CN110589832A - SiC nanowire and preparation method and application thereof - Google Patents
SiC nanowire and preparation method and application thereof Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
Abstract
The invention provides a preparation method of a SiC nanowire, wherein the SiC nanowire is prepared by adopting a hot wire chemical vapor deposition method, and the specific method of the hot wire chemical vapor deposition method comprises the following steps: providing a substrate, and cleaning and drying the surface of the substrate; placing the substrate obtained by treatment in a deposition chamber of hot wire chemical vapor deposition equipment; introducing mixed gas containing carbon source gas and silicon source gas, keeping the distance between the substrate and the filament inside the equipment to be 16-18 mm, and under the conditions that the power of the filament is 6800-7000W and the temperature of the filament is 600-800 ℃; and preparing the SiC nanowire. The preparation method has simple process, low production cost and high speed; the length and the thickness of the prepared SiC nanowire can be accurately controlled, and the prepared SiC nanowire is uniform and stable and has high purity.
Description
Technical Field
The invention relates to the field of semiconductor and battery cathode materials, in particular to a SiC nanowire and a preparation method and application thereof.
Background
In recent years, semiconductor nanowires have unique electrical, optical, mechanical and other properties, and have wide application prospects in the field of novel nano optoelectronic devices, so that great attention is paid to researchers. The silicon carbide (SiC) semiconductor material is a third-generation semiconductor material developed after a first-generation element semiconductor material (Si) and a second-generation compound semiconductor material (GaAs, GaP, InP and the like), has the characteristics of indirect wide forbidden band, large breakdown electric field, high thermal conductivity, high electron saturation drift velocity and the like, and has great application prospect in the preparation of optoelectronic devices working under the extreme end environment of high temperature, high frequency, high power, radiation resistance and the like. At present, the research of SiC semiconductor materials focuses on two aspects, namely the growth of SiC single crystals and the synthesis of SiC nanowires. Besides the performance of a wide-band-gap semiconductor of the SiC nanowire, the SiC nanowire has more specificity in the aspects of mechanical property, luminous property, field emission property and the like due to a nanometer size effect, a specific morphology and an internal special structure and defects, so that the research on the synthesis, the structure and the performance of the SiC nanowire is of great significance. And secondly, the SiC nanowire has an excellent framework structure and can be used as a battery cathode material.
The SiC nanowire has the characteristics of indirect wide forbidden band, large breakdown electric field, high thermal conductivity, high electron saturation drift velocity and the like, so that the SiC nanowire has huge application prospect in the preparation of optoelectronic devices working under the extreme environments of high temperature, high frequency, high power, radiation resistance and the like. A great deal of time and energy is also put into the preparation of the SiC nanowires in all countries of the world, but the effect is not ideal. At present, the preparation of SiC nanowires still has the defects of complex preparation process, long time consumption, low yield, low purity and uneven thickness of the prepared SiC nanowires, difficult control of reaction and the like. The prepared nanowire has a complex preparation process and a long preparation period, the diameter of the prepared nanowire is not uniform, the purity of the prepared nanowire is low, and the service performance of a photoelectronic device or an electrochemical energy storage device prepared by the non-uniform nanowire can be greatly influenced.
Disclosure of Invention
The invention aims to provide a SiC nanowire and a preparation method and application thereof, and aims to solve the problems that in the prior art, the preparation process of the SiC nanowire is complicated, and the prepared SiC nanowire is low in purity and uneven in thickness.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of SiC nanowires is provided, wherein the SiC nanowires are prepared by a hot filament chemical vapor deposition method, and the specific method of the hot filament chemical vapor deposition method comprises the following steps:
providing a substrate, and cleaning and drying the surface of the substrate;
placing the substrate obtained by treatment in a deposition chamber of hot wire chemical vapor deposition equipment; introducing mixed gas containing carbon source gas and silicon source gas, keeping the distance between the substrate and the filament inside the equipment to be 16-18 mm, and under the conditions that the power of the filament is 6800-7000W and the temperature of the filament is 600-800 ℃; and preparing the SiC nanowire.
Correspondingly, the SiC nanowire is prepared by the preparation method of the SiC nanowire.
And the application of the SiC nanowire, wherein the SiC nanowire is applied to optoelectronic devices, electrochemical energy storage devices and battery materials.
