CN111088477A - Preparation of VO2Method for making thin film - Google Patents

Preparation of VO2Method for making thin film Download PDF

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Publication number
CN111088477A
CN111088477A CN201811238298.4A CN201811238298A CN111088477A CN 111088477 A CN111088477 A CN 111088477A CN 201811238298 A CN201811238298 A CN 201811238298A CN 111088477 A CN111088477 A CN 111088477A
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substrate
film
atom beam
flow velocity
cleaning
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CN201811238298.4A
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不公告发明人
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Nantong An Art Design Co Ltd
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Nantong An Art Design Co Ltd
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Priority to CN201811238298.4A priority Critical patent/CN111088477A/en
Publication of CN111088477A publication Critical patent/CN111088477A/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a method for preparing VO2The film preparation method comprises the following steps: using ultrasonic cleaner to clean Al2O3Cleaning the surface of the substrate with deionized water, cleaning with an acetone solution and absolute ethyl alcohol in sequence, and drying; cleaning the Al2O3Transferring the single crystal substrate to a high vacuum growth chamber, and vacuumizing to make background pressure better than 1 × 10‑6Pa, rotating the substrate, heating the substrate to 610-630 ℃, after the metal vanadium powder is heated to an evaporation state, opening a gas activation source and introducing oxygen, spraying vanadium atom beams and active oxygen atom beams onto the substrate for reaction, wherein the film growth time is 34-36min, and after the film deposition is finished, introducing N2Naturally cooling the vacuum chamber to below 150 deg.C, and taking out. The prepared semi-transparent film has smooth surface and light yellow colorClear VO2The film has good crystallization, high purity, uniform and compact surface and good mid-infrared modulation characteristic.

