CN110240198B - Preparation method of single crystal potassium tantalate film - Google Patents
Preparation method of single crystal potassium tantalate film Download PDFInfo
- Publication number
- CN110240198B CN110240198B CN201910561077.9A CN201910561077A CN110240198B CN 110240198 B CN110240198 B CN 110240198B CN 201910561077 A CN201910561077 A CN 201910561077A CN 110240198 B CN110240198 B CN 110240198B
- Authority
- CN
- China
- Prior art keywords
- reaction kettle
- single crystal
- reaction
- niobium
- substrate
- 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
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation method of a single crystal potassium tantalate film. The method comprises the steps of taking tantalum pentoxide and potassium hydroxide as main raw materials, taking the potassium hydroxide as a mineralizer, stirring strongly at room temperature, adding a niobium-doped strontium titanate substrate, and carrying out hydrothermal treatment at high temperature to obtain the single crystal potassium tantalate film. The niobium-doped strontium titanate substrate is a single-polished single crystal substrate and has the orientation of (001). The invention adopts a hydrothermal method to prepare the single crystal potassium tantalate film for the first time. The preparation method has the advantages of simple process, easy control, no pollution, low cost and easy large-scale production; the prepared product is a high-quality large-area single crystal film, forms a high-quality heterojunction interface with the substrate, and has wide potential application prospect in the fields of information storage, spin electronic devices, sensors and the like.
Description
Technical Field
The invention relates to a preparation method of a single crystal potassium tantalate film, and belongs to the field of functional material preparation.
Background
KTaO3The crystal has larger refractive index and dielectric constant, lower dielectric loss, wider light-transmitting wave band and KTaO3The crystal is mainly applied to digital deflectors, adjustable microwave devices and various integrated optical windows. Further, KTaO3The crystal also has a more obvious secondary electro-optic effect and has certain application in laser modulators. However, the application of potassium tantalate is limited because the curie temperature of potassium tantalate is low and it is not easy to grow large-size single crystal thin film at low cost.
Meanwhile, transistors, lasers and solar cells all utilize the phenomenon of a heterogeneous interface, and oxide heterojunctions, particularly perovskite oxide heterojunctions, are one of the hot researches in the field of material science research. For example, interfacial two-dimensional electron gas, ferromagnetic properties found in strontium titanate/lanthanum aluminate (STO/LAO) systems have attracted considerable attention by researchers. However, the existing method for preparing the oxide heterojunction, especially the heterojunction with the atomic-scale flat interface, mainly comprises oxide molecular beam epitaxy and pulsed laser deposition, has complex equipment, high price and strict experimental condition requirements, so that the search for a simple, effective and high-yield method for preparing the oxide heterojunction is extremely important and urgent for actual production and scientific research.
The invention firstly adopts a hydrothermal method to epitaxially grow a high-quality single-crystal potassium tantalate film on the exposed surface of the niobium-doped strontium titanate substrate (100), and can obtain an atomically flat interface. The method has the advantages of simple process, easy control, no pollution, low cost and easy large-scale production.
Disclosure of Invention
The invention aims to provide a preparation method of a single crystal potassium tantalate film, which has the advantages of low cost, simple process and easy control of the process and can obtain a high-quality heterojunction interface.
The invention is realized by adopting the following technical scheme:
a preparation method of a single crystal potassium tantalate film comprises the following steps:
1) dissolving potassium hydroxide in a liner of a reaction kettle filled with deionized water, and fully stirring to obtain a potassium hydroxide solution with the molar concentration of 6-10 mol/L;
2) adding 0.5-5mmol of tantalum pentoxide into the sodium hydroxide aqueous solution prepared in the step 1) under the stirring state, adjusting the volume of reaction materials in the inner container of the reaction kettle to 70% -80% of the volume of the inner container of the reaction kettle by using deionized water, and stirring for 2-3h to obtain a suspension of a reaction precursor;
3) ultrasonically treating the single-crystal niobium-doped strontium titanate substrate in acetone, ethanol, deionized water and ethanol in sequence for at least 10min, drying at 60-80 ℃, vertically placing the dried niobium-doped strontium titanate substrate in a reaction kettle liner filled with suspension of a reaction precursor in the step 2), and enabling the distance between the niobium-doped strontium titanate substrate and the bottom of the reaction kettle liner to be 1-2 cm;
4) and (3) placing the inner container of the reaction kettle in the step 3) into the reaction kettle, sealing, preserving at 140-200 ℃ for 2-24 h for hydrothermal treatment, naturally cooling the reaction kettle to room temperature, unloading the kettle, washing a reaction product by deionized water and absolute ethyl alcohol, filtering, and drying to obtain the single crystal potassium tantalate film.
