CN112410880B - Flexible self-supporting single crystal Fe with self-regulating growth orientation3O4Preparation of thin film material, thin film material and single crystal structure - Google Patents

Flexible self-supporting single crystal Fe with self-regulating growth orientation3O4Preparation of thin film material, thin film material and single crystal structure Download PDF

Info

Publication number
CN112410880B
CN112410880B CN202011301146.1A CN202011301146A CN112410880B CN 112410880 B CN112410880 B CN 112410880B CN 202011301146 A CN202011301146 A CN 202011301146A CN 112410880 B CN112410880 B CN 112410880B
Authority
CN
China
Prior art keywords
sto
single crystal
sao
substrate
layer
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.)
Active
Application number
CN202011301146.1A
Other languages
Chinese (zh)
Other versions
CN112410880A (en
Inventor
李江宇
钟高阔
安峰
欧云
訾孟飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenzhen Institute of Advanced Technology of CAS
Original Assignee
Shenzhen Institute of Advanced Technology of CAS
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shenzhen Institute of Advanced Technology of CAS filed Critical Shenzhen Institute of Advanced Technology of CAS
Priority to CN202011301146.1A priority Critical patent/CN112410880B/en
Publication of CN112410880A publication Critical patent/CN112410880A/en
Application granted granted Critical
Publication of CN112410880B publication Critical patent/CN112410880B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • 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
    • 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
    • C23C14/085—Oxides of iron group metals
    • 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
    • C23C14/088—Oxides of the type ABO3 with A representing alkali, alkaline earth metal or Pb and B representing a refractory or rare earth metal
    • 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
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • C30B23/025—Epitaxial-layer growth characterised by the substrate
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C30B29/32—Titanates; Germanates; Molybdates; Tungstates
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape

Abstract

The application discloses a flexible self-supporting single crystal Fe with self-regulating growth orientation3O4Preparation of thin film materials, thin film materials and single crystal structures. The preparation method comprises the following steps: selecting a substrate with a specific crystal plane orientation; preparing a pre-dissolving layer on a selected substrate with a specific crystal face orientation; preparing single crystal Fe after preparing orientation control layer on pre-dissolving layer3O4Film, substrate/pre-dissolved layer/orientation control layer/Fe3O4A multilayer epitaxial structure; soaking the obtained multilayer epitaxial structure in solvent to dissolve the pre-dissolved layer, the substrate and the orientation control layer/Fe3O4Separating epitaxial structure to obtain flexible self-supporting monocrystal Fe with specific crystal face orientation3O4A film. The method obtains the flexible self-supporting single crystal Fe with different growth orientations through self-regulation and control according to requirements3O4The film material is favorable for growing epitaxial heterojunction with different lattice parameters on the film material, and greatly expands the single crystal Fe3O4The thin film material is applied to the field of wearable electronic products.