Description

Preparation of VO2Method for making thin film
Technical Field
The invention relates to a method for preparing VO2A method of making a thin film.
Background
VO2The material is a functional material with phase change property, and the phase change temperature is close to room temperature and is about 68 ℃. At around the phase transition temperature, VO2The forbidden band width of the material will change, phase transition of the insulator-metal body occurs, various physical parameters of the material, such as refractive index, infrared transmittance, resistivity, etc., will change, and macroscopically show that the optical and electrical physical properties before and after phase transition are mutated, which is a current research hotspot. People can design the energy-saving glass for the green building for preventing high-temperature infrared rays by utilizing the characteristic that the infrared transmittance is greatly reduced before and after phase change, and can also be applied to the field of laser protection, and the research is based on VO2In the form of a film. VO has been reported2Film made ofThe preparation methods comprise a vacuum evaporation method, a magnetron sputtering method, a pulse laser deposition method and certain chemical methods, such as a sol-gel method and the like, and VO with phase change characteristics is successfully prepared through reports2However, the quality of the thin film is not ideal due to different principles of various methods and different process flows, which mainly reflects in that the crystallinity of the thin film and a substrate is not high, the uniformity and the compactness are not enough, the large-area growth cannot be realized, the components of the thin film are not pure, and the like. The current method capable of accurately controlling various parameters of film growth is a molecular beam epitaxy method, and VO with high quality can be prepared2And (3) epitaxial growth of a monocrystalline film. Due to Al2O3And VO2Good lattice matching relation, easy to use molecular beam epitaxy method to Al2O3Growing single crystal VO on substrate2A film. Further, Al2O3The film has good transmittance to visible light and infrared light, and satisfies VO2Practical application and optical property research of the film.
Disclosure of Invention
The invention aims to provide a method for preparing VO2A method of making a thin film.
The invention is realized by the following technical scheme:
preparation of VO2A method of making a film comprising the steps of: al by ultrasonic cleaner2O3Washing the surface of the substrate with deionized water for 25-35min, then washing with acetone solution and absolute ethyl alcohol for 20-30min, and finally taking out and drying with a blower; cleaning the Al2O3Transferring the single crystal substrate to a high vacuum growth chamber, and vacuumizing to make background pressure better than 1 × 10-6Rotating a substrate, heating the substrate to 610-630 ℃, after 10-20 parts of metal vanadium powder is heated to an evaporation state, opening a gas activation source and introducing oxygen, spraying a vanadium atom beam and an active oxygen atom beam onto the substrate for reaction, observing the digital change of a crystal oscillator film thickness instrument, controlling the flow velocity of the vanadium atom beam to be 1.2-1.4nm/min, and controlling the flow velocity of the oxygen atom beam to be 3.8-4.2cm by using a gas flowmeter3Min, the film growth time is 34-36min, and after the film deposition is finished, the residual oxygen is preventedContinuous oxidation of VO2Film, introducing protective gas N2Naturally cooling the vacuum chamber to below 150 ℃, and taking out to obtain the product; the raw materials are in parts by weight.
Preferably, in the method, the Al is cleaned by an ultrasonic cleaner2O3The substrate surface was rinsed with deionized water for 30 min.
Preferably, in the method, the washing is carried out for 25min by using an acetone solution and absolute ethyl alcohol sequentially.
Preferably, in the method, the substrate is heated to 620 ℃.
Preferably, in the method, the flow velocity of the vanadium atom beam is controlled to be 1.3 nm/min.
Preferably, in the method, the flow velocity of the oxygen atom beam is controlled to be 4.0cm by using a gas flowmeter3/min。
Preferably, in the method, the film growth time is 35 min.
The invention has the technical effects that:
the method is simple, convenient, fast and easy to operate, and the prepared VO has smooth surface and is light yellow and semitransparent2The film has good crystallization, high purity, uniform and compact surface and good mid-infrared modulation characteristic, and shows that VO is utilized2The film has certain feasibility for realizing the mid-infrared laser protection.
Detailed Description
The following describes the substance of the present invention with reference to the examples.
Example 1
Preparation of VO2A method of making a film comprising the steps of: al by ultrasonic cleaner2O3Cleaning the surface of the substrate with deionized water for 30min, cleaning with acetone solution and anhydrous ethanol for 25min, and blow-drying with a blower; cleaning the Al2O3Transferring the single crystal substrate to a high vacuum growth chamber, and vacuumizing to make background pressure better than 1 × 10-6Pa, rotating the substrate, heating the substrate to 620 ℃, after 15 parts of metal vanadium powder is heated to an evaporation state, opening a gas activation source and introducing oxygen, and adding vanadiumSpraying atomic beam and active oxygen atomic beam onto substrate for reaction, observing digital change of crystal oscillator film thickness meter, controlling flow velocity of vanadium atomic beam at 1.3nm/min, and controlling flow velocity of oxygen atomic beam at 4.0cm by gas flowmeter3Min, the film growth time is 35min, and after the film deposition is finished, VO is continuously oxidized for preventing residual oxygen2Film, introducing protective gas N2Naturally cooling the vacuum chamber to below 150 ℃, and taking out to obtain the product; the raw materials are in parts by weight.
Example 2
Preparation of VO2A method of making a film comprising the steps of: al by ultrasonic cleaner2O3Washing the surface of the substrate with deionized water for 25min, then washing with acetone solution and absolute ethyl alcohol for 20min, and finally taking out and drying with a blower; cleaning the Al2O3Transferring the single crystal substrate to a high vacuum growth chamber, and vacuumizing to make background pressure better than 1 × 10-6Pa, rotating the substrate, heating the substrate to 610 ℃, after 10 parts of metal vanadium powder is heated to an evaporation state, opening a gas activation source and introducing oxygen, spraying a vanadium atom beam and an active oxygen atom beam onto the substrate for reaction, observing the digital change of a crystal oscillator film thickness instrument, controlling the flow velocity of the vanadium atom beam to be 1.2nm/min, and controlling the flow velocity of the oxygen atom beam to be 3.8cm by using a gas flowmeter3The growth time of the film is 34min, and after the deposition of the film is finished, VO is continuously oxidized by residual oxygen2Film, introducing protective gas N2Naturally cooling the vacuum chamber to below 150 ℃, and taking out to obtain the product; the raw materials are in parts by weight.
Example 3
Preparation of VO2A method of making a film comprising the steps of: al by ultrasonic cleaner2O3Cleaning the surface of the substrate with deionized water for 35min, cleaning with acetone solution and anhydrous ethanol for 30min, and blow-drying with a blower; cleaning the Al2O3Transferring the single crystal substrate to a high vacuum growth chamber, and vacuumizing to make background pressure better than 1 × 10-6Pa, rotating the substrate and heating the substrate to 630 ℃ in 20 parts of metal vanadium powderHeating to evaporation state, opening gas activation source and introducing oxygen, spraying vanadium atom beam and active oxygen atom beam onto substrate for reaction, observing digital change of crystal oscillator film thickness instrument, controlling flow velocity of vanadium atom beam at 1.4nm/min, and controlling flow velocity of oxygen atom beam at 4.2cm by gas flow meter3The growth time of the film is 36min, and VO is continuously oxidized by residual oxygen after the film deposition is finished2Film, introducing protective gas N2Naturally cooling the vacuum chamber to below 150 ℃, and taking out to obtain the product; the raw materials are in parts by weight.
The method is simple, convenient, fast and easy to operate, and the prepared VO has smooth surface and is light yellow and semitransparent2The film has good crystallization, high purity, uniform and compact surface and good mid-infrared modulation characteristic, and shows that VO is utilized2The film has certain feasibility for realizing the mid-infrared laser protection.

