CN111204805A - Vanadium dioxide nanowire and preparation method and application thereof - Google Patents
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Abstract
The invention relates to the technical field of semiconductors, and provides a vanadium dioxide nanowire and a preparation method and application thereof, aiming at solving the problems of long growth period, low efficiency and small range of the traditional preparation process of the vanadium dioxide nanowire, wherein the vanadium dioxide nanowire is prepared by an epitaxial growth method, the vanadium dioxide nanowires are distributed in the same direction, the length of the vanadium dioxide nanowire is 3-13 mu m, the diameter of the vanadium dioxide nanowire is 0.3-1.2 mu m, and the length-diameter ratio of the vanadium dioxide nanowire is 2.5-43. The invention can realize the uniform epitaxial growth of the vanadium dioxide nanowire on the centimeter-sized substrate, has certain directionality, and the length of the vanadium dioxide nanowire can reach the micron-sized; the preparation method belongs to a physical vapor deposition method, and has the advantages of low cost, short period, high efficiency and high repeatability.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a large-scale epitaxially grown vanadium dioxide nanowire and a preparation method and application thereof.
Background
Vanadium is a group VB element, and in the oxides of vanadium, vanadium exists in +2, +3, +4, +5 or mixed valence states. Vanadium dioxide (VO2) is a typical metal-insulating phase change material. The resistance is reversibly changed by 3-5 orders of magnitude near the critical temperature (68 ℃), and the characteristics are accompanied with the conversion of optical and magnetic properties (from antiferromagnetic to paramagnetic), so that the vanadium dioxide has wide application prospects in the fields of field effect tubes, sensors, thermistors, optical information storage and the like. Several common methods for preparing nanowires include physical vapor deposition, foreign metal catalyzed gas-liquid-solid (VLS) method, etc. Dense nanowire arrays can produce similar effects to nano-pillars in nanocomposites, which can achieve volume strain with greater flexibility in material selection.
Although the vanadium dioxide nanowire can be prepared by the traditional physical vapor transport method, the vanadium dioxide powder is required to be used as a source, vanadium pentoxide is used as a catalyst, silicon is used as a substrate in the process, the growth period is long, the efficiency is low, the range is small, and the grown nanowire has no directionality; exotic metal catalyzed gas-liquid-solid processes require the formation of supersaturated eutectic liquids in order to minimize the unintentional doping effects of the catalyst on vanadium dioxide, another low vapor pressure metal catalyst that is quite difficult.
Chinese patent documents disclose a preparation method of an A-phase vanadium dioxide nanowire, and the application publication number is CN103663556A, in the invention, the addition of a surfactant enables an intermediate phase B to be rapidly converted into the A-phase vanadium dioxide, and the A-phase vanadium dioxide nanowire with excellent appearance and length-diameter ratio is formed, the prepared A-phase vanadium dioxide nanowire is very pure and very stable, but the vanadium dioxide nanowire prepared by the method has no directionality.
Based on the above analysis, a fast and effective method for realizing large-scale directional epitaxial growth of vanadium dioxide nanowires is still lacking at the present stage, and therefore a preparation method for directional nanowires capable of realizing large-scale epitaxial growth is urgently needed to be found.
Disclosure of Invention
The invention provides a vanadium dioxide nanowire which is epitaxially grown along a substrate in a large scale in order to overcome the problem that the traditional nanowire is not directional.
The invention provides a preparation method for large-scale epitaxial growth of vanadium dioxide nanowires, which aims to overcome the problems of long growth period, low efficiency and small range of the traditional preparation process of vanadium dioxide nanowires.
The invention also provides application of the vanadium dioxide nanowire in the fields of field effect tubes, sensors, thermistors and optical information storage.
In order to achieve the purpose, the invention adopts the following technical scheme:
the vanadium dioxide nanowires are prepared by an epitaxial growth method, are distributed in the same direction, and have the length of 3-13 microns, the diameter of 0.3-1.2 microns and the length-diameter ratio of 2.5-43.