Description

Flexible self-supporting single crystal Fe with self-regulating growth orientation3O4Preparation of thin film material, thin film material and single crystal structure
Technical Field
The present application relates to the field of flexible self-supporting crystal structure growth orientation, more specifically it relates to a flexible self-supporting single crystal Fe with self-controlled growth orientation3O4Preparation of thin film materials, thin film materials and single crystal structures.
Background
In recent years, with the development of science and technology, flexible wearable electronic devices such as electronic skins, smart fabrics, implantable medical devices and the like are receiving increasingly wide attention, and the demand for wearable flexible information storage devices is also increasing. Most of the conventional flexible information storage materials are based on organic polymer materials, but the materials have the problems of narrow service temperature range, large volume, slow response speed, high energy consumption and the like all the time when being applied, and the problems are not solved properly all the time.
Based on the above situation, many researchers in the industry have moved the focus of flexible intelligent materials to inorganic materials, and magnetic oxides, as one of the richest resources on the earth, can be widely applied to the fields of information storage, signal detection, biomedicine and the like, especially ferroferric oxide (Fe)3O4) The magnetic material has the advantages of simple preparation, wide iron element source, high saturation magnetization at room temperature, stable chemical property, no toxicity, no harm, biocompatibility and the like, and is one of the most widely applied magnetic materials.
Amorphous inorganic oxide films have been obtained by various methods in research and, in order to meet the requirements of flexible wearable electronics, flexible inorganic single crystal smart materials have also been developed, such as flexible self-supporting single crystal Fe based on inorganic single crystal materials prepared from mica flakes3O4Thin films, but flexible materials based on mica sheets can only be bent and cannot be stretched, and have the limitation of fixed orientation; flexible self-supporting single crystal Fe3O4The film can only achieve a single orientation due to lattice adaptation and energy problems and the epitaxial relationship is STO [001 ]]//SAO[001]//Fe3O4[111]Wherein STO is SrTiO3SAO is Sr3Al2O6The film with the epitaxial structure cannot meet the requirements of various flexible wearable electronic devices at present.
Disclosure of Invention
Flexible self-supporting single crystal Fe for improving single orientation3O4The application provides a flexible self-supporting sheet with self-regulating growth orientationCrystalline Fe3O4Preparation of thin film materials, thin film materials and single crystal structures.
In a first aspect, the present application provides a flexible self-supporting single crystal of Fe with self-controlled growth orientation3O4The preparation method of the film material adopts the following technical scheme:
flexible self-supporting single crystal Fe capable of self-regulating growth orientation3O4The preparation method of the film material comprises the following steps: (1) selecting a substrate with a specific crystal face orientation; (2) preparing a pre-dissolving layer on a selected substrate with a specific crystal face orientation; (3) preparing a layer of orientation control layer on the pre-dissolving layer and then preparing single crystal Fe3O4Film, substrate/pre-dissolved layer/orientation control layer/Fe3O4The multilayer epitaxial structure of (1); (4) soaking the obtained multilayer epitaxial structure in solvent to dissolve the pre-dissolved layer, the substrate and the orientation control layer/Fe3O4Separating epitaxial structure to obtain flexible self-supporting monocrystal Fe with specific crystal face orientation3O4A film.
By adopting the preparation method, the application can obtain the flexible self-supporting single crystal Fe with various specific growth orientations in a self-regulating and stable manner according to the requirements3O4Thin film material, single crystal Fe3O4The film material has different growth orientations, which is beneficial to growing epitaxial heterojunctions with different lattice parameters on the film material to construct a novel multiferroic heterostructure, and simultaneously, because different growth orientations can lead the sample to have the difference of anisotropy and magnetic property, the development of spinning electronic devices with different requirements is facilitated, and the single crystal Fe is greatly expanded3O4The application of the film material in the field of wearable electronic products; and single crystal Fe with various specific growth orientations prepared by the method3O4The film has excellent flexibility and self-supporting characteristics, can be stretched in multiple directions, is beneficial to promoting the development of a flexible spinning electronic device without substrate constraint, and better meets the requirements of a flexible wearable electronic device; the whole preparation method is simple, easy to produce, stable in product quality, more environment-friendly, and greatly reduces the production cost and the post production costThe treatment cost is low, and the popularization and the production are more facilitated.
Preferably, the thickness of the pre-dissolving layer is 20-100nm, and the thickness of the orientation regulating layer is 10-50 nm.
The thickness of the pre-dissolving layer is controlled to be 20-100nm, so that the rapid dissolving of the pre-dissolving layer and the surface flatness of the pre-dissolving layer can be guaranteed, the subsequent process is not obviously influenced, the orientation can be regulated and controlled by controlling the thickness of the orientation regulating and controlling layer to be 10-50 nm, and the performance of the film is not obviously influenced.
Preferably, the method comprises the following steps: (1) selecting an STO substrate with a specific crystal face orientation; (2) preparing an SAO layer on the STO substrate with the selected specific crystal face orientation; (3) preparing a STO layer on the SAO layer and then preparing single crystal Fe3O4Film formation of STO/SAO/STO/Fe3O4An epitaxial structure; (4) the obtained STO/SAO/STO/Fe3O4Soaking the epitaxial structure in solvent to dissolve the SAO layer, STO substrate and STO/Fe3O4Separating epitaxial structure to obtain flexible self-supporting monocrystal Fe with specific crystal face orientation3O4A film.
Preferably, a single crystal SAO layer is prepared in the step (2), an STO layer is prepared in the step (3), and a single crystal Fe3O4The film is prepared by pulse laser deposition, the thickness of the SAO layer is 20-100nm, the thickness of the STO layer is 10-50 nm, and the single crystal Fe3O4The thickness of the film is 50 to 200 nm.
