CN114197035A - Perovskite thin film and epitaxial preparation method thereof - Google Patents
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- 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
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- 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
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- C30B29/22—Complex oxides
Abstract
The invention belongs to the technical field of functional thin film material preparation, and discloses a perovskite thin film and an epitaxial preparation method thereof. Through the reaction of Sr3Al2O6Doping Ca to regulate Sr3Al2O6The lattice constant of the sacrificial layer realizes the epitaxial growth of different perovskite films, and the prepared single crystal film has good compactness, high stability, high growth speed, good repeatability and stoichiometric ratio consistent with that of the target material, namely Sr3Al2O6The film growing on the surface of the film can not be adversely affected in the dissolving process, and the crystal is regulated and controlledThe lattice constant makes it possible to act as a sacrificial layer for other materials.
Description
Technical Field
The invention belongs to the technical field of functional thin film material preparation, and particularly relates to a perovskite thin film and an epitaxial preparation method thereof.
Background
At present, in functional thin film materials in recent years, perovskite oxides attract people to pay great attention with abundant structural, electrical, magnetic and optical properties, and the properties expand the application potential of novel functional electronic materials. However, previous studies have focused on three-dimensional materials stacked one on top of the other, with layers being connected by weak van der waals interactions. The substrate or the sacrificial layer can show abundant physical properties by regulating and controlling the pressure to which the substrate or the sacrificial layer is subjected, the type of rare earth elements, the epitaxial stress to which the film is subjected, the stoichiometric ratio and the doping concentration. The perovskite-type rare earth nickelate is prepared into a thin film, which can be expected to exhibit specific properties more advantageous to reality. In addition, the peeling of the film from the substrate to obtain a flexible two-dimensional material is of great physical significance throughout the condensed state.
In an epitaxial film, strain can play a role in an additional degree of freedom, expanding the parameter space for adjusting the material performance. Most notably, thin film growth methods can be used to achieve atom-controlled heterostructures, multilayer structures, and superlattices of constituent oxides. For the preparation of ultra-thin films or artificially structured oxide films of functional perovskite structures, chemically and structurally compatible substrates and sacrificial layers are of critical importance, since the interfacial interactions between the capping film and the substrate surface critically control the growth quality and subsequent properties of the film. Notably, metal oxide perovskites are also important as substrates, as many of the single crystals that are useful as substrates are perovskites or perovskite-related structures.
Through the above analysis, the problems and defects of the prior art are as follows:
(1) material growth techniques, such as physical/chemical vapor deposition, molecular beam epitaxy, etc., are generally limited to lattice matching and processing compatibility between substrates and films, and from film to film.
(2) The growth types of the films corresponding to the substrate with the fixed lattice constant are limited, and the epitaxial growth of the films of different types is limited.
(3) The two-dimensional material obtained by the conventional method is mainly obtained by etching, high-energy laser irradiation, and the like, but these techniques are too complicated and affect the thin film.
The difficulty in solving the above problems and defects is: the perovskite thin films of different types are grown through regulating and controlling the lattice constant of the substrate, and the lattice matching degree of the substrate and the thin films is the most difficult problem.
The significance of solving the problems and the defects is as follows: the method has great significance for the whole condensed state physics in order to realize the epitaxial growth of more abundant perovskite thin film types, regulate and control the physical properties of the two-dimensional material and strip the thin film from the substrate to obtain the flexible two-dimensional material.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a perovskite thin film and an epitaxial preparation method thereof.
The invention is realized in such a way that the epitaxial preparation method of the perovskite thin film comprises the following steps:
by laser pulses at SiTO3Respectively depositing Sr on the substrate3Al2O6、Sr2CaAl2O6And SrCa2Al2O6The sacrificial layer film is formed by growing different kinds of perovskite type films by regulating and controlling the lattice constant of the sacrificial layer.