The vanadium dioxide nanowire is a one-dimensional monoclinic phase vanadium dioxide nanowire, can realize uniform epitaxial growth on a centimeter-sized substrate, has certain directionality, can reach the micron-sized length, and can generate an effect similar to that of a nano column in a nano composite material due to the dense nanowire array, so that the volume strain can be realized, and the flexibility in material selection is higher.
A preparation method of vanadium dioxide nanowires comprises the following steps:
(1) cleaning the substrate;
(2) putting a vanadium source and a substrate into a heating container, then putting the heating container into a tube furnace, and controlling the vacuum degree in the furnace to be below 10 Pa; the heating container can be a heating vessel made of refractory materials such as quartz boats, crucibles and the like;
(3) introducing oxygen-argon mixed gas, heating the tube furnace, and preserving heat;
(4) introducing pure argon, cooling and then preserving heat;
(5) cooling and taking out the substrate, namely preparing the vanadium dioxide nanowire on the surface of the substrate; the cooling mode is natural cooling, and the sample can be taken out when the temperature reaches below 100 ℃.
The method belongs to a physical vapor deposition method, and has the advantages of low cost, short period, high efficiency and high repeatability; the vanadium dioxide nanowire can realize uniform epitaxial growth on a centimeter-sized substrate, has certain directionality, and the length of the vanadium dioxide nanowire can reach the micron-sized.
Preferably, in step (1), the substrate is a sapphire substrate; the sapphire substrate is cut in the r direction, the base surface is a (1-102) crystal face, and the single surface is polished.
Preferably, in the step (1), the cleaning process is to adopt absolute ethyl alcohol and deionized water to alternately circulate and ultrasonically clean for 10-20 min.
Preferably, in the step (2), the vanadium source is vanadium pentoxide.
Preferably, in step (2), the substrate is placed in the following manner: and (3) enabling the front surface of the substrate to face downwards, and enabling the front surface of the substrate to be 4-6 cm away from a vanadium source.
Preferably, in the step (3), the flow rate of the oxygen-argon mixed gas is 80 to 100 sccm. In the step, the flow of the gas is strictly controlled, and a growth template of vanadium pentoxide for the growth of the vanadium dioxide nanowire cannot be formed when the flow is too high or too low.
Preferably, in the step (3), the volume fraction of oxygen in the oxygen-argon mixed gas is 20%, and the volume fraction of argon is 80%. The proportion of gas in the oxygen-argon mixed gas is critical, wherein the over-high oxygen input can cause that the vanadium pentoxide can not be reduced into vanadium dioxide to form V6O13、V3O7When the oxygen is introduced into the vanadium oxide, the vanadium pentoxide is reduced into vanadium dioxide to form V2O3、V3O5And the like.
Preferably, in the step (4), the flow rate of the pure argon is 80-100 sccm. In the step, the effect of replacing gas with pure argon gas is to form a nanowire array, so that the growth of nanowires is promoted, the length of the grown nanowires is short due to too low flow of the pure argon gas, and the nanowires cannot be nucleated due to too high flow.
Preferably, in the step (3), the pressure in the furnace is controlled to be 110-150 Pa.
Preferably, in the step (3), the temperature rise time and the heat preservation time are both 30-40 min; the heat preservation temperature is 850-900 ℃.
Preferably, in the step (4), the temperature reduction range is reduced by 20 ℃ on the basis of the heat preservation temperature in the step (3); the heat preservation time is 10-15 min.
The vanadium dioxide nanowire has the characteristics of obvious quantum size effect, small size effect, surface effect, interface effect and the like, and can be widely applied to the fields of field effect tubes, sensors, thermistors, optical information storage and the like.
Therefore, the invention has the following beneficial effects:
(1) the invention can realize the uniform epitaxial growth of the vanadium dioxide nanowire on the centimeter-sized substrate, has certain directionality, and the length of the vanadium dioxide nanowire can reach the micron-sized;
(2) the preparation method belongs to a physical vapor deposition method, and has the advantages of low cost, short period, high efficiency and high repeatability;
(3) the vanadium dioxide nanowire has the characteristics of obvious quantum size effect, small size effect, surface effect, interface effect and the like, and can be widely applied to the fields of field effect tubes, sensors, thermistors, optical information storage and the like.
