CN110358959A - A kind of magnetostrictive thin film composite material and preparation method - Google Patents
A kind of magnetostrictive thin film composite material and preparation method Download PDFInfo
- Publication number
- CN110358959A CN110358959A CN201810311956.1A CN201810311956A CN110358959A CN 110358959 A CN110358959 A CN 110358959A CN 201810311956 A CN201810311956 A CN 201810311956A CN 110358959 A CN110358959 A CN 110358959A
- Authority
- CN
- China
- Prior art keywords
- layer
- magnetostrictive
- thin film
- composite material
- film composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F10/00—Thin magnetic films, e.g. of one-domain structure
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F10/00—Thin magnetic films, e.g. of one-domain structure
- H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
- H01F10/10—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
- H01F10/12—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
- H01F10/126—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing rare earth metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Thin Magnetic Films (AREA)
- Investigating Or Analyzing Materials By The Use Of Ultrasonic Waves (AREA)
Abstract
A kind of magnetostrictive thin film composite material and preparation method, the film composite material are sequentially compounding by protective layer, magnetostrictive layer, flexible substrate layer, the chemical formula of the magnetostrictive layer are as follows: (Tb1‑xDyx‑δNδ)(Fe1‑yMy)zWherein 0.60≤x≤0.80,0≤y≤0.2,1.8≤z≤2.2,0≤δ≤0.3, M represents combination one kind or two or more in B, Al, Si, Ti, V, Cr, Mn, Co, Ni, Zn, Ga, Nb, Ta and W, and N represents combination one kind or two or more in other rare earth elements in addition to Tb and Dy.Magnetostrictive thin film composite material interface combined strength bination of the invention is high, structure is simple, effectively prevents the damage of magnetostrictive layer, has good piezomagnetic coefficient (d33), alternative frequency eddy-current loss is small, performance is stable, size is frivolous, is very suitable to prepare magnetic-sonic transducer and Ultrasonic Nondestructive sensor.
Description
Technical field
The invention belongs to magnetic functional material and preparation technical fields and magnetic-sound mechanical switch and sound wave non-destructive testing technology
Field, and in particular to a kind of magnetostrictive thin film composite material and preparation method.
Background technique
Wei Deman (Weidman) effect based on magnetostriction materials of the principle of magnetostriction type ultrasonic guided wave transducer
Answer, to magnetostriction materials apply different directions bias magnetic field and excitation field and make its generate torsional wave, torsional wave to
Sectional area, which changes, when propagation encounters defect in survey part can generate echo, by being widely used in echo-signal analysis processing
Field of non destructive testing.Magnetostriction materials in common non-destructive testing ultrasonic guided wave transducer have FeCo strip, Ni strip
Deng these materials are easy to process, have preferable flexible, can be adapted for the detection of the non-planar part to be measured such as tubing.But this
The saturation magnetostriction of a little materials is lower, has considerable restraint to detection effect and conversion efficiency.
Terbium dysprosium ferrum (TbDyFe) rare earth ultra-magnetostriction material has the magnetostriction much higher than other non-rare earth alloys
Can, have the characteristics that high-energy density, high-magnetostriction coefficient, high sensitivity, has one in the defence and militaries such as naval's sonar field
Fixed application.Although terbium dysprosium ferrum material has very high λ111, but the material has MgCu2Type structure, brittleness is big, and tension is strong
Degree is very low, and almost without plastic deformation, magnetizing field is higher, and in addition a high proportion of high cost problem of heavy rare earth element bring also limits
It has been made in the application of other field.Researcher improves it by filming using disadvantage, even the two dimension of terbium dysprosium ferrum is thin
Film, still with the Magnetostriction of 200~800ppm.
For magnetostrictive thin film, good piezomagnetic coefficient d33=(d λ/dH)maxIt is the basis of application, therefore is directed to mangneto
The raising of self-adhering film low field magnetosensitive performance is always the emphasis of research.Low field magnetosensitive performance mainly with the magnetic anisotropy of film
Can be related, it is expressed as follows:
Wherein, Es、EdAnd EσRespectively indicate the uniaxial anisotropy energy, demagnetization energy and magnetoelastic energy of film, KeffectIt is thin
Film effective magnetic anisotropy constant, θ are the angle of stress direction and magnetization orientation, KsFor uniaxial anisotropy constant, N is demagnetization
The factor, μ0For space permeability, MsFor saturation magnetization, λsFor saturation magnetostriction constant, σ is inter-laminar stress.
