CN117418190A - Preparation and application of silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film - Google Patents
Preparation and application of silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film Download PDFInfo
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- CN117418190A CN117418190A CN202210808061.5A CN202210808061A CN117418190A CN 117418190 A CN117418190 A CN 117418190A CN 202210808061 A CN202210808061 A CN 202210808061A CN 117418190 A CN117418190 A CN 117418190A
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- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 title claims abstract description 42
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 24
- 239000004332 silver Substances 0.000 title claims abstract description 24
- 230000027311 M phase Effects 0.000 title claims abstract description 23
- 238000004544 sputter deposition Methods 0.000 claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 238000004140 cleaning Methods 0.000 claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 13
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 12
- 230000005855 radiation Effects 0.000 claims abstract description 10
- 238000002834 transmittance Methods 0.000 claims abstract description 10
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 8
- 238000005057 refrigeration Methods 0.000 claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract 2
- 239000010703 silicon Substances 0.000 claims abstract 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 30
- 229910052786 argon Inorganic materials 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002105 nanoparticle Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000012495 reaction gas Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 31
- 229910000831 Steel Inorganic materials 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 239000010959 steel Substances 0.000 description 8
- 238000000151 deposition Methods 0.000 description 7
- 238000005265 energy consumption Methods 0.000 description 6
- 238000004377 microelectronic Methods 0.000 description 6
- 230000008021 deposition Effects 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 230000008859 change Effects 0.000 description 3
- 238000005137 deposition process Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Classifications
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
-
- 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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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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)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to preparation and application of a silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film, which sequentially comprises the steps of preparing silver nanoparticles and preparing a vanadium dioxide film, wherein the preparation comprises the basic operation flows of cleaning a substrate (common glass slide, silicon and the like), setting sputtering parameters, vacuumizing, performing magnetron sputtering at normal temperature, annealing in a tube furnace, setting a reaction gas atmosphere and the like. The invention also relates to application of the silver nanoparticle-ultrathin vanadium dioxide composite structure film in the fields of intelligent window energy-saving glass and radiation refrigeration, and solves the problems of low visible light transmittance, poor near infrared and far infrared modulation capability and the like of the traditional vanadium dioxide film.
Description
Technical Field
The invention relates to the field of microelectronic device preparation, in particular to a magnetron sputtering growth material technology; in particular to a preparation process and a preparation method of a composite structure of silver nano particles and an ultrathin M-phase vanadium dioxide film grown on a substrate.
Technical Field
Among various energy consumption, the building energy consumption is about more than one third of the social energy consumption, so that the energy consumption of the building is reduced, the energy consumption can be greatly reduced, and further, the carbon emission is reduced. The intelligent window adjusts the solar wave band (400-2500 nm) through self-adaption so as to adjust indoor illumination and temperature change; radiant refrigeration cools buildings by radiating the energy of the building through the earth's atmospheric window (8000-13000 nm) into the cold outer space. Therefore, reducing building energy consumption through intelligent window and radiation refrigeration has become a research hotspot. The transmittance and modulation efficiency of solar wave bands and atmospheric window wave bands are affected before and after the phase change of the vanadium dioxide film, the modulation efficiency of light before and after the phase change of the single-layer ultrathin vanadium dioxide film is lower, and the modulation effect on radiation refrigeration is opposite to practical application.
Vanadium dioxide (VO) 2 ) The metal-semiconductor phase transition occurs at the phase transition temperature point of 68 ℃, and simultaneously the mutation of the properties such as electricity, mechanics, magnetism, optics and the like is accompanied; the ultrathin silver metal film has better visible light transmittance and stronger near infrared and middle-far infrared reflectivity. In order to improve the transmittance of the silver metal film in visible light and near infrared, the nano particles are creatively embedded into the ultrathin vanadium dioxide film to replace the silver film, so that the transmittance of the visible light can be ensured, and the adjustment of near infrared and middle-far infrared wave bands can be realized. With the development of microelectronic devices towards miniaturization, the growth of ultrathin nanocomposite films has become a research hotspot in the field of improving the performance of microelectronic devices.