As the pulse laser deposition method for preparing the epitaxial heterostructure requires a material with a relatively good lattice matching degree, tests show that the lattice matching degree of the STO substrate with the crystal plane orientation of (001) and the SAO is only 1.4%, a better SAO epitaxial heterostructure can be obtained, a single crystal SAO layer can be dissolved in water, other substrates often have a relatively large lattice matching degree, and the epitaxial heterostructure is difficult to obtain if the STO substrate with the crystal plane orientation of (011), so that the material selection of the substrate plays a crucial role in preparing the epitaxial heterostructure.
The SAO target material used in the application has the characteristic of water solubility, and high-quality single crystal can be prepared on an STO substrate by a pulse laser deposition methodEpitaxial SAO layer, STO layer and single crystal magnetic Fe3O4Thin film material, and the thickness of STO layer can be controlled to be 10-50 nm, for single crystal Fe3O4The properties of the film are substantially unaffected.
The single crystal SAO layer can be fully dissolved in water and can not be dissolved in the single crystal Fe3O4The surface of the film is remained, and single crystal Fe with better quality can be obtained3O4A film; and single crystal Fe grown after STO layer is grown on SAO3O4The film can be completely separated from the STO substrate after being soaked in water; in addition, through experimental tests, the surface flatness is more difficult to control when the single crystal SAO layer is too thick, so that the thickness of the single crystal SAO layer is preferably 20-100nm, the thickness of the STO layer is preferably 10-50 nm, and the thickness of the single crystal Fe is preferably selected3O4The thickness of the film is 50-200 nm, so that the requirements of the flexible wearable electronic device can be better met.
Preferably, the deposition temperature is 650-750 ℃ when the single crystal SAO layer is prepared in the step (2), 650-750 ℃ when the STO layer is prepared in the step (3), and the single crystal magnetic Fe is prepared in the step (4)3O4The deposition temperature of the film is 350-450 ℃, the laser energy is 250-350 mJ, and the frequency is 5-15 Hz.
Preferably, in the step (2), before the pulsed laser deposition, the background vacuum in the growth cavity is pumped to 5 × 10-7Below Torr, and maintaining the partial pressure of oxygen flowing during deposition at 1X 10-6~5×10-6Torr。
By adopting the preparation method, the laser energy is controlled to be 250-350 mJ, so that the rapid deposition rate can be ensured, the phenomenon that large particles are generated on a deposition layer due to overlarge energy can be avoided, and the improvement of Fe is facilitated3O4Flatness and smoothness of the film surface; the frequency is controlled to be between 5Hz and 15Hz, so that the rapid deposition rate is kept, and the Fe content is increased3O4The purity and quality of the film, when the frequency is higher, the particles deposited on the film have not moved, the next batch of sputtered particles have fallen, thus will cause and pile up and form the inhomogeneous film, when the frequency is too low, the interval time is too long, the impurity will enter the film, reduce the quality of the film; will be provided withOxygen partial pressure is controlled at 1X 10-6~5×10-6The Torr is beneficial to the formation of preferred orientation of the film, the balance of chemical ratio is also beneficial to be ensured, and the defects of the internal structure of the film are reduced, thereby improving the quality of the film.
Preferably, the step (2) comprises the steps of: (a) adhering the STO substrate in the step (1) to the SiC heat conducting strip by using silver paste, and then placing the SiC heat conducting strip on a drying table to heat and dry the silver paste; (b) then, the SiC heat conducting strip adhered with the STO substrate is placed on a laser heating table in a growth cavity of a pulse laser deposition system, and the background in the growth cavity is vacuumized to 5 multiplied by 10-7The STO substrate is heated to the deposition temperature of SAO below Torr, and flowing oxygen is filled into the growth cavity to reach the target oxygen partial pressure in the heating process; (c) then starting a laser to bombard the SAO target material to deposit the SAO on the STO substrate for 5-25 min; the step (3) comprises the following steps: keeping the temperature at 650-750 ℃, keeping the oxygen partial pressure constant, bombarding the STO target material by laser to deposit an STO layer on the STO/SAO surface for 5-10 min, and then reducing the temperature to Fe3O4The deposition temperature is 350-450 ℃, the oxygen partial pressure is kept unchanged, and laser is used for bombarding Fe3O4Target material of Fe3O4Depositing on the surface of STO/SAO/STO for 20-80 min to obtain STO/SAO/STO/Fe3O4And (3) epitaxial heterostructure.
The application relates to a pulse laser method for preparing a single crystal SAO layer, an STO layer and a single crystal Fe3O4The deposition temperature, dynamic oxygen partial pressure, laser energy, deposition time and the like in the film process are optimized, and the single crystal SAO layer with preferred orientation growth, smooth surface and excellent water solubility, the STO layer and the Fe layer with high quality are prepared3O4A film.
Preferably, the substrate having a specific crystal plane orientation in step (1) is subjected to a cleaning process, the cleaning process comprising the steps of: a. Soaking a substrate with a specific crystal face orientation in acetone, and ultrasonically cleaning for 3-20 min at 40-70 ℃; b. Soaking the substrate with the specific crystal face orientation in absolute ethyl alcohol, and ultrasonically cleaning for 1-6 min; c. Then soaking the substrate with the specific crystal face orientation in deionized water, and ultrasonically cleaning for 1-6 min; d. And finally, drying the substrate with the specific crystal face orientation by using nitrogen.
The method can ensure that the surface of the substrate is smooth and clean through the pretreatment step, thereby being beneficial to preparing and obtaining a high-quality single crystal SAO layer and also being a follow-up high-quality STO layer and Fe3O4The preparation of the film provides a good basis.
Preferably, the step (4) specifically comprises the following steps: (A) using organic polymer as support plate and substrate/pre-dissolved layer/orientation control layer/Fe3O4Epitaxial structure of Fe3O4Tightly attaching the film; (B) heating the treated sample at the softening point of the organic polymer support plate; (C) then soaking the sample in deionized water for 30-60 min to completely dissolve the pre-dissolved layer; (D) finally, Fe will be adhered to3O4Taking out the organic polymer support plate of the film to prepare the flexible self-supporting single crystal Fe with different growth orientations3O4A material.
Preferably, the heating temperature in the step (B) is 80-100 ℃, the heating time is 10-20 min, and the organic polymer support plate is attached to the heating table heated in the step (B).