According to minimum energy principle, in order to obtain good low field magnetosensitive, need to reduce K as far as possibleeffect, specifically mention
High method can be summarized as following four: adjust the ingredient of film, the decrystallized and nano-crystallization of film changes the interior of film
Stress state and multilayer film coupling.Make film direction of easy axis deflect into direction in face by these types of method, improves film
Saturation magnetization and saturation magnetostriction constant.
Summary of the invention
One of the objects of the present invention is to provide a kind of novel magnetostrictive thin film composite material, the material magnetostriction
It is functional, conversion efficiency is high, performance is stable.
To achieve the above object, the present invention takes following technical scheme:
A kind of magnetostrictive thin film composite material, the film composite material is by protective layer, magnetostrictive layer, flexible substrate layer
It is sequentially compounding,
The chemical formula of the magnetostrictive layer are as follows: (Tb1-xDyx-δNδ)(Fe1-yMy)z, wherein 0.60≤x≤0.80,0≤y
≤ 0.2,1.8≤z≤2.2,0≤δ≤0.3, M represent in B, Al, Si, Ti, V, Cr, Mn, Co, Ni, Zn, Ga, Nb, Ta and W a kind
Or combination of more than two kinds, N represent combination one kind or two or more in other rare earth elements in addition to Tb and Dy.
That present invention is generally directed to traditional magnetostriction type ultrasonic guided wave energy exchange material magnetostriction coefficients and conversion efficiency is low,
The shortcomings such as detection effect difference propose a kind of completely new magnetostrictive thin film composite material, by flexible substrate and rare earth
Giant magnetostrictive thin film is combined, and additional shields, not only plays anti-oxidation, scratch resistance effect to magnetostrictive thin film,
And Magnetostriction is effectively improved compared with traditional material, conversion efficiency is good, and alternative frequency eddy-current loss is small, performance stabilization,
Preparation is simple, is very suitable for ultrasonic guided wave energy exchange and senser element.The substrate layer that the present invention uses be it is flexible, can be fitted in
It is applied widely in the non-planar materials such as pipeline, there is higher use value in energy converter and non-destructive testing sensor.
Preferably, the ingredient of the protective layer is combination one kind or two or more in Ta, Cr, Al, Zn, Cu, W, or it is
Epoxy resin, polyvinyl alcohol, combination one kind or two or more in PET.
Preferably, the magnetostrictive layer be single layer magnetostrictive thin film material, or for magnetostrictive thin film layer with it is soft
The multi-layer compound structure of magnetic thin film layer composition.
Preferably, the material of the flexible substrate layer be polyimides (PI), polyvinyl alcohol (PVA), polyester (PET),
One kind or two or more combination in magnetically soft alloy band.
Preferably, the chemical formula of the soft magnetic film layer or magnetically soft alloy band are as follows: FexCoyM100-x-y、FexNiyM100-x-y、
FexSiyM100-x-yIn any, wherein atomic ratio 0≤x≤100,0≤y≤100, M represent B, Al, Si, Ni, Ti, V, Cr, Mn,
One kind or two or more combination in Co, Ni, Zn, Ga, Nb, Ta and W.
Preferably, the protective layer with a thickness of 0.01-1000 μm, the magnetostrictive layer with a thickness of 0.001-
1000 μm, the flexible substrate layer with a thickness of 0.05-2mm.
An object of the present invention, which also resides in, provides a kind of magnetostrictive thin film composite material of the present invention preparation side
Method includes the following steps:
(1) flexible substrate material is processed into flakiness；
(2) magnetostrictive layer is deposited on the flexible substrate thin slice obtained by step (1)；
(3) protective layer is deposited on the magnetostrictive layer prepared.
Thin slice is cleaned up after processing flakiness in step (1).
It can according to need the annealing or unannealed processing for carrying out different temperatures after magnetostrictive layer deposition.As excellent
It selects, makes annealing treatment 10-90min at 300-600 DEG C after magnetostrictive layer deposition in step (2).
The deposition method for depositing protective layer in magnetostrictive layer or step (3) in step (2) on flexible substrate thin slice is
Any one of magnetron sputtering, pulse laser deposition, electron beam evaporation, multi-arc ion plating process, swabbing firing process and cladding process.
Deposition method in step (2) and step (3) may be the same or different.
The compound of flexible substrate and magnetostrictive thin film has certain a flexible and toughness in method of the invention, attached
Add protective layer, anti-oxidation, scratch resistance effect can also be played to magnetostrictive thin film, advantageously ensures that composite material magnetostriction
Performance, the stabilization of conversion efficiency.Relatively thin magnetostrictive thin film also efficiently avoids vortex damage of the material under alternative frequency
Consumption, improves the conversion efficiency of material.
