CN114783768B - SrFeO for improving interface mismatch strain 2.0 Method for film magnetic performance and application - Google Patents
SrFeO for improving interface mismatch strain 2.0 Method for film magnetic performance and application Download PDFInfo
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- 230000005291 magnetic effect Effects 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000010408 film Substances 0.000 claims abstract description 150
- 239000000758 substrate Substances 0.000 claims abstract description 33
- 239000011241 protective layer Substances 0.000 claims abstract description 30
- 239000013078 crystal Substances 0.000 claims abstract description 29
- 229910002367 SrTiO Inorganic materials 0.000 claims abstract description 28
- 230000008021 deposition Effects 0.000 claims abstract description 28
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000010410 layer Substances 0.000 claims abstract description 8
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- 239000013077 target material Substances 0.000 claims abstract description 8
- 239000010409 thin film Substances 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 229910002294 SrAl0.5Ta0.5O3 Inorganic materials 0.000 claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 21
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- 239000001301 oxygen Substances 0.000 claims description 21
- 230000005415 magnetization Effects 0.000 claims description 11
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- 239000000463 material Substances 0.000 abstract description 6
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- 238000012360 testing method Methods 0.000 description 19
- 238000010438 heat treatment Methods 0.000 description 13
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
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- 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
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- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- 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
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
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- 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
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- 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
- C23C14/5846—Reactive treatment
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- 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
- H01F41/20—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 by evaporation
- H01F41/205—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 by evaporation by laser ablation, e.g. pulsed laser deposition [PLD]
Abstract
The invention discloses an interface mismatch strain lifting SrFeO 2.0 A method and application of film magnetic property relate to the application field of material technology. The method comprises the following steps: (1) Bombardment of SrFeO on single crystal substrates with pulsed laser 3 SrFeO preparation by target material 2.5 Thin film, single crystal substrate and SrFeO 2.5 Interface mismatch strain is generated between the films; the single crystal substrate comprises KTaO 3 、(LaAlO 3 ) 0.3 (SrAl 0.5 Ta 0.5 O 3 ) 0.7 、LaAlO 3 、YAlO 3 The interface mismatch strain ranges from-8.0% to 2.0%; the SrFeO 2.5 The thickness of the film is 10nm-50nm; (2) CaH is carried out 2 Powder and SrFeO 2.5 Sealing and sintering the film in a high vacuum state to obtain SrFeO 2.0 A film. The invention prepares the crystal with the pulse laser deposition and the soft chemical topological structure phase change on different monocrystal substrates<001>Oriented SrFeO 2.0 /SrTiO 3 Two-layer film system in which SrTiO is coated 3 The film is a structural protective layer. The interface mismatch strain effect between the substrate and the film can obviously improve SrFeO 2.0 The magnetic property of the film provides thought for the related basic and application research of the high Wen Tieci insulating oxide film.
Description
Technical Field
The invention relates to the field of material technology application, in particular to an interface mismatch strain lifting SrFeO 2.0 Method for film magnetic performance and application thereof.
Background
Current highly integrated information technology puts new demands on electronic materials/devices in terms of efficiency, power consumption, etc. The conventional electronic device performs information processing mainly with the charge of electrons as a degree of freedom. Recently, an electronic material having both ferromagnetic and insulating properties can be loaded with both the charge and spin of electronsThe information storage and processing work is beneficial to the further development of electronic information technology, and is also a necessary condition for developing the next generation of low-dissipation quantum spin electronic devices. However, such electronic materials having both ferromagnetic and electrical insulating properties have been recently reported. Existing SrFeO 2.5 The film is an antiferromagnetic material and has no macroscopic magnetization and hysteresis loop. At the same time, srFeO 2.0 The polycrystalline bulk material or thick film does not have obvious magnetization and other characteristics. The invention realizes SrFeO by interface mismatch strain effect 2.0 The magnetic regulation and control of the film provides material support for the development of high-temperature low-dissipation quantum ferromagnetic insulation spin electronic devices.
