CN111893569A - Vanadium dioxide crystal with good appearance and strong crystallinity, and preparation and application thereof - Google Patents

Vanadium dioxide crystal with good appearance and strong crystallinity, and preparation and application thereof Download PDF

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CN111893569A
CN111893569A CN202010668883.9A CN202010668883A CN111893569A CN 111893569 A CN111893569 A CN 111893569A CN 202010668883 A CN202010668883 A CN 202010668883A CN 111893569 A CN111893569 A CN 111893569A
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container
crucible
crystal
good appearance
placing
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CN111893569B (en
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谢伟广
曾文
陈楠
张宇靖
赖浩杰
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Jinan University
University of Jinan
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—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
    • C30B1/00—Single-crystal growth directly from the solid state
    • C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing

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Abstract

The invention belongs to the technical field of crystal materials, and discloses VO with good appearance and strong crystallinity2Crystal and preparation method and application thereof. The invention adopts an improved CVD method to prepare VO2The crystal specifically comprises the following steps: (1) will V2O5The powder is dissolved in water to give V2O5Adding the precursor solution into a container, drying to obtain V at the bottom of the container2O5The precursor is used as an evaporation source; (2) placing the substrate over the container, and then placing the substrate and the container with V2O5The container of the precursor is placed in a heat treatment furnace together, vacuumized and subjected to heat treatment to obtain VO with good appearance and strong crystallinity2And (4) crystals. The preparation method has the advantages of simple process, low temperature, high repeatability, high utilization rate of raw materials and prepared VO2The crystal has the advantages of good appearance, smooth surface, strong crystallinity, good growth orientation, single phase and the like, and has good application prospect in the field of microelectronic devices.

Description

Vanadium dioxide crystal with good appearance and strong crystallinity, and preparation and application thereof
Technical Field
The invention belongs to the technical field of crystal materials, and particularly relates to vanadium dioxide (VO) with good appearance and strong crystallinity2) Crystal and preparation method and application thereof.
Background
Vanadium dioxide (VO)2) The transformation from a monoclinic structure to a rutile phase structure occurs at 68 ℃, and the unique metal-insulator transition characteristic (MIT) is accompanied by the sudden change of various properties such as electricity, mechanics, magnetism, optics and the like, so that the metal-insulator transition material has wide application prospect. VO (vacuum vapor volume)2Thin film materials have been the focus of research for a long time, and in recent years, electronic devices are developed toward miniaturization, so that low-dimensional nanomaterials are more and more emphasized.
Since Guiton et al used Chemical Vapor Deposition (CVD) to grow well-defined nanowires, one-dimensional single crystal VO was started2Research on nano materials develops VO in the field of nano materials2The phase transformation mechanism and the structural performance are deeply researched. Meanwhile, the surface effect and the quantum size effect of the one-dimensional material also make VO2Has excellent performance and is beneficial to VO2The application in the field of microelectronic devices.
Preparation of VO2The methods of the nano material include a vapor deposition method, a hydrothermal method, a sol-gel method, a thermal reduction method and the like. The solution preparation method is easy to realize to VO2Doping different ions, but obtaining VO with regular appearance and high quality is difficult2. Although VO with single phase and good crystallinity can be realized by the CVD growth method2The preparation of the nano material, however, requires the simultaneous control of the gas flow and partial pressure of various auxiliary gases (such as oxygen, argon, etc.), and the position of the substrate, which causes the problems of complicated operation and poor repeatability. In addition, VO is prepared by the current CVD method2The nano-crystal needs a large amount of precursor as a reaction source, causes the waste of raw materials, and utilizes VO2The powder is used as a precursor, and the reaction temperature is too high (over 1000 ℃). How to prepare VO with regular appearance, good crystallinity and excellent performance on the premise of simple and convenient operation and reasonable cost2The crystal material, which ensures the repeatability at the same time, is the current preparation of high-quality VO2A great problem with crystalline materials.
Disclosure of Invention
In order to overcome the defects of the prior art and solve the problem of high-quality VO at present2The problems of harsh preparation conditions, low raw material utilization rate, difficulty in ensuring regular morphology, low repeatability and the like in the preparation of nano materials are solved, and the invention aims to provide the VO with good morphology and strong crystallinity2A method for preparing the crystal.