Drawings
FIG. 1 is a schematic view showing the structure of an apparatus used in the production process of the present invention.
Figure 2 is a low-magnification SEM image of vanadium dioxide nanowires prepared in example 1.
Figure 3 is a high-magnification SEM image of vanadium dioxide nanowires prepared in example 1.
Figure 4 is a low-magnification SEM image of vanadium dioxide nanowires prepared in example 2.
Figure 5 is a high-magnification SEM image of vanadium dioxide nanowires made in example 2.
Figure 6 is a low-magnification SEM image of vanadium dioxide nanowires made in example 3.
Figure 7 is a high-magnification SEM image of vanadium dioxide nanowires made in example 3.
Figure 8 is a low-magnification SEM image of vanadium dioxide nanowires made in example 4.
Figure 9 is a high-magnification SEM image of vanadium dioxide nanowires made in example 4.
Figure 10 is a physical representation of vanadium dioxide nanowires obtained by epitaxial growth of example 4 on a 0.8cm by 1.2cm sapphire substrate.
Figure 11 is a current-voltage graph of vanadium dioxide nanowires prepared in example 4.
Fig. 12 is an SEM image of vanadium dioxide nanowires prepared in comparative example 1.
Fig. 13 is an SEM image of vanadium dioxide nanowires prepared in comparative example 2.
Fig. 14 is an SEM image of vanadium dioxide nanowires prepared in comparative example 3.
In fig. 1: sapphire substrate 1, vanadium source 2, vacuum pump 3, sampler 4, quartz boat 5, gas circuit 6.
Detailed Description
The technical solution of the present invention is further specifically described below by using specific embodiments and with reference to the accompanying drawings.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
The following examples of the invention were all carried out in an apparatus as shown in FIG. 1: the operation steps of the equipment are as follows:
(1) placing the sapphire substrate 1 with the front surface facing downwards and vanadium pentoxide (vanadium source 2) in a quartz boat 5 in a drawing mode, placing the quartz boat in a tube furnace by using a sampler, and closing all gas paths 6;
(2) setting a program of temperature and time of the tube furnace in advance, turning on the vacuum pump 3, and continuously adjusting to enable the vacuum pump to reach a specified range;
(3) opening a gas path, introducing oxygen-argon mixed gas, and introducing pure argon after a specified time;
(4) and after naturally cooling, stopping introducing the gas, closing the vacuum pump 3, discharging the gas in the tube furnace out of the room, and taking out the substrate by using the sampler 4.
Example 1
(1) Alternately and repeatedly cleaning the sapphire substrate by using absolute ethyl alcohol and deionized water;
(2) putting vanadium pentoxide powder serving as a source into a quartz boat, putting the sapphire substrate at a position 4cm away from the source with the front surface facing downwards into a tube furnace, starting a vacuum pump, and reducing the vacuum degree to below 10 Pa; the sapphire substrate is cut in the r direction, a base plane is a (1-102) crystal plane, and single surface polishing is carried out;
(3) introducing 100sccm of mixed gas with the oxygen-argon content ratio of 20% to 80% into the furnace, keeping the pressure in the furnace at 130Pa, heating the tubular furnace to 870 ℃ within 30min, and keeping the temperature for 30 min;
(4) reducing the temperature to 850 ℃ within 5min, replacing the oxygen-argon mixed gas with pure argon, keeping the flow and the pressure unchanged, and keeping the temperature for 10 min;
(5) naturally cooling to below 100 ℃, taking out the substrate, and obtaining the vanadium dioxide nanowire on the surface of the substrate.
SEM tests were performed on the vanadium dioxide nanowires prepared in example 1, and the results are shown in fig. 2 and 3: most vanadium dioxide nanowires growing on the sapphire substrate have definite directionality, few nanowires have uncertain directions and belong to epitaxial growth, the length is about 3 micrometers, the diameter is 0.3-1.2 micrometers, and the length-diameter ratio is 2.5-43; the growth range is about 0.8cm x 1.2cm, and the thickness and the length are uniform.