The preparation method of the SiC nanowire provided by the invention adopts a hot filament chemical vapor deposition method for preparation, and particularly, the SiC nanowire is grown on the surface of the substrate through hot filament chemical vapor deposition by controlling the distance between the substrate and the filament, the power of the filament and the temperature of the filament in a straight-through manner, so that the length and the thickness of the prepared SiC nanowire can be accurately controlled, and the prepared SiC nanowire is uniform, stable and high in purity. The preparation method has simple process and low production cost, but greatly improves the production rate and greatly enhances the production controllability, thereby being beneficial to the large-scale production and application of SiC nanowire materials.
The SiC nanowire provided by the invention is prepared by the preparation method of the SiC nanowire. Compared with the SiC nanowire prepared in the prior art, the SiC nanowire prepared by the preparation method of the SiC nanowire has the advantages of controllable size, uniformity, stability, higher purity and contribution to wide application under the condition that the diameter of the SiC nanowire is different from dozens of to hundreds of nanometers.
The SiC nanowire is applied to optoelectronic devices, electrochemical energy storage devices and battery materials; by using the SiC nanowire, the good performance stability of a photoelectronic device, an electrochemical energy storage device and a battery material can be kept, and the excellent characteristics of long-term use can be kept.
Drawings
Fig. 1 is a diagram of an apparatus for preparing SiC nanowires by hot filament chemical vapor deposition provided in an embodiment of the present invention.
Fig. 2 is an electron microscope analysis diagram of the SiC nanowire prepared by the hot filament chemical vapor deposition method provided in embodiment 1 of the present invention.
Fig. 3 is an electron microscope analysis diagram of the SiC nanowire prepared by the hot filament chemical vapor deposition method provided in embodiment 1 of the present invention.
Fig. 4 is an electron microscope analysis diagram of the SiC nanowire prepared by the hot filament chemical vapor deposition method provided in embodiment 2 of the present invention.
FIG. 5 is an electron microscope analysis diagram of SiC nanowires prepared by a preparation method in the prior art according to a comparative example of the present invention.
Detailed Description
In order to make the objects, technical solutions and technical effects of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments obtained by a person of ordinary skill in the art without any inventive step in connection with the embodiments of the present invention shall fall within the scope of protection of the present invention.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The embodiment of the invention provides a preparation method of a SiC nanowire, the SiC nanowire is prepared by adopting a hot filament chemical vapor deposition method, the hot filament chemical vapor deposition refers to heating decomposition of carbon substances by using a glow tungsten filament and activation of chemical vapor phase reaction, and the method has the characteristics of simple equipment and easily controlled process conditions.
Specifically, the hot wire chemical vapor deposition method specifically comprises the following steps:
s01, providing a substrate, and cleaning and drying the surface of the substrate;
s02, placing the substrate obtained by treatment in a deposition chamber of hot wire chemical vapor deposition equipment; introducing mixed gas containing carbon source gas and silicon source gas, keeping the distance between the substrate and the filament inside the equipment to be 16-18 mm, and under the conditions that the power of the filament is 6800-7000W and the temperature of the filament is 600-800 ℃; and preparing the SiC nanowire. Specifically, in step S01, a substrate selected from any one of a cobalt-based alloy substrate, a nickel-based alloy substrate, and an iron-based substrate such as stainless steel is provided. When the hot wire chemical vapor deposition method is adopted for preparing the SiC nanowire, any one of the cobalt-based alloy substrate, the nickel-based alloy substrate and the iron-based substrate such as stainless steel is selected, the substrates contain at least one metal of nickel, cobalt and iron, and the metal of nickel, cobalt, iron and the like possibly plays a catalytic role in the hot wire chemical vapor deposition preparation process, so that the generation of the SiC nanowire is facilitated. In a preferred embodiment of the invention, the substrate is tungsten carbide.
Preferably, the thickness of the substrate is 1-5 mm. If the selected substrate is thin, the hardness of the substrate is not enough due to the fact that the substrate is too thin, and when the SiC nanowire grows, the SiC nanowire can be influenced, so that the growth of the SiC nanowire is influenced and is not beneficial to growth; if the substrate is chosen to be thicker, it is not favorable to control the distance between the substrate and the filament, and the growth of the SiC nanowire is also affected.