Further, the epitaxial preparation method of the perovskite thin film specifically comprises the following steps:
step one, high-purity SrCO is mixed3、Al2O3And CaCO3Mixing the raw materials according to different proportions, decarburizing in a muffle furnace at 1200 ℃, grinding and tabletting the decarburized mixed powder, and sintering in the muffle furnace to respectively obtain Sr3Al2O6、Sr2CaAl2O6And SrCa2Al2O6A target material;
step two, La2O3And Ni2O3Uniformly mixing and grinding the mixture according to a certain proportion, pressing a target by using a tabletting machine, and sintering the mixture in a muffle furnace to obtain LaNiO3A target material;
step three, Sr is added3Al2O6Target material, LaNiO3Target and treated SrTiO3Putting the substrates into a pulsed laser deposition system together, and sequentially placing the substrates on SrTiO3Sequentially growing Sr on the substrate by epitaxy3Al2O6And LaNiO3A single crystal thin film;
step four, Sr is performed according to the step three2CaAl2O6、PrNiO3Target material replacing Sr3Al2O6Target material, LaNiO3The target material is used for carrying out epitaxial growth of different films;
step five, SrCa is carried out according to the step three2Al2O6、NdNiO3Target material replacing Sr3Al2O6Target material, LaNiO3Carrying out epitaxial growth of different films on the target material again;
step six, respectively coating Sr with a bench type spin coater3Al2O6-LaNiO3、Sr2CaAl2O6-PrNiO3And SrCa2Al2O6-NdNiO3Coating a layer of PMMA (polymethyl methacrylate) on the surface of the film in a suspending way, heating, and putting the film into water for dissolving after cooling to room temperature;
step seven, waiting for Sr3Al2O6、Sr2CaAl2O6And SrCa2Al2O6Dissolution, PMMA and LaNiO3After the film floats on the water surface, the film is salvaged and dried by using a Si sheet to prepare a sample.
Further, in step one, Sr3Al2O6SrCO in target preparation3And Al2O3In a ratio of 3:1, Sr2CaAl2O6SrCO in target preparation3、Al2O3And CaCO3In a ratio of 2:1:2, SrCa2Al2O6SrCO in target preparation3、Al2O3And CaCO3The ratio was 1:2: 1.
Further, in the step one, when the decarburized mixed powder is ground, the grinding time is 40-60 minutes, the target pressing pressure of a tablet press during tablet forming is 20-25MPa, the target pressing time is 15-20 minutes, and the size of a die for target pressing is 1 inch; when the material is placed into a muffle furnace for sintering, the pre-calcining temperature is 1250 ℃, the sintering temperature is 1300 ℃, the sintering time is 12-14 hours, and the heating rate and the cooling rate are 5 ℃/min.
Further, in step two, La2O3And Ni2O3The ratio of the grinding time to the target pressing time is 1:1, the grinding time is 40-60 minutes, the target pressing pressure of a tabletting machine is 20-25MPa, the target pressing time is 10-20 minutes, the size of a die for pressing the target is 1 inch, the sintering temperature is 1250 ℃, the sintering time is 12-14 hours, and the temperature rising speed is 5 ℃/min.
Further, in step three, SiTO3The distance between the substrate and the target is 50-60 mm.
Further, in step three, the pulsed laser deposition system deposits Sr3Al2O6The temperature of the sacrificial layer is 700-800 ℃, and the air pressure is 10-4～10-5mtorr with energy density of 0.8-1.0 J.cm-2Then in Sr3Al2O6Further depositing LaNiO on the sacrificial layer3The temperature is 600-650 ℃, the air pressure is 150-200mtorr, and the energy density is 1.0-1.2J-cm-2。
Further, in the third step, in the sixth step, the rotating speed of the desktop spin coater is 3000-4000 rpm, the heating temperature is 100-120 ℃, the heating time lasts 10-20 minutes, the cooling time is 10-20 minutes, the drying temperature is 80-100 ℃, and the drying time is 10-20 minutes.
Further, in the seventh step, the glue removing time of PMMA is 40 minutes, the drying temperature is 70 ℃, and the time is 12-15 minutes.
By combining all the technical schemes, the invention has the advantages and positive effects that:
through the reaction of Sr3Al2O6Doping Ca to regulate Sr3Al2O6The lattice constant of the sacrificial layer realizes the epitaxial growth method of different perovskite thin films. In addition, Sr3Al2O6、Sr2CaAl2O6And SrCa2Al2O6Has water solubility, and can be dissolved in water only by putting the two-dimensional material LaNiO3 into water, thereby realizing the peeling of the flexible two-dimensional material LaNiO3 from the STO substrate. The prepared single crystal film has good compactness, high stability, high growth speed, good repeatability and consistent stoichiometric ratio with a target material. Unlike the conventional method, Sr is3Al2O6The film growing on the film can not be adversely affected in the dissolving process, and the crystal lattice constant of the film can be adjusted to be used as a sacrificial layer of other materials.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained from the drawings without creative efforts.
Fig. 1 is a flowchart of an epitaxial preparation method of a perovskite thin film according to an embodiment of the present invention.