The traditional nano composite structure film preparation method mainly comprises a one-time preparation scheme such as a vacuum evaporation method, a sputtering method, a chemical vapor deposition method, a physical vapor deposition method, a pulse laser deposition method and the like. Because the quality of the film has a strong relation with equipment, the high cost brought by high performance hinders the development of the film to the industrialization, low cost and microminiaturization targets, so that the optimization of the traditional preparation process and the development of the multi-band-regulated, high-quality, low-cost and high-performance composite film structure preparation process become the problems to be solved.
Disclosure of Invention
First, the technical problem to be solved
In view of the above-mentioned shortcomings of the existing ultrathin M-phase vanadium dioxide film applied to the fields of microelectronics such as intelligent windows and radiation refrigeration, the invention provides a silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film and a preparation process method thereof, which comprise the steps of preparation of an embedded structure of the silver nanoparticle composite vanadium dioxide film, setting of magnetron sputtering parameters and annealing process parameters, and the like, and the silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film is prepared by the method, and the difference value between complex refractive indexes n and k of the composite structure is utilized at high temperature, so that the modulating capability of a vanadium dioxide single-layer film in visible light and near infrared band is improved, and the development process of microelectronics is promoted.
(II) technical scheme
In order to achieve the above purpose, the invention provides a method for preparing an M-phase ultrathin vanadium dioxide film, which is characterized by comprising the following steps:
step 1, sequentially placing a substrate into a beaker containing an acetone solution, absolute ethyl alcohol and deionized water, respectively ultrasonically cleaning for 15min, and finally drying for 10min in an oven;
step 2, turning on a magnetron sputtering device to control a main power supply and a water cooler, and turning on a cavity;
step 3, cleaning the substrate by using a nitrogen gun, fixing the substrate on a sample table, and closing the cavity;
step 4, introducing argon (24 sccm), wherein the sputtering power is 30W, the sputtering pressure is 2pa, and the sputtering time is 1s;
and 5, taking out the sample, placing the sample on a ceramic plate, then placing the sample into a quartz tube (30 cm), and finally placing the sample into a tube furnace. Setting annealing parameters: argon is introduced, the flow rate is 55sccm, the heating rate is 5 ℃/min, the temperature is raised to 400 ℃, and the heat preservation time is 40min; and naturally cooling to 100 ℃ after the heat preservation step is finished, and closing the tube furnace.
Step 6, taking out the sample from the tube furnace, opening a chamber of the magnetron sputtering equipment, putting the sample in the chamber, and cleaning the sample by using a nitrogen gun;
step 7, waiting for the pressure of the vacuum chamber to be reduced to 4 x 10 -4 Pa, introducing argon (48 sccm), sputtering pressure of 2Pa, sputtering power of 120W, and sputtering time of 2min;
step 8, taking out a sample, and placing the sample into a tube furnace; setting annealing parameters: argon is introduced, the flow rate is 40sccm, the flow rate of oxygen is 2sccm, the heating rate is 5 ℃/min, the temperature is raised to 400 ℃, and the heat preservation time is 40min; and naturally cooling to 100 ℃ after the heat preservation step is finished, and closing the tube furnace.
The method has the advantages that the silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film is successfully prepared, the visible light transmittance and the middle-far infrared reflectivity are ensured, and the near infrared modulation capability is improved. The composite structure film of the invention can maintain the visible light transmittance and simultaneously enhance the self-adaptive temperature modulation heat radiation capability and the near infrared regulation capability, thereby further promoting the development of the intelligent window and the radiation refrigeration field.
Drawings
FIG. 1 is a flow chart of a silver nanoparticle-ultrathin M-phase vanadium dioxide composite structural film preparation according to an embodiment of the disclosure.
FIG. 2 is a graph showing the temperature resistance characteristics of a silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film prepared on a glass slide substrate in the invention.
