CN104451543A - Vanadium ferrite-bismuth ferrite multiferroic composite film with exchange bias effect and preparation method of composite film - Google Patents
Vanadium ferrite-bismuth ferrite multiferroic composite film with exchange bias effect and preparation method of composite film Download PDFInfo
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Abstract
The invention relates to a vanadium ferrite-bismuth ferrite multiferroic composite film with an exchange bias effect and a preparation method of the composite film. The method comprises the following steps: carrying out epitaxial growth to form a BiFeO3 film on an SrTiO3 single crystal substrate by using a megnetron sputtering technology; preparing a vanadium ferrite Fe3-xVxO4 (x is smaller than or equal to 0.6 and greater than or equal to 0.1) film by using metal Fe target and V target co-sputtering; and achieving the epitaxial growth together with the BiFeO3 film. The multiferroic composite film is formed by vanadium ferrite and bismuth ferrite; and the condition that the BiFeO3-Fe3-xVxO4 composite film has the exchange bias effect is found out for the first time. Due to the BiFeO3-Fe3-xVxO4 epitaxial composite structure, the research range of the multiferroic composite structure is expanded; a simple and cheap preparation technology for an epitaxial heterostructure, which can be put into industrial popularization, is provided; the method disclosed by the invention has the advantages of simpleness in target selection and good application value in multiferroic storage devices and the like.
Description
Technical field
Patent of the present invention relates to a kind of preparation method of multiferroic laminated film, more specifically, is a kind of vanadium iron oxysome-bismuth ferrite many iron laminated film and preparation method with exchange bias effect.
Background technology
Multi-ferroic material is a kind of both magnetic and ferroelectric Multifunction material." multiferroic " refers to that (typical material is as BiMnO at single-phase compounds material
3, YMnO
3and BiFeO
3) in ferromagnetic order and ferroelectric sequence exist simultaneously, comprise ferromegnetism, antiferromagnetism, ferroelectricity and ferroelasticity etc.Because various physical influence is in same system, so will inevitably interact between each effect, thus make it not only possess single independently " iron " character, coupling also by various " multiferroic " realizes the mutual regulation and control between difference in functionality and produces some new physical influences, has therefore greatly widened the range of application of ferroic material.Based on ferroelectricity and ferromegnetism (antiferromagnetism) widespread use in modern science and technology, people easily expect the two to combine, namely said " magnetoelectricity " material afterwards.Utilize the compound of multi-ferroic material and spin polarization(SP) material, people can realize the regulation and control of electric field to material magnetotransport, can effectively reduce the power consumption of electron device, have obvious using value.As the representative of multi-ferroic material, bismuth ferrite (BiFeO
3) there are abundant magnetic, electrical property, there is higher ferroelectrie Curie temperature and antiferromagnetic Ne&1&el temperature.BiFeO
3the ferroelectricity had and weak magnetic, utilize magnetic oxide and BiFeO
3extension compound, will more abundant coupling effect be there is in interface.This type of composite structure can be widely used in the multiferroic storing device of electromagnetism cross complaint.
Based on above-mentioned purpose, select ferrospinel material and BiFeO
3extension compound, preparation multiferroic composite structure.Ferrospinel membrane structure is stablized, and has the advantages such as room-temperature ferromagnetic, becomes the ideal chose preparing multiferroic composite structure with ferroelectric material compound.As the main mechanism of magnetoelectric composite film magnetoelectric effect, exchange bias effect is understanding the interface coupling mechanism of many iron/ferromagnetic of antiferromagnetic/ferromagnetic system, and the character of particularly electroluminescent magnetoelectric effect has very important meaning.Exchange bias effect is by a large amount of in the manufacturing and designing of magnetic head, and the exchange bias effect in many iron composite structures, is more conducive to realize electroluminescent exchange biased, in the design of information recording device, has potential using value.
In previous research work, BiFeO
3many iron composite structures of base have metal simple-substance (as Fe, CO, Ni etc.) same to BiFeO
3compound.But this class formation Presence of an interface metal is easily oxidized etc., and reduce magneto-electric coupled, namely the exchange bias effect of composite structure is on the low side.In addition, investigator is had to utilize sol-gel method to prepare BiFeO
3with calcium titanium ore manganose oxide (La
1-xsr
xmnO
3) etc. the ceramic powder of compound.Consider from application point, pulverous material cannot be applied on a storage device, and therefore, experimenter utilizes the method for pulsed laser deposition to prepare BiFeO
3/ La
1-xsr
xmnO
3epitaxial structure, but, La
1-xsr
xmnO
3curie temperature lower, the interface coupling effect of bi-material is on the low side, reduces exchange bias effect.
