CN112938893B - Vanadium dioxide monocrystal driver and preparation method and application thereof - Google Patents

Vanadium dioxide monocrystal driver and preparation method and application thereof Download PDF

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CN112938893B
CN112938893B CN202110181070.1A CN202110181070A CN112938893B CN 112938893 B CN112938893 B CN 112938893B CN 202110181070 A CN202110181070 A CN 202110181070A CN 112938893 B CN112938893 B CN 112938893B
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driver
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CN112938893A (en
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程春
石润
陈勇
申楠
孔伟光
甘翊辰
王子旭
赵娅萱
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Southwest University of Science and Technology
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Abstract

The invention provides a vanadium dioxide monocrystal driver and a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) Mixing vanadium pentoxide powder and silicon dioxide powder according to the mass ratio of (1-2) to 1 to obtain vanadium source powder; (2) Placing the growth substrate right above the vanadium source powder obtained in the step (1), and placing the growth substrate into a heating system; (3) And (3) vacuumizing the heating system in the step (2), introducing protective gas, and starting a heating program to perform chemical vapor deposition reaction to obtain the vanadium dioxide monocrystal driver. The invention controllably applies the M2 phase and the T phase to the vanadium dioxide monocrystal driver, fully utilizes the M2-R phase change and the T-M2 phase change to realize the theoretical optimal driving performance, reduces the energy loss in the driving process, and improves the stability and the corrosion resistance of the driver.

Description

Vanadium dioxide monocrystal driver and preparation method and application thereof
Technical Field
The invention belongs to the technical field of advanced micro-nano drivers, relates to a single crystal driver, and particularly relates to a vanadium dioxide single crystal driver, and a preparation method and application thereof.
Background
Researchers have found that the M1 phase vanadium dioxide converts to R phase vanadium dioxide when heated to 68 ℃ and produces a compressive strain of about 1% along the [001] direction of the R phase, a characteristic that allows the vanadium dioxide to be used in the fabrication of thermally driven devices. In recent years, scholars at home and abroad find that the vanadium dioxide thermal excitation micro-driver can simultaneously meet the application requirements of high frequency, high amplitude and high output power. Among them, the driver based on vanadium dioxide single crystal micro-nanowires (grown in [001] direction of R phase) exhibits the most excellent driving capability.
In 2010, wu Junqiao of the national laboratory of Lorentebergy, U.S. teaches that combining vanadium dioxide single crystal nanowires with metallic chromium into a dual crystal drive yields up to 2.5X10 4 m -1 Curvature change of (2) and 7J/cm 3 Theoretical work density (Journal of Applied Physics 108,083538 (2010)). In 2013, the subject group explores the performance limit of the double-crystal micro-driver of vanadium dioxide nanowires and chromium, and discovers that the device can also realize the working speed of kilohertz level, and the efficiency of converting heat energy into mechanical energy can reach 0.85%. Meanwhile, the work also finds that the bi-crystal interface stress when the driver is bent can induce the generation of metastable M2 phase vanadium dioxide, and the M2 phase to R phase transition can generate strain as high as 2 percent. Thus, the bilayer device can produce greater amplitude and higher energy conversion efficiency (-3.4%) (Wang K, cheng C, cardona E, et al Performance limits of microactuation with vanadium dioxide as a solid engine [ J)]ACS nano,2013,7 (3): 2266-2272). In 2019, the inventor group developed a preparation method of a monocrystal vanadium dioxide nanowire driver, by means of tungsten doping and space asymmetric distribution of reaction conditions, a lateral oxygen concentration gradient and a lateral asymmetric phase change are formed in the prepared monocrystal nanowire, so that bidirectional self-bending behavior of a single vanadium dioxide nanowire is realized, driving performance of the monocrystal vanadium dioxide nanowire driver is equivalent to that of a twin crystal vanadium dioxide nanowire driver, and the monocrystal vanadium dioxide nanowire driver shows better cycle stability than that of the twin crystal driver (Shi R, cai X, wang W, et al Single-Crystalline Vanadium Dioxide Actuators [ J ]].Advanced Functional Materials,2019,29(20):1900527)。
However, the driving capability of the nanowire/metal bimorph driver is directly affected by the double-layer thickness ratio and the interface contact condition, so that there are objective problems of poor stability, poor corrosion resistance and the like caused by the falling of the coating. While the heretofore developed single crystal drives overcome the problems in the twin crystal drives, M2-R phase transitions are not utilized to achieve the theoretical optimal driving performance. The generation of M2 phase in the bicrystal system cannot be reasonably controlled and utilized, so how to controllably apply the M2 phase to the vanadium dioxide single crystal driver is still a key problem. In addition, a transition phase T phase exists between the M1 phase and the M2 phase, and researchers find that the transition from the T phase to the M2 phase can generate linear strain of up to 0.7%, and meanwhile, the energy required by the transition is far lower than that required by the transition from the M1 phase or the M2 phase to the R phase, so that whether the T phase can be introduced into a driver to reduce the energy loss in the driving process becomes an important consideration in the design and the preparation process of the driving device.