The invention also aims to provide VO with good appearance and strong crystallinity obtained by the preparation method2And (4) crystals.
It is still another object of the present invention to provide the VO having good morphology and strong crystallinity2Use of the crystals.
In order to achieve the purpose, the invention adopts the following technical scheme:
VO with good appearance and strong crystallinity2A method for preparing a crystal comprising the steps of:
(1) will V2O5The powder is dissolved in water to give V2O5Adding the precursor solution into a container, drying to obtain V at the bottom of the container2O5The precursor is used as an evaporation source.
(2) Placing the substrate over the container, and then placing the substrate and the container with V2O5The container of the precursor is placed in a heat treatment furnace together, vacuumized and subjected to heat treatment to obtain monocrystal VO with good appearance and strong crystallinity2And (4) crystals.
In the step (1), the V2O5The concentration of the precursor solution is 0.015 to 0.045g/mL, preferably 0.015 g/mL.
In the step (1), the V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 15-35 μ L/cm2(ii) a Preferably 25. mu.L/cm2。
In the step (1), the V2O5The powder purity is preferably higher than 99.5%.
In the step (1), the V is2O5Dissolving the powder in water, preferably V2O5The powder was added to water and stirred until dissolved. The stirring can be performed by normal-temperature magnetic stirring at the rotation speed of 1000-1500 rpm; preferably 1500 revolutions per minute.
In step (1), preferably, the container may be made of quartz, alumina, Si, SiO2And the like.
The container is preferably a small circular crucible, the diameter of the small circular crucible is 5-8mm, and the depth of the small circular crucible is 5-10 mm; preferably a small crucible of 5mm diameter and 6mm depth.
Further, in order to grow VO in batch2The container can be prepared into small circular crucibles in an array, the diameter of each small circular crucible is 5-8mm, and the depth of each small circular crucible is 5-10 mm; preferably, the crucible has a diameter of 5mm and a depth of 6 mm. The number of crucibles may be determined according to the inner space of the heat treatment furnace, and the container may be composed of a 4 x 4 array of circular crucibles, for example, a quartz tube furnace having a diameter of 50 mm.
In the step (1), the drying can be heating drying or natural drying; preferably, the mixture is heated and dried at a constant temperature of 80 ℃.
In the step (2), the heat treatment furnace can be a tube furnace, a bell-type furnace and other common heat treatment instruments.
In the step (2), the top surface of the container is completely attached to the polished surface of the substrate; preferably, the inner bottom of the container is spaced from the substrate polishing surface by 5 to 10mm, preferably 6 mm.
In the step (2), the substrate can be any one of a sapphire substrate, a quartz substrate and the like, preferably the sapphire substrate is used, which is beneficial to VO2During growth, the growth is selected to be preferred. The polishing surface of the substrate is opposite the container.
Preferably, the substrate can be cleaned before use; the cleaning can comprise the following specific steps: the substrate was placed in ethanol and sonicated for 30 minutes, and this step was repeated as necessary.
In the step (2), the vacuum condition is 3-8Pa, and preferably 5 Pa.
In the step (2), the heating rate of the heat treatment is 10-20 ℃/min, preferably 15 ℃/min.
In the step (2), the temperature of the heat treatment is 750-1000 ℃, and is preferably 800 ℃; the constant temperature duration of the heat treatment is 60-300min, preferably 240 min.
The invention adopts an improved CVD method to prepare VO2Crystals, VO obtained by preparation2The crystal has good appearance, smooth surface, single phase and strong crystallinity, and has good application prospect in the field of microelectronic devices.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. in the preparation method provided by the invention, V2O5The precursor solution has simple preparation process, only needs water as a solvent, has low cost, and is safer and more environment-friendly; at the same time V2O5The precursor escapes from the bottom of the heating container in the form of gas molecules under the action of high temperature and is directly deposited on the substrate, and V can be utilized to the maximum extent2O5The precursor further reduces the production cost. In addition, the special array crucible is adopted, the batch preparation can be realized, and the industrial VO realization is facilitated2Large-scale production of crystals.