FIG. 2 is a schematic diagram of an embodiment of the present invention
Lattice constants of a wide variety of perovskite thin films and commercially available substrates
FIG. 3 shows Sr prepared in example 1 of the present invention3Al2O6、Sr2CaAl2O6And SrCa2Al2O6XRD pattern of single crystal thin film, wherein Sr2CaAl2O6Lattice constant different from that of STO substrateOften close, resulting in overlapping peak positions, so the display is not obvious.
FIG. 4 shows Sr grown on STO substrate in sequence prepared in example 1 of the present invention3Al2O6-LaNiO3、Sr2CaAl2O6-PrNiO3And SrCa2Al2O6-NdNiO3XRD pattern of single crystal film.
FIG. 5 shows Sr in example 1 of the present invention3Al2O6-LaNiO3The process diagram of gradual dissolution in water.
FIG. 6 shows a flexibly conductive LaNiO under an optical microscope in example 1 of the present invention3Figure (a).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In view of the problems of the prior art, the present invention provides a perovskite thin film and an epitaxial preparation method thereof, and the present invention is described in detail below with reference to the accompanying drawings.
As shown in fig. 1, the method for epitaxially preparing a perovskite thin film according to an embodiment of the present invention includes:
s101, mixing high-purity SrCO3、Al2O3And CaCO3Mixing the raw materials according to different proportions, decarburizing in a muffle furnace at 1200 ℃, grinding and tabletting the decarburized mixed powder, and sintering in the muffle furnace to respectively obtain Sr3Al2O6、Sr2CaAl2O6And SrCa2Al2O6A target material;
s102, mixing La2O3And Ni2O3Uniformly mixing and grinding the mixture according to a certain proportion, pressing a target by using a tabletting machine, and sintering the mixture in a muffle furnace to obtain LaNiO3A target material;
s103, adding Sr3Al2O6Target material, LaNiO3Target and treated SrTiO3Putting the substrates into a pulsed laser deposition system together, and sequentially placing the substrates on SrTiO3Sequentially growing Sr on the substrate by epitaxy3Al2O6And LaNiO3A single crystal thin film;
s104, Sr is performed according to the third step2CaAl2O6、PrNiO3Target material replacing Sr3Al2O6Target material, LaNiO3The target material is used for carrying out epitaxial growth of different films;
s105, mixing SrCa according to the third step2Al2O6、NdNiO3Target material replacing Sr3Al2O6Target material, LaNiO3Carrying out epitaxial growth of different films on the target material again;
s106, respectively coating Sr with a bench type spin coater3Al2O6-LaNiO3、Sr2CaAl2O6-PrNiO3And SrCa2Al2O6-NdNiO3Coating a layer of PMMA (polymethyl methacrylate) on the surface of the film in a suspending way, heating, and putting the film into water for dissolving after cooling to room temperature;
s107, to be Sr3Al2O6、Sr2CaAl2O6And SrCa2Al2O6Dissolution, PMMA and LaNiO3After the film floats on the water surface, the film is salvaged and dried by using a Si sheet to prepare a sample.
The invention is further described with reference to specific examples.
Example 1
The method for realizing the epitaxial growth of the perovskite thin film by regulating and controlling the lattice constant of the sacrificial layer comprises the following steps of:
(1)Sr3Al2O6the target material is according to SrCO3And Al2O3In a ratio of 3:1, Sr2CaAl2O6Target SrCO3、Al2O3And CaCO3In a ratio of 2:1:2, SrCa2Al2O6SrCO of target material3、Al2O3And CaCO3The proportion is 1:2:1, grinding time is 40 minutes after mixing, the pressure of a pressing target of a tabletting machine is 20-25MPa, the pressing target time is 20 minutes, the size of a die for pressing the target is 1 inch, the precalcination temperature is 1250 ℃, the sintering temperature is 1300 ℃, the sintering time is 12 hours, and the heating rate and the cooling rate are 5 ℃/min.