FIG. 3 is a schematic diagram of a silver nanoparticle-ultrathin M-phase vanadium dioxide composite structural film prepared on a glass slide substrate according to the invention.
FIG. 4 is a scanning electron microscope image of 10nm silver nanoparticles grown on a glass slide substrate according to the present invention.
FIG. 5 is a scanning electron microscope image of a 30nm vanadium dioxide film grown on a glass slide substrate in accordance with the present invention.
FIG. 6 is an X-ray diffraction pattern of a 30nm vanadium dioxide thin film of the present invention.
[ symbolic description ]
1-substrate (glass slide)
2-silver nanoparticles
3-M phase vanadium dioxide film
Detailed Description
The invention provides a preparation method and application of a silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film. The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments of the present invention, and should not be taken as limiting the scope of the present invention.
The invention provides a preparation process of a silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film, which utilizes a physical vapor deposition method through magnetron sputtering equipment to optimize an experimental step scheme, deeply clean a chamber environment, optimize an annealing step, set sputtering power and gas atmosphere, set chamber air pressure, sputtering time, annealing temperature and gas flow, effectively prepare the silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film, effectively maintain visible light transmittance, and improve the heat radiation modulating capability and near infrared regulating capability.
The preparation method comprises the following specific steps:
step 1: preparation before deposition
A1: cleaning a substrate
And ultrasonically cleaning the substrate to ensure the surface cleaning. The cleaning process of the substrate is as follows: pouring a proper amount of absolute ethyl alcohol into the beaker, and ultrasonically cleaning for 15min to ensure that impurity dust in the beaker is removed; placing the substrate into a clean beaker, and respectively ultrasonically cleaning the substrate for 15min by using acetone and absolute ethyl alcohol; and finally, taking out the cleaned substrate, transferring the substrate to a tray, and putting the tray into an oven for drying for 15min.
A2: starting up preparation:
and opening the main gate and each path of split gate of the magnetron sputtering equipment, and opening the water pump. The inflation valve and the low vacuum gauge are opened, and when the vacuum representation number is equal to the atmospheric pressure, the chamber is opened.
A3: and (3) adding a target material and a substrate:
a silver metal target is placed on the rf target and the substrate is assembled on a turntable. After confirming that the target and the substrate are on the same straight line, the chamber is closed.
Step 2: deposition process
A1: vacuumizing:
and closing the flow limiting valve, opening the mechanical pump, opening the backing valve, and opening the molecular pump when the low vacuum gauge number is less than 5 Pa.
A2: setting parameters:
when the pressure drop in the cavity is less than 1 x 10 < -4 > Pa, the flow limiting valve is closed, the flowmeter is opened, the argon steel cylinder valve is opened, the pressure reducing valve of the steel cylinder is regulated to be less than 0.3MPa, and the indication number of the flowmeter is regulated to be 24sccm.
A3: turning on deposition
When the pressure of the air in the chamber is lower than a certain pressure, the sputtering power is regulated to be 30w, the pre-sputtering is carried out for 10min, and the sputtering time is set to be 1s.
Step 3: end of deposition
And (3) adjusting the sputtering current and the voltage to be zero, closing a sputtering power supply, closing a flowmeter, closing a steel cylinder valve, closing a molecular pump, closing a backing valve, closing a mechanical pump, opening an inflation valve, opening a cavity when the low vacuum representation number is equal to the atmospheric pressure, and taking out a sample.
Step 5: annealing process
A1: starting up preparation:
and (3) opening each power supply, opening a vacuum meter, opening an air inlet valve, and opening a flange when the pressure in the quartz hearth is equal to the atmospheric pressure.
A2: placing a sample:
the samples were placed on ceramic plates and centered in a quartz tube (30 cm) and then placed into a quartz hearth, the flange closed, and the air inlet valve closed.
A3: setting gas parameters:
when the vacuum degree in the hearth is lower than 30Pa, respectively opening an argon steel bottle, opening an air inlet valve, adjusting a gas flowmeter, and setting the argon flow rate to 55sccm.
