercivity, thus improve the overall performance of Fe-based amorphous material.
These are only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (10)
1. a Fe-based amorphous material, it is characterised in that the composition of described Fe-based amorphous material is Fe100-a-b-cMcBbAa, M be Si,
Any one or more in Zr, Nb, Cr, P, Al, Co, Ni, Ti, A is N and/or C, 0.5≤a≤2at%, 9≤b≤14at%,
0≤c≤10at%；Described Fe-based amorphous material includes noncrystal substrate layer and the surface layer being positioned on described noncrystal substrate layer, described
Surface layer is FeA enriched layer.
Fe-based amorphous material the most according to claim 1, it is characterised in that the thickness of described surface layer is 5nm～5 μm.
Fe-based amorphous material the most according to claim 1, it is characterised in that A is N, the structure of described surface layer includes
α″-Fe16N2。
Fe-based amorphous material the most according to claim 1, it is characterised in that when A is N, along away from described noncrystal substrate
On the direction of layer, described surface layer is 50nm～FeN concentration at 5 μm is the highest at thickness.
Fe-based amorphous material the most according to claim 1, it is characterised in that when A is C, along away from described noncrystal substrate
On the direction of layer, described surface layer is that the FeC concentration at 5nm～50nm is the highest at thickness.
Fe-based amorphous material the most according to any one of claim 1 to 5, it is characterised in that described Fe-based amorphous material
Thickness is 15～35 μm.
7. the preparation method of the Fe-based amorphous material according to any one of a claim 1 to 6, it is characterised in that described preparation
Method comprises the following steps:
Preparing noncrystal substrate material, the composition of described noncrystal substrate material is Fe100-a-b-cMcBbAa, M is Si, Zr, Nb,
Any one or more in Cr, P, Al, Co, Ni, Ti, A is N and/or C, 0.5≤a≤2at%, 9≤b≤14at%,
0≤c≤10at%；
Described noncrystal substrate material carries out surface process to form described Fe-based amorphous material.
Preparation method the most according to claim 7, it is characterised in that the step that described surface processes includes: use containing A's
Described noncrystal substrate material is carried out in ion implanting, and the step of described ion implanting by ion beam, the energy of described ion beam
Amount is 50～500keV, and base reservoir temperature is 100～300 DEG C.
Preparation method the most according to claim 7, it is characterised in that the step that described surface processes includes:
Determine the crystallization temperature T1 of described Fe-based amorphous material；
Containing A atmosphere, (T1-100)～(T1+10) temperature range under described noncrystal substrate material is carried out heat treatment；
Described Fe-based amorphous material is obtained after being cooled to room temperature.
Preparation method the most according to claim 9, it is characterised in that the step of described heat treatment includes:
Step S1, containing A atmosphere, (T1-100)～(T1-50) temperature range under carry out heat treatment 10～30min；
Step S2, continue containing A atmosphere, (T1-20)～(T1+10) temperature range under carry out heat treatment 3～10min；
Repeating said steps S1 and described step S2N time, N is 5～10.
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