Disclosure of Invention
The invention aims to solve the technical problems that the prior art refers to a method for improving SrFeO by combining pulse laser deposition and topology structure regulation means to provide an interface mismatch strain 2.0 Method for film magnetic performance and application thereof.
In order to solve the problems, the invention provides the following technical scheme:
in a first aspect, the present invention provides an interface mismatch strain lifted SrFeO 2.0 A method of film magnetic properties comprising the steps of: (1) Bombardment of SrFeO on single crystal substrates with pulsed laser 3 SrFeO preparation by target material 2.5 Thin film, single crystal substrate and SrFeO 2.5 Interface mismatch strain is generated between the films; the single crystal substrate comprises KTaO 3 、 (LaAlO 3 ) 0.3 (SrAl 0.5 Ta 0.5 O 3 ) 0.7 、LaAlO 3 、YAlO 3 The interface mismatch strain ranges from-8.0% to 2.0%; the SrFeO 2.5 The thickness of the film is 10nm-50nm; (2) CaH is carried out 2 Powder and SrFeO 2.5 Sealing and sintering the film in a high vacuum state to obtain SrFeO 2.0 A film.
Further, the interface mismatch strain ranges from-7.12% to-0.02%.
Further, the SrFeO 2.0 The saturation magnetization of the film at 10K is 65emu/cc-165 emu/cc。
Further, the SrFeO 2.0 The saturation magnetization of the film at 300K is 23emu/cc to 130emu/cc.
Further, the step (1) and the step (2) also comprise the preparation of SrTiO 3 A step of protecting the layer; the preparation of SrTiO 3 The protective layer comprises the following steps: using pulsed laser light at SrFeO 2.5 Covering the surface of the film with a layer of SrTiO 3 A protective layer; the SrTiO 3 The thickness of the protective layer is less than or equal to 3nm.
Further, in the step (1), srFeO is prepared 2.5 When the film is prepared, the temperature is 600-680 ℃, and the deposition oxygen pressure is 0.01Pa-5.0Pa.
Further, the preparation of SrTiO 3 The protective layer is prepared at 550-650 deg.c and deposited oxygen pressure less than or equal to 0.01Pa.
Further, the laser source of the pulse laser is KrF excimer laser with the wavelength of 248nm, the laser pulse width of 10ns and the laser energy density of 1.0J/cm 2 -3.0J/cm 2 The laser frequency is 2Hz-5Hz.
Further, the vacuum degree in the step (2) is 1×10 or more -2 Pa, the temperature is 200-400 ℃, and the sintering time is more than 20 hours.
In a second aspect, the invention also provides the interface mismatch strain lifting SrFeO 2.0 The application of the method for the magnetic property of the film in the high Wen Tieci insulating oxide film.
The invention is to SrFeO 2.0 The structure and magnetism of the film are regulated and controlled, the magnetic performance of the film is effectively improved through interface mismatch strain, and SrFeO with high-quality epitaxy is obtained 2.0 A film. In the range of-7.12% to-0.02% of interface mismatch strain, srFeO 2.0 The magnetic properties of the film at 10K and 300K are enhanced with the increase of the interface mismatch strain value. The heterojunction system has ferromagnetic and insulating characteristics higher than room temperature, and provides material support for development of high-integration and low-power consumption electronic information devices.
The invention utilizes pulse laser deposition and soft chemical topological structure phase change method to prepare the material on different monocrystal substratesHas the following components<001>Oriented SrFeO 2.0 /SrTiO 3 Two-layer film system in which SrTiO is coated 3 The film is a structural protective layer. The interface mismatch strain effect between the substrate and the film can obviously improve SrFeO 2.0 The magnetic property of the film provides thought for the related basic and application research of the high Wen Tieci insulating oxide film.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows SrFeO obtained after pulse laser deposition according to examples 1-4 of the present invention 2.5 XRD pattern of the film;
FIG. 2 shows SrFeO obtained after topological phase transition in examples 1-4 of the present invention 2.0 XRD pattern of the film;
FIG. 3 shows SrFeO obtained after topological phase transition in examples 1-4 of the present invention 2.0 M-T curve of the film at 10K-300K;
FIG. 4 shows SrFeO obtained after topological phase transition in examples 1-4 of the present invention 2.0 M-H curve of film at 10K;
FIG. 5 shows SrFeO obtained after topological phase transition in examples 1-4 of the present invention 2.0 M-H curve of film at 300K;
FIG. 6 shows the SrFeO obtained after the topology phase transition of example 5 of the present invention 2.0 XRD pattern of the film after 60 days of storage;
FIG. 7 shows SrFeO obtained after topological phase transition in comparative example 1 of the present invention 2.0 XRD pattern of the film after 10 days of storage.