A4: setting temperature parameters:
when the gas flow rate and the pressure in the furnace are stable, setting the heating rate to be 5 ℃/min, the heating time to be 80min, the heat preservation temperature to be 400 ℃, the heat preservation time to be 40min, the cooling rate to be 5 ℃/min, the cooling time to be 50min, and naturally cooling to 100 ℃ after the heat preservation step is finished to stop working. After the setting is completed, clicking the 'Turn On', pressing the 'Start', and starting the tube furnace.
A6: and (3) annealing is finished:
the screen displays "Stop", presses "turnoff", closes the flow meter, closes the air inlet valve, closes the cylinder valve, closes the baffle, closes the mechanical pump, and takes out the sample.
Step 6: preparation before depositing vanadium metal
A1: starting up preparation:
and opening the main gate and each path of split gate of the magnetron sputtering equipment, and opening the water pump. The V2 control valve, low vacuum gauge, is opened and the chamber is opened when the vacuum gauge number is equal to atmospheric pressure.
A2: and (3) adding a target material and a substrate:
and placing a vanadium metal target on the convection target, and assembling the substrate on the rotary table. After confirming that the target, sputtering hole and target are on the same straight line, the chamber is closed.
Step 7: deposition process
A1: vacuumizing:
and (3) opening the mechanical pump, the electromagnetic valve and the low vacuum gauge, and opening the molecular pump and opening the gate valve to start vacuumizing when the low vacuum gauge number is smaller than 10 Pa.
A2: setting parameters:
when the pressure in the chamber is reduced to 4.0 x 10 -4 And opening a flowmeter below Pa, opening an argon steel cylinder valve, adjusting a steel cylinder pressure reducing valve to be smaller than 0.3MPa, adjusting the indicating number of the flowmeter to be 48sccm, opening a V3 control valve, adjusting a gate valve, and adjusting the sputtering pressure to be 2Pa.
A3: opening deposition:
the sputtering power was adjusted to 120w, and pre-sputtering was performed for 10min with the sputtering time set to 2min.
Step 8: deposition end:
and (3) adjusting the sputtering current and the voltage to zero, closing a sputtering power supply, closing a flowmeter, closing a steel cylinder valve, closing a V3 control valve, closing a gate valve, closing a molecular pump, closing an electromagnetic valve, closing a mechanical pump, opening a V2 control valve, opening a cavity when the low vacuum representation number is equal to the atmospheric pressure, and taking out a sample.
Step 9: annealing process
A1: starting up preparation:
and (3) opening each power supply, opening a vacuum meter, opening an air inlet valve, and opening a flange when the pressure in the quartz hearth is equal to the atmospheric pressure.
A2: and (3) equipment large cleaning:
the chamber and the like are cleaned by a dust collector, and finally the quartz tube and the ceramic plate are cleaned in all directions by using dust-free paper.
A3: placing a sample:
the sample was placed in the ceramic wafer and centered in a quartz tube (30 cm) and then placed in a quartz hearth, the flange was closed, and the air inlet valve was closed.
A4: setting gas parameters:
when the vacuum degree in the hearth is lower than 30Pa, respectively opening an argon and oxygen steel bottle, opening an air inlet valve, adjusting a gas flowmeter, sequentially opening argon and oxygen, setting the flow rate of the argon to be 40sccm, and setting the flow rate of the oxygen to be 0.5sccm.
A5: setting temperature parameters:
when the gas flow rate and the pressure in the furnace are stable, setting the heating rate to be 5 ℃/min, the heating time to be 80min, the heat preservation temperature to be 400 ℃, the heat preservation time to be 40min, the cooling rate to be 5 ℃/min, the cooling time to be 50min, and naturally cooling to 100 ℃ after the heat preservation step is finished to stop working. After the setting is completed, clicking the 'Turn On', pressing the 'Start', and starting the tube furnace.