Preferably, the organic polymer support plate is one of PDMS, PEN or PET, and has a thickness of 50-500 μm.
The application is realized by supporting an organic polymer plate with Fe3O4The close adhesion of the film and the heating on the heating stage are both to make the organic polymer support plate and Fe after the single crystal SAO layer is dissolved in water3O4The film is more closely attached to prevent Fe3O4The film falls off the organic polymer support plate; the surface of the organic polymer support plate becomes softer when the organic polymer support plate is heated, which is beneficial to the organic polymer support plate and Fe3O4The film is better combined; the use of water as a solvent for dissolving the pre-dissolved layer can dissolve the single crystal SAO layer without affecting Fe3O4The structure and the property of the film are favorable for ensuring Fe3O4The quality of the film.
In a second aspect, the present application provides a flexible self-supporting single crystal of Fe3O4The film material adopts the following technical scheme:
flexible self-supporting single crystal Fe3O4A film material of the self-regulating flexible self-supporting single crystal Fe3O4The film material is prepared by a method for preparing growth orientation, namely single crystal Fe3O4The thickness of the film is 50-200 nm, and the film is monocrystalline Fe3O4Is a cubic crystal system, and the unit cell parameters are as follows: a = 8.394A.
Flexible self-supporting single crystal Fe with different growth orientations produced by the present application3O4The thin film material has different growth orientations, which is beneficial to growing epitaxial heterojunctions with different lattice parameters on the thin film material, and meanwhile, the difference of magnetic properties caused by the different growth orientations is also beneficial to developing spintronic devices with different requirements.
In a third aspect, the present application provides a single crystal structure, which adopts the following technical solution:
a single crystal structure which is sequentially STO/SAO/STO/Fe3O4Wherein STO is STO substrate with crystal orientation of (001), SAO is single crystal SAO layer epitaxially grown on STO substrate with crystal phase in epitaxial relationship of STO [001 ]]//SAO[001]Fe grown on STO/SAO/STO layer3O4Being single crystal Fe3O4Film with an epitaxial growth relationship of STO [001 ]]//SAO[001]//STO[001]//Fe3O4[001]。
In summary, the present application has at least one of the following advantages:
1. the present application creatively proposes single crystal Fe3O4The method for self-regulating growth orientation of the film material can obtain flexible self-supporting single crystal Fe with various specific growth orientations in a self-regulating and stable manner3O4Thin film material, facilitating the growth of single crystal Fe in different orientations3O4Epitaxial heterojunctions with different lattice parameters are grown on the thin film material to construct a novel multiferroic heterostructure, and the different growth orientations can cause the sample to have anisotropyThe difference of magnetic properties is beneficial to developing the spintronic devices with different requirements, and the single crystal Fe is greatly expanded3O4Application of thin film material in field of wearable electronic products, and single crystal Fe with various specific growth orientations prepared by using method3O4The film has excellent flexibility and self-supporting characteristics, can be stretched in multiple directions, is beneficial to promoting the development of a flexible spinning electronic device without substrate constraint, and better meets the requirements of a flexible wearable electronic device; the whole preparation method is simple and environment-friendly, the product quality is stable, and the production cost and the post-treatment cost are greatly reduced.
2. The application relates to a pulse laser method for preparing a single crystal SAO layer, an STO layer and a single crystal Fe3O4The deposition temperature, dynamic oxygen partial pressure, laser energy, deposition time and the like in the film process are optimized, and the single crystal SAO layer with preferred orientation growth, smooth surface and excellent water solubility, the STO layer and the Fe layer with high quality are prepared3O4A film.
3. The preparation process of the etching method in the application is very simple, the single crystal SAO layer can be dissolved only by using water, and simultaneously Fe is not influenced3O4The structure and the property of the film are energy-saving and environment-friendly.
4. The organic polymer support plate is contacted with Fe3O4The close adhesion of the film and the heating on the heating stage are both to make the organic polymer support plate and Fe after the single crystal SAO layer is dissolved in water3O4The film is more closely attached to prevent Fe3O4The film falls off from the organic polymer support plate; the surface of the organic polymer supporting plate can be softer when the organic polymer supporting plate is heated, and the organic polymer supporting plate and the Fe are favorably used3O4The film bonds better.
5. Flexible self-supporting single crystal Fe with different growth orientations prepared by the method3O4The film material has different growth orientations, which is beneficial to growing epitaxial heterojunctions with different lattice parameters on the film material, and the prepared single crystal Fe with different growth orientations3O4The film has excellent flexibility and can be stretched, folded orThe operation of twisting, the self-supporting characteristic is excellent, do not receive the substrate constraint.
Drawings
FIG. 1 shows STO/SAO/Fe prepared in comparative example 13O4And XRD pattern after water dissolution;
FIG. 2 shows STO/SAO/Fe prepared in comparative example 13O4Schematic orientation diagram of (a);
FIG. 3 shows STO/SAO/STO/Fe prepared in example 13O4And XRD pattern after water dissolution;
FIG. 4 shows STO/SAO/STO/Fe prepared in example 13O4Schematic orientation diagram of (a);
FIG. 5 shows STO/SAO/Fe obtained in comparative example 13O4EDS spectra of (a);
FIG. 6 shows STO/SAO/STO/Fe prepared in example 13O4EDS spectra of (a);
FIG. 7 shows STO/SAO/Fe obtained in comparative example 13O4And an M-H hysteresis loop in a bent state after water dissolution;
FIG. 8 shows STO/SAO/STO/Fe prepared in example 13O4And an M-H hysteresis loop in a bent state after water dissolution;
FIG. 9 shows STO/SAO/STO/Fe prepared in example 13O4The MFM test domain structure of (1).
Detailed Description
For better understanding of the present invention, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings of the embodiments of the present application. It is to be understood that the described embodiments are merely a few embodiments of the present application and not all embodiments. Based on the embodiments in the present application, other embodiments obtained by persons of ordinary skill in the art with the understanding of the inventive concepts in the present application are within the scope of the present application.