Preferably, in the step of surface cleaning and drying the substrate, an organic solvent is used to perform surface cleaning on the substrate. The substrate is cleaned by an organic solvent, mainly for removing impurities on the surface of the substrate and keeping the surface of the substrate clean and free of impurities, so that the grown SiC nanowire has high purity and is not influenced by the impurities. In a preferred embodiment of the present invention, the specific method for surface cleaning the substrate is as follows: and (3) selecting absolute ethyl alcohol, and placing the substrate in the absolute ethyl alcohol for ultrasonic cleaning for ten minutes to ensure that the substrate is clean and dustless.
Preferably, the substrate subjected to surface cleaning is subjected to a drying treatment to remove the solvent subjected to surface cleaning, so that the substrate is kept dry and tidy. It is further preferred that the drying process is carried out under an inert gas atmosphere so that the substrate does not undergo some other reaction and impurities are not formed. In a preferred embodiment of the present invention, a specific method of drying a substrate subjected to surface cleaning is as follows: and selecting nitrogen as inert gas atmosphere, and drying the substrate subjected to surface cleaning in the nitrogen atmosphere by blow drying.
Specifically, in step S02, the processed substrate is placed in a deposition chamber of a hot-wire chemical vapor deposition apparatus; preferably, the substrate obtained by the treatment is placed in a hot filament chemical vapor deposition device for treatment as shown in the attached figure 1, wherein a filament is used as a heat source and is arranged at the top end in the device; a substrate is placed directly below the filament; the base is placed above the heat conduction plate, the heat conduction plate is placed above the water cooling table, and the filament is made of tantalum wires. Preferably, the heat conducting disc is a graphite disc. In the preferred embodiment of the invention, nine tantalum wires with the length of 29cm and the distance of 1cm are selected as the filament. Specifically, mixed gas containing carbon source gas and silicon source gas is introduced, the introduced mixed gas contains the carbon source gas and the silicon source gas, carbon sources and silicon sources are mainly provided for preparing SiC nanowires, and the growth of the SiC nanowires is facilitated. Preferably, the carbon source gas is selected from methane, the purity of the methane is more than 99.99%, and methane gas with higher purity is provided, so that SiC nanowires grown in the reaction process have higher purity; preferably, the silicon source gas is selected from tetramethylsilane, and the volume percentage of the tetramethylsilane is 1% and the volume percentage of the hydrogen gas is 99% based on 100% of the total volume of the tetramethylsilane. If the ventilation amount of the tetramethylsilane is too large, the SiC nanowire cannot be obtained, and the SiC particle material is prepared; if the ventilation amount of tetramethylsilane is too small, the SiC nanowire cannot be obtained, and the diamond material is prepared.
Preferably, the mixed gas further comprises hydrogen, and the hydrogen is provided to provide an inert gas environment for the reaction, so as to avoid introducing impurities in the reaction.
More preferably, the ventilation amounts of the mixed gas are: 32-35 sccm of methane, 800-810 sccm of hydrogen and 80-81 sccm of tetramethylsilane. In the preferred embodiment of the invention, the ventilation amount of the mixed gas is 32sccm of methane; 800sccm of hydrogen; tetramethylsilane 80 sccm.
Specifically, the distance between the substrate and a filament inside the equipment is kept to be 16-18 mm, and under the conditions that the power of the filament is 6800-7000W and the temperature of the filament is 600-800 ℃; and controlling the distance between the substrate and the filament inside the equipment and the power of the filament, so as to control the temperature of the reaction and enable the temperature of the filament to be 600-800 ℃. If the distance between the filaments is too close or the power of the filaments is too high, the temperature is too high, and the SiC nanowires cannot be obtained under the condition of higher temperature during growth, but the diamond material is prepared; if the filament distance is too far or the filament power is too low, the temperature is too low, and the SiC nanowire cannot be obtained under the condition of higher temperature during growth, but the SiC particle material is prepared instead of the molded SiC nanowire material.
Preferably, the pressure inside the hot wire chemical vapor deposition equipment is 1500-1800 Pa, and the internal pressure is set to be 1500-1800 Pa, so that normal reaction is facilitated.
Preferably, in the step of preparing the SiC nanowire, the preparation time is 0.5-3 hours. The SiC nanowires are grown in the time, if the growth time is too short, the number of the obtained SiC nanowires is small, the adhesion force with the substrate is strong, and the SiC nanowires are difficult to separate; if the growth time is too long, the obtained SiC nanowires are too rich and are easy to partially fall off to cause unnecessary waste, and simultaneously, the SiC nanowires are easy to fall off from the substrate to influence the collection.