A6: and (3) annealing is finished:
the screen displays "Stop", presses "turnoff", closes the flow meter, closes the air inlet valve, closes the cylinder valve, closes the baffle, closes the mechanical pump, and takes out the sample.
The preparation process of the silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film provided by the invention effectively maintains the visible light transmittance and improves the heat radiation modulation capability and the near infrared regulation capability. The silver nano particles and the vanadium dioxide film are prepared by adopting a two-step method, the preparation process and conditions are optimized, the requirements of the intelligent window and the radiation refrigeration field on performance are met, and the preparation cost is reduced. The invention has a pushing effect on the development of microelectronic devices.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it will be apparent that the foregoing is merely illustrative of the present invention and that various modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the invention.
Claims (5)
1. A preparation process of a silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film comprises a substrate (common glass slide, silicon and the like), silver nanoparticles and a vanadium dioxide film, and is characterized in that the silver nanoparticles and the ultrathin M-phase vanadium dioxide film are respectively prepared by utilizing a magnetron sputtering method, and a sandwich structure is innovatively provided, wherein the silver nanoparticles, the silver nanoparticles (10 nm) and the vanadium dioxide film (30 nm) are respectively arranged on the substrate. The specific operation steps are as follows:
step 1, sequentially placing a substrate into a beaker containing an acetone solution, absolute ethyl alcohol and deionized water, respectively ultrasonically cleaning for 15min, and finally drying for 10min in an oven;
step 2, turning on a magnetron sputtering control main power supply and a water cooler, and turning on a cavity;
step 3, cleaning the substrate by using a nitrogen gun, fixing the substrate on a sample table, and closing the cavity;
step 4, reducing the pressure of the vacuum chamber to 1 x 10 -4 Argon (24 sccm) is then introduced under Pa, the sputtering power is 30W, the sputtering pressure is 2Pa, and the sputtering time is 1s;
and 5, taking out the sample, placing the sample on a ceramic plate, then placing the sample in a 30cm quartz tube, and finally placing the sample in a tube furnace. Setting annealing parameters: argon is introduced, the flow rate is 55sccm, the heating rate is 5 ℃/min, the temperature is raised to 400 ℃, and the heat preservation time is 40min; and naturally cooling to 100 ℃ after the heat preservation step is finished, and closing the tube furnace.
Step 6, taking out the sample from the tube furnace, opening a chamber of the magnetron sputtering equipment, putting the sample in the chamber, and cleaning the sample by using a nitrogen gun;
step 7, setting sputtering parameters, and reducing the pressure of the vacuum chamber to 4×10 -4 Pa, introducing argon (48 sccm), sputtering pressure of 2Pa, sputtering power of 120W, and sputtering time of 2min;
step 8, taking out a sample, and placing the sample into a tube furnace; setting annealing parameters: argon is introduced, the flow rate is 40sccm, the flow rate of oxygen is 2sccm, the heating rate is 5 ℃/min, the temperature is raised to 400 ℃, and the heat preservation time is 40min; and naturally cooling to 100 ℃ after the heat preservation step is finished, and closing the tube furnace.
2. The preparation and application of the silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film according to claim 1, wherein the silver nanoparticle and vanadium dioxide film are compounded into an embedded structure.
3. The preparation and application of the silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film according to claim 1, wherein the silver nanoparticle doped in the film is 5nm-20nm, and the thickness of the vanadium dioxide film is 10nm-50nm.
4. The preparation and application of the silver nanoparticle-ultrathin M-phase vanadium dioxide composite structural film according to any one of claims 2-4, wherein the silver nanoparticle-ultrathin M-phase vanadium dioxide composite structural film is applied to visible light-transmitting structures with adjustable near infrared and mid-infrared transmittance, and related structures are applied to intelligent windows, radiation refrigeration and laser protection.
5. The preparation and application of the silver nanoparticle-ultrathin M-phase vanadium dioxide composite structure film according to claim 1, wherein the process flow of preparing silver nanoparticles and then preparing the vanadium dioxide film is respectively utilized by magnetron sputtering and annealing.
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