Flexible inorganic single crystal intelligent material is an important material indispensable in flexible wearable electronic devices, but flexible self-supporting single crystal Fe prepared based on mica sheets3O4The film can be bent only and can not be stretched, and can be storedLimitations in fixed orientation; flexible self-supporting single crystal Fe of another related technology3O4The film has the limitation of single growth orientation due to the problems of lattice adaptation and energy, and only the single orientation is obtained and the epitaxial relationship is STO [001 ]]//SAO[001]//Fe3O4[111]The film of (2) can not meet the requirements of various flexible wearable electronic devices at present.
The self-regulation flexible self-supporting single crystal Fe is realized by introducing the orientation regulation layer3O4The growth orientation of the film material produces single crystal Fe with various specific growth orientations3O4Film, to obtain in single crystal Fe3O4The purpose of growing epitaxial heterojunction with different lattice parameters in different growth orientations of the film material is greatly expanded, and the single crystal Fe is greatly expanded3O4The thin film material is applied to the field of wearable electronic products.
For the purpose of facilitating understanding of the technical solutions of the present application, the following detailed description of the present application is made with reference to the accompanying drawings 1 to 9 and the embodiments, but the present application is not limited to the scope of protection.
Example 1
Flexible self-supporting single crystal Fe capable of self-regulating growth orientation3O4The preparation method of the film material comprises the following steps:
(1) selecting an STO (001) substrate and pretreating the substrate, wherein the method specifically comprises the following steps:
a. soaking STO (001) substrate in acetone, and ultrasonically cleaning at 60 deg.C for 10 min;
b. then soaking the STO (001) substrate in absolute ethyl alcohol, and ultrasonically cleaning for 5 min;
c. then soaking the STO (001) substrate in deionized water, and ultrasonically cleaning for 5 min;
d. the STO (001) substrate was finally dried with nitrogen.
(2) Preparing a single crystal SAO layer, an STO layer and Fe on a pretreated STO (001) substrate in sequence by adopting a pulse laser deposition method3O4The film material specifically comprises the following steps:
(a) adhering the STO (001) substrate pretreated in the step (1) on a SiC heat conducting sheet by using silver paste, and heating and drying;
(b) then placing the SiC heat-conducting strip adhered with the STO (001) substrate on a laser heating table in a growth cavity of a pulse laser deposition system, and vacuumizing the background in the growth cavity to 5 multiplied by 10-7Torr below, the STO (001) substrate is heated to 700 deg.C, and oxygen gas is introduced into the growth chamber to reach 3 × 10-6Torr oxygen partial pressure, setting the laser energy of a laser to be 300mJ and the frequency to be 10 Hz;
(c) then starting a laser to bombard the SAO target material to deposit the SAO on the STO (001) substrate for 20 min;
(d) keeping the temperature of the STO (001) substrate and the oxygen pressure in the cavity unchanged, starting a laser to bombard the STO target material, and depositing a STO layer on the surface of the STO/SAO for 5 min;
(e) finally, the temperature of the STO (001) substrate is reduced to 400 ℃, the oxygen partial pressure in the growth cavity is kept unchanged, and the laser is started again to bombard Fe3O4Target material of Fe3O4Depositing on the surface of STO/SAO for 60min to obtain STO/SAO/Fe3O4A material.
(3) STO/SAO/STO/Fe prepared by the steps3O4Soaking the material in deionized water to dissolve the single crystal SAO layer to obtain self-supporting STO/Fe3O4The film material specifically comprises the following steps:
(A) supports with STO/SAO/STO/Fe by organic polymers3O4Fe of sample3O4Tightly attaching the film;
(B) then placing the processed sample on a heating table at 90 ℃ and heating for 10 min;
(C) then soaking the sample in deionized water for 50min to completely dissolve the single crystal SAO layer;
(D) finally, Fe will be adhered to3O4Taking out the PDMS supporting plate of the film to prepare the self-supporting STO/Fe3O4A material.
Prepared self-supporting STO/Fe3O4The film material is single crystal of cubic system, single crystal Fe3O4The unit cell parameters are as follows: a =8.394 a, the unit cell parameters of the STO crystal are: a =3.905 a, unit cell parameters of the SAO crystal: a = 15.844A.
Comparative example 1
Single-crystal Fe without STO layer prepared by the above method3O4The material comprises the following specific steps:
(1) selecting an STO (001) substrate and pretreating the substrate, wherein the method specifically comprises the following steps:
a. soaking STO (001) substrate in acetone, and ultrasonically cleaning at 60 deg.C for 10 min;
b. then soaking the STO (001) substrate in absolute ethyl alcohol, and ultrasonically cleaning for 5 min;
c. then soaking the STO (001) substrate in deionized water, and ultrasonically cleaning for 5 min;
d. the STO (001) substrate was finally dried with nitrogen.
(2) Preparing a single crystal SAO layer and Fe sequentially on a pretreated STO (001) substrate by adopting a pulse laser deposition method3O4The film material specifically comprises the following steps:
(a) adhering the STO (001) substrate pretreated in the step (1) on a SiC heat conducting sheet by using silver paste, and heating and drying;
(b) then placing the SiC heat-conducting strip adhered with the STO (001) substrate on a laser heating table in a growth cavity of a pulse laser deposition system, and vacuumizing the background in the growth cavity to 5 multiplied by 10-7Torr below, the STO (001) substrate is heated to 700 deg.C, and oxygen gas is introduced into the growth chamber to reach 3 × 10-6Torr oxygen partial pressure, setting the laser energy of a laser to be 300mJ and the frequency to be 10 Hz;
(c) then starting a laser to bombard the SAO target material to deposit the SAO on the STO (001) substrate for 20min, and then reducing the temperature of the STO (001) substrate to 400 ℃ while keeping the oxygen partial pressure in the growth cavity unchanged;
(d) finally, the laser is turned on againBombardment of Fe3O4Target material of Fe3O4Depositing on the surface of STO/SAO for 60min to obtain STO/SAO/Fe3O4A material.
(3) STO/SAO/Fe prepared by the steps3O4Soaking the material in deionized water to dissolve the single crystal SAO layer to obtain self-supporting Fe3O4The film material specifically comprises the following steps:
(A) supports with organic polymers and STO/SAO/Fe3O4Fe of sample3O4Tightly attaching the film;
(B) then placing the processed sample on a heating table at 90 ℃ and heating for 10 min;
(C) then soaking the sample in deionized water for 50min to completely dissolve the single crystal SAO layer;
(D) finally, Fe will be adhered to3O4Taking out the PDMS supporting plate of the film to prepare self-supporting single crystal Fe3O4A material.
