CN115506009A - Preparation method of in-situ nitrogen-doped epitaxial oxide single crystal film - Google Patents
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- CN115506009A CN115506009A CN202211083022.XA CN202211083022A CN115506009A CN 115506009 A CN115506009 A CN 115506009A CN 202211083022 A CN202211083022 A CN 202211083022A CN 115506009 A CN115506009 A CN 115506009A
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- 239000013078 crystal Substances 0.000 title claims abstract description 22
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 40
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 230000008021 deposition Effects 0.000 claims abstract description 14
- 239000013077 target material Substances 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 42
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000010409 thin film Substances 0.000 claims description 14
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 claims description 12
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical group O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 11
- 239000004408 titanium dioxide Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims 4
- 230000001105 regulatory effect Effects 0.000 abstract description 8
- 230000001276 controlling effect Effects 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 description 18
- 230000007704 transition Effects 0.000 description 11
- 238000004549 pulsed laser deposition Methods 0.000 description 10
- 239000012212 insulator Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 230000006872 improvement Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000005137 deposition process Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 3
- -1 nitrogen ions Chemical class 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000005468 ion implantation Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004176 ammonification Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006471 dimerization reaction Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- DUSYNUCUMASASA-UHFFFAOYSA-N oxygen(2-);vanadium(4+) Chemical group [O-2].[O-2].[V+4] DUSYNUCUMASASA-UHFFFAOYSA-N 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
-
- 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
- C30B23/002—Controlling or regulating
- C30B23/005—Controlling or regulating flux or flow of depositing species or vapour
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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
- C30B29/16—Oxides
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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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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Abstract
The invention provides a preparation method of an in-situ nitrogen-doped epitaxial oxide single crystal film, which comprises the following steps: cleaning a substrate, placing the substrate in a cavity of pulse laser deposition equipment, introducing a mixture of oxygen and nitrogen, performing pulse laser deposition on the substrate by using a pure target material of an oxide after the atmosphere in the cavity is uniform and stable, and annealing in the same atmosphere environment after deposition is completed. By adopting the technical scheme of the invention, the doping of nitrogen element is realized by regulating and controlling the atmosphere during epitaxial growth, the preparation of the doped oxide film can be realized without selecting a specific target material, and the method is simple, convenient and effective; the secondary treatment of the film is not involved, and the prepared high-quality film is not damaged.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a preparation method of an in-situ nitrogen-doped epitaxial oxide single crystal film.
Background
The oxide film material plays an important role in the development of modern science and technology. Many techniques have been developed for preparing functional oxide films, such as solution methods, spin-coating methods, magnetron sputtering, molecular beam deposition, pulsed laser deposition, and the like. Among them, pulsed Laser Deposition (PLD) has many advantages as a current hot-gate means for epitaxial growth of thin films, such as high crystalline quality of thin films, stable stoichiometric ratio, etc. The nitrogen doping has a remarkable effect on regulating and controlling the function of the oxide film, such as regulating and controlling the phase change temperature, the on-off ratio and the like of the vanadium dioxide film. Since PLD is commonly used for epitaxial growth of thin films in oxygen environment, nitrogen doping of thin films is usually performed by using a nitrogen-doped target method, i.e., selecting a nitrogen-doped target, or by using some post-processing methods, such as ion implantation, ammonification, and the like. The nitrogen-doped target method comprises the steps of sintering a nitrogen-doped target in advance and then carrying out epitaxial growth. The ion implantation mainly adopts a prepared oxide film sample, the oxide film sample is placed in high vacuum, and then nitrogen doping is realized through N ion beam bombardment; the ammoniation treatment is to place the prepared oxide film in ammonia atmosphere and at high temperature to realize nitrogen doping.
Although the doped epitaxial growth of the oxide film can be realized by bombarding the nitrogen-doped target material, two problems exist, firstly, the nitrogen doping content is the same as that of the target material, so different target materials need to be fired according to different contents, and continuous adjustment cannot be realized in the epitaxial growth process; secondly, some targets are not easy to fire after nitrogen doping, and the cost is higher than that before doping. The post-treatment means is simple and effective in nitrogen doping, but the post-treatment means often damages the crystal quality of the original epitaxial growth film and influences the functional performance of the film. At present, the bottleneck in the aspect of preparing the nitrogen-doped functional oxide thin film material with high epitaxial quality is that no preparation method capable of realizing in-situ nitrogen-doped growth exists. Compared with oxygen, the nitrogen has lower activity and stronger bond energy, and the conventional vapor deposition preparation method is difficult to separate nitrogen into nitrogen ions and participate in the film deposition process. No disclosure is found in the PLD technology about the performance research of the nitrogen-introduced control film.
Disclosure of Invention
Aiming at the technical problems, the invention discloses a preparation method of an in-situ nitrogen-doped epitaxial oxide single crystal film, and the obtained film has high epitaxial quality and realizes certain content doping, thereby realizing the performance regulation of a functional oxide film and meeting the requirements of the functional oxide film on material science research and engineering application.