Example 2
(1) Repeatedly cleaning the sapphire substrate by using absolute ethyl alcohol and deionized water;
(2) putting vanadium pentoxide powder serving as a source into a quartz boat, putting the sapphire substrate at a position 5cm away from the source with the front surface facing downwards into a tube furnace, starting a vacuum pump, and reducing the vacuum degree to below 10 Pa;
(3) introducing 100sccm oxygen-argon mixture with a content ratio of 20% to 80%, maintaining the pressure at about 130Pa, and maintaining the temperature of a tube furnace at about 870 deg.C for 30 min;
(4) reducing the temperature to about 850 ℃ within 5min, replacing the oxygen-argon mixed gas with pure argon, keeping the flow and the pressure unchanged, and keeping the temperature for 10 min;
(5) naturally cooling to below 100 ℃, taking out the substrate, and obtaining the vanadium dioxide nanowire on the surface of the substrate.
SEM tests were performed on the vanadium dioxide nanowires prepared in example 2, and the results are shown in fig. 4 and 5: most vanadium dioxide nanowires growing on the sapphire substrate have definite directionality, the length is about 10 mu m, the diameter is 0.3-1.2 mu m, and the length-diameter ratio is 2.5-43; the growth range was about 0.8cm by 1.2cm, and the nanowires grown under this process condition had a higher density and a longer length compared to the method of example 1.
Example 3
(1) Repeatedly cleaning the sapphire substrate by using absolute ethyl alcohol and deionized water;
(2) putting vanadium pentoxide powder serving as a source into a quartz boat, putting the sapphire substrate at a position 6cm away from the source with the front surface facing downwards into a tube furnace, starting a vacuum pump, and reducing the vacuum degree to below 10 Pa;
(3) introducing 100sccm oxygen-argon mixture with a content ratio of 20% to 80%, maintaining the pressure at about 130Pa, and maintaining the temperature of a tube furnace at about 870 deg.C for 30 min;
(4) reducing the temperature to about 850 ℃ within 5min, replacing the oxygen-argon mixed gas with pure argon, keeping the flow and the pressure unchanged, and keeping the temperature for 10 min;
(5) naturally cooling to below 100 ℃, taking out the substrate, and obtaining the vanadium dioxide nanowire on the surface of the substrate.
SEM tests were performed on the vanadium dioxide nanowires prepared in example 3, and the results are shown in fig. 6 and 7. Most vanadium dioxide nanowires growing on the sapphire substrate have a uniform direction, the length is about 7 microns, the diameter is 0.3-1.2 microns, and the length-diameter ratio is 2.5-43; the growth range is about 0.8cm x 1.2cm, the thickness difference is large, and the cross section of the grown nanowire is obviously observed to be rectangular.
Example 4
(1) Repeatedly cleaning the sapphire substrate by using absolute ethyl alcohol and deionized water;
(2) putting vanadium pentoxide powder serving as a source into a quartz boat, putting the sapphire substrate at a position 5cm away from the source with the front surface facing downwards into a tube furnace, starting a vacuum pump, and reducing the vacuum degree to below 10 Pa;
(3) firstly, introducing 100sccm of mixed gas with the oxygen-argon content ratio of 20 percent and 80 percent, keeping the pressure at about 130Pa, and keeping the temperature of a tubular furnace at about 870 ℃ for 30 min;
(4) secondly, reducing the temperature to about 850 ℃ within 5min, replacing the oxygen-argon mixed gas with pure argon, keeping the flow and the pressure unchanged, and keeping the temperature for 20 min;
(5) naturally cooling to below 100 ℃, taking out the substrate, and obtaining the vanadium dioxide nanowire on the surface of the substrate.