How to prepare the emphasis that the multiferroic laminated film with strong interface magnetoelectric effect becomes Study and appliance.
Summary of the invention
Ferromagnetic substance spinel vanadium iron oxysome and ferroelectric material bismuth ferrite is utilized to form compound multi-iron material; Utilize simple magnetron sputtering method to prepare BiFeO
3-Fe
3-xv
xo
4(0.1≤x≤0.6) many iron extension heterofilm; This invention exploits a kind of new multiferroic composite structure, achieve a kind of preparation method with the multiferroic composite structure of large exchange bias effect.
We select ferrospinel material.First, ferrospinel material is with Sauerstoffatom close-packed, and lattice parameter is easy to realize with BiFeO
3extension is mated; Secondly, containing Fe element in ferrospinel, easily same BiFeO is gone out at interface
3in Fe occur exchange interaction, strengthen magnetoelectric effect.3rd, compare La
1-xsr
xmnO
3, ferrospinel, far above the Curie temperature of room temperature, more easily realizes room temperature exchange biased.Fe
3o
4be the Typical Representative of ferrospinel, there is the features such as high-curie temperature.But, Fe
3o
4film preparation condition is very harsh, and therefore we select preparation to be comparatively easy to binary spinel oxide-vanadium iron oxysome Fe
3-xv
xo
4(0.1≤x≤0.6).Spinel vanadium iron oxysome Fe
3-xv
xo
4have a cube inverse spinel structure, wherein, crystalline network makes close-packed with Sauerstoffatom, in the face-centered cubic lattice that 32 Sauerstoffatoms are formed, has 64 tetrahedral interstices (A position) and 32 octahedral interstices (B position).Wherein, 64 tetrahedron A positions are occupied by 8 Fe, and 32 octahedral B positions occupy 16 positions wherein altogether by Fe and V.In addition, utilize spinel vanadium iron oxysome can increase oxygen level in Sample Preparation Procedure, reduce the defects such as the Lacking oxygen at interface, improve interfacial coupling constant, be conducive to obtaining strong exchange bias effect.
How by the oxide material (BiFeO of two kinds of complex constructions
3and Fe
3-xv
xo
4) extension compound, realize the strong magneto-electric coupled difficult problem becoming research and produce, do not have the research of the extension Heteroepitaxy of bi-material at present.Realize the epitaxial heterostructures of this bi-material, need (1) first epitaxy BiFeO
3film, require to have high quality, surfaceness is low, is convenient to further epitaxy spinel ferrite body thin film; (2) at BiFeO
3further epitaxy ferrospinel Fe on epitaxial film
3-xv
xo
4film forms epitaxial heterostructures.Because two kinds of films are in interface epitaxy, the interface crystal lattice structure had, is easy to realize strong interface coupling.
1.BiFeO
3the epitaxy of film:
Experimentally, people prepare BiFeO
3the technology of film has magnetron sputtering, pulsed laser deposition or sol-gel etc.In existing report, utilize the BiFeO of magnetron sputtering or preparation of sol-gel
3film is non epitaxial growth; And the means that tradition prepares epitaxial film are pulse laser sink to the bottom or molecular beam epitaxy technique apparatus expensive, cost high, technical sophistication.By contrast, magnetically controlled sputter method is a kind of economical and practical and method for manufacturing thin film capable of being industrialized.We are by regulating BiFeO
3the growth conditions of film, the high-quality epitaxial film that utilized magnetron sputtering technique to prepare.
2. the epitaxy of spinel ferrite body thin film:
Experimentally, people utilize ceramic target to prepare spinel ferrite body thin film, and we achieve and utilize metal Fe target and V target at Ar and O
2atmosphere in reactive sputtering method prepare spinel vanadium iron ferrite thin film and realize it at BiFeO
3film Epitaxial growth.