Therefore, how to provide a vanadium dioxide single crystal driver, a preparation method and application thereof, wherein an M2 phase and a T phase are controllably applied to the vanadium dioxide single crystal driver, and the M2-R phase change and the T-M2 phase change are fully utilized to realize the theoretical optimal driving performance, so that the energy loss in the driving process is reduced, the stability and the corrosion resistance of the driver are improved, and the problem which needs to be solved by the current technicians in the field is solved.
Disclosure of Invention
The invention aims to provide a vanadium dioxide single crystal driver, and a preparation method and application thereof, wherein an M2 phase and a T phase are controllably applied to the vanadium dioxide single crystal driver, so that M2-R phase change and T-M2 phase change are fully utilized to realize theoretical optimal driving performance, energy loss in a driving process is reduced, and stability and corrosion resistance of the driver are improved.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a vanadium dioxide single crystal driver, the method comprising the steps of:
(1) Mixing vanadium pentoxide powder and silicon dioxide powder according to the mass ratio of (1-2) to 1 to obtain vanadium source powder;
(2) Placing the growth substrate right above the vanadium source powder obtained in the step (1), and placing the growth substrate into a heating system;
(3) And (3) vacuumizing the heating system in the step (2), introducing protective gas, and starting a heating program to perform chemical vapor deposition reaction to obtain the vanadium dioxide monocrystal driver.
In the present invention, step (1) is to mix the vanadium pentoxide powder with the silicon dioxide powder in the mass ratio of (1-2): 1, for example, it may be 1:1, 1.1:1, 1.2:1, 1.3:1, 1.4:1, 1.5:1, 1.6:1, 1.7:1, 1.8:1, 1.9:1 or 2:1, but not limited to the listed values, and other non-listed values within the range of values are equally applicable.
According to the invention, the method of mixing silicon dioxide into vanadium pentoxide is adopted to effectively regulate the oxygen partial pressure of a reaction system, so that excessive oxygen permeates into the synthesized vanadium dioxide micro-nano wire, and the metastable M2 phase and the metastable T phase are promoted to exist stably at room temperature. Meanwhile, the formation of the lateral oxygen concentration gradient of the vanadium dioxide micro-nano wire is realized through the self liquid layer auxiliary growth mode of the low-temperature low-pressure vanadium pentoxide reduction reaction, and the T-M2 single crystal driver with good driving capability is prepared. The energy required for converting the T phase into the M2 phase is only 20% of that of converting the M1 phase into the R phase, and the driving amplitude can reach 70% of that of an M1-R type driver, so that the energy-saving single crystal driver can be used as a high-efficiency single crystal driver with low energy consumption.
Preferably, the vanadium source powder in step (1) is further mixed with tungsten dioxide powder.
Preferably, the tungsten dioxide powder comprises 20-40% of the total mass of the vanadium source powder, for example 20%, 22%, 24%, 26%, 28%, 30%, 32%, 34%, 36%, 38% or 40%, but is not limited to the recited values, and other non-recited values within this range are equally applicable.