2. VO with good appearance and strong crystallinity provided by the invention2The preparation method of the crystal adopts a strategy of solution-assisted solid-phase high-temperature reduction to carry out single-crystal VO2The preparation of the crystal overcomes the defect that the solution method is difficult to prepare VO with regular appearance2The nano material and the gas phase deposition method have the difficulties of higher material temperature and lower yield; compared with the existing CVD growth method, the method overcomes the defects of low utilization rate of raw materials, harsh conditions, low repeatability and the like.
3. The preparation method of the invention not only has the characteristics of simple preparation process, lower temperature and high repeatability, but also prepares the VO2The crystal has the advantages of good appearance, smooth surface, strong crystallinity, good growth orientation, single phase and the like.
Drawings
FIG. 1 is a diagram of the preparation of single crystal VO in the present invention2Process schematic of the crystal.
FIG. 2 shows a single crystal VO prepared in example 1 of the present invention2Physical picture of crystal.
FIG. 3 shows a single crystal VO prepared in example 1 of the present invention2XRD pattern of the crystal.
FIG. 4 shows a single crystal VO prepared in example 1 of the present invention2AFM characterization of the crystal.
FIG. 5 is a diagram showing the batch preparation of VO according to the present invention2The design of the array circular crucible of the crystal is shown in the specification, wherein A is a three-dimensional schematic diagram, and B is a top view.
FIG. 6 is a physical representation of the product prepared in comparative example 1 of the present invention.
FIG. 7 is a physical representation of the product prepared in comparative example 2 of the present invention.
FIG. 8 is a physical representation of the product prepared in comparative example 3 of the present invention.
FIG. 9 is a physical representation of the product prepared in comparative example 4 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples and drawings, but the present invention is not limited thereto. All the raw materials and reagents used in the present invention are commercially available raw materials and reagents, unless otherwise specified. For process parameters not specifically noted, reference may be made to conventional techniques. In the examples, the components are used in g and mL in parts by mass.
Example 1: VO with good appearance and strong crystallinity2Preparation of crystals
The process schematic of the preparation method of the invention is shown in figure 1.
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On a small circular crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing a crucible on a quartz support plate, placing the crucible in a tube furnace for heat treatment, placing the quartz support plate in the center of a quartz tube of the tube furnace, tightly closing a valve at the gas inlet end of the quartz tube of the tube furnace, connecting the gas exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 15 ℃/min, and maintaining for 240 min; closing the tube furnace, and naturally cooling to room temperature to obtain the monocrystal VO with good appearance and strong crystallinity2And (4) crystals.
For the prepared monocrystal VO with good appearance and strong crystallinity2The crystal is subjected to morphology characterization tests, and the results are shown in figures 2-4.
Characterization of the single crystal VO prepared above with an optical microscope2The crystal morphology is shown in FIG. 2, and the obtained VO can be seen from FIG. 22The crystal has good appearance and smooth surface and is a flaky crystal;
adopting XRD to prepare VO with good appearance2As a result of phase analysis of the crystal, as shown in FIG. 3, it was found that all XRD diffraction peaks obtained were VO2And only the (011) and (022) crystal face diffraction peaks show that the VO prepared by the embodiment has excellent crystallinity2Single crystal, and grows along the (011) plane with good growth orientation.
Further AFM characterization is shown in FIG. 4, where the growing VO can be seen2The crystals appeared smooth with no obvious defects and had a thickness of about 170 nm.
Example 2: VO with good appearance and strong crystallinity2Preparation of crystals
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 1.5 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.03g/mL of V2O5A precursor solution.
And (3) selecting a quartz substrate, immersing the quartz substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 15 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On the small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 8 mm; placing the small crucible on a quartz support plate, placing the small crucible in a tube furnace for heat treatment, placing the quartz support plate in the middle of a quartz tube of the tube furnace, tightly closing a valve at the air inlet end of the quartz tube of the tube furnace, connecting the air exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 15 ℃/min, and maintaining for 240 min; closing the tube furnace, and naturally cooling to room temperature to obtain the monocrystal VO with good appearance and strong crystallinity2And (4) crystals.