Magnetostrictive thin film composite material interface combined strength bination of the invention is high, structure is simple, effectively prevents mangneto stretches
The damage of contracting layer has good piezomagnetic coefficient (d33), alternative frequency eddy-current loss is small, performance is stable, size is frivolous, very suitable
Conjunction prepares magnetic-sonic transducer and Ultrasonic Nondestructive sensor.
In addition, can effectively improve magnetostrictive thin film by the annealing of certain condition in preparation method of the present invention
Interior state, reduce the magnetic anisotropy energy of parallel film surface use direction, improve the Magnetostriction of material.
Detailed description of the invention
Fig. 1 is the magnetostrictive thin film composite structure schematic diagram of 1-4 of the embodiment of the present invention；
Fig. 2 is the magnetostrictive thin film composite structure schematic diagram of 5-8 of the embodiment of the present invention；
In figure: 1- flexible substrate, 2- protective layer, 3- magnetostrictive layer.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
As shown in Figure 1, being a kind of magnetostrictive thin film composite structure schematic diagram provided by the invention, in the composite junction
Protective layer 2, magnetostrictive layer 3, flexible substrate layer 1 are arranged successively in structure, and flexible substrate layer is carried out single side throwing first when processing
Light；After substrate is cleaned, magnetostrictive layer is prepared in the burnishing surface deposition of the substrate；Then compound one layer of layer upper layer is stretched in mangneto
Protective layer obtains film magnetoelectric composite structure shown in Fig. 1.Specific preparation method is visible: embodiment 1-6.
As shown in Fig. 2, being a kind of magnetostrictive thin film composite structure schematic diagram provided by the invention, in the composite junction
Protective layer 2, magnetostrictive layer 3, flexible substrate layer 1, magnetostrictive layer 3, protective layer 2 are arranged successively in structure, first will when processing
Flexible substrate layer carries out twin polishing；After substrate is cleaned, preparation magnetostriction is deposited respectively in the bilateral burnishing surface of the substrate
Layer；The compound one layer of protective layer in layer upper layer then is stretched in mangneto, obtains film magnetoelectric composite structure shown in Fig. 2.Specific preparation
Method is visible: embodiment 7-12.
Embodiment 1
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: polyimides (PI) substrate is processed into size
For the thin slice of 20 × 20 × 0.3mm, single-sided polishing after cleaning up, uses the method for magnetically controlled DC sputtering at room temperature
(the Tb that a layer thickness is 10 μm is deposited in the burnishing surface of substrate0.3Dy0.7)Fe1.95Magnetostrictive thin film, after deposition
Continue the Ta layer that deposition thickness is 100nm and be used as protective layer in magnetostrictive thin film surface layer.
After the completion of material preparation, by flexible composite under the static magnetic field of 5000Oe, magnetostriction coefficient is
200ppm.At room temperature by flexible composite, 5s is magnetized along the direction plane x by permanent-magnet and then passes through integrated coil
Apply the alternating magnetic field along the direction plane y, the electromechanical coupling of material is measured under the conditions of coil power 80%, stimulating frequency 128kHz
Collaboration number reaches 20% or more, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude at the position sample 0.6m
2.0V。
Embodiment 2
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: polyimides (PI) substrate is processed into size
For the thin slice of 20 × 20 × 0.3mm, single-sided polishing after cleaning up, uses spin-coating method in the polishing of substrate at room temperature
(the Tb that one layer of face coating a layer thickness is 100 μm0.3Dy0.7)Fe1.95The mixture of phosphatization fine powder and macromolecule organic solution applies
Continue to coat a layer thickness to be 10 μm of polyester (PET) as protective layer on surface layer after covering, at 80 DEG C after the completion of material preparation
The dry 2h of vacuum oven.
By flexible composite under the static magnetic field of 5000Oe, characterization magnetostriction coefficient is 400ppm.Flexibility is multiple
Condensation material magnetizes 5s along the direction plane x at room temperature, by permanent-magnet, then, is applied by integrated coil along the direction plane y
Alternating magnetic field, under the conditions of coil power 80%, stimulating frequency 128kHz measure material electromechanical coupling factor reach 20%
More than, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude 2.1V at the position sample 0.6m.