Detailed Description
The technical solutions in the embodiments will be clearly and completely described below with reference to the drawings in the embodiments of the present invention. It will be apparent that the embodiments described below are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to explore the high Wen Tieci insulating oxide film, the interface mismatch strain provided by the invention is applied to promote SrFeO 2.0 Method for preparing SrFeO by using film magnetic property 2.0 A film. SrFeO is prepared by utilizing pulse laser deposition technology 2.5 SrFeO obtained after film and topological phase transition 2.0 XRD testing (XRD: X-ray diffraction) of the film; srFeO obtained after topological phase transformation 2.0 The films were placed in an integrated property measurement system (Physical Property Measurement System) at 10K-300K for corresponding magnetic property testing.
SrFeO 2.0 The preparation method of the film comprises the following steps:
the laser pulse deposition technology is utilized, the laser source is KrF excimer laser with the wavelength of 248nm, the laser pulse width of 10ns and the laser energy density of 1.0J/cm 2 -3.0J/cm 2 The laser frequency is 2-5Hz.
Adjusting the vacuum degree of a vacuum cavity in a pulse laser deposition system, and when the vacuum degree in the vacuum cavity is equal to the vacuum degree<2×10 -5 Heating monocrystalline substrate to 600-680 deg.C under Pa, introducing oxygen into the chamber, and depositing SrFeO under oxygen pressure of 0.01-5Pa 3 Bombarding target material, and obtaining SrFeO after pulse laser deposition 2.5 A film. To fully utilize the interface strain effect, srFeO is controlled 2.5 The thickness of the film is 10-50nm. Pulse laser deposition is carried out again, and SrFeO is formed 2.5 SrTiO is covered on the surface of the film 3 Protective layer, srTiO 3 The growth temperature of the protective layer is 550-650 ℃, the deposition oxygen pressure is less than or equal to 0.01Pa, srTiO 3 The thickness of the protective layer is less than or equal to 3nm. Then the mixture was kept under a dynamic oxygen atmosphere for 10 minutes and then cooled to room temperature. And then SrFeO is added 2.5 Film and CaH 2 Mixing the powder, sealing at ultra-high vacuum degree of not less than 10 -2 Pa in a quartz tube. Sintering the quartz tube for more than 20 hours at the temperature of more than 200 ℃ to enable the quartz tube to generate topological phase change to obtain stable SrFeO 2.0 A film. In addition, oxygen in the air and SrFeO 2.0 SrFeO in film 2.0 Contact of the film system results in a film phase structure from SrFeO 2.0 Oxidation to SrFeO 2.5 ，SrTiO 3 The protective layer can avoid air and SrFeO 2.0 SrFeO in film 2.0 Contacting the film system to maintain SrFeO 2.0 Stability of the film.
Example 1: srFeO 2.0 /KTO
The crystal face orientation is selected as<001>KTaO of (a) 3 (KTO for short, hereinafter the same) single crystal substrate having a lattice constant ofSrFeO is directly prepared on the single crystal substrate by utilizing the pulse laser deposition technology 2.5 Film and SrTiO 3 And (3) a protective layer.