The preparation method of the SiC nanowire provided by the invention adopts a hot filament chemical vapor deposition method for preparation, and particularly, the SiC nanowire is grown on the surface of the substrate through hot filament chemical vapor deposition by controlling the distance between the substrate and the filament, the power of the filament and the temperature of the filament in a straight-through manner, so that the length and the thickness of the prepared SiC nanowire can be accurately controlled, and the prepared SiC nanowire is uniform, stable and high in purity. The preparation method has simple process and low production cost, but greatly improves the production rate and greatly enhances the production controllability, thereby being beneficial to the large-scale production and application of SiC nanowire materials.
Correspondingly, the embodiment of the invention also provides the SiC nanowire material, and the SiC nanowire material is prepared by the preparation method of the SiC nanowire material. Compared with the SiC nanowire prepared in the prior art, the SiC nanowire prepared by the preparation method of the SiC nanowire has the advantages of controllable size, uniformity, stability, higher purity and contribution to wide application under the condition that the diameter of the SiC nanowire is different from dozens of to hundreds of nanometers.
Preferably, the diameter of the SiC nanowire is 20-50 nm, and the prepared SiC nanowire is uniform in size, 20-50 nm in diameter, fine in diameter and controllable in size, and is beneficial to wide application.
Preferably, the purity of the SiC nanowire is more than or equal to 90%. The SiC nanowire prepared by the method has high purity, and is obtained by analyzing by a scanning electron microscope, on the substrate, the purity of the SiC nanowire is more than or equal to 90 percent, other impurities are hardly generated, and the application of the high-purity SiC nanowire is wider.
Correspondingly, the invention also provides an application of the SiC nanowire, and the SiC nanowire is applied to optoelectronic devices, electrochemical energy storage devices and battery materials. By using the SiC nanowire, the good performance stability of a photoelectronic device, an electrochemical energy storage device and a battery material can be kept, and the excellent characteristics of long-term use can be kept.
The following further describes specific embodiments.
Example 1
A preparation method of SiC nanowires is provided, wherein the SiC nanowires are prepared by a hot filament chemical vapor deposition method, and the specific method of the hot filament chemical vapor deposition method comprises the following steps:
providing a tungsten carbide substrate, ultrasonically cleaning the substrate for ten minutes by using alcohol, and blow-drying the substrate by using nitrogen for later use;
placing the treated substrate in hot wire chemical vapor deposition equipment, wherein nine flat wires with the length of 29cm and the distance of 1cm are used as filaments in the equipment, and a graphite plate is used as a heat conduction plate; keeping the distance between the substrate and a filament inside the equipment to be 16mm, setting the power of the filament to be 6800W, and setting the temperature of the filament to be 600 ℃; introducing mixed gas of methane, hydrogen and tetramethylsilane for reaction, wherein the ventilation rate of the mixed gas is 32sccm of methane, 800sccm of hydrogen and 80sccm of tetramethylsilane respectively; reacting for three hours to prepare the SiC nanowire, wherein the diameter of the SiC nanowire is 20-50 nm; the purity is more than or equal to 90 percent.
Example 2
A preparation method of SiC nanowires is provided, wherein the SiC nanowires are prepared by a hot filament chemical vapor deposition method, and the specific method of the hot filament chemical vapor deposition method comprises the following steps:
providing a tungsten carbide substrate, ultrasonically cleaning the substrate for ten minutes by using alcohol, and blow-drying the substrate by using nitrogen for later use;
placing the treated substrate in hot wire chemical vapor deposition equipment, wherein nine flat wires with the length of 29cm and the distance of 1cm are used as filaments in the equipment, and a graphite plate is used as a heat conduction plate; keeping the distance between the substrate and a filament inside the equipment to be 18mm, setting the power of the filament to be 7000W, and setting the temperature of the filament to be 800 ℃; introducing mixed gas of methane, hydrogen and tetramethylsilane for reaction, wherein the ventilation rate of the mixed gas is 32sccm of methane, 800sccm of hydrogen and 80sccm of tetramethylsilane respectively; reacting for three hours to prepare the SiC nanowire, wherein the diameter of the SiC nanowire is 20-50 nm; the purity is more than or equal to 90 percent.