In the above technical scheme, further, the reaction kettle is a polytetrafluoroethylene inner container and a stainless steel sleeve closed reaction kettle, and the substrate is placed on a polytetrafluoroethylene frame.
Furthermore, the purity of the tantalum pentoxide is not lower than 99.99%, and the purity of the potassium hydroxide is not lower than chemical purity.
Further, the niobium-doped strontium titanate substrate is a single-polished single crystal substrate and has the orientation of (001).
Furthermore, the thickness of the prepared potassium tantalate film is 20-300 nm.
The invention has the beneficial effects that:
according to the invention, the potassium tantalate film is prepared by a hydrothermal method under the condition that only tantalum pentoxide and potassium hydroxide are used as raw materials. The hydrothermal method can realize the synthesis of potassium tantalate with the stoichiometry maintained at a lower temperature, and meanwhile, the reaction environment is a liquid phase, so that the uniform nucleation and diffusion of crystallization reaction are facilitated, and the crystallization performance of the product is good. In the preparation method, the hydrothermal method is completely adopted for one-step growth of potassium tantalate crystals for the first time, and the niobium-doped strontium titanate (Nb-SrTiO) is introduced3) The conductive substrate regulates and controls the growth of potassium tantalate crystals through the combined action of charge transfer of an interface and heterogeneous nucleation. The method can prepare the high-quality large-area monocrystal potassium tantalate film in the hydrothermal environment and form a high-quality heterojunction interface with the substrate. The invention has simple process, easy control, no pollution, low cost and easy production.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a single crystal potassium tantalate thin film produced in accordance with the present invention;
FIG. 2 is an X-ray diffraction pattern (XRD) of a single crystal potassium tantalate film prepared in accordance with the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) image of a cross section of a single crystal potassium tantalate thin film produced in accordance with the present invention.
Detailed Description
The technical scheme of the invention is further illustrated by the following specific examples.
Example 1
1) Dissolving potassium hydroxide with certain mass in deionized water, and fully stirring to obtain a potassium hydroxide solution with the molar concentration of 6 mol/L;
2) under the stirring state, adding 1mmol of tantalum pentoxide into the sodium hydroxide aqueous solution prepared in the step 1), adjusting the volume of reaction materials in the inner container of the reaction kettle to 80% of the volume of the inner container of the reaction kettle by using deionized water, stirring for 2h to obtain a suspension of a reaction precursor, and placing the suspension in the inner container of polytetrafluoroethylene;
3) carrying out ultrasonic treatment on a single-crystal niobium-doped strontium titanate substrate in acetone, ethanol, deionized water and ethanol for 10min in sequence, drying at 60 ℃, and vertically placing the dried niobium-doped strontium titanate substrate at a position 1cm away from the bottom of a liner of a reaction kettle;
4) and (3) placing the inner container of the reaction kettle, which is provided with the reaction materials and the substrate in the step 3), in the reaction kettle, sealing, storing at 200 ℃ for 12h for hydrothermal treatment, naturally cooling the reaction kettle to room temperature, unloading the kettle, repeatedly washing a reaction product by using deionized water and absolute ethyl alcohol, filtering, and drying to obtain the single crystal potassium tantalate film.