Example 3: VO with good appearance and strong crystallinity2Preparation of crystals
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5The powder was mixed with 1 part by volume of water and stirred at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.045g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 35 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On the small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 10 mm; placing the small crucible on a quartz support plate, placing the small crucible in a tube furnace for heat treatment, placing the quartz support plate in the middle of a quartz tube of the tube furnace, tightly closing a valve at the air inlet end of the quartz tube of the tube furnace, connecting the air exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 15 ℃/min, and maintaining for 240 min; closing the tube furnace, and naturally cooling to room temperature to obtain the monocrystal VO with good appearance and strong crystallinity2And (4) crystals.
Example 4: VO with good appearance and strong crystallinity2Preparation of crystals
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On the small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing the small crucible on a quartz support plate, placing the small crucible in a tube furnace for heat treatment, placing the quartz support plate in the middle of a quartz tube of the tube furnace, tightly closing a valve at the air inlet end of the quartz tube of the tube furnace, connecting the air exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 3Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 15 ℃/min, and maintaining for 240 min; closing the tube furnace, and naturally cooling to room temperature to obtain the monocrystal VO with good appearance and strong crystallinity2And (4) crystals.
Example 5: VO with good appearance and strong crystallinity2Preparation of crystals
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On the small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing the small crucible on a quartz support plate, placing the small crucible in a tube furnace for heat treatment, placing the quartz support plate in the middle of a quartz tube of the tube furnace, tightly closing a valve at the air inlet end of the quartz tube of the tube furnace, connecting the air exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 8Pa, the heat treatment is ready to be started, and the tube furnace is arranged at the speed of 15 ℃/minHeating to 800 deg.C, and maintaining for 240 min; closing the tube furnace, and naturally cooling to room temperature to obtain the monocrystal VO with good appearance and strong crystallinity2And (4) crystals.
Example 6: VO with good appearance and strong crystallinity2Preparation of crystals
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On the small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing the small crucible on a quartz support plate, placing the small crucible in a tube furnace for heat treatment, placing the quartz support plate in the middle of a quartz tube of the tube furnace, tightly closing a valve at the air inlet end of the quartz tube of the tube furnace, connecting the air exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 10 ℃/min, and maintaining for 240 min; closing the tube furnace, and naturally cooling to room temperature to obtain the monocrystal VO with good appearance and strong crystallinity2And (4) crystals.
Example 7: VO with good appearance and strong crystallinity2Preparation of crystals
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On the small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing the small crucible on a quartz support plate, placing the small crucible in a tube furnace for heat treatment, placing the quartz support plate in the middle of a quartz tube of the tube furnace, tightly closing a valve at the air inlet end of the quartz tube of the tube furnace, connecting the air exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 20 ℃/min, and maintaining for 240 min; closing the tube furnace, and naturally cooling to room temperature to obtain the monocrystal VO with good appearance and strong crystallinity2And (4) crystals.
Example 8: VO with good appearance and strong crystallinity2Preparation of crystals
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5Powder precursor as vaporAnd (4) originating.
Step (2): placing the sapphire substrate in a chamber containing V2O5On the small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing the small crucible on a quartz support plate, placing the small crucible in a tube furnace for heat treatment, placing the quartz support plate in the middle of a quartz tube of the tube furnace, tightly closing a valve at the air inlet end of the quartz tube of the tube furnace, connecting the air exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 900 ℃ at the speed of 15 ℃/min, and maintaining for 240 min; closing the tube furnace, and naturally cooling to room temperature to obtain the monocrystal VO with good appearance and strong crystallinity2And (4) crystals.
Example 9: VO with good appearance and strong crystallinity2Preparation of crystals
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On the small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing a small crucible on a quartz support plate, placing the small crucible into a tube furnace for heat treatment, placing the quartz support plate in the center of a quartz tube of the tube furnace, tightly closing a valve at the air inlet end of the quartz tube of the tube furnace, connecting the air exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tubeEmpty; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 1000 ℃ at the speed of 15 ℃/min, and maintaining for 240 min; closing the tube furnace, and naturally cooling to room temperature to obtain the monocrystal VO with good appearance and strong crystallinity2And (4) crystals.