The laser source of the pulse laser deposition system is KrF excimer laser, the laser wavelength is 248nm, the laser pulse width is 10ns, and the laser frequency is 3Hz. Adjusting the vacuum degree of a cavity in a pulse laser deposition system to be 1 multiplied by 10 -5 Pa, heating the heating support to 660 ℃, then introducing oxygen to maintain 1Pa, and setting the laser energy density to 2.8J/cm 2 For SrFeO 3 Bombarding target material to obtain 20nm SrFeO by controlling the number of pulse laser 2.5 A film. XRD testing of the film was performed as shown in FIG. 1 to obtain SrFeO 2.5 Out-of-plane lattice constant c of film film Is that
Pulse laser deposition is carried out again, the temperature of the heating support is increased to 600 ℃, then oxygen is introduced to maintain 0.01Pa, and SrFeO is formed 2.5 SrTiO is covered on the surface of the film 3 And (3) a protective layer. By controlling the number of pulse laser, srTiO of 3nm is obtained 3 And (3) a protective layer. Then the mixture was kept under a dynamic oxygen atmosphere for 10 minutes and then cooled to room temperature.
To epitaxially grow SrFeO 2.5 Film and purity of 99% CaH 2 Powder at 1X 10 -2 Sealing in quartz tube under Pa vacuum condition, placing in a tube furnace at 250deg.C, and performing soft chemical reaction to obtain SrFeO 2.5 Phase transition of film into SrFeO 2.0 A film. XRD testing of the film was performed as shown in FIG. 2 to obtain SrFeO 2.0 Out-of-plane lattice constant c of film film Is thatKTO single crystal substrate and SrFeO 2.0 Is-0.02% (i.e., the interface mismatch strain is-0.02%).
The samples were then placed in an integrated property measurement system (Physical Property Measurement System) for corresponding magnetic property testing. As shown in FIGS. 3-5, the test results showed that SrFeO on KTO substrate 2.0 The film has poor magnetic properties and negligible saturation magnetization and hysteresis loop.
Example 2: srFeO 2.0 /LSAT
The crystal face orientation is selected as<001>Of (LaAlO) 3 ) 0.3 (SrAl 0.5 Ta 0.5 O 3 ) 0.7 (abbreviated as LSAT, hereinafter the same) single crystal substrate having a lattice constant ofSrFeO is directly prepared on the single crystal substrate by utilizing the pulse laser deposition technology 2.5 Film and SrTiO 3 And (3) a protective layer.
The laser source of the pulse laser deposition system is KrF excimer laser, the laser wavelength is 248nm, the laser pulse width is 10ns, and the laser frequency is 3Hz. Adjusting the vacuum degree of a cavity in a pulse laser deposition system to be 1 multiplied by 10 -5 Pa, heating the heating support to 660 ℃, then introducing oxygen to maintain 1Pa, and setting the laser energy density to 2.8J/cm 2 For SrFeO 3 Bombarding target material to obtain 20nm SrFeO by controlling the number of pulse laser 2.5 A film. XRD testing of the film was performed as shown in FIG. 1 to obtain SrFeO 2.5 Out-of-plane lattice constant c of film film Is that
Pulse laser deposition is carried out again, the temperature of the heating support is increased to 600 ℃, and then oxygen is introduced to maintain at 0.01Pa, at SrFeO 2.5 SrTiO is covered on the surface of the film 3 And (3) a protective layer. By controlling the number of pulse laser, srTiO of 3nm is obtained 3 And (3) a protective layer. Then the mixture was kept under a dynamic oxygen atmosphere for 10 minutes and then cooled to room temperature.
To epitaxially grow SrFeO 2.5 Film and purity of 99% CaH 2 Powder at 1X 10 -2 Sealing in quartz tube under Pa vacuum condition, placing in a tube furnace at 250deg.C for 40 hr, and performing softening chemical reaction to obtain SrFeO 2.5 Phase transition of thin film into SrFeO 2.0 A film. XRD testing of the film was performed as shown in FIG. 2 to obtain SrFeO 2.0 Out-of-plane lattice constant c of film film Is thatLSAT single crystal substrate and SrFeO 2.0 The degree of mismatch of the film was-3.08% (i.e., the interfacial mismatch strain was-3.08%).
The samples were then placed in an integrated property measurement system (Physical Property Measurement System) for corresponding magnetic property testing. Test of SrFeO at 10K and 300K 2.0 The hysteresis loop of the film, as shown in FIGS. 3-5, reached a saturation magnetization of 65emu/cc at 10K and 23emu/cc at 300K.