Example 2
1) Dissolving potassium hydroxide with certain mass in deionized water, and fully stirring to obtain a potassium hydroxide solution with the molar concentration of 8 mol/L;
2) under the stirring state, adding 1mmol of tantalum pentoxide into the sodium hydroxide aqueous solution prepared in the step 1), adjusting the volume of reaction materials in the inner container of the reaction kettle to 80% of the volume of the inner container of the reaction kettle by using deionized water, stirring for 2h to obtain a suspension of a reaction precursor, and placing the suspension in the inner container of polytetrafluoroethylene;
3) carrying out ultrasonic treatment on a single-crystal niobium-doped strontium titanate substrate in acetone, ethanol, deionized water and ethanol for 10min in sequence, drying at 60 ℃, and vertically placing the dried niobium-doped strontium titanate substrate at a position 1cm away from the bottom of a liner of a reaction kettle;
4) and (3) placing the inner container of the reaction kettle, which is provided with the reaction materials and the substrate in the step 3), in the reaction kettle, sealing, storing at 200 ℃ for 12h for hydrothermal treatment, naturally cooling the reaction kettle to room temperature, unloading the kettle, repeatedly washing a reaction product by using deionized water and absolute ethyl alcohol, filtering, and drying to obtain the single crystal potassium tantalate film.
Example 3
1) Dissolving potassium hydroxide with certain mass in deionized water, and fully stirring to obtain a potassium hydroxide solution with the molar concentration of 8 mol/L;
2) under the stirring state, adding 1mmol of tantalum pentoxide into the sodium hydroxide aqueous solution prepared in the step 1), adjusting the volume of reaction materials in the inner container of the reaction kettle to 80% of the volume of the inner container of the reaction kettle by using deionized water, stirring for 2h to obtain a suspension of a reaction precursor, and placing the suspension in the inner container of polytetrafluoroethylene;
3) carrying out ultrasonic treatment on a single-crystal niobium-doped strontium titanate substrate in acetone, ethanol, deionized water and ethanol for 10min in sequence, drying at 60 ℃, and vertically placing the dried niobium-doped strontium titanate substrate at a position 1cm away from the bottom of a liner of a reaction kettle;
4) and (3) placing the inner container of the reaction kettle, which is provided with the reaction materials and the substrate in the step 3), in the reaction kettle, sealing, preserving at 200 ℃ for 8 hours for hydrothermal treatment, naturally cooling the reaction kettle to room temperature, unloading the kettle, repeatedly washing a reaction product by deionized water and absolute ethyl alcohol, filtering, and drying to obtain the single crystal potassium tantalate film.
Example 4
1) Dissolving potassium hydroxide with certain mass in deionized water, and fully stirring to obtain a potassium hydroxide solution with the molar concentration of 10 mol/L;
2) under the stirring state, adding 5mmol of tantalum pentoxide into the sodium hydroxide aqueous solution prepared in the step 1), adjusting the volume of reaction materials in the inner container of the reaction kettle to 70% of the volume of the inner container of the reaction kettle by using deionized water, stirring for 3h to obtain a suspension of a reaction precursor, and placing the suspension in the inner container of polytetrafluoroethylene;
3) carrying out ultrasonic treatment on a single-crystal niobium-doped strontium titanate substrate in acetone, ethanol, deionized water and ethanol for 10min in sequence, drying at 80 ℃, and vertically placing the dried niobium-doped strontium titanate substrate at a position 1cm away from the bottom of a liner of a reaction kettle;
4) and (3) placing the inner container of the reaction kettle, which is provided with the reaction materials and the substrate in the step 3), in the reaction kettle, sealing, storing at 200 ℃ for 12h for hydrothermal treatment, naturally cooling the reaction kettle to room temperature, unloading the kettle, repeatedly washing a reaction product by using deionized water and absolute ethyl alcohol, filtering, and drying to obtain the single crystal potassium tantalate film.