In the invention, the total mass of the vanadium source powder is the total mass of the vanadium source powder mixed with the tungsten dioxide powder, namely the sum of the mass of the vanadium pentoxide powder, the mass of the silicon dioxide powder and the mass of the tungsten dioxide powder.
According to the invention, the oxygen content in a vanadium dioxide system can be selectively reduced by adding the reducible tungsten dioxide doping agent, so that the oxygen concentration gradient is increased, coexistence of an M2 phase and an R phase is realized, the maximum bending driving behavior is realized, and the prepared M2-R type single crystal driver reaches the performance limit of the vanadium dioxide driver from all aspects.
In the invention, the tungsten dioxide powder accounts for less than 50% of the total mass of the vanadium source powder, otherwise, the lateral oxygen concentration gradient is too high, so that the vanadium dioxide nanowire is severely corroded, and the driving behavior cannot be realized.
In the invention, the mixing in the step (1) is performed in a quartz boat.
Preferably, the growth substrate of step (2) comprises a quartz plate.
Preferably, the surface average particle size of the quartz plate is 300 to 340 mesh, for example, 300 mesh, 305 mesh, 310 mesh, 315 mesh, 320 mesh, 325 mesh, 330 mesh, 335 mesh or 340 mesh, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In the invention, the surface average granularity is specifically expressed as the average mesh number of quartz sand on the surface of the quartz plate.
Preferably, the distance between the growth substrate and the vanadium source powder in the step (2) is 0.1-1cm, for example, 0.1cm, 0.2cm, 0.3cm, 0.4cm, 0.5cm, 0.6cm, 0.7cm, 0.8cm, 0.9cm or 1cm, but not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
In the invention, the heating system in the step (2) is a tube furnace.
Preferably, the absolute vacuum degree of the vacuum in the step (3) is less than or equal to 10Pa, for example, 1Pa, 2Pa, 3Pa, 4Pa, 5Pa, 6Pa, 7Pa, 8Pa, 9Pa or 10Pa, but is not limited to the recited values, and other non-recited values in the range of the values are equally applicable.
Preferably, the shielding gas in step (3) includes any one of nitrogen, argon or helium.
Preferably, the flow rate of the shielding gas in the step (3) is 7-20sccm, for example, 7sccm, 8sccm, 10sccm, 12sccm, 14sccm, 16sccm, 18sccm or 20sccm, but the present invention is not limited to the recited values, and other non-recited values within the recited values are equally applicable.
Preferably, the pressure of the protective gas introduced into the heating system in the step (3) is 2-4Torr, and may be, for example, 2Torr, 2.2Torr, 2.4Torr, 2.6Torr, 2.8Torr, 3Torr, 3.2Torr, 3.4Torr, 3.6Torr, 3.8Torr or 4Torr, but not limited to the above values, and other non-enumerated values within the above values may be equally applied.
Preferably, the temperature increasing program in the step (3) specifically includes: heating to a first temperature in a first time period, then heating to a second temperature at a first heating rate, maintaining for a second time period, and finally cooling.