Therefore, we utilize magnetron sputtering technique to prepare BiFeO
3epitaxial film and spinel vanadium iron oxysome (Fe
3-xv
xo
4) epitaxial film, realize the heteroepitaxial growth of bi-material first, by changing Fe
3-xv
xo
4oxygen proportion in membrane-film preparation process, finds the BiFeO prepared under high oxygen ratio
3-Fe
3-xv
xo
4extension composite structure has large exchange bias effect, realizes ferromagnetic/ferroelectric coupling of sull.This BiFeO
3-Fe
3-xv
xo
4extension composite structure, has expanded the research range of many iron composite structures; The preparation method of this composite structure, providing can be a kind of simple, cheap and can the technology of preparing of epitaxial heterostructures of industrialization promotion.
Technical scheme of the present invention is as follows:
Have vanadium iron oxysome-bismuth ferrite many iron laminated film of exchange bias effect, membrane structure formula is: BiFeO
3-Fe
3-xv
xo
4, wherein 0.1≤x≤0.6.
The preparation method with vanadium iron oxysome-bismuth ferrite many iron laminated film of exchange bias effect of the present invention, step is as follows:
(1) magnetron sputtering method prepares BiFeO
3epitaxial film;
(2) reactive sputtering growth Fe
3-xv
xo
4epitaxial film, 0.1≤x≤0.6;
(3) BiFeO is prepared
3-Fe
3-xv
xo
4laminated film, its structural representation is shown in Fig. 1.
Magnetron sputtering method prepares BiFeO
3epitaxial film condition is:
(1) target selecting 10%Bi excessive, base reservoir temperature 600 ~ 700 DEG C; Oxygen compares with argon gas: (4.0 ~ 10.0): 100; Sputtering pressure is 0.5 ~ 1.5Pa; Sputter rate: 1.8 nm/min;
(2) BiFeO
3epitaxial film thickness 10 ~ 30 nanometer, choice of the substrates SrTiO
3monocrystal chip.
Reactive sputtering growth Fe
3-xv
xo
4epitaxial film condition is:
(1) three target magnetic control sputtering devices are adopted, two d.c. sputtering target heads are installed respectively metal purity be 99.99% Fe target and purity be 99.99% V target, sputter equipment three target all upward RC sample position tilts, with the angle about 60 degree of horizontal plane;
(2) single crystal substrates is positioned over sample rack position, Heating temperature 450 DEG C; Pass into the scope of sputtering oxygen and argon gas: (1.6 ~ 4.0)/100, sputtering pressure 2.0Pa;
(3) open shielding power supply, Fe target applies the electric current of 0.2A and the volts DS of 360V, V target applies the volts DS of 0.04 ~ 0.16A and 360V; Film growth rate 8 nm/min;
(4) control Fe
3-xv
xo
4epitaxial film thickness 5 ~ 30 nanometer, closes shielding power supply.
Fig. 2 is extension Fe
3-xv
xo
4the x ray diffration pattern x (x is respectively 0.1 and 0.6) of (0.1≤x≤0.6) film, wherein (a) figure illustrates Fe
3-xv
xo
4along the growth of (00l) direction, (b) figure is Fe
3-xv
xo
4the diffraction peak in (111) direction, it is orderly that tetragyre symmetry describes lattice, and Fig. 2 (a) and (b) together illustrate Fe
3-xv
xo
4the epitaxial growth of (0.1≤x≤0.6) film.
Selection monocrystal chip is SrTiO
3substrate, then obtain BiFeO
3/ SrTiO
3; Study exchange bias effect for x=0.2, use BiFeO obtained above
3/ SrTiO
3for single crystal substrates, select the sputtering power 0.08A*360V (corresponding x=0.2) of V target, preparation Fe
2.8v
0.2o
4/ BiFeO
3/ SrTiO
3; As shown in Figure 3, high-resolution-ration transmission electric-lens photo display Fe
2.8v
0.2o
4/ BiFeO
3for epitaxial structure.
By Fe
2.8v
0.2o
4/ BiFeO
3/ SrTiO
3laminated film is cooled to low temperature 3K from room temperature under the externally-applied magnetic field of 1 tesla, measures the magnetzation curve of laminated film at 3K temperature;
BiFeO is read from magnetzation curve
3-Fe
2.8v
0.2o
4the exchange bias effect of laminated film, the BiFeO prepared under more different oxygen proportion
3-Fe
2.8v
0.2o
4the exchange bias effect of laminated film.In Fig. 4, open circles be oxygen/argon than the sample being 4.0/100, filled box be oxygen/argon than the sample being 2.0/100, can see, oxygen/argon shows large exchange bias effect than the sample being 4.0/100, has-400Oe during 3K.Large exchange bias effect illustrates that there is strong coupling effect ferromagnetic/ferroelectric interface.