(2) La2O3And Ni2O3Uniformly mixing according to the ratio of 1:1, grinding for 30-40 minutes, putting the ground powder into a 1-inch mold, pressing a target by using the pressure of 20-25Mpa for 10-20 minutes, taking out, sintering at the high temperature of 1300-1350 ℃ in a muffle furnace for 12-20 hours to obtain about 9g of LaNiO3A target material;
(3) sr is3Al2O6Target material, LaNiO3Target and treated SrTiO3Putting the substrates into a pulsed laser deposition system together, and firstly, SrTiO3Epitaxially growing Sr on the substrate3Al2O6The temperature of the single crystal film is 700--4-10- 5mtorr with energy density of 0.8-1.0 J.cm-2(ii) a Then in the grown Sr3Al2O6Epitaxial growth of LaNiO on monocrystal film3The single crystal film has a temperature of 600-700 deg.C, a gas pressure of 200mtorr, and an energy density of 1.0-1.2J-cm-2；
(4) Respectively placing the film samples obtained in the step (3) on a bench spin coater, coating a layer of polymethyl methacrylate (PMMA) on the surface of the film samples at the rotating speed of 3000-4000 rpm, heating the samples to the temperature of 100-120 ℃, continuing for 10-20 minutes, cooling for 10-20 minutes at room temperature, and then placing the samples into water for dissolving; after a period of time, Sr3Al2O6Dissolution, PMMA and LaNiO3Floating the film on the water surface, fishing the film by using a Si sheet, and drying the film on a heating table at the temperature of 80-100 ℃ for 10-20 minutes.
(5) Soaking the sample in acetone for 30-40 min to remove PMMA, taking out, and drying on a heating table at 60-70 ℃ for 3-5 min to obtain the film separated from the substrate.
Example 2
The present embodiment is different from the first embodiment in that SrTiO is used in step (3)3Epitaxially growing Sr on the substrate2CaAl2O6The temperature of the single crystal film is 700--4-10-5mtorr with energy density of 0.8-1.1 J.cm-2(ii) a The rest is the same as the first embodiment.
Example 3
This example differs from example 1 in that SrTiO is used in step (3)3Epitaxially growing SrCa on the substrate2Al2O6The temperature of the single crystal film is 600-700 ℃, and the air pressure is 10-4-10-5mtorr with energy density of 0.8-1.0 J.cm-2(ii) a The rest is the same as the first embodiment.
Analysis of results
As shown in FIG. 2, in
Lattice constants of a wide variety of perovskite thin films and commercially available substrates
The lattice constants of the substrate and the scientifically meaningful multifunctional perovskite vary widely, and the diversity of the substrates is evident from the figure, meaning that for a given material, the lattice constant of the thin film can be manipulated to produce a multilayer structure thin film in its most natural state.
Sr was obtained in example 13Al2O6、Sr2CaAl2O6And SrCa2Al2O6The result of XRD pattern analysis of the sacrificial layer film is shown in figure 3. from figure 3, it can be seen that the film prepared by the pulsed laser deposition method in the experiment has high diffraction peak intensity, sharp diffraction peak and small half-height width, which indicates that the film has good crystallization and pure product.
SrTiO formulations for examples 1, 2 and 33Sr is sequentially deposited on the substrate3Al2O6And LaNiO3The XRD single crystal diffraction pattern after the film,from FIG. 4, Sr can be seen3Al2O6And LaNiO3Thin films have been successfully grown epitaxially.
Sr is shown for example 13Al2O6After the picture is continuously dissolved by deionized water, the PMMA supports the LaNiO3 film and finally is separated from SrTiO3The substrate, the result is shown in FIG. 5.
LaNiO showing flexibility after transfer for example 13The optical microscopy of the film shows that the film is relatively intact after transfer, the result of which is shown in FIG. 6.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A method for epitaxial preparation of a perovskite thin film, the method comprising:
using laser pulses at SiTO3Respectively depositing Sr on the substrate3Al2O6、Sr2CaAl2O6And SrCa2Al2O6Sacrificial layer film, and different kinds of perovskite type film are grown by regulating and controlling the lattice constant of the sacrificial layer.