Preferably, the first period of time is 25-35min, for example, 25min, 26min, 27min, 28min, 29min, 30min, 31min, 32min, 33min, 34min or 35min, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the first temperature is 500 to 600 ℃, for example, 500 ℃, 510 ℃, 520 ℃, 530 ℃, 540 ℃, 550 ℃, 560 ℃, 570 ℃, 580 ℃, 590 ℃, or 600 ℃, but the first temperature is not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the first heating rate is 8-12 ℃/min, for example, 8 ℃/min, 8.5 ℃/min, 9 ℃/min, 9.5 ℃/min, 10 ℃/min, 10.5 ℃/min, 11 ℃/min, 11.5 ℃/min or 12 ℃/min, but the first heating rate is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the second temperature is 800 to 900 ℃, for example, 800 ℃, 810 ℃, 820 ℃, 830 ℃, 840 ℃, 850 ℃, 860 ℃, 870 ℃, 880 ℃, 890 ℃, or 900 ℃, but the second temperature is not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the second period of time is 1-10min, for example, 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
As a preferred technical solution of the first aspect of the present invention, the preparation method includes the following steps:
(1) Mixing vanadium pentoxide powder and silicon dioxide powder according to the mass ratio of (1-2) to 1 to obtain vanadium source powder; and mixing tungsten dioxide powder accounting for 20-40% of the total weight of the vanadium source powder;
(2) Placing a quartz plate with the surface average granularity of 300-340 meshes as a growth substrate at a position which is 0.1-1cm above the vanadium source powder obtained in the step (1), and placing the quartz plate into a heating system;
(3) Vacuumizing the heating system in the step (2) until the absolute vacuum degree is less than or equal to 10Pa, introducing nitrogen, argon or helium with the flow of 7-20sccm to the air pressure of the heating system of 2-4Torr, and starting a heating program to perform chemical vapor deposition reaction to obtain the vanadium dioxide monocrystal driver; the temperature-raising program specifically comprises the following steps: heating to 500-600deg.C within 25-35min, heating to 800-900deg.C at 8-12deg.C/min, maintaining for 1-10min, and cooling.
In a second aspect, the present invention provides a vanadium dioxide single crystal driver prepared by the preparation method according to the first aspect.
The type of the vanadium dioxide single crystal driver obtained by the invention comprises an M2-R type single crystal driver, a T-M2 type single crystal driver and an M1-R type single crystal driver, wherein the length range of the single crystal driver is 10 mu M-1mm, and the width range of the single crystal driver is 200nm-30 mu M.
In a third aspect, the present invention provides a use of a vanadium dioxide single crystal driver as described in the second aspect in micro-nano driving.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the method of mixing silicon dioxide into vanadium pentoxide is adopted to effectively adjust the oxygen partial pressure of a reaction system, so that excessive oxygen permeates into the synthesized vanadium dioxide micro-nano wire, and the metastable M2 phase and T phase are promoted to exist stably at room temperature;
(2) According to the invention, through the self liquid layer auxiliary growth mode of the low-temperature low-pressure vanadium pentoxide reduction reaction, the formation of the lateral oxygen concentration gradient of the vanadium dioxide micro-nanowire is realized, and the T-M2 type monocrystal driver with good driving capability is prepared; the energy required by the transformation of the T phase to the M2 phase is only 20% of that of the M1 phase to the R phase, and the driving amplitude can reach 70% of that of an M1-R type monocrystal driver, so that the energy-saving monocrystal driver can be used as a high-efficiency monocrystal driver with low energy consumption;
(3) According to the invention, the oxygen content in a vanadium dioxide system can be selectively reduced by adding the reducible tungsten dioxide doping agent, so that the oxygen concentration gradient is increased, coexistence of an M2 phase and an R phase is realized, the maximum bending driving behavior is realized, and the prepared M2-R type single crystal driver reaches the performance limit of the vanadium dioxide driver from all aspects.
Drawings
FIG. 1 is an optical image and Raman spectrum of an asymmetric domain pattern of a vanadium dioxide single crystal drive provided in example 1;
FIG. 2 is an optical photograph of the temperature swing driving behavior of the vanadium dioxide single crystal driver provided in example 1;
FIG. 3 is an optical image and Raman spectrum of an asymmetric domain pattern of a vanadium dioxide single crystal drive provided in example 2;
FIG. 4 is an optical photograph of the temperature swing driving behavior of the vanadium dioxide single crystal driver provided in example 2;
FIG. 5 is an optical photograph of vanadium dioxide nanowires provided in example 5 that are etched with excess tungsten;
fig. 6 is a schematic diagram showing the operation principle of two novel single crystal drivers obtained in example 1 and example 2.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a vanadium dioxide single crystal driver and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Mixing 3mg of vanadium pentoxide powder and 2mg of silicon dioxide powder in a quartz boat according to the mass ratio of 1.5:1 to obtain vanadium source powder; and mixing tungsten dioxide powder accounting for 30 percent of the total weight of the vanadium source powder;
(2) Placing a quartz plate with the surface average granularity of 320 meshes as a growth substrate at a position which is 0.5cm above the vanadium source powder obtained in the step (1), and placing the quartz plate into a tube furnace;
(3) Vacuumizing the tubular furnace in the step (2) to an absolute vacuum degree of 5Pa, introducing argon with a flow of 15sccm to a gas pressure of 3Torr in the tubular furnace, and starting a heating program to perform a chemical vapor deposition reaction to obtain the vanadium dioxide monocrystal driver; the temperature-raising program specifically comprises the following steps: heating to 550 ℃ within 30min, then heating to 850 ℃ at 10 ℃/min, maintaining for 5min, and finally cooling.