Effect of the present invention is as follows:
1. utilize spinel vanadium iron oxysome and bismuth ferrite to form many iron epitaxial heterostructures, become a kind of new compound multi-iron material, expand the research range of many iron composite structures;
2. adopt reaction cosputtering method successfully to prepare spinel Fe first
3-xv
xo
4epitaxial film, physical properties is stablized;
3. adopt magnetically controlled sputter method to realize the epitaxy of two kinds of complex oxide vanadium iron oxysomes-bismuth ferrite multiferroic laminated film first, compare other film preparing technology, magnetron sputtering more easily realizes suitability for industrialized production;
4. finding the vanadium iron exchange bias effect that oxysome-bismuth ferrite multiferroic laminated film is large, is-400Oe under low temperature, is conducive to realizing multiferroic and stores.
Accompanying drawing explanation
Fig. 1 vanadium iron oxysome-bismuth ferrite complex thin film structure schematic diagram.
The Fe of Fig. 2 (a) MgO monocrystal chip Epitaxial growth
3-xv
xo
4the x ray diffration pattern x (x is respectively 0.1 and 0.6) of (0.1≤x≤0.6) film.
The Fe of (001) orientation of Fig. 2 (b) MgO monocrystal chip Epitaxial growth
3-xv
xo
4the X-ray of (x is respectively 0.1 and 0.6) film
scanning spectra.
Fig. 3 BiFeO
3-Fe
2.8v
0.2o
4the high resolution transmission electron microscopy image of laminated film, wherein (1) is BiFeO
3, (2) are Fe
2.8v
0.2o
4.
Fig. 4 BiFeO
3-Fe
2.8v
0.2o
4the magnetzation curve figure of laminated film, wherein, open circles be oxygen/argon than the sample being 4.0/100, filled box is that oxygen/argon is than the sample being 2.0/100.
Embodiment
According to our analysis to the exchange bias effect that sample prepared in the present invention carries out, below preferred forms is described in detail:
There is vanadium iron oxysome-bismuth ferrite many iron laminated film of exchange bias effect and the specific implementation step of preparation method:
1. magnetron sputtering method prepares BiFeO
3epitaxial film:
(1) target selecting 10%Bi excessive, regulates necessary processing parameter to realize film forming.Reaction parameter comprises: monocrystal chip base reservoir temperature, sputtering atmosphere, sputter rate, anneal environment etc.Condition is: base reservoir temperature 650 DEG C; Oxygen compares with argon gas: 7.0:100; Sputtering pressure: 1Pa; Sputter rate: 1.8 nm/min;
(2) BiFeO
3epitaxial film thickness 20 nanometer, choice of the substrates SrTiO
3monocrystal chip, as shown in Figure 3, high resolution transmission electron microscopy display BiFeO
3epitaxial structure.
2. reactive sputtering growth Fe
3-xv
xo
4epitaxial film:
(1) three target magnetic control sputtering devices are adopted, two d.c. sputtering target heads are installed respectively metal purity be 99.99% Fe target and purity be 99.99% V target, sputter equipment three target all upward RC sample position tilts, with the angle about 60 degree of horizontal plane;
(2) single crystal substrates is positioned over sample rack position, Heating temperature 450 DEG C; Pass into the scope of sputtering oxygen and argon gas: 4.0/100, sputtering pressure 2.0Pa; In this step, select different single crystal substrates, as MgO, SrTiO
3deng, the extension Fe that different base grows can be obtained
3-xv
xo
4(0.1≤x≤0.6) film;
(3) open shielding power supply, Fe target applies the electric current of 0.2A and the volts DS of 360V, V target applies the volts DS of 0.04A (x=0.1), 0.08A (x=0.2), 0.16A (x=0.16) and 360V; Film growth rate 8 nm/min;
(4) control Fe
3-xv
xo
4epitaxial film thickness 15 nanometer, closes shielding power supply.
Fe when Fig. 2 has reacted x=0.1 and 0.6
3-xv
xo
4the epitaxial structure of film, Fe when Fig. 3 gives x=0.2
3-xv
xo
4the epitaxial structure of film.