Claims (7)

1. Preparation of VO2A method of making a film, comprising the steps of: al by ultrasonic cleaner2O3Washing the surface of the substrate with deionized water for 25-35min, then washing with acetone solution and absolute ethyl alcohol for 20-30min, and finally taking out and drying with a blower; cleaning the Al2O3Transferring the single crystal substrate to a high vacuum growth chamber, and vacuumizing to make background pressure better than 1 × 10-6Rotating a substrate, heating the substrate to 610-630 ℃, after 10-20 parts of metal vanadium powder is heated to an evaporation state, opening a gas activation source and introducing oxygen, spraying a vanadium atom beam and an active oxygen atom beam onto the substrate for reaction, observing the digital change of a crystal oscillator film thickness instrument, controlling the flow velocity of the vanadium atom beam to be 1.2-1.4nm/min, and controlling the flow velocity of the oxygen atom beam to be 3.8-4.2cm by using a gas flowmeter3The growth time of the film is 34-36min, and VO is continuously oxidized by residual oxygen after the film deposition is finished2Film, introducing protective gas N2Naturally cooling the vacuum chamber to below 150 ℃, and taking out to obtain the product; the raw materials are in parts by weight.
2. The method of claim 1, wherein: al by ultrasonic cleaner2O3The substrate surface was rinsed with deionized water for 30 min.
3. The method of claim 1, wherein: washing with acetone solution and anhydrous ethanol for 25 min.
4. The method of claim 1, wherein: the substrate was heated to 620 ℃.
5. The method of claim 1, wherein: controlling the flow velocity of the vanadium atom beam at 1.3 nm/min.
6. The method of claim 1, wherein: controlling the oxygen atom beam flow velocity to be 4.0cm by using a gas flowmeter3/min。
7. The method of claim 1, wherein: the film growth time is 35 min.
CN201811238298.4A 2018-10-23 2018-10-23 Preparation of VO2Method for making thin film Pending CN111088477A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112126895A (en) * 2020-09-22 2020-12-25 北京航空航天大学合肥创新研究院 Preparation method of vanadium dioxide single crystal film

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112126895A (en) * 2020-09-22 2020-12-25 北京航空航天大学合肥创新研究院 Preparation method of vanadium dioxide single crystal film

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