SEM tests were performed on the vanadium dioxide nanowires prepared in example 4, and the results are shown in fig. 8 and 9: most vanadium dioxide nanowires growing on the sapphire substrate have definite directionality, the length is about 13 microns, the diameter is 0.3-1.2 microns, and the length-diameter ratio is 2.5-43; the length difference is large, the growth density is large, and the thickness degree is uniform. The physical diagram of the vanadium dioxide nanowire of the present embodiment is shown in fig. 10, and the growth range is about 0.8cm x 1.2 cm. The current-voltage curve of the vanadium dioxide nanowire prepared by the embodiment is shown in fig. 11, which shows that the metal-insulator transition characteristic is good, and the vanadium dioxide nanowire has significant quantum size effect, small size effect, surface effect and interface effect, and can be widely applied to the fields of field effect tubes, sensors, thermistors, optical information storage and the like.
Example 5
(1) Alternately and repeatedly cleaning the sapphire substrate by using absolute ethyl alcohol and deionized water;
(2) putting vanadium pentoxide powder serving as a source into a quartz boat, putting the sapphire substrate with the front surface facing downwards at a position 6cm away from the source, putting the quartz boat into a tube furnace, starting a vacuum pump, and reducing the vacuum degree to below 10 Pa; the sapphire substrate is cut in the r direction, a base plane is a (1-102) crystal plane, and single surface polishing is carried out;
(3) introducing 80sccm of mixed gas with the oxygen-argon content ratio of 20 percent to 80 percent into the furnace, keeping the pressure in the furnace at 110Pa, heating the tubular furnace to 850 ℃ within 30min, and keeping the temperature for 40 min;
(4) reducing the temperature to 830 ℃ within 5min, replacing the oxygen-argon mixed gas with pure argon, keeping the flow and the pressure unchanged, and keeping the temperature for 12 min;
(5) naturally cooling to below 100 ℃, taking out the substrate, and obtaining the vanadium dioxide nanowire on the surface of the substrate.
Example 6
(1) Alternately and repeatedly cleaning the sapphire substrate by using absolute ethyl alcohol and deionized water;
(2) putting vanadium pentoxide powder serving as a source into a quartz boat, putting the sapphire substrate at a position 4.5cm away from the source with the front surface facing downwards into a tube furnace, starting a vacuum pump, and reducing the vacuum degree to below 10 Pa; the sapphire substrate is cut in the r direction, a base plane is a (1-102) crystal plane, and single surface polishing is carried out;
(3) introducing oxygen argon with the content ratio of 90sccm into the furnace as 20%: keeping the pressure in the furnace at 120Pa for 80% of mixed gas, heating the tube furnace to 900 ℃ within 30min, and keeping the temperature for 30 min;
(4) reducing the temperature to 875 ℃ within 5min, replacing the oxygen-argon mixed gas with pure argon, controlling the flow of the pure argon to be 80sccm, controlling the pressure in the furnace to be 110Pa, and keeping the temperature for 15 min;
(5) naturally cooling to below 100 ℃, taking out the substrate, and obtaining the vanadium dioxide nanowire on the surface of the substrate.
Comparative example 1 (gas flow rate too large)
Comparative example 1 is different from example 4 in that the flow rate of the gas introduced in step (3) and step (4) was 130sccm, and the rest of the process was identical to example 4.
The morphology of the vanadium dioxide nanowire prepared in the comparative example 1 is shown in fig. 12, and it can be seen that the prepared nanowire has extremely uneven thickness and small growth density, and even the grown nanowire is flat, because the template for nanowire growth cannot be well formed due to too high oxygen-argon mixed gas, and when the content of pure argon is too high, the nanowire cannot be normally nucleated in the growth process.
Comparative example 2 (sapphire crystal plane: 0001)
The difference between the comparative example 2 and the example 2 is that the crystal plane of the sapphire substrate used in the step (2) is (0001), the morphology of the vanadium dioxide prepared in the comparative example 2 is shown in fig. 13, and it can be seen that the prepared nanowires do not show an array of upright growth, and grow to show a growth direction of 60 ° or 120 °. Because the nanowire follows the principle of lattice matching in the growth process of the substrate, the two crystal planes of sapphire are different, so that the appearances of the nanowire are different.
Comparative example 3 (vanadium dioxide as vanadium source and silicon wafer as substrate)
Comparative example 3 the method of the example was not used, and a tube furnace was used as well, the operation was carried out for 1h from room temperature to 600 ℃, then 1h from 600 ℃ to 900 ℃, the temperature was maintained for 4h, and finally the temperature was naturally reduced, the pressure was maintained at 290-310 Pa and the flow rate was maintained at 35sccm throughout the process.