In contrast, the technical scheme adopted by the invention is as follows:
a method for preparing an in-situ nitrogen-doped epitaxial oxide single crystal thin film comprises the following steps: cleaning a substrate, placing the substrate in a cavity of pulse laser deposition equipment, introducing a mixture of oxygen and nitrogen, performing pulse laser deposition on the substrate by using a pure target material of an oxide after the atmosphere in the cavity is uniform and stable, and annealing in the same atmosphere environment after deposition is finished.
By adopting the technical scheme, the nitrogen doping is realized while the high-quality monocrystalline oxide film is epitaxially grown by regulating and controlling the gas environment in the PLD cavity during the epitaxial growth. Because the pulsed laser bombards the surface of the target material, the plasma plume emitted has extremely high energy, and when the plasma plume collides with nitrogen gas molecules in the cavity, the gas molecules can be ionized into a mixture of atoms, ions and electrons and transmitted to the surface of the substrate material, so that the plasma plume participates in the epitaxial growth of the thin film. Because the in-situ growth technology is adopted, doping post-treatment is not needed, and the crystal quality of the film is effectively ensured. In addition, the atmosphere in the cavity can be reasonably regulated, the same target material can be realized, and different nitrogen doping concentrations can be continuously regulated.
As a further improvement of the invention, the oxide is vanadium dioxide. By adopting the technical scheme, the reduction of the metal insulator transition temperature of the vanadium dioxide film is realized by nitrogen doping, and the higher the doping concentration is, the more the reduction of the phase transition temperature is.
As a further improvement of the invention, the substrate is made of titanium dioxide.
As a further improvement of the invention, the condition parameters of the pulsed laser deposition are as follows: the temperature is 380 to 420 ℃, the total air pressure in the cavity is 15 to 25mTorr, the laser energy density is 1.0 to 1.2J/cm & lt 2 & gt, and the pulse frequency is 10 Hz. Further preferably, the condition parameters of the pulsed laser deposition are as follows: the temperature is 400 ℃, the total air pressure in the cavity is 20 mTorr, the laser energy density is 1.1J/cm < 2 >, and the pulse frequency is 10 Hz.
As a further improvement of the invention, after the deposition is finished, the temperature is preserved for 5 min in the original epitaxial atmosphere environment, and then annealing is carried out.
As a further improvement of the invention, the volume ratio of oxygen to nitrogen is 1. By adopting the technical scheme, the ideal metal insulator transition performance can be obtained by controlling the volume ratio of the oxygen to the nitrogen to be 1.
Compared with the prior art, the invention has the following beneficial effects:
firstly, by adopting the technical scheme of the invention, the doping of nitrogen element is realized by regulating and controlling the atmosphere during epitaxial growth, the preparation of the doped oxide film can be realized without selecting a specific target material, and the method is simple, convenient and effective; the secondary treatment of the film is not involved, and the prepared high-quality film is not damaged.
Secondly, compared with other prior arts, the nitrogen-doped vanadium dioxide thin film prepared by the technical scheme of the invention not only regulates and controls the transition temperature of the metal insulator, but also effectively improves the crystal quality, and the effect comes from the introduction of nitrogen, thereby not only providing a nitrogen source for doping, but also providing internal force for the growth process of the thin film, and reducing the lattice mismatch. Particularly, under the optimized nitrogen-oxygen atmosphere condition, the nitrogen-doped vanadium dioxide has lower transition temperature and higher on-off ratio, and is expected to be applied to high-performance intelligent switching devices.
Drawings
FIG. 1 is a comparative XRD diagram of films deposited in examples 1 to 3 of the present invention and comparative examples 1 to 2.
FIG. 2 is a microscopic morphology of films deposited in examples 1 to 3 and comparative examples 1 to 2 of the present invention.
FIG. 3 is an XPS comparison of films deposited in examples 1 to 3 of the present invention and comparative examples 1 to 2.
FIG. 4 is a graph showing the N contents of films deposited in examples 1 to 3 of the present invention and comparative examples 1 to 2.
FIG. 5 is a temperature resistance curve of films deposited in examples 1 to 3 and comparative examples 1 to 2 of the present invention.
Figure 6 is a XRD comparison of the films deposited in example 1 of the present invention and comparative example 3.
FIG. 7 is a graph showing the temperature resistance curves of the films deposited in example 1 of the present invention and comparative example 3.
Detailed Description
Preferred embodiments of the present invention are described in further detail below.
Example 1
Titanium dioxide is selected as a substrate, and cleaning and drying are carried out. Before the film is deposited, introducing atmosphere into the PLD cavity, regulating the proportion of oxygen and nitrogen entering the cavity by using a flow meter, controlling the volume ratio of oxygen to nitrogen to be 1.
Example 2
In this example, the volume ratio of oxygen to nitrogen was 2.
Example 3
In this example, the volume ratio of oxygen to nitrogen was 1.
Comparative example 1
In this comparative example, pure nitrogen was used as the gas to be introduced on the basis of example 1.
Comparative example 2
In this comparative example, pure oxygen was used as the gas to be introduced on the basis of example 1.