2. The method for epitaxial production of a perovskite thin film as claimed in claim 1, wherein the method for epitaxial production of a perovskite thin film specifically comprises the steps of:
step one, high-purity SrCO is mixed3、Al2O3And CaCO3Mixing the raw materials according to different proportions, decarburizing in a muffle furnace at 1200 ℃, grinding and tabletting the decarburized mixed powder, and sintering in the muffle furnace to respectively obtain Sr3Al2O6、Sr2CaAl2O6And SrCa2Al2O6A target material;
step two, La2O3And Ni2O3Uniformly mixing and grinding the mixture according to a certain proportion, pressing a target by using a tabletting machine, and sintering the mixture in a muffle furnace to obtain LaNiO3A target material;
step three, Sr is added3Al2O6Target material, LaNiO3Target and treated SrTiO3Putting the substrates into a pulsed laser deposition system together, and sequentially placing the substrates on SrTiO3Sequentially growing Sr on the substrate by epitaxy3Al2O6And LaNiO3A single crystal thin film;
step four, Sr is performed according to the step three2CaAl2O6、PrNiO3Target material replacing Sr3Al2O6Target material, LaNiO3The target material is used for carrying out epitaxial growth of different films;
step five, SrCa is carried out according to the step three2Al2O6、NdNiO3Target material replacing Sr3Al2O6Target material, LaNiO3Carrying out epitaxial growth of different films on the target material again;
step six, respectively coating Sr with a bench type spin coater3Al2O6-LaNiO3、Sr2CaAl2O6-PrNiO3And SrCa2Al2O6-NdNiO3Coating a layer of PMMA (polymethyl methacrylate) on the surface of the film in a suspending way, heating, and putting the film into water for dissolving after cooling to room temperature;
step seven, waiting for Sr3Al2O6、Sr2CaAl2O6And SrCa2Al2O6Dissolution, PMMA and LaNiO3After the film floats on the water surface, the film is salvaged and dried by using a Si sheet to prepare a sample.
3. The process for the epitaxial production of a perovskite thin film as claimed in claim 2, wherein in step one, Sr is3Al2O6SrCO in target preparation3And Al2O3In a ratio of 3:1, Sr2CaAl2O6SrCO in target preparation3、Al2O3And CaCO3In a ratio of 2:1:2, SrCa2Al2O6SrCO in target preparation3、Al2O3And CaCO3The ratio was 1:2: 1.
4. The method for epitaxial production of a perovskite thin film as claimed in claim 2, wherein in the step one, when the decarburized mixed powder is ground, the grinding time is 40 minutes, the target pressing pressure of a tablet press during tablet forming is 20 to 25MPa, the target pressing time is 20 minutes, and the size of a die for target pressing is 1 inch; when the material is placed into a muffle furnace for sintering, the pre-calcining temperature is 1250 ℃, the sintering temperature is 1300 ℃, the sintering time is 12 hours, and the heating rate and the cooling rate are 5 ℃/min.
5. The method for epitaxial production of a perovskite thin film as claimed in claim 2, wherein in the second step, La is added2O3And Ni2O3The ratio of the grinding time to the target pressing time is 1:1, the grinding time is 60 minutes, the target pressing pressure of a tabletting machine is 20MPa, the target pressing time is 10-20 minutes, the size of a die for pressing the target is 1 inch, the sintering temperature is 1250 ℃, the sintering time is 12 hours, and the temperature rising speed is 5 ℃/min.
6. The process for the epitaxial production of perovskite thin film as claimed in claim 2, wherein in step three, SiTO3The distance between the substrate and the target is 50-60 mm.
7. The process for epitaxial growth of perovskite thin film as claimed in claim 2, wherein in step three, the pulsed laser deposition system deposits Sr3Al2O6The temperature of the sacrificial layer is 700-800 ℃, and the air pressure is 10-4～10-5mtorr with energy density of 0.8-1.0 J.cm-2Then in Sr3Al2O6Further depositing on the sacrificial layerProduct LaNiO3The temperature is 600-650 ℃, the air pressure is 200mtorr, and the energy density is 1.0-1.2J-cm-2。
8. The epitaxial preparation method of the perovskite thin film as claimed in claim 2, wherein in the third step, in the sixth step, the rotating speed of a bench-type spin coater is 3000-4000 rpm, the heating temperature is 100-120 ℃, the heating time lasts 10-20 minutes, the cooling time is 10-20 minutes, the drying temperature is 80-100 ℃, and the drying time is 10-20 minutes.
9. The method for epitaxial growth of perovskite thin film as claimed in claim 2, wherein in the seventh step, the glue removing time of PMMA is 40 minutes, the drying temperature is 70 ℃, and the time is 12 minutes.
10. A perovskite thin film produced by the method for epitaxial production of a perovskite thin film according to any one of claims 1 to 9.
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| CN113322511A (en) * | 2021-05-27 | 2021-08-31 | 中国科学院宁波材料技术与工程研究所 | Flexible self-supporting perovskite oxide single crystal thin film with perpendicular magnetic anisotropy in different crystal directions and preparation thereof |
| CN113481602A (en) * | 2021-07-06 | 2021-10-08 | 电子科技大学 | Preparation method of infinite-layer nickelate film with superconducting characteristic |
| CN114086118A (en) * | 2021-11-09 | 2022-02-25 | 电子科技大学长三角研究院(湖州) | Self-supporting flexible film and preparation method thereof |
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