Example 10: VO with good appearance and strong crystallinity2Preparation of crystals
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5Precursor solution, as shown in fig. 1.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On the small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing the small crucible on a quartz support plate, placing the small crucible in a tube furnace for heat treatment, placing the quartz support plate in the middle of a quartz tube of the tube furnace, tightly closing a valve at the air inlet end of the quartz tube of the tube furnace, connecting the air exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 15 ℃/min, and maintaining for 60 min; closing the tube furnace, and naturally cooling to room temperature to obtain the monocrystal VO with good appearance and strong crystallinity2Crystal
Example 11: VO with good appearance and strong crystallinity2Preparation of crystals
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Powder, adding 3 parts by volumeStirring the water (2) for 48 hours at 1500 rpm on a magnetic stirrer to obtain 0.015g/mL of V2O5Precursor solution, as shown in fig. 1.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On the small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing the small crucible on a quartz support plate, placing the small crucible in a tube furnace for heat treatment, placing the quartz support plate in the middle of a quartz tube of the tube furnace, tightly closing a valve at the air inlet end of the quartz tube of the tube furnace, connecting the air exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 15 ℃/min, and maintaining for 300 min; closing the tube furnace, and naturally cooling to room temperature to obtain the monocrystal VO with good appearance and strong crystallinity2Crystal
Example 12: VO with good appearance and strong crystallinity2Bulk preparation of crystals
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5The precursor solution was added to a 4X 4 array of small circular crucibles (see FIG. 5), V2O5The ratio of the amount of precursor solution to the inner bottom area of the containerIs 25 mu L/cm2Heating and drying at constant temperature of 80 ℃ to obtain a certain amount of V on a small crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing 16 pieces of 10 × 10mm sapphire substrate in a chamber containing V2O5On a 4 multiplied by 4 array circular small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; directly placing the small 4X 4 array circular crucibles into a tube furnace for heat treatment, placing the small 4X 4 array circular crucibles into the center of a quartz tube of the tube furnace, tightly closing a valve at the air inlet end of the quartz tube of the tube furnace, connecting the air exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 15 ℃/min, and maintaining for 240 min; closing the tube furnace, naturally cooling to room temperature, and obtaining the monocrystal VO with good appearance and strong crystallinity in batches2And (4) crystals.
Comparative example 1: v2O5Adding excess precursor solution
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 40 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On a small circular crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing the crucible on a quartz carrier plate, placing the crucible into a tube furnace for heat treatment, and placing the crucible into the tube furnace for heat treatmentThe quartz support plate is placed in the right center of the quartz tube of the tube furnace, the valve at the air inlet end of the quartz tube of the tube furnace is tightly closed, and the air exhaust end of the quartz tube is connected with a common mechanical pump to vacuumize the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 15 ℃/min, and maintaining for 240 min; closing the tube furnace, naturally cooling to room temperature to obtain VO with disordered appearance and stacked mutually as shown in figure 62And (4) crystals.
Comparative example 2: excessive heat treatment temperature
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On a small circular crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing a crucible on a quartz support plate, placing the crucible in a tube furnace for heat treatment, placing the quartz support plate in the center of a quartz tube of the tube furnace, tightly closing a valve at the gas inlet end of the quartz tube of the tube furnace, connecting the gas exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 1100 ℃ at the speed of 15 ℃/min, and maintaining for 240 min; closing the tube furnace, naturally cooling to room temperature to obtain block VO with disordered appearance, mutual stacking and large thickness as shown in figure 72And (4) crystals.
Comparative example 3: evaporation source is too far away from the substrate
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On a round small crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 10 mm; placing a crucible on a quartz support plate, placing the crucible in a tube furnace for heat treatment, placing the quartz support plate in the center of a quartz tube of the tube furnace, tightly closing a valve at the gas inlet end of the quartz tube of the tube furnace, connecting the gas exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 15 ℃/min, and maintaining for 240 min; closing the tube furnace, naturally cooling to room temperature to obtain VO with irregular shape as shown in figure 82And (4) crystals.