An XRD contrast diagram of the films obtained in the examples 1 to 3 and the comparative examples 1 to 2 is shown in figure 1, an SEM contrast diagram is shown in figure 2, an energy spectrum contrast diagram is shown in figure 3, and an N content contrast diagram is shown in figure 4, so that the method of the embodiment can realize effective regulation of the nitrogen doping content from about 0-4% in the environment with the same nitrogen-oxygen ratio.
The temperature resistance curves of the films obtained in the examples 1 to 3 and the comparative examples 1 to 2 are shown in fig. 5, and it can be seen that the transition temperature of the metal insulator of the vanadium dioxide film is reduced by nitrogen doping, and the higher the doping concentration is, the more the phase transition temperature is reduced. In the volume ratio of nitrogen to oxygen of 1:1, a desired metal-insulator transition property can be obtained.
Comparative example 3
The comparative example differs from example 1 in that the ratio of oxygen and nitrogen varies during the deposition process. Specifically, during the deposition process, the flow ratio of nitrogen and oxygen to the chamber is changed instantaneously, the nitrogen ratio is reduced to 1,2min after the volume ratio of nitrogen to oxygen is 0.5.
The XRD contrast patterns of the films deposited in example 1 and comparative example 3 are shown in fig. 6, and the temperature resistance curves are shown in fig. 7, it can be seen that the nitrogen-oxygen gas ratio in comparative example 1 fluctuates, the obtained sample is not a single-phase structure, and the obtained film has poorer metal-insulator transition performance, specifically, the transition is not sharp, and the temperature range is more relaxed; exhibit a multi-segment transition; the switching ratio is decreased. Therefore, the fluctuation of the air pressure easily causes the uneven components of the film, and further the transformation performance of the metal insulator is greatly influenced.
In the epitaxial growth process of the single crystal substrate, the crystal structure and the lattice parameter of the single crystal substrate are the same as or similar to those of the epitaxial film, so that the high-quality single crystal epitaxial film can be obtained more easily. Titanium dioxide and vanadium dioxide both have rutile structures and are similar in structure, but the lattice parameters of the titanium dioxide and the vanadium dioxide are greatly different (the unit cell volume of the vanadium dioxide is smaller than that of the titanium dioxide), so that under normal conditions, vanadium dioxide single crystals can be epitaxially grown in the PLD technology, but the general crystal quality is poor. In the embodiment of the invention, nitrogen is doped, on one hand, nitrogen ions are slightly larger than cations to cause certain lattice expansion, and during epitaxial growth, lattice mismatch between the nitrogen ions and the substrate is reduced, so that the preparation of a high-quality single-crystal vanadium dioxide film is facilitated; on the other hand, nitrogen doping introduces hole carriers, inhibits V-V dimerization in the vanadium dioxide structure, plays a role in stabilizing a rutile phase, and is also favorable for maintaining high crystallization quality of the rutile phase.
The foregoing is a further detailed description of the invention in connection with specific preferred embodiments and it is not intended to limit the invention to the specific embodiments described. For those skilled in the art to which the invention pertains, numerous simple deductions or substitutions may be made without departing from the spirit of the invention, which shall be deemed to belong to the scope of the invention.
Claims (6)
1. A method for preparing an in-situ nitrogen-doped epitaxial oxide single crystal thin film is characterized by comprising the following steps: cleaning a substrate, placing the substrate in a cavity of pulse laser deposition equipment, introducing a mixture of oxygen and nitrogen, performing pulse laser deposition on the substrate by using a pure target material of an oxide after the atmosphere in the cavity is uniform and stable, and annealing in the same atmosphere environment after deposition is completed.
2. The method for producing an in-situ nitrogen-doped epitaxial oxide single-crystal thin film according to claim 1, wherein: the condition parameters of the pulse laser deposition are as follows: the temperature is 380 to 420 ℃, the total air pressure in the cavity is 15 to 25mTorr, and the laser energy density is 1.0 to 1.2J/cm 2 And the pulse frequency is 10 Hz.
3. The method for producing an in-situ nitrogen-doped epitaxial oxide single-crystal thin film according to claim 2, characterized in that: the condition parameters of the pulse laser deposition are as follows: the temperature is 400 ℃, the total air pressure in the cavity is 20 mTorr, and the laser energy density is 1.1J/cm 2 And the pulse frequency is 10 Hz.
4. The method for producing an in-situ nitrogen-doped epitaxial oxide single-crystal thin film according to claim 3, wherein: and after the deposition is finished, keeping the temperature for 5 min in the original epitaxial atmosphere environment, and then annealing.
5. The method for preparing an in-situ nitrogen-doped epitaxial oxide single crystal film according to any one of claims 1 to 4, wherein: and introducing a mixture of oxygen and nitrogen, wherein the volume ratio of the oxygen to the nitrogen is 1.
6. The method for producing an in-situ nitrogen-doped epitaxial oxide single-crystal thin film according to claim 5, wherein: the oxide is vanadium dioxide, and the substrate is made of titanium dioxide.
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