Example 3: srFeO 2.0 /LAO
The crystal face orientation is selected as<001>LaAlO of (F) 3 (abbreviated as LAO, hereinafter the same) single crystal substrate having a lattice constant ofSrFeO is directly prepared on the single crystal substrate by utilizing the pulse laser deposition technology 2.5 Film and SrTiO 3 And (3) a protective layer.
The laser source of the pulse laser deposition system is KrF excimer laser, the laser wavelength is 248nm, the laser pulse width is 10ns, and the laser frequency is 3Hz. Adjusting the vacuum degree of a cavity in a pulse laser deposition system to be 1 multiplied by 10 -5 Pa, heating the heating support to 660 ℃, then introducing oxygen to maintain 1Pa, and setting the laser energy density to 2.8J/cm 2 For SrFeO 3 Bombarding the target material, and obtaining 20n by controlling the number of pulse lasersm SrFeO 2.5 A film. XRD testing of the film was performed as shown in FIG. 1 to obtain SrFeO 2.5 Out-of-plane lattice constant c of film film Is that
Pulse laser deposition is carried out again, the temperature of the heating support is increased to 600 ℃, then oxygen is introduced to maintain 0.01Pa, and SrFeO is formed 2.5 SrTiO is covered on the surface of the film 3 And (3) a protective layer. By controlling the number of pulse laser, srTiO of 3nm is obtained 3 And (3) a protective layer. Then the mixture was kept under a dynamic oxygen atmosphere for 10 minutes and then cooled to room temperature.
To epitaxially grow SrFeO 2.5 Film and purity of 99% CaH 2 Powder at 1X 10 -2 Sealing in quartz tube under Pa vacuum condition, placing in a tube furnace at 250deg.C for 40 hr, and performing softening chemical reaction to obtain SrFeO 2.5 Phase transition of thin film into SrFeO 2.0 A film. XRD testing of the film was performed as shown in FIG. 2 to obtain SrFeO 2.0 Out-of-plane lattice constant c of film film Is thatLAO single crystal substrate and SrFeO 2.0 The degree of mismatch of the film was-4.99% (i.e., the interfacial mismatch strain was-4.99%).
The samples were then placed in an integrated property measurement system (Physical Property Measurement System) for corresponding magnetic property testing. SrFeO at 10K and 300K was tested on LAO substrates 2.0 The hysteresis loop of the film, as shown in FIGS. 3-5, has a saturation magnetization of 90emu/cc at 10K and 35emu/cc at 300K.
Example 4: srFeO 2.0 /YAO
The crystal face orientation is selected as<001>YAlO of (A) 3 (abbreviated as YAO, hereinafter the same) single crystal substrate having a lattice constant ofSrFeO is directly prepared on the single crystal substrate by utilizing the pulse laser deposition technology 2.5 Film and SrTiO 3 And (3) a protective layer.
The laser source of the pulse laser deposition system is KrF excimer laser, the laser wavelength is 248nm, the laser pulse width is 10ns, and the laser frequency is 3Hz. Adjusting the vacuum degree of a cavity in a pulse laser deposition system to be 1 multiplied by 10 -5 Pa, heating the heating support to 660 ℃, then introducing oxygen to maintain 1Pa, and setting the laser energy density to 2.8J/cm 2 For SrFeO 3 Bombarding target material to obtain 20nm SrFeO by controlling the number of pulse laser 2.5 A film. XRD testing of the film was performed as shown in FIG. 1 to obtain SrFeO 2.5 Out-of-plane lattice constant c of film film Is that
Pulse laser deposition is carried out again, the temperature of the heating support is increased to 600 ℃, then oxygen is introduced to maintain 0.01Pa, and SrFeO is formed 2.5 SrTiO is covered on the surface of the film 3 And (3) a protective layer. By controlling the number of pulse laser, srTiO of 3nm is obtained 3 And (3) a protective layer. Then the mixture was kept under a dynamic oxygen atmosphere for 10 minutes and then cooled to room temperature.