3. prepare BiFeO
3-Fe
3-xv
xo
4(x=0.2) laminated film measure its exchange bias effect (structural representation is shown in Fig. 1):
(1) monocrystal chip is selected to be SrTiO in step 1
3substrate, then obtain BiFeO
3/ SrTiO
3;
(2) study exchange bias effect for x=0.2, use BiFeO obtained above
3/ SrTiO
3for the single crystal substrates of step 2, select the sputtering power 0.08A*360V (corresponding x=0.2) of V target, preparation Fe
2.8v
0.2o
4/ BiFeO
3/ SrTiO
3; Its epitaxial structure is shown in Fig. 3.
(3) by Fe
2.8v
0.2o
4/ BiFeO
3/ SrTiO
3laminated film is cooled to low temperature 3K from room temperature under the externally-applied magnetic field of 1 tesla, measures the magnetzation curve of laminated film at 3K temperature; As Fig. 4.
(4) from magnetzation curve, BiFeO is read
3-Fe
2.8v
0.2o
4the exchange bias effect of laminated film, as can see from Figure 4, oxygen/argon is-400Oe when 3K than the exchange bias effect of the sample (open circle curve) being 4.0/100.
Involved in the present invention a kind of there is exchange bias effect vanadium iron oxysome-bismuth ferrite multiferroic laminated film and preparation method utilize BiFeO
3with Fe
3-xv
xo
4(0.1≤x≤0.6) forms multiferroic composite structure; Realize BiFeO
3-Fe
3-xv
xo
4prepared by (0.1≤x≤0.6) complex thin film structure extension; Late Cambrian BiFeO
3-Fe
3-xv
xo
4laminated film has large exchange bias effect and interface coupling.This inventive method has target and selects advantage simple, have good using value in multiferroic storing device etc.
Claims (4)
1. there is vanadium iron oxysome-bismuth ferrite many iron laminated film of exchange bias effect, it is characterized in that membrane structure formula is: BiFeO
3-Fe
3-xv
xo
4, wherein 0.1≤x≤0.6.
2. the preparation method of many iron laminated film described in claim 1, is characterized in that step is as follows:
(1) magnetron sputtering method prepares BiFeO
3epitaxial film;
(2) reactive sputtering growth Fe
3-xv
xo
4epitaxial film, 0.1≤x≤0.6;
(3) BiFeO is prepared
3-Fe
3-xv
xo
4laminated film.
3. the method for claim 1, is characterized in that magnetron sputtering method prepares BiFeO
3epitaxial film condition is:
(1) target selecting 10%Bi excessive, base reservoir temperature 600 ~ 700 DEG C; Oxygen compares with argon gas: (4.0 ~ 10.0): 100; Sputtering pressure is 0.5 ~ 1.5Pa; Sputter rate: 1.8 nm/min;
(2) BiFeO
3epitaxial film thickness 10 ~ 30 nanometer, choice of the substrates SrTiO
3monocrystal chip.
4. the method for claim 1, is characterized in that reactive sputtering growth Fe
3-xv
xo
4epitaxial film condition is:
(1) three target magnetic control sputtering devices are adopted, two d.c. sputtering target heads are installed respectively metal purity be 99.99% Fe target and purity be 99.99% V target, sputter equipment three target all upward RC sample position tilts, with the angle about 60 degree of horizontal plane;
(2) single crystal substrates is positioned over sample rack position, Heating temperature 450 DEG C; Pass into the scope of sputtering oxygen and argon gas: (1.6 ~ 4.0)/100, sputtering pressure 2.0Pa;
(3) open shielding power supply, Fe target applies the electric current of 0.2A and the volts DS of 360V, V target applies the volts DS of 0.04 ~ 0.16A and 360V; Film growth rate 8 nm/min;
(4) control Fe
3-xv
xo
4epitaxial film thickness 5 ~ 30 nanometer, closes shielding power supply.
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CN114551717A (en) * | 2022-02-10 | 2022-05-27 | 中国矿业大学 | Perovskite type alkaline earth vanadate film ferroelectric heterostructure and preparation method thereof |
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2014
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CN114551717A (en) * | 2022-02-10 | 2022-05-27 | 中国矿业大学 | Perovskite type alkaline earth vanadate film ferroelectric heterostructure and preparation method thereof |
CN114551717B (en) * | 2022-02-10 | 2023-12-05 | 中国矿业大学 | Perovskite alkaline earth vanadate thin film ferroelectric heterostructure and preparation method thereof |
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