The vanadium dioxide single crystal driver obtained in the embodiment is an M2-R type single crystal driver, part of samples show larger lateral oxygen concentration gradient, an asymmetric domain pattern of one side M2 phase and one side R phase is shown in figure 1 when the temperature is raised, the single crystal driver generates great bidirectional bending behavior when the temperature is changed due to the fact that strain of 1.7% is generated when the M2 phase is converted to the R phase, and the process is reversible when the temperature is lowered.
Example 2
The embodiment provides a vanadium dioxide single crystal driver and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Mixing 3mg of vanadium pentoxide powder and 2mg of silicon dioxide powder in a quartz boat according to the mass ratio of 1.5:1 to obtain vanadium source powder;
(2) Placing a quartz plate with the surface average granularity of 300 meshes as a growth substrate at a position which is 1cm above the vanadium source powder obtained in the step (1), and placing the quartz plate into a tube furnace;
(3) Vacuumizing the tubular furnace in the step (2) to an absolute vacuum degree of 1Pa, introducing nitrogen with a flow of 7sccm to a gas pressure of 2Torr in the tubular furnace, and starting a heating program to perform a chemical vapor deposition reaction to obtain the vanadium dioxide monocrystal driver; the temperature-raising program specifically comprises the following steps: heating to 500 ℃ within 25min, then heating to 800 ℃ at 8 ℃/min, maintaining for 10min, and finally cooling.
The vanadium dioxide single crystal driver obtained in this embodiment is a T-M2 single crystal driver, a part of samples show a smaller lateral oxygen concentration gradient, an asymmetric domain pattern of one side M2 phase and one side T phase is shown in fig. 3 when the temperature is raised, and the single crystal driver also generates a bidirectional bending behavior when the temperature is changed (see fig. 4) due to the fact that the strain of 0.7% is generated when the T phase is converted into the M2 phase, and the process is reversible when the temperature is lowered.
Example 3
The embodiment provides a vanadium dioxide single crystal driver and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Mixing 4mg of vanadium pentoxide powder and 2mg of silicon dioxide powder in a quartz boat according to a mass ratio of 2:1 to obtain vanadium source powder; and mixing tungsten dioxide powder accounting for 20 percent of the total weight of the vanadium source powder;
(2) Placing a quartz plate with the surface average granularity of 340 meshes as a growth substrate at a position which is 0.1cm above the vanadium source powder obtained in the step (1), and placing the quartz plate into a tube furnace;
(3) Vacuumizing the tubular furnace in the step (2) to an absolute vacuum degree of 10Pa, introducing helium with a flow of 20sccm to a gas pressure of 4Torr in the tubular furnace, and starting a heating program to perform a chemical vapor deposition reaction to obtain the vanadium dioxide monocrystal driver; the temperature-raising program specifically comprises the following steps: heating to 600 ℃ within 35min, then heating to 900 ℃ at 12 ℃/min, maintaining for 1min, and finally cooling.
The vanadium dioxide single crystal driver obtained in the embodiment is an M1-R type single crystal driver, part of samples show smaller lateral oxygen concentration gradient, asymmetric domain patterns of one side M1 phase and one side R phase are shown when the temperature is raised, and the single crystal driver can generate bidirectional bending behavior when the temperature is changed due to the fact that strain of 1% is generated when the M1 phase is converted into the R phase, and the process is reversible when the temperature is lowered.