Comparative example 4: too short a heat treatment time
Step (1): 0.045 part by mass of V with a purity of 99.5 percent is weighed2O5Adding 3 volume parts of water into the powder, and stirring at 1500 rpm for 48 hours on a magnetic stirrer to obtain 0.015g/mL of V2O5A precursor solution.
And (3) selecting a sapphire substrate, immersing the sapphire substrate in alcohol, carrying out ultrasonic treatment for 30 minutes, repeating the operation steps for 3 times, and drying.
Handle V2O5Adding the precursor solution into a small circular crucible, V2O5Dosage and container of precursor solutionThe ratio of the inner bottom area is 25 mu L/cm2Heating and drying at a constant temperature of 80 ℃ to obtain a certain amount of V on a crucible2O5The powder precursor is used as an evaporation source.
Step (2): placing the sapphire substrate in a chamber containing V2O5On a small circular crucible of the precursor, the top surface of the small crucible is completely attached to the polished surface of the sapphire substrate, and the distance between the bottom in the crucible and the polished surface of the substrate is 5 mm; placing a crucible on a quartz support plate, placing the crucible in a tube furnace for heat treatment, placing the quartz support plate in the center of a quartz tube of the tube furnace, tightly closing a valve at the gas inlet end of the quartz tube of the tube furnace, connecting the gas exhaust end of the quartz tube with a common mechanical pump, and vacuumizing the quartz tube; when the vacuum index is 5Pa, preparing to start heat treatment, heating the tube furnace to 800 ℃ at the speed of 15 ℃/min, and maintaining for 40 min; the tube furnace was closed and naturally cooled to room temperature to obtain the unshaped, uncrystallized vanadium oxide shown in FIG. 9.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. VO with good appearance and strong crystallinity2A method for producing a crystal, characterized by comprising the steps of:
(1) will V2O5The powder is dissolved in water to give V2O5Adding the precursor solution into a container, drying to obtain V at the bottom of the container2O5The precursor is used as an evaporation source;
(2) placing the substrate over the container, and then placing the substrate and the container with V2O5The container of the precursor is placed in a heat treatment furnace together, vacuumized and subjected to heat treatment to obtain monocrystal VO with good appearance and strong crystallinity2And (4) crystals.
2. The topographically well defined of claim 1VO having high crystallinity2A method for producing a crystal, characterized by: in the step (1), the V2O5The concentration of the precursor solution is 0.015-0.045 g/mL.
3. VO with good appearance and strong crystallinity according to claim 12A method for producing a crystal, characterized by: in the step (1), the V2O5The ratio of the amount of the precursor solution to the inner bottom area of the container is 15-35 μ L/cm2。
4. VO with good appearance and strong crystallinity according to claim 12A method for producing a crystal, characterized by: the container is made of quartz, alumina, Si and SiO2Is prepared by one of the following steps; in the step (2), the substrate is one of a sapphire substrate and a quartz substrate.
5. VO with good appearance and strong crystallinity according to claim 12A method for producing a crystal, characterized by: in the step (2), the top surface of the container is attached to the polished surface of the substrate; the distance between the bottom in the container and the substrate is 5-10 mm.
6. VO with good appearance and strong crystallinity according to claim 12A method for producing a crystal, characterized by: in the step (2), the vacuum condition is 3-8 Pa.
7. VO with good appearance and strong crystallinity according to claim 12A method for producing a crystal, characterized by: in the step (2), the heating rate of the heat treatment is 10-20 ℃/min.
8. VO with good appearance and strong crystallinity according to claim 12A method for producing a crystal, characterized by: in the step (2), the temperature of the heat treatment is 750-1000 ℃; the constant temperature duration of the heat treatment is 60-300 min.
9. VO with good appearance and strong crystallinity2Crystals, characterized by being prepared by the process according to any one of claims 1 to 8.
10. VO according to claim 92The crystal is applied in the field of microelectronic devices.
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CN106637404A (en) * 2016-12-06 2017-05-10 东华理工大学 Method for growing large-area mono-crystal vanadium dioxide thin film by utilizing tubular furnace
CN111392685A (en) * 2020-03-05 2020-07-10 华中科技大学 Two-dimensional self-assembled M1/M2-VO2Homojunction nanosheet and preparation method thereof

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