Embodiment 3
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: by chemical formula be Fe48Co50V2Rolled iron cobalt
Thin slice is processed into the thin slice that size is 50 × 30 × 0.5mm, and single-sided polishing after cleaning up, uses direct current at room temperature
The method of magnetron sputtering deposits the (Tb that a layer thickness is 10 μm in the burnishing surface of substrate0.3Dy0.7)Fe1.95Magnetostriction it is thin
Film continues Ta layer that deposition thickness is 100nm as protective layer on magnetostrictive thin film surface layer after deposition.Film has deposited
Bi Hou, the in-situ annealing 1h at 600 DEG C.
After the completion of material preparation, by flexible composite under the static magnetic field of 5000Oe, magnetostriction coefficient is
350ppm.At room temperature by flexible composite, 5s is magnetized along the direction plane x by permanent-magnet and then passes through integrated coil
Apply the alternating magnetic field along the direction plane y, the electromechanical coupling of material is measured under the conditions of coil power 80%, stimulating frequency 128kHz
Collaboration number reaches 25% or more, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude at the position sample 0.6m
2.5V (saturation).
Embodiment 4
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: by chemical formula be Fe48Co50V2Rolled iron cobalt
Thin slice is processed into the thin slice that size is 20 × 20 × 0.5mm, and single-sided polishing after cleaning up, uses spin coating at room temperature
(the Tb that method is 100 μm in one layer of burnishing surface coating a layer thickness of substrate0.3Dy0.7)Fe1.95Phosphatization fine powder and macromolecule are organic
The mixture of solution continues to coat a layer thickness to be 10 μm of polyvinyl alcohol as protective layer, material system after coating on surface layer
The dry 2h of vacuum oven after the completion of standby at 80 DEG C.
By flexible composite under the static magnetic field of 5000Oe, characterization magnetostriction coefficient is 500ppm.Flexibility is multiple
Condensation material magnetizes 5s along the direction plane x at room temperature, by permanent-magnet, then, is applied by integrated coil along the direction plane y
Alternating magnetic field, under the conditions of coil power 80%, stimulating frequency 128kHz measure material electromechanical coupling factor reach 20%
More than, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude 2.5V (saturation) at the position sample 0.6m.
Embodiment 5
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: by chemical formula be Fe48Ni50Zn2Rolling it is thin
Piece is processed into the thin slice that size is 20 × 20 × 0.5mm, and single-sided polishing after cleaning up, uses DC magnetic at room temperature
The method for controlling sputtering deposits the (Tb that a layer thickness is 10 μm in the burnishing surface of substrate0.2Dy0.7Pr0.1)(Fe1.9Nb0.2) mangneto
Self-adhering film continues Ta layer that deposition thickness is 100nm as protective layer on magnetostrictive thin film surface layer after deposition.Film
After deposition, the in-situ annealing 1h at 600 DEG C.
After the completion of material preparation, by flexible composite under the static magnetic field of 5000Oe, magnetostriction coefficient is
300ppm.At room temperature by flexible composite, 5s is magnetized along the direction plane x by permanent-magnet and then passes through integrated coil
Apply the alternating magnetic field along the direction plane y, the electromechanical coupling of material is measured under the conditions of coil power 80%, stimulating frequency 128kHz
Collaboration number reaches 20% or more, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude at the position sample 0.6m
2.4V。
Embodiment 6
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: be processed into the rolled sheet that chemical formula is Ni
Size is the thin slice of 20 × 20 × 0.5mm, single-sided polishing, after cleaning up, at room temperature using spin-coating method in substrate
(the Tb that one layer of burnishing surface coating a layer thickness is 1000 μm0.4Dy0.5Pr0.1)(Fe1.6Co0.4) phosphatization fine powder and macromolecule it is organic
The mixture of solution continues to coat a layer thickness to be 10 μm of polyvinyl alcohol as protective layer, material system after coating on surface layer
The dry 2h of vacuum oven after the completion of standby at 80 DEG C.
By flexible composite under the static magnetic field of 5000Oe, characterization magnetostriction coefficient is 400ppm.Flexibility is multiple
Condensation material magnetizes 5s along the direction plane x at room temperature, by permanent-magnet, then, is applied by integrated coil along the direction plane y
Alternating magnetic field, under the conditions of coil power 80%, stimulating frequency 128kHz measure material electromechanical coupling factor reach 25%
More than, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude 2.5V (saturation) at the position sample 0.6m.Implement
Example 7
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: polyimides (PI) substrate is processed into size
For the thin slice of 20 × 20 × 0.3mm, twin polishing after cleaning up, uses the method for magnetically controlled DC sputtering at room temperature
(the Tb for being 10 μm in the two-sided a layer thickness of deposition respectively of the burnishing surface of substrate0.3Dy0.7)Fe1.95Magnetostrictive thin film, deposition
After magnetostrictive thin film surface layer continue respectively deposition thickness be 100nm Ta layer be used as protective layer.