To epitaxially grow SrFeO 2.5 Film and purity of 99% CaH 2 Powder at 1X 10 -2 Sealing in quartz tube under Pa vacuum condition, placing in a tube furnace at 250deg.C for 40 hr, and performing softening chemical reaction to obtain SrFeO 2.5 Phase transition of thin film into SrFeO 2.0 A film. XRD testing of the film was performed as shown in FIG. 2 to obtain SrFeO 2.0 Out-of-plane lattice constant c of film film Is thatYAO single crystal substrate and SrFeO 2.0 The degree of mismatch of the film was-7.12% (i.e., the interfacial mismatch strain was-7.12%).
The samples were then placed in an integrated property measurement system (Physical Property Measurement System) for corresponding magnetic property testing. As shown in FIGS. 3-5, srFeO acts in contrast to the LAO substrate 2.0 The film has further enhanced magnetic properties when YAO substrates are used. At 10K, srFeO 2.0 The saturation magnetization of the YAO film is as high as 165emu/cc. At 300K, srFeO 2.0 YAO filmUp to 130emu/cc, good room temperature ferromagnetism can be achieved.
As can be found from the test results, KTaO is adopted 3 、(LaAlO 3 ) 0.3 (SrAl 0.5 Ta 0.5 O 3 ) 0.7 、LaAlO 3 、 YAlO 3 The interface mismatch strain range generated by the single crystal substrate and the film is-8.0% -2.0%, when the interface mismatch strain is increased from-0.02% to-7.12%, srFeO 2.0 The saturation magnetization of the film is obviously improved. At SrFeO 2.0 LAO, and SrFeO 2.0 Under the action of larger interface mismatch strain such as/YAO, the magnetism of the material is obviously enhanced.
SrFeO 2.0 Surface coating and structural stability of films
Example 5
Preparation of SrFeO on LAO single crystal substrate by pulse laser deposition technique 2.5 Film in SrFeO 2.5 Growing an ultrathin SrTiO layer on the film 3 A protective layer, by being combined with CaH 2 The powder is subjected to chemical reaction in quartz tube to make SrFeO 2.5 The film undergoes phase change to SrFeO 2.0 A film. For SrFeO obtained after topological phase transformation 2.0 XRD testing of the films and films after 60 days of storage was performed as shown in FIG. 6, STO/SrFeO 2.0 No significant structural changes were observed after 60 days of storage in the atmospheric environment for the LAO system.
Comparative example 1
Preparation of SrFeO on LAO single crystal substrate by pulse laser deposition technique 2.5 Film by combining with CaH 2 The powder is subjected to chemical reaction in quartz tube to make SrFeO 2.5 The film undergoes phase change to SrFeO 2.0 A film. Comparative example 1 compared to example 5 except that there is no SrTiO 3 The other conditions are the same outside the protective layer. For SrFeO obtained after topological phase transformation 2.0 XRD testing of the film and the film after 60 days of storage was performed, as shown in FIG. 7, and the XRD results showed SrFeO 2.0 Weakening of the phase, and appearance of the hetero-phase, indicates that the SrFeO 2.0 The film is obviously unstable in structure after being stored for 10 days in an atmospheric environment.
It can be seen that in SrFeO 2.5 Growing an ultrathin SrTiO layer on the film 3 The protective layer can effectively improve the structural stability.
In summary, the invention utilizes strain (-7.1% -0.02%) generated at the interface by different substrates to make SrFeO 2.0 The in-plane and out-of-plane lattices of the film deform. SrFeO when the in-plane lattice thereof is more compressed 2.0 The magnetic properties of the film are significantly and gradually increased. In addition, the invention utilizes SrTiO 3 The protective layer maintains SrFeO 2.0 Stability of the film (FIGS. 6-7).
In the foregoing embodiments, the descriptions of the embodiments are focused on, and for those portions of one embodiment that are not described in detail, reference may be made to the related descriptions of other embodiments.
While the invention has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes and substitutions of equivalents may be made and equivalents will be apparent to those skilled in the art without departing from the scope of the invention. Therefore, the protection scope of the invention is subject to the protection scope of the claims.