XRD test analysis was performed on the sample materials prepared in example 1 and comparative example 1.
As shown in FIG. 1, it is apparent from XRD that in comparative example 1, in addition to the STO basal peak, there are a single-crystal SAO phase preferentially growing in the (008), (0012) orientation and a single-crystal Fe phase preferentially growing in the (111), (222), (333) and (444) orientations3O4Phase, illustrating a monocrystalline SAO layer and monocrystalline Fe3O4The crystallinity of the film is good. Referring to FIG. 2, the water-dissolved sample had only single-crystal Fe preferentially grown in the (111), (222), (333), and (444) orientations3O4Phase, illustrating the STO substrate and Fe3O4The film was successfully released and no SAO remained.
As shown in FIG. 3, it is apparent from XRD that example 1 has a single SAO phase preferentially growing in the (008) orientation and a single Fe phase preferentially growing in the (004) orientation in addition to the STO basal peak, as compared with comparative example 13O4Phase, illustrating a monocrystalline SAO layer and monocrystalline Fe3O4The crystallinity of the film is good. Reference is then made to4, presence of single crystal Fe preferentially grown in (004) orientation in the water-dissolved sample3O4The phases and the weak STO phase preferentially growing along the (002) orientation confirmed that a flexible self-supporting STO/Fe was obtained3O4And the film realizes the change of growth orientation.
For STO/SAO/STO/Fe3O4The lattice mismatch degree of the sample material is calculated, the lattice mismatch degree of the STO substrate layer and the SAO epitaxial layer is (3.905-15.844/4)/3.905 = -1.43%, the lattice mismatch degree of the SAO epitaxial layer and the STO regulating layer is (15.844/4-3.905)/3.961 =1.41%, and the lattice mismatch degree of the STO regulating layer and Fe3O4The lattice mismatch degree of the film is (3.905-8.394/2)/3.905 = -7.48%, and the film is good in lattice match and beneficial to growing high-quality materials.
EDS test analysis was performed on the sample materials in example 1 and comparative example 1.
As shown in FIG. 5, the elements Fe and O are Fe3O4Thin film and uniform distribution of Sr, Al, O in single crystal SAO layer, STO, SAO, Fe3O4Clear interfaces exist among three phases, and no interface diffusion phenomenon exists, so that the material prepared in the comparative example 1 has a high-quality epitaxial heterostructure. Comparing fig. 6, it is evident that Fe, O, Sr, Al, and O are also uniformly distributed in each layer, and a clear interface exists between each phase, and there is no interface diffusion phenomenon, which indicates that the material prepared in example 1 also has a high-quality epitaxial heterostructure, so that it is known that the presence of the STO layer does not affect the performance of the material, and further, the requirements of the flexible electronic device can be better satisfied.
Hysteresis loop measurements were performed on the sample materials in example 1 and comparative example 1.
Comparing FIGS. 7 and 8, it can be seen from the M-H hysteresis curve of comparative example 1 that Fe is in either a flat state or a bent state3O4(111) The thin film shows a hysteresis loop in which saturation can be measured in both in-plane (IP) and out-of-plane (OP), and the hysteresis loop exhibits a typical ferromagnetic characteristic shape, confirming Fe3O4(111) Room temperature ferromagnetism of the film. While it can be seen from the M-H hysteresis curve of example 1 that in either the flat state or the bent state,Fe3O4(001) the thin film also shows a hysteresis loop in saturation both in-plane (IP) and out-of-plane (OP), and the hysteresis loop also exhibits a typical ferromagnetic characteristic shape, confirming Fe3O4(001) Room temperature ferromagnetism of the film.
As can be seen from FIG. 7, Fe in the flat state3O4(111) The film has an IP coercive field of 300Oe and Fe in a bent state3O4(111) The film has an IP coercive field of 380Oe and Fe in a flat state3O4(111) The film has an OP coercive field of 530Oe and Fe in a bent state3O4(111) The OP coercive field of the film was 380 Oe. Under the external magnetic field of 15000Oe, Fe in a flat state3O4(111) Coercive field and Fe in bent state of thin film3O4(111) The coercive force field of the film is not obviously changed, and the saturation magnetization and the residual magnetization of the film are stable, thereby proving that Fe is in different mechanical states3O4(111) The film has stable magnetic performance.
Comparison of FIG. 8, Fe3O4(001) The IP coercive force fields of the film in a flat state and a bent state are 480Oe, and Fe in the flat state3O4(001) The film has an OP coercive field of 330Oe and Fe in a bent state3O4(001) The OP coercivity field of the film was 290 Oe. Under the external magnetic field of 15000Oe, Fe in a flat state3O4(001) Coercive field and Fe in bent state of thin film3O4(001) The coercive force field of the film is not obviously changed and the saturation magnetization and the residual magnetization of the film are stable, thereby proving that the Fe is in different mechanical states3O4(001) The film also has stable magnetic performance and can be well applied to electronic devices. The film is compared with Fe in comparative example 13O4(111) The magnetic property difference exists between the films, but the magnetic easy axis of the films is not obviously changed.
The sample material from example 1 was subjected to the MFM test.
As shown in FIG. 9, the MFM test (0Oe) was first conducted on the sample material in example 1 in the initial state, and the results showed that the sample hadAnd a clear magnetic domain structure is obtained, then the magnetic domain structure is not changed after a 300OeIP magnetic field is applied, which indicates that 300Oe does not reach the sample coercive field, the IP magnetic field is continuously increased to 400Oe, the magnetic domain structure is not changed, and when the IP magnetic field is increased to 500Oe, a slight change of a magnetic signal is found, so that the magnetic field is confirmed to exceed the sample coercive field and is consistent with the obtained M-H result. Subsequently, by applying 1500OeIP magnetic field, the magnetic domain structure was found to be completely changed, which shows that the application of IP magnetic field can regulate the magnetic performance of the sample. When the IP field was increased to 3000Oe, the domain structure was found to be the same as that when the 1500OeIP field was applied, which means that the sample had saturated when the 1500OeIP field was applied, also consistent with the M-H results. Next, by observing the change of the magnetic domain by applying an IP magnetic field in the opposite direction, it was found that the magnetic domain obtained when the magnetic field was increased to-3000 Oe was exactly opposite to that obtained when the 3000OeIP magnetic field was applied, confirming that the obtained STO/SAO/STO/Fe3O4The magnetic property of the heterojunction sample can be reversibly regulated by an external IP magnetic field.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (2)