Example 5
1) Dissolving potassium hydroxide with certain mass in deionized water, and fully stirring to obtain a potassium hydroxide solution with the molar concentration of 6 mol/L;
2) under the stirring state, adding 0.5mmol of tantalum pentoxide into the sodium hydroxide aqueous solution prepared in the step 1), adjusting the volume of reaction materials in the inner container of the reaction kettle to 80% of the volume of the inner container of the reaction kettle by using deionized water, stirring for 2h to obtain a suspension of a reaction precursor, and placing the suspension in the inner container of polytetrafluoroethylene;
3) carrying out ultrasonic treatment on a single-crystal niobium-doped strontium titanate substrate in acetone, ethanol, deionized water and ethanol for 10min in sequence, drying at 60 ℃, and vertically placing the dried niobium-doped strontium titanate substrate at a position 1cm away from the bottom of a liner of a reaction kettle;
4) and (3) placing the inner container of the reaction kettle, which is provided with the reaction materials and the substrate in the step 3), in the reaction kettle, sealing, storing at 200 ℃ for 12h for hydrothermal treatment, naturally cooling the reaction kettle to room temperature, unloading the kettle, repeatedly washing a reaction product by using deionized water and absolute ethyl alcohol, filtering, and drying to obtain the single crystal potassium tantalate film.
As can be seen from fig. 1 and 2, the embodiment of the present invention successfully produces a single crystal potassium tantalate thin film, the potassium tantalate is grown on the oriented (001) strontium niobate-doped titanate substrate, and the orientation of the potassium tantalate is consistent with the orientation of the substrate, and the thin film has a flat surface; as can be seen from FIG. 3, the thickness of the single-crystal potassium tantalate film obtained by the present invention was 238 nm.
Claims (3)
1. The preparation method of the single crystal potassium tantalate film is characterized by comprising the following steps of:
1) dissolving potassium hydroxide in a liner of a reaction kettle filled with deionized water, and fully stirring to obtain a potassium hydroxide solution with the molar concentration of 6-8 mol/L;
2) under the stirring state, adding 1mmol of tantalum pentoxide into the potassium hydroxide aqueous solution prepared in the step 1), adjusting the volume of reaction materials in the inner container of the reaction kettle to 80% of the volume of the inner container of the reaction kettle by using deionized water, and stirring for 2h to obtain a suspension of a reaction precursor;
3) ultrasonically treating the single-crystal niobium-doped strontium titanate substrate in acetone, ethanol, deionized water and ethanol in sequence for at least 10min, drying at 60 ℃, vertically placing the dried niobium-doped strontium titanate substrate in a reaction kettle liner filled with suspension of a reaction precursor in the step 2), and enabling the distance between the niobium-doped strontium titanate substrate and the bottom of the reaction kettle liner to be 1 cm; the niobium-doped strontium titanate substrate is a single-polished single crystal substrate with the orientation of (001);
4) and (3) placing the inner container of the reaction kettle in the step 3) into the reaction kettle, sealing, preserving at 200 ℃ for 8-12 h for hydro-thermal treatment, naturally cooling the reaction kettle to room temperature, unloading the kettle, washing a reaction product by deionized water and absolute ethyl alcohol, filtering, and drying to obtain the single crystal potassium tantalate film.
2. The method for preparing the single-crystal potassium tantalate film of claim 1, wherein the reaction vessel is a polytetrafluoroethylene inner container and a stainless steel sleeve closed reaction vessel, and the niobium-doped strontium titanate substrate is placed on a polytetrafluoroethylene frame.