Claims (9)
1. SrFeO for improving interface mismatch strain 2.0 A method of film magnetic properties comprising the steps of: (1) Bombardment of SrFeO on single crystal substrates with pulsed laser 3 SrFeO preparation by target material 2.5 Thin film, single crystal substrate and SrFeO 2.5 Interface mismatch strain is generated between the films; the single crystal substrate comprises KTaO 3 、(LaAlO 3 ) 0.3 (SrAl 0.5 Ta 0.5 O 3 ) 0.7 、LaAlO 3 、YAlO 3 The interface mismatch strain ranges from-8.0% to 2.0%; the SrFeO 2.5 The thickness of the film is 10nm-50nm; (2) CaH is carried out 2 Powder and SrFeO 2.5 Sealing and sintering the film in a high vacuum state to obtain SrFeO 2.0 A film;
the step (1) and the step (2) also comprise the preparation of SrTiO 3 A step of protecting the layer; the preparation of SrTiO 3 The protective layer comprises the following steps: using pulsed laser light at SrFeO 2.5 Covering the surface of the film with a layer of SrTiO 3 A protective layer; the SrTiO 3 The thickness of the protective layer is less than or equal to 3nm.
2. The interface mismatched strain lifted SrFeO of claim 1 2.0 A method of film magnetic properties, characterized in that the interface mismatch strain ranges from-7.12% to-0.02%.
3. The interface mismatched strain lifted SrFeO of claim 2 2.0 A method for film magnetic properties, characterized in that the SrFeO 2.0 The saturation magnetization of the film at 10K is 65emu/cc-165emu/cc.
4. An interface mismatched strain lifted SrFeO according to claim 3 2.0 A method for film magnetic properties, characterized in that the SrFeO 2.0 The saturation magnetization of the film at 300K is 23emu/cc to 130emu/cc.
5. The interface mismatched strain lifted SrFeO of claim 1 2.0 A method for film magnetic properties, characterized in that in step (1), srFeO is prepared 2.5 When the film is prepared, the temperature is 600-680 ℃, and the deposition oxygen pressure is 0.01Pa-5.0Pa.
6. The interface mismatched strain lifted SrFeO according to claim 5 2.0 A method for preparing SrTiO film magnetic properties is characterized in that 3 The protective layer is prepared at 550-650 deg.c and deposited oxygen pressure less than or equal to 0.01Pa.
7. The interface mismatched strain lifted SrFeO according to claim 6 2.0 The method for the magnetic performance of the film is characterized in that the laser source of the pulse laser is KrF excimer laser with the wavelength of 248nm, the laser pulse width of 10ns and the laser energy density of 1.0J/cm 2 -3.0J/cm 2 The laser frequency is 2Hz-5Hz.
8. The interface mismatched strain lifted SrFeO of claim 7 2.0 A method for magnetic properties of a thin film, characterized in that the vacuum degree in the step (2) is 1X 10 or more -2 Pa, the temperature is 200-400 ℃, and the sintering time is more than 20 hours.
9. The interface mismatch strain lifted SrFeO of any of claims 1-8 2.0 The application of the method for the magnetic property of the film in the high Wen Tieci insulating oxide film.
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| CA2212827A1 (en) * | 1996-08-13 | 1998-02-13 | Sumitomo Electric Industries, Ltd. | Superconducting film structure comprising oxide superconductor layer and protective layer and method for preparing the same |
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| US6803071B1 (en) * | 2003-01-10 | 2004-10-12 | The United States Of America As Represented By The Secretary Of The Army | Paraelectric thin film semiconductor material and method for producing the same |
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| CA2212827A1 (en) * | 1996-08-13 | 1998-02-13 | Sumitomo Electric Industries, Ltd. | Superconducting film structure comprising oxide superconductor layer and protective layer and method for preparing the same |
| US6803071B1 (en) * | 2003-01-10 | 2004-10-12 | The United States Of America As Represented By The Secretary Of The Army | Paraelectric thin film semiconductor material and method for producing the same |
| WO2004086422A1 (en) * | 2003-03-25 | 2004-10-07 | Minebea Co., Ltd. | Ferrite magnet and method for production thereof |
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