1. Flexible self-supporting single crystal Fe capable of self-regulating growth orientation3O4The preparation method of the film material is characterized by comprising the following steps:
(1) selecting an STO (001) substrate and pretreating the substrate, wherein the method specifically comprises the following steps:
a. soaking STO (001) substrate in acetone, and ultrasonically cleaning at 60 deg.C for 10 min;
b. then soaking the STO (001) substrate in absolute ethyl alcohol, and ultrasonically cleaning for 5 min;
c. then soaking the STO (001) substrate in deionized water, and ultrasonically cleaning for 5 min;
d. finally, the STO (001) substrate is dried by nitrogen;
(2) a pulse laser deposition method is adopted to prepare a single crystal SAO layer, an STO layer and an Fe3O4 film material on a pretreated STO (001) substrate in sequence, and the method specifically comprises the following steps:
(a) adhering the STO (001) substrate pretreated in the step (1) to the SiC heat conducting strip by using silver paste, and then heating and drying;
(b) placing the SiC heat conducting strip adhered with the STO (001) substrate on a laser heating table in a growth cavity of a pulse laser deposition system, vacuumizing the background in the cavity to be below 5 multiplied by 10 < -7 > Torr, heating the STO (001) substrate to 700 ℃, filling flowing oxygen into the cavity to reach 3 multiplied by 10 < -6 > Torr oxygen partial pressure in the heating process, and setting the laser energy of a laser to be 300mJ and the frequency to be 10 Hz;
(c) then starting a laser to bombard the SAO target material to deposit the SAO on the STO (001) substrate for 20 min;
(d) keeping the temperature of an STO (001) substrate and the oxygen pressure in the cavity unchanged, starting a laser to bombard an STO target material, and depositing a STO layer on the surface of the STO/SAO, wherein the thickness is 20-100nm, the deposition time is 5min, and the deposition temperature is 650-750 ℃;
(e) finally, reducing the temperature of the STO (001) substrate to 400 ℃, simultaneously keeping the oxygen partial pressure unchanged, starting the laser again to bombard the Fe3O4 target material, so that Fe3O4 is deposited on the STO/SAO surface for 60min, and preparing the STO/SAO/Fe3O4 material;
(3) soaking the STO/SAO/STO/Fe3O4 material prepared in the steps in deionized water to dissolve the single crystal SAO layer, thereby obtaining the self-supporting STO/Fe3O4 thin film material, which comprises the following steps:
(A) closely attaching an organic polymer support plate to a Fe3O4 film of the STO/SAO/STO/Fe3O4 sample;
(B) then placing the processed sample on a heating table at 90 ℃ and heating for 10 min;
(C) then soaking the sample in deionized water for 50min to completely dissolve the single crystal SAO layer;
(D) finally, taking out the PDMS supporting plate attached with the Fe3O4 film to prepare a self-supporting STO/Fe3O4 material;
the prepared self-supporting STO/Fe3O4 film material is a single crystal of a cubic system, and the unit cell parameters of the single crystal Fe3O4 are as follows: a =8.394 a, the unit cell parameters of the STO crystal are: a =3.905 a, unit cell parameters of the SAO crystal: a = 15.844A.
2. A single crystal structure characterized by a self-regulating growth orientation of flexible self-supporting single crystal Fe as claimed in claim 13O4The film material is prepared by the preparation method, and the single crystal structure is STO/SAO/STO/Fe in sequence3O4Wherein STO is STO substrate with crystal orientation of (001), SAO is single crystal SAO layer epitaxially grown on STO substrate with crystal phase in epitaxial relationship of STO [001 ]]//SAO[001]Fe grown on STO/SAO/STO layer3O4Being single crystal Fe3O4Film with an epitaxial growth relationship of STO [001 ]]//SAO[001]//STO[001]//Fe3O4[001]。
CN202011301146.1A 2020-11-19 2020-11-19 Flexible self-supporting single crystal Fe with self-regulating growth orientation3O4Preparation of thin film material, thin film material and single crystal structure Active CN112410880B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011301146.1A CN112410880B (en) 2020-11-19 2020-11-19 Flexible self-supporting single crystal Fe with self-regulating growth orientation3O4Preparation of thin film material, thin film material and single crystal structure