Example 4
The embodiment provides a vanadium dioxide single crystal driver and a preparation method thereof, wherein the preparation method is changed from the step (1): mixing 2.5mg of vanadium pentoxide powder and 2.5mg of silicon dioxide powder in a quartz boat according to a mass ratio of 1:1 to obtain vanadium source powder; and mixing tungsten dioxide powder accounting for 30 percent of the total weight of the vanadium source powder; the other conditions are the same as those of example 1, and thus, a description thereof will not be repeated here.
The vanadium dioxide single crystal driver obtained in the embodiment is an M2-R type single crystal driver, part of samples show larger lateral oxygen concentration gradient, asymmetric domain patterns of one side M2 phase and one side R phase are shown when the temperature is raised, and the single crystal driver generates great bidirectional bending behavior when the temperature is changed due to the fact that strain of 1.7% is generated when the M2 phase is converted to the R phase, and the process is reversible when the temperature is lowered.
Example 5
The embodiment provides a vanadium dioxide single crystal driver and a preparation method thereof, wherein the preparation method is changed from the step (1): mixing 3mg of vanadium pentoxide powder and 2mg of silicon dioxide powder in a quartz boat according to the mass ratio of 1.5:1 to obtain vanadium source powder; and mixing tungsten dioxide powder accounting for 50 percent of the total weight of the vanadium source powder; the other conditions are the same as those of example 1, and thus, a description thereof will not be repeated here.
The vanadium dioxide nanowires obtained in this example are severely corroded, and cannot realize driving behavior (see fig. 5).
Comparative example 1
The comparative example provides a vanadium dioxide single crystal driver and a preparation method thereof, and the preparation method is the same as that of example 1 except that the vanadium source powder in step (1) is changed to 5mg of vanadium pentoxide powder, no silicon dioxide powder or tungsten dioxide powder is added, and the other conditions are the same as those of example 1, so that no description is given here.
The vanadium dioxide nanowires obtained in this comparative example are all M1 phase crystals, and there are no stable M2 phase and T phase, so that the driving behavior cannot be achieved.
It can be seen that the two novel single crystal drivers obtained in example 1 and example 2 operate on the following principles (see fig. 6):
(1) For an M2-R type single crystal drive: the side with lower oxygen content is firstly changed into R phase when the temperature is raised, and the other side is changed into M2 phase, and the driver bends towards the side occupied by the R phase because the M2 phase is longer than the R phase in the axial direction;
(2) For a T-M2 type single crystal drive: the side with the lower oxygen content becomes the M2 phase at first at the time of temperature rise, and the other side is the T phase at this time, and the driver bends to the side occupied by the T phase because the M2 phase is longer than the T phase in the axial direction.
In conclusion, the method of mixing silicon dioxide into vanadium pentoxide is adopted to effectively adjust the oxygen partial pressure of a reaction system, so that excessive oxygen permeates into the synthesized vanadium dioxide micro-nano wire, and the metastable M2 phase and the metastable T phase are promoted to exist stably at room temperature; in addition, the formation of the lateral oxygen concentration gradient of the vanadium dioxide micro-nano wire is realized through the self liquid layer auxiliary growth mode of the low-temperature low-pressure vanadium pentoxide reduction reaction, and the T-M2 single crystal driver with good driving capability is prepared; the energy required for converting the T phase into the M2 phase is only 20% of that of converting the M1 phase into the R phase, and the driving amplitude can reach 70% of that of an M1-R type single crystal driver, so that the energy-saving single crystal driver can be used as a high-efficiency single crystal driver with low energy consumption. According to the invention, the oxygen content in the vanadium dioxide system can be selectively reduced by adding the reducible tungsten dioxide doping agent, so that the oxygen concentration gradient is increased, coexistence of an M2 phase and an R phase is realized, the maximum bending driving behavior is realized, and the prepared M2-R type single crystal driver reaches the performance limit of the vanadium dioxide driver from all aspects.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.