Example 3
A preparation method of SiC nanowires is provided, wherein the SiC nanowires are prepared by a hot filament chemical vapor deposition method, and the specific method of the hot filament chemical vapor deposition method comprises the following steps:
providing a tungsten carbide substrate, ultrasonically cleaning the substrate for ten minutes by using alcohol, and blow-drying the substrate by using nitrogen for later use;
placing the treated substrate in hot wire chemical vapor deposition equipment, wherein nine flat wires with the length of 29cm and the distance of 1cm are used as filaments in the equipment, and a graphite plate is used as a heat conduction plate; keeping the distance between the substrate and a filament inside the equipment to be 17mm, setting the power of the filament to be 6900W, and setting the temperature of the filament to be 700 ℃; introducing mixed gas of methane, hydrogen and tetramethylsilane for reaction, wherein the ventilation rate of the mixed gas is 32sccm of methane, 800sccm of hydrogen and 80sccm of tetramethylsilane respectively; and reacting for three hours to prepare the SiC nanowire, wherein the diameter of the SiC nanowire is 20-50 nm, and the purity is more than or equal to 90%.
Example 4
A preparation method of SiC nanowires is provided, wherein the SiC nanowires are prepared by a hot filament chemical vapor deposition method, and the specific method of the hot filament chemical vapor deposition method comprises the following steps:
providing a cobalt-based alloy substrate, ultrasonically cleaning the substrate for ten minutes by using alcohol, and blow-drying the substrate by using nitrogen for later use;
placing the treated substrate in hot wire chemical vapor deposition equipment, wherein nine flat wires with the length of 29cm and the distance of 1cm are used as filaments in the equipment, and a graphite plate is used as a heat conduction plate; keeping the distance between the substrate and a filament inside the equipment to be 18mm, setting the power of the filament to be 7000W, and setting the temperature of the filament to be 800 ℃; introducing mixed gas of methane, hydrogen and tetramethylsilane for reaction, wherein the ventilation rate of the mixed gas is 32sccm of methane, 800sccm of hydrogen and 80sccm of tetramethylsilane respectively; and reacting for three hours to prepare the SiC nanowire, wherein the diameter of the SiC nanowire is 20-50 nm, and the purity is more than or equal to 90%.
Example 5
A preparation method of SiC nanowires is provided, wherein the SiC nanowires are prepared by a hot filament chemical vapor deposition method, and the specific method of the hot filament chemical vapor deposition method comprises the following steps:
providing a stainless steel substrate, ultrasonically cleaning the substrate for ten minutes by using alcohol, and blow-drying the substrate by using nitrogen for later use;
placing the treated substrate in hot wire chemical vapor deposition equipment, wherein nine flat wires with the length of 29cm and the distance of 1cm are used as filaments in the equipment, and a graphite plate is used as a heat conduction plate; keeping the distance between the substrate and a filament inside the equipment to be 18mm, setting the power of the filament to be 7000W, and setting the temperature of the filament to be 800 ℃; introducing mixed gas of methane, hydrogen and tetramethylsilane for reaction, wherein the ventilation rate of the mixed gas is 32sccm of methane, 800sccm of hydrogen and 80sccm of tetramethylsilane respectively; and reacting for three hours to prepare the SiC nanowire, wherein the diameter of the SiC nanowire is 20-50 nm, and the purity is more than or equal to 90%.
Example 6
A preparation method of SiC nanowires is provided, wherein the SiC nanowires are prepared by a hot filament chemical vapor deposition method, and the specific method of the hot filament chemical vapor deposition method comprises the following steps:
providing a tungsten carbide substrate, ultrasonically cleaning the substrate for ten minutes by using alcohol, and blow-drying the substrate by using nitrogen for later use;
placing the treated substrate in hot wire chemical vapor deposition equipment, wherein nine flat wires with the length of 29cm and the distance of 1cm are used as filaments in the equipment, and a graphite plate is used as a heat conduction plate; keeping the distance between the substrate and a filament inside the equipment to be 16mm, setting the power of the filament to be 6800W, and setting the temperature of the filament to be 600 ℃; introducing mixed gas of methane, hydrogen and tetramethylsilane for reaction, wherein the ventilation rate of the mixed gas is 35sccm of methane, 810sccm of hydrogen and 81sccm of tetramethylsilane; and reacting for three hours to prepare the SiC nanowire, wherein the diameter of the SiC nanowire is 20-50 nm, and the purity is more than or equal to 90%.