3. The method of claim 1, wherein the purity of said tantalum pentoxide is not less than 99.99% and the purity of said potassium hydroxide is not less than chemical purity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910561077.9A CN110240198B (en) | 2019-06-26 | 2019-06-26 | Preparation method of single crystal potassium tantalate film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910561077.9A CN110240198B (en) | 2019-06-26 | 2019-06-26 | Preparation method of single crystal potassium tantalate film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110240198A CN110240198A (en) | 2019-09-17 |
| CN110240198B true CN110240198B (en) | 2020-10-23 |
Family
ID=67889508
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910561077.9A Active CN110240198B (en) | 2019-06-26 | 2019-06-26 | Preparation method of single crystal potassium tantalate film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110240198B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602524A (en) * | 2009-07-07 | 2009-12-16 | 桂林理工大学 | A kind of hydrothermal synthesis method of potassium tantalite powder |
| CN109825873A (en) * | 2019-03-26 | 2019-05-31 | 浙江大学 | A kind of preparation method of monocrystalline bismuth ferrite thin film |
| CN109898137A (en) * | 2019-03-26 | 2019-06-18 | 浙江大学 | A kind of preparation method of sodium tantalate monocrystal thin films |
-
2019
- 2019-06-26 CN CN201910561077.9A patent/CN110240198B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602524A (en) * | 2009-07-07 | 2009-12-16 | 桂林理工大学 | A kind of hydrothermal synthesis method of potassium tantalite powder |
| CN109825873A (en) * | 2019-03-26 | 2019-05-31 | 浙江大学 | A kind of preparation method of monocrystalline bismuth ferrite thin film |
| CN109898137A (en) * | 2019-03-26 | 2019-06-18 | 浙江大学 | A kind of preparation method of sodium tantalate monocrystal thin films |
Non-Patent Citations (1)
| Title |
|---|
| La(1-x)SrxCrO3薄膜脉冲激光沉积制备及性能研究;胡万景;《中国优秀硕士学位论文全文数据库 基础科学辑》;20190115;第16-17页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110240198A (en) | 2019-09-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Vajargah et al. | Sol–gel derived ZnO thin films: effect of amino-additives | |
| CN109825873B (en) | Preparation method of single-crystal bismuth ferrite film | |
| CN105624782B (en) | A kind of preparation method of gallium oxide film | |
| CN102260046B (en) | Microwave synthesis method of zinc oxide film with oriented nanorod structure | |
| CN106986373A (en) | A kind of preparation method of ZnO nanorod | |
| Zhao et al. | Nucleation and growth of ZnO nanorods on the ZnO-coated seed surface by solution chemical method | |
| CN103253708B (en) | Solvothermal preparation method of niobium pentoxide nanowire by use of acetic acid | |
| CN110128134B (en) | Preparation method of lead titanate film with niobium-doped strontium titanate as substrate | |
| CN102050481A (en) | Method for preparing zinc oxide nano material | |
| CN112960660A (en) | Black phosphorus nanobelt material and preparation method thereof | |
| CN109913813B (en) | Epitaxial orientation lithium niobate thin film and preparation method thereof | |
| CN112750919B (en) | Perovskite nanowire heterojunction and preparation method thereof | |
| CN110240198B (en) | Preparation method of single crystal potassium tantalate film | |
| CN104628263A (en) | Method for preparing indium oxide octahedral nanocrystal film | |
| CN105236472A (en) | Preparation method of SnO2 nano-wire array | |
| CN112176394A (en) | Preparation method of lanthanum-doped bismuth ferrite single crystal film | |
| CN109594067B (en) | Method for preparing rutile phase titanium dioxide nanowire array growing in preferred orientation of (001) crystal face | |
| CN110230100B (en) | Preparation method of monocrystal potassium niobate film | |
| Wang et al. | Fabrication and morphology control of BaWO4 thin films by microwave assisted chemical bath deposition | |
| CN109879310A (en) | A kind of preparation method of single-crystal strontium titanate film | |
| CN1295752C (en) | Semiconductor substrate material of compound ZnO nano-line on silicon wafer and preparation method thereof | |
| Ievlev et al. | Synthesis of lithium niobate during crystallization of amorphous Li–Nb–O film | |
| CN101619484B (en) | Method for growing single crystal indium oxide film on conductive substrate | |
| CN111533170A (en) | Disk-shaped (K, Na) NbO prepared by two-step hydrothermal method3Crystal and method | |
| Yu et al. | Perpendicular branching in crystal growth of 3D architecture-tuned cadmium hydroxide arrays: from oriented tripods to faceted crystals |
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 |