At room temperature by flexible composite, 5s is magnetized along the direction plane x by permanent-magnet, then, by integrating line
Circle applies the alternating magnetic field along the direction plane y, and the electromechanics of material is measured under the conditions of coil power 80%, stimulating frequency 128kHz
The coefficient of coup reaches 20% or more, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude at the position sample 0.6m
2.2V。
Embodiment 8
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: polyimides (PI) substrate is processed into size
For the thin slice of 20 × 20 × 0.3mm, twin polishing after cleaning up, uses spin-coating method in the polishing of substrate at room temperature
(the Tb that a layer thickness is 100 μm is respectively coated in face0.3Dy0.7)Fe1.95The mixture of phosphatization fine powder and macromolecule organic solution applies
Continue to coat a layer thickness to be 10 μm of epoxy resin as protective layer on surface layer after covering, at 80 DEG C after the completion of material preparation
Vacuum oven dries 2h.
At room temperature by flexible composite, 5s is magnetized along the direction plane x by permanent-magnet, then, by integrating line
Circle applies the alternating magnetic field along the direction plane y, and the electromechanics of material is measured under the conditions of coil power 80%, stimulating frequency 128kHz
The coefficient of coup reaches 20% or more, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude at the position sample 0.6m
2.4V。
Embodiment 9
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: by chemical formula be Fe48Co50V2Rolled iron cobalt
Thin slice is processed into the thin slice that size is 50 × 30 × 0.5mm, and twin polishing after cleaning up, uses direct current at room temperature
The method of magnetron sputtering deposits the (Tb that a layer thickness is 10 μm in the burnishing surface of substrate respectively0.3Dy0.7)Fe1.95Magnetostriction
Film continues the Ta layer that deposition thickness is 100nm on magnetostrictive thin film surface layer after deposition respectively and is used as protective layer.Film
After deposition, the in-situ annealing 1h at 600 DEG C.
At room temperature by flexible composite, 5s is magnetized along the direction plane x by permanent-magnet, then, by integrating line
Circle applies the alternating magnetic field along the direction plane y, and the electromechanics of material is measured under the conditions of coil power 80%, stimulating frequency 128kHz
The coefficient of coup reaches 25% or more, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude at the position sample 0.6m
2.5V (saturation).
Embodiment 10
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: by chemical formula be Fe48Co50V2Rolled iron cobalt
Thin slice is processed into the thin slice that size is 20 × 20 × 0.5mm, and twin polishing after cleaning up, uses spin coating at room temperature
(the Tb that a layer thickness is 100 μm is respectively coated in the burnishing surface of substrate in method0.3Dy0.7)Fe1.95Phosphatization fine powder and macromolecule are organic
The mixture of solution continues to coat a layer thickness respectively to be 10 μm of epoxy resin as protective layer, material after coating on surface layer
The dry 2h of vacuum oven after the completion of material preparation at 80 DEG C.
At room temperature by flexible composite, 5s is magnetized along the direction plane x by permanent-magnet, then, by integrating line
Circle applies the alternating magnetic field along the direction plane y, and the electromechanics of material is measured under the conditions of coil power 80%, stimulating frequency 128kHz
The coefficient of coup reaches 20% or more, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude at the position sample 0.6m
2.5V (saturation).
Embodiment 11
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: polyimides (PI) substrate is processed into size
For the thin slice of 20 × 20 × 0.3mm, twin polishing after cleaning up, uses spin-coating method in the polishing of substrate at room temperature
(the Tb that a layer thickness is 100 μm is respectively coated in face0.2Dy0.6Pr0.1Ce0.1)(Fe1.9Zn0.1) phosphatization fine powder and macromolecule it is organic molten
The mixture of liquid continues to coat a layer thickness to be 10 μm of epoxy resin as protective layer, material preparation after coating on surface layer
After the completion in 80 DEG C of the dry 2h of vacuum oven.