The morphology of the finally grown nanowires in the comparative example 3 is shown in fig. 14, and it can be seen that the nanowires have disordered growth directions and uneven thickness, cannot form array vertical growth, and have a small growth range.
The above description is only a preferred embodiment of the present invention, and does not limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (10)
1. The vanadium dioxide nanowires are characterized by being prepared by an epitaxial growth method, the vanadium dioxide nanowires are distributed in the same direction, the length of each vanadium dioxide nanowire is 3-13 microns, the diameter of each vanadium dioxide nanowire is 0.3-1.2 microns, and the length-diameter ratio of each vanadium dioxide nanowire is 2.5-43.
2. The method for preparing vanadium dioxide nanowires according to claim 1, comprising the steps of:
(1) cleaning the substrate;
(2) putting a vanadium source and a substrate into a heating container, then putting the heating container into a tube furnace, and controlling the vacuum degree in the furnace to be below 10 Pa;
(3) introducing oxygen and argon mixed gas, heating the tube furnace, and preserving heat;
(4) introducing pure argon, cooling and then preserving heat;
(5) and cooling and taking out the substrate, namely preparing the vanadium dioxide nanowire on the surface of the substrate.
3. The method for epitaxially growing large-scale vertical vanadium dioxide nanowires according to claim 2, wherein in the step (1), the vanadium source is vanadium pentoxide; the substrate is a sapphire substrate; the sapphire substrate is cut in the r direction, the base surface is a (1-102) crystal face, and the single surface is polished.
4. The method for epitaxially growing the large-scale vertical vanadium dioxide nanowires according to claim 2, wherein in the step (1), the cleaning process is ultrasonic cleaning with absolute ethyl alcohol and deionized water alternately and circularly for 10-20 min.
5. The method for epitaxially growing large-scale vertical vanadium dioxide nanowires according to claim 2, wherein in the step (2), the substrate is placed in a manner that: and (3) enabling the front surface of the substrate to face downwards, and enabling the front surface of the substrate to be 4-6 cm away from a vanadium source.
6. The method for epitaxially growing large-scale vertical vanadium dioxide nanowires according to claim 2, wherein in the step (3), the flow rate of the oxygen-argon mixed gas is 80-100 sccm; the volume fraction of oxygen in the oxygen-argon mixed gas is 20%, and the volume fraction of argon is 80%; in the step (4), the flow rate of the pure argon is 80-100 sccm.
7. The method for epitaxially growing the large-scale vertical vanadium dioxide nanowires according to claim 2, wherein in the step (3), the pressure in the tube is controlled to be 110-150 Pa.
8. The method for epitaxially growing the large-scale vertical vanadium dioxide nanowire according to claim 2, wherein in the step (3), the temperature rise time and the temperature preservation time are both 30-40 min; the heat preservation temperature is 850-900 ℃.
9. The method for epitaxially growing the large-scale vertical vanadium dioxide nanowires according to claim 2, wherein in the step (4), the temperature reduction range is reduced by 20-25 ℃ on the basis of the heat preservation temperature in the step (3); the heat preservation time is 10-15 min.
10. Use of vanadium dioxide nanowires according to claim 1 in the field of field effect tubes, sensors, thermistors, optical information storage.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111876826A (en) * | 2020-07-13 | 2020-11-03 | 暨南大学 | High-quality grass-shaped vanadium pentoxide crystal, preparation method thereof and low-dimensional material based on high-quality grass-shaped vanadium pentoxide crystal |
| CN112225250A (en) * | 2020-10-16 | 2021-01-15 | 成都先进金属材料产业技术研究院有限公司 | Method for self-reducing hydrothermal synthesis of vanadium dioxide nano powder |
| CN112225250B (en) * | 2020-10-16 | 2022-05-24 | 成都先进金属材料产业技术研究院有限公司 | Method for self-reduction hydrothermal synthesis of vanadium dioxide nano powder |
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