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011301146.1A CN112410880B (en) 2020-11-19 2020-11-19 Flexible self-supporting single crystal Fe with self-regulating growth orientation3O4Preparation of thin film material, thin film material and single crystal structure

Publications (2)

Publication Number Publication Date
CN112410880A CN112410880A (en) 2021-02-26
CN112410880B true CN112410880B (en) 2022-04-19

Family

ID=74774776

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011301146.1A Active CN112410880B (en) 2020-11-19 2020-11-19 Flexible self-supporting single crystal Fe with self-regulating growth orientation3O4Preparation of thin film material, thin film material and single crystal structure

Country Status (1)

Country Link
CN (1) CN112410880B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113698194A (en) * 2021-06-16 2021-11-26 中国科学院深圳先进技术研究院 Flexible self-supporting BaTiO3-CoFe2O4Multiferroic self-assembled nanostructure and preparation method thereof
CN113675330B (en) * 2021-07-09 2023-08-22 中国科学院深圳先进技术研究院 By CoFe 2 O 4 Piezoelectric material for directionally regulating and controlling growth orientation of PMN-PT film and preparation method thereof
CN115537738A (en) * 2022-10-26 2022-12-30 桂林电子科技大学 Preparation method of M-type ferrite heterojunction film with high remanence ratio and single orientation

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5670218A (en) * 1995-10-04 1997-09-23 Hyundai Electronics Industries Co., Ltd. Method for forming ferroelectric thin film and apparatus therefor
CN111270306A (en) * 2020-03-19 2020-06-12 西安交通大学 Preparation method of flexible epitaxial monocrystal ferrite film
CN111540826A (en) * 2020-04-22 2020-08-14 西安交通大学 Flexible functional film based on composite transition layer and preparation method thereof
CN111733452B (en) * 2020-04-30 2021-09-21 深圳先进技术研究院 Flexible self-supporting single crystal magnetic Fe3O4Preparation of thin film material, thin film material and application thereof, and single crystal structure

Also Published As

Publication number Publication date
CN112410880A (en) 2021-02-26

Similar Documents

Publication Publication Date Title
CN112410880B (en) Flexible self-supporting single crystal Fe with self-regulating growth orientation3O4Preparation of thin film material, thin film material and single crystal structure
CN111733452B (en) Flexible self-supporting single crystal magnetic Fe3O4Preparation of thin film material, thin film material and application thereof, and single crystal structure
CN108517555B (en) Method for obtaining large-area high-quality flexible self-supporting monocrystalline oxide film based on Van der Waals epitaxy
CN107146761B (en) Preparation method of yttrium iron garnet/bismuth heterogeneous film with giant magneto-optical effect
CN108385166A (en) Regulate and control the method for ferrite single crystal thin film magnetic using bending stress
CN104193316B (en) Yttrium iron garnet film and preparation method thereof
CN108039408A (en) A kind of preparation method of flexibility hafnium oxide based ferroelectric film
CN108660417B (en) Self-supporting Ga2O3Film and preparation method thereof
CN109994315B (en) Magnetoelectric composite material combined by ferroelectric film of magnetic nano fiber and preparation method thereof
CN115714035A (en) Flexible self-supporting ferroelectric film and preparation method thereof
US9437823B2 (en) Production device for a graphene thin film
CN113322511B (en) Flexible self-supporting perovskite oxide single crystal thin film with perpendicular magnetic anisotropy in different crystal directions and preparation thereof
CN109972136B (en) Preparation method of oriented growth P (VDF-TrFE) film
CN100366786C (en) Novel metallic film preparation technology on liquid phase substrate surface
CN113745092A (en) Preparation method of flexible self-supporting perovskite oxide single crystal thin film with different crystal orientations
CN108531857B (en) Method for regulating and controlling residual polarization and coercive field of barium titanate single crystal film by utilizing bending deformation
CN105441877A (en) Resistance type thermal evaporation technology for preparing ferromagnetic material Fe3Si film
CN114086118B (en) Self-supporting flexible film and preparation method thereof
CN114808140B (en) Two-dimensional monocrystalline ferroferric oxide nano material and preparation method thereof
WO2022262235A1 (en) Flexible self-supporting batio3-cofe2o4 multiferroic self-assembled nanomaterial and preparation method therefor
CN111129286B (en) Flexible magnetoelectric heterojunction and preparation method thereof
CN112382718A (en) C-axis vertical preferred orientation AlN piezoelectric film and preparation method thereof
CN107287563A (en) A kind of extension stronitum stannate cobalt thin film and preparation method thereof
CN110783460A (en) Non-volatile memory device with flexible multi-state magnetic and holding ferroelectric regulation and control characteristics
CN101343723A (en) Method of manufacturing permalloy iron core film

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