At room temperature by flexible composite, 5s is magnetized along the direction plane x by permanent-magnet, then, by integrating line
Circle applies the alternating magnetic field along the direction plane y, and the electromechanics of material is measured under the conditions of coil power 80%, stimulating frequency 128kHz
The coefficient of coup reaches 20% or more, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude at the position sample 0.6m
2.2V。
Embodiment 12
The magnetostrictive thin film composite material and preparation method thereof of the present embodiment are as follows: by chemical formula be Fe50Co50Rolled iron cobalt
Thin slice is processed into the thin slice that size is 50 × 30 × 0.5mm, and twin polishing after cleaning up, uses direct current at room temperature
The method of magnetron sputtering deposits the (Tb that a layer thickness is 10 μm in the burnishing surface of substrate respectively0.2Dy0.6Pr0.2)(Fe1.9Co0.1)
Magnetostrictive thin film, continue the Ta layer conduct that deposition thickness is 100nm respectively on magnetostrictive thin film surface layer after deposition
Protective layer.After film deposits, the in-situ annealing 1h at 600 DEG C.
At room temperature by flexible composite, 5s is magnetized along the direction plane x by permanent-magnet, then, by integrating line
Circle applies the alternating magnetic field along the direction plane y, and the electromechanics of material is measured under the conditions of coil power 80%, stimulating frequency 128kHz
The coefficient of coup reaches 25% or more, MSGW ultrasonic guided wave detecting instrument sign edge echo signal amplitude at the position sample 0.6m
2.4V (saturation), (under the conditions of corresponding, the echo-signal amplitude of end face passes through more single FeCo material in 2.2V or less)
Compound prepares material, and performance parameter makes moderate progress.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (10)
1. a kind of magnetostrictive thin film composite material, which is characterized in that the film composite material is by protective layer, magnetostriction
Layer, flexible substrate layer are sequentially compounding,
The chemical formula of the magnetostrictive layer are as follows: (Tb1-xDyx-δNδ)(Fe1-yMy)z, wherein 0.60≤x≤0.80,0≤y≤
0.2,1.8≤z≤2.2,0≤δ≤0.3, M represent in B, Al, Si, Ti, V, Cr, Mn, Co, Ni, Zn, Ga, Nb, Ta and W a kind or
Combination of more than two kinds, N represent combination one kind or two or more in other rare earth elements in addition to Tb and Dy.
2. magnetostrictive thin film composite material according to claim 1, which is characterized in that the ingredient of the protective layer is
One kind or two or more combination in Ta, Cr, Al, Zn, Cu, W.
3. magnetostrictive thin film composite material according to claim 1, which is characterized in that the ingredient of the protective layer is ring
Oxygen resin, polyvinyl alcohol, combination one kind or two or more in PET.
4. magnetostrictive thin film composite material according to claim 1-3, which is characterized in that the magnetostriction
Layer is single layer magnetostrictive thin film material.
5. magnetostrictive thin film composite material according to claim 1-3, which is characterized in that the magnetostriction
Layer is the multi-layer compound structure of magnetostrictive thin film layer and soft magnetic film layer composition.
6. magnetostrictive thin film composite material according to claim 1-5, which is characterized in that the flexible substrate
The material of layer is polyimides, polyvinyl alcohol, PET, combination one kind or two or more in magnetically soft alloy band.
7. magnetostrictive thin film composite material according to claim 5 or 6, which is characterized in that the soft magnetic film layer or
The chemical formula of magnetically soft alloy band are as follows: FexCoyM100-x-y、FexNiyM100-x-y、FexSiyM100-x-yIn any, wherein atomic ratio 0
≤ x≤100,0≤y≤100, M represent in B, Al, Si, Ni, Ti, V, Cr, Mn, Co, Ni, Zn, Ga, Nb, Ta and W a kind or 2 kinds
Above combination.
8. magnetostrictive thin film composite material according to claim 1-7, which is characterized in that the protective layer
With a thickness of 0.01-1000 μm, the magnetostrictive layer with a thickness of 0.001-1000 μm, the flexible substrate layer with a thickness of
0.05-2mm。
9. a kind of described in any item magnetostrictive thin film composite material and preparation method thereofs of claim 1-8, include the following steps:
(1) flexible substrate material is processed into flakiness；
(2) magnetostrictive layer is deposited on the flexible substrate thin slice obtained by step (1)；
(3) protective layer is deposited on the magnetostrictive layer prepared.