Example 7
A preparation method of SiC nanowires is provided, wherein the SiC nanowires are prepared by a hot filament chemical vapor deposition method, and the specific method of the hot filament chemical vapor deposition method comprises the following steps:
providing a tungsten carbide substrate, ultrasonically cleaning the substrate for ten minutes by using alcohol, and blow-drying the substrate by using nitrogen for later use;
placing the treated substrate in hot wire chemical vapor deposition equipment, wherein nine flat wires with the length of 29cm and the distance of 1cm are used as filaments in the equipment, and a graphite plate is used as a heat conduction plate; keeping the distance between the substrate and a filament inside the equipment to be 16mm, setting the power of the filament to be 6800W, and setting the temperature of the filament to be 600 ℃; introducing mixed gas of methane, hydrogen and tetramethylsilane for reaction, wherein the ventilation rate of the mixed gas is 34sccm of methane, 805sccm of hydrogen and 81sccm of tetramethylsilane; and reacting for three hours to prepare the SiC nanowire, wherein the diameter of the SiC nanowire is 20-50 nm, and the purity is more than or equal to 90%.
Example 8
A preparation method of SiC nanowires is provided, wherein the SiC nanowires are prepared by a hot filament chemical vapor deposition method, and the specific method of the hot filament chemical vapor deposition method comprises the following steps:
providing a tungsten carbide substrate, ultrasonically cleaning the substrate for ten minutes by using alcohol, and blow-drying the substrate by using nitrogen for later use;
placing the treated substrate in hot wire chemical vapor deposition equipment, wherein nine flat wires with the length of 29cm and the distance of 1cm are used as filaments in the equipment, and a graphite plate is used as a heat conduction plate; keeping the distance between the substrate and a filament inside the equipment to be 16mm, setting the power of the filament to be 6800W, and setting the temperature of the filament to be 600 ℃; introducing mixed gas of methane, hydrogen and tetramethylsilane for reaction, wherein the ventilation rate of the mixed gas is 32sccm of methane, 800sccm of hydrogen and 80sccm of tetramethylsilane respectively; reacting for 2 hours to prepare the SiC nanowire, wherein the diameter of the SiC nanowire is 20-50 nm, and the purity is more than or equal to 90%.
Example 9
A preparation method of SiC nanowires is provided, wherein the SiC nanowires are prepared by a hot filament chemical vapor deposition method, and the specific method of the hot filament chemical vapor deposition method comprises the following steps:
providing a tungsten carbide substrate, ultrasonically cleaning the substrate for ten minutes by using alcohol, and blow-drying the substrate by using nitrogen for later use;
placing the treated substrate in hot wire chemical vapor deposition equipment, wherein nine flat wires with the length of 29cm and the distance of 1cm are used as filaments in the equipment, and a graphite plate is used as a heat conduction plate; keeping the distance between the substrate and a filament inside the equipment to be 16mm, setting the power of the filament to be 6800W, and setting the temperature of the filament to be 600 ℃; introducing mixed gas of methane, hydrogen and tetramethylsilane for reaction, wherein the ventilation rate of the mixed gas is 32sccm of methane, 800sccm of hydrogen and 80sccm of tetramethylsilane respectively; and reacting for 1 hour to prepare the SiC nanowire, wherein the diameter of the SiC nanowire is 20-50 nm, and the purity is more than or equal to 90%.
Example 10
A preparation method of SiC nanowires is provided, wherein the SiC nanowires are prepared by a hot filament chemical vapor deposition method, and the specific method of the hot filament chemical vapor deposition method comprises the following steps:
providing a tungsten carbide substrate, ultrasonically cleaning the substrate for ten minutes by using alcohol, and blow-drying the substrate by using nitrogen for later use;
placing the treated substrate in hot wire chemical vapor deposition equipment, wherein nine flat wires with the length of 29cm and the distance of 1cm are used as filaments in the equipment, and a graphite plate is used as a heat conduction plate; keeping the distance between the substrate and a filament inside the equipment to be 16mm, setting the power of the filament to be 6800W, and setting the temperature of the filament to be 600 ℃; introducing mixed gas of methane, hydrogen and tetramethylsilane for reaction, wherein the ventilation rate of the mixed gas is 32sccm of methane, 800sccm of hydrogen and 80sccm of tetramethylsilane respectively; and reacting for 0.5 hour to prepare the SiC nanowire, wherein the diameter of the SiC nanowire is 20-50 nm, and the purity is more than or equal to 90%.