Claims (11)

1. A method for preparing a vanadium dioxide single crystal driver, the method comprising the steps of:
(1) Mixing vanadium pentoxide powder and silicon dioxide powder according to the mass ratio of (1-2) to 1 to obtain vanadium source powder;
(2) Placing the growth substrate right above the vanadium source powder obtained in the step (1), and placing the growth substrate into a heating system;
(3) Vacuumizing the heating system in the step (2) and introducing protective gas, and starting a heating program to perform chemical vapor deposition reaction to obtain the vanadium dioxide monocrystal driver; the temperature-raising program specifically comprises the following steps: heating to 500-600deg.C within 25-35min, heating to 800-900deg.C at 8-12deg.C/min, maintaining for 1-10min, and cooling.
2. The method according to claim 1, wherein the vanadium source powder of step (1) is further mixed with tungsten dioxide powder.
3. The preparation method according to claim 2, wherein the tungsten dioxide powder accounts for 20-40% of the total mass of the vanadium source powder.
4. The method of claim 1, wherein the growth substrate of step (2) comprises a quartz plate.
5. The method according to claim 4, wherein the surface average particle size of the quartz plate is 300 to 340 mesh.
6. The method of claim 1, wherein the growth substrate in step (2) is spaced from the vanadium source powder by a distance of 0.1cm to 1cm.
7. The method according to claim 1, wherein the absolute vacuum degree of the vacuum in the step (3) is 10Pa or less.
8. The method of claim 1, wherein the shielding gas in step (3) comprises any one of nitrogen, argon or helium.
9. The method according to claim 1, wherein the flow rate of the shielding gas in the step (3) is 7-20sccm.
10. The method according to claim 1, wherein the pressure of the protective gas introduced into the heating system in the step (3) is 2to 4Torr.
11. The preparation method according to any one of claims 1 to 10, characterized in that the preparation method comprises the steps of:
(1) Mixing vanadium pentoxide powder and silicon dioxide powder according to the mass ratio of (1-2) to 1 to obtain vanadium source powder; and mixing tungsten dioxide powder accounting for 20-40% of the total weight of the vanadium source powder;
(2) Placing a quartz plate with the surface average granularity of 300-340 meshes as a growth substrate at a position which is 0.1-1cm above the vanadium source powder obtained in the step (1), and placing the quartz plate into a heating system;
(3) Vacuumizing the heating system in the step (2) until the absolute vacuum degree is less than or equal to 10Pa, introducing nitrogen, argon or helium with the flow of 7-20sccm to the air pressure of the heating system of 2-4Torr, and starting a heating program to perform chemical vapor deposition reaction to obtain the vanadium dioxide monocrystal driver; the temperature-raising program specifically comprises the following steps: heating to 500-600deg.C within 25-35min, heating to 800-900deg.C at 8-12deg.C/min, maintaining for 1-10min, and cooling.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106187318A (en) * 2016-07-15 2016-12-07 天津大学 A kind of preparation method of the ceramic base Vanadium dioxide nanometer rod structure of freedom and on-plane surface growth
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
CN110699670A (en) * 2019-11-13 2020-01-17 西安近代化学研究所 Preparation method of vanadium dioxide film
CN111850684A (en) * 2019-04-30 2020-10-30 中国科学技术大学 Preparation method of vanadium dioxide-based single crystal and vanadium dioxide-based single crystal

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106187318A (en) * 2016-07-15 2016-12-07 天津大学 A kind of preparation method of the ceramic base Vanadium dioxide nanometer rod structure of freedom and on-plane surface growth
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
CN111850684A (en) * 2019-04-30 2020-10-30 中国科学技术大学 Preparation method of vanadium dioxide-based single crystal and vanadium dioxide-based single crystal
CN110699670A (en) * 2019-11-13 2020-01-17 西安近代化学研究所 Preparation method of vanadium dioxide film

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