10. preparation method according to claim 9, which is characterized in that in step (2) magnetostrictive layer deposition after
10-90min is made annealing treatment at 300-600 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810311956.1A CN110358959B (en) | 2018-04-09 | 2018-04-09 | Magnetostrictive film composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810311956.1A CN110358959B (en) | 2018-04-09 | 2018-04-09 | Magnetostrictive film composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110358959A true CN110358959A (en) | 2019-10-22 |
| CN110358959B CN110358959B (en) | 2021-03-19 |
Family
ID=68212153
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810311956.1A Active CN110358959B (en) | 2018-04-09 | 2018-04-09 | Magnetostrictive film composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110358959B (en) |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994000695A1 (en) * | 1992-06-20 | 1994-01-06 | Robert Bosch Gmbh | Magnetostrictive transducer |
| CN1392194A (en) * | 2002-07-02 | 2003-01-22 | 武汉理工大学 | Poly meta-fluoroethylene/lead zirconate titanate/terbium dysprosium iron composite material sheet with magnetoelectric property and its preparation |
| US20050116831A1 (en) * | 2003-12-01 | 2005-06-02 | Anis Zribi | Contactless humidity/chemical vapor sensor device and associated method of fabrication |
| CN101599340A (en) * | 2009-04-08 | 2009-12-09 | 南京航空航天大学 | Direct magnetic coupling preparation method of magneto strictive multiplayer film |
| CN101748407A (en) * | 2010-01-20 | 2010-06-23 | 中国船舶重工集团公司第七二五研究所 | Preparation method of surface composite coating of Tb-Dy-Fe magnetostrictive material |
| US7927439B1 (en) * | 2008-08-08 | 2011-04-19 | The United States Of America As Represented By The Secretary Of The Navy | Shock compression sensitivity change on command of explosives containing SMART materials |
| CN102044626A (en) * | 2009-10-20 | 2011-05-04 | 北京有色金属研究总院 | Film magnetoelectric composite material and preparation method thereof |
| CN104900799A (en) * | 2014-03-04 | 2015-09-09 | 中国科学院宁波材料技术与工程研究所 | Structural unit with adjustable and controllable exchange bias field, preparation method and adjusting and controlling method thereof |
| CN105098000A (en) * | 2014-05-16 | 2015-11-25 | 北京纳米能源与系统研究所 | Composite structure of regulating LED luminous intensity through magnetic field, and manufacturing method |
| CN106505147A (en) * | 2016-10-25 | 2017-03-15 | 中南大学 | A kind of miniature, flexible magnetic electric compound material and preparation method thereof |
| KR20170057806A (en) * | 2015-11-17 | 2017-05-25 | 삼성전자주식회사 | Magnetic junctions having a magnetoelastic free layer programmable using spin transfer torque |
| CN106868379A (en) * | 2017-03-13 | 2017-06-20 | 北京科技大学 | A kind of high-entropy alloy with big magnetostriction coefficient and preparation method thereof |
| EP2377126B1 (en) * | 2009-01-14 | 2017-09-27 | Headway Technologies, Inc. | A novel free lyer/capping layer for high performance mram mtj |
| CN107474618A (en) * | 2017-08-25 | 2017-12-15 | 中国科学院宁波材料技术与工程研究所 | A kind of high-temperature electromagnetic wave absorbent, microwave absorbing coating and preparation method thereof |
-
2018
- 2018-04-09 CN CN201810311956.1A patent/CN110358959B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994000695A1 (en) * | 1992-06-20 | 1994-01-06 | Robert Bosch Gmbh | Magnetostrictive transducer |
| CN1392194A (en) * | 2002-07-02 | 2003-01-22 | 武汉理工大学 | Poly meta-fluoroethylene/lead zirconate titanate/terbium dysprosium iron composite material sheet with magnetoelectric property and its preparation |
| US20050116831A1 (en) * | 2003-12-01 | 2005-06-02 | Anis Zribi | Contactless humidity/chemical vapor sensor device and associated method of fabrication |
| US7927439B1 (en) * | 2008-08-08 | 2011-04-19 | The United States Of America As Represented By The Secretary Of The Navy | Shock compression sensitivity change on command of explosives containing SMART materials |
| EP2377126B1 (en) * | 2009-01-14 | 2017-09-27 | Headway Technologies, Inc. | A novel free lyer/capping layer for high performance mram mtj |
| CN101599340A (en) * | 2009-04-08 | 2009-12-09 | 南京航空航天大学 | Direct magnetic coupling preparation method of magneto strictive multiplayer film |
| CN102044626A (en) * | 2009-10-20 | 2011-05-04 | 北京有色金属研究总院 | Film magnetoelectric composite material and preparation method thereof |