Comparative example
The SiC is prepared by adopting the method for preparing SiC in the prior art.
Further analysis is performed on the SiC nanowires prepared in the above examples 1-2 and comparative example, and electron microscope analysis graphs of the SiC nanowire prepared in the example 1 are shown in the attached drawings 2 and 3, which clearly show that the prepared SiC material has a nanowire structure, is uniform in size, has no impurities, and is high in purity. An electron microscope analysis chart of the SiC nanowire prepared in the embodiment 2 is shown in a figure 4, and the prepared SiC nanowire is of a nanowire structure, the diameter of the SiC nanowire is 20-50 nm, the size of the SiC nanowire is controllable, and the SiC nanowire is uniform in size; and the purity reaches more than 90 percent, the purity is higher, and no impurities exist. An electron microscope analysis chart of the SiC material prepared by the comparative example is shown in FIG. 5, and the prepared SiC material is in an agglomerated granular shape and is not in a dispersed linear shape; non-uniform in size; meanwhile, as can be seen from the figure, the SiC material is doped with diamond impurities, the white particles are diamonds, the black particles are SiC, wherein the content of the diamond impurities is 25% -35%, the content of the SiC is 65% -75%, and the purity is low; the SiC material has different particle sizes of 30-80 nm, and the size is not controllable, so that the subsequent use is not facilitated.
In conclusion, the SiC nanowires prepared by the hot wire chemical vapor deposition method provided by the invention have the advantages of controllable size, uniformity, stability, higher purity and contribution to wide application.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The preparation method of the SiC nanowire is characterized in that the SiC nanowire is prepared by adopting a hot wire chemical vapor deposition method, and the specific method of the hot wire chemical vapor deposition method comprises the following steps:
providing a substrate, and cleaning and drying the surface of the substrate;
placing the substrate obtained by treatment in a deposition chamber of hot wire chemical vapor deposition equipment; introducing mixed gas containing carbon source gas and silicon source gas, keeping the distance between the substrate and the filament inside the equipment to be 16-18 mm, and under the conditions that the power of the filament is 6800-7000W and the temperature of the filament is 600-800 ℃; and preparing the SiC nanowire.
2. The method of producing the SiC nanowire according to claim 1, wherein in the step of producing the SiC nanowire, an internal pressure of the deposition chamber is 1500 to 1800 Pa.
3. The method for preparing SiC nanowires according to claim 1, wherein the mixed gas further comprises hydrogen, and/or;
the carbon source gas is selected from methane, and the purity of the methane is more than 99.99%; and/or the presence of a gas in the gas,
the silicon source gas is selected from tetramethylsilane, and the silicon source gas comprises, by volume, 1% of tetramethylsilane and 99% of hydrogen, wherein the total volume of the tetramethylsilane is 100%.
4. The method for producing SiC nanowires according to claim 3, wherein the mixed gas has a ventilation amount of: 32-35 sccm of methane, 800-810 sccm of hydrogen and 80-81 sccm of tetramethylsilane.
5. The method for preparing SiC nanowires according to any one of claims 1 to 4, wherein in the step of preparing SiC nanowires, the preparation time is 0.5 to 3 hours.
6. The method for preparing SiC nanowires according to any one of claims 1 to 4, wherein the substrate is selected from any one of a cobalt-based alloy substrate, a nickel-based alloy substrate, and an iron-based substrate such as stainless steel.
7. The method for preparing SiC nanowires according to any one of claims 1 to 4, wherein the substrate has a thickness of 1 to 5 mm.
8. An SiC nanowire, characterized in that the SiC nanowire is prepared by the method for preparing an SiC nanowire according to any one of claims 1 to 7.
9. The SiC nanowire of claim 8, wherein the SiC nanowire has a diameter of 20-50 nm; and/or the presence of a gas in the gas,
the purity of the SiC nanowire is more than or equal to 90 percent.
10. The application of the SiC nanowire is characterized in that the SiC nanowire is applied to optoelectronic devices, electrochemical energy storage devices and battery materials.
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