| CN101748407A (en) * | 2010-01-20 | 2010-06-23 | 中国船舶重工集团公司第七二五研究所 | Preparation method of surface composite coating of Tb-Dy-Fe magnetostrictive material |
| CN104900799A (en) * | 2014-03-04 | 2015-09-09 | 中国科学院宁波材料技术与工程研究所 | Structural unit with adjustable and controllable exchange bias field, preparation method and adjusting and controlling method thereof |
| CN105098000A (en) * | 2014-05-16 | 2015-11-25 | 北京纳米能源与系统研究所 | Composite structure of regulating LED luminous intensity through magnetic field, and manufacturing method |
| KR20170057806A (en) * | 2015-11-17 | 2017-05-25 | 삼성전자주식회사 | Magnetic junctions having a magnetoelastic free layer programmable using spin transfer torque |
| CN106505147A (en) * | 2016-10-25 | 2017-03-15 | 中南大学 | A kind of miniature, flexible magnetic electric compound material and preparation method thereof |
| CN106868379A (en) * | 2017-03-13 | 2017-06-20 | 北京科技大学 | A kind of high-entropy alloy with big magnetostriction coefficient and preparation method thereof |
| CN107474618A (en) * | 2017-08-25 | 2017-12-15 | 中国科学院宁波材料技术与工程研究所 | A kind of high-temperature electromagnetic wave absorbent, microwave absorbing coating and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110358959B (en) | 2021-03-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Johnson et al. | A wireless biosensor using microfabricated phage-interfaced magnetoelastic particles | |
| US20120098530A1 (en) | Piezoelectric/magnetostrictive composite magnetic sensor | |
| Park et al. | High magnetic field sensitivity in Pb (Zr, Ti) O3–Pb (Mg1/3Nb2/3) O3 single crystal/Terfenol-D/Metglas magnetoelectric laminate composites | |
| CN102867645B (en) | Method for improving thermostability of anisotropic magnetoresistance permalloy film | |
| CN102044626A (en) | Film magnetoelectric composite material and preparation method thereof | |
| Zhu et al. | Magnetostrictive properties and detection efficiency of TbDyFe/FeCo composite materials for nondestructive testing | |
| Qi et al. | Magnetostriction of Fe-Ga coatings and their application in ultrasonic guided wave sensing | |
| Shin et al. | Elastically coupled magneto-electric elements with highly magnetostrictive amorphous films and PZT substrates | |
| CN110358959A (en) | A kind of magnetostrictive thin film composite material and preparation method | |
| Bi et al. | Magnetoelectric Ni–Pb (Zr, Ti) O3–Ni trilayers prepared by electroless deposition | |
| Quandt et al. | Magnetic vector field sensor using magnetoelectric thin-film composites | |
| Savin et al. | Effect of phase separation in an Fe 20 Ni 80/Fe 50 Mn 50 structure with exchange coupling | |
| Pan et al. | Magnetoelectric coupling and the hydrogen effect on Ni–PZT–Ni trilayers made by electrodeposition | |
| Liu et al. | Effects of anisotropy and spin-asymmetry of ferromagnetic materials in ferromagnetic/Cr2O3/ferromagnetic trilayers | |
| Zou et al. | Observation of the transition state of domain wall displacement and GMI effect of FINEMET/graphene composite ribbons | |
| Mizuguchi | Control of anomalous Nernst effect in spintronic materials | |
| Choi et al. | Fabrication and simulation of a piezoelectric PIN-PMN-PT thin film for ultrahigh-frequency ultrasonic transducers | |
| Wang et al. | The effect of in situ magnetic field on magnetic properties and residual stress of fe-based amorphous film | |
| CN101359716B (en) | Co(x)C(1-x)/Co/Si multilayered structure granule film material having room temperature low field large magnetic resistance effect | |
| CN100470868C (en) | FexCl-x/Fe/Si multilayer coating material with low field room temperature huge magnetic resistance effect | |
| Huang et al. | Joule magnetostriction and volume magnetostriction of Iron Gallium thin films | |
| Egelhoff et al. | 400-fold reduction in saturation field by interlayering | |
| Rheem et al. | Depth profile of transverse permeability spectrum in an annealed Co-based amorphous ribbon | |
| CN102916127A (en) | High-performance magnetic impedance composite material | |
| Liu et al. | Influence of the thickness of BiFeO3 on the ferromagnet properties of layered multiferroic CoFe2O4–BiFeO3 films |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 100088, 2, Xinjie street, Xicheng District, Beijing Patentee after: GRIREM ADVANCED MATERIALS Co.,Ltd. Patentee after: Youyan rare earth high technology Co., Ltd Address before: 100088, 2, Xinjie street, Xicheng District, Beijing Patentee before: GRIREM ADVANCED MATERIALS Co.,Ltd. Patentee before: Guoke rare earth new material Co., Ltd |