CN115312373B - Preparation method of SiC nanowire functional film - Google Patents

Preparation method of SiC nanowire functional film Download PDF

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CN115312373B
CN115312373B CN202211003031.3A CN202211003031A CN115312373B CN 115312373 B CN115312373 B CN 115312373B CN 202211003031 A CN202211003031 A CN 202211003031A CN 115312373 B CN115312373 B CN 115312373B
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silicon carbide
nanowire
film
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nanowires
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CN115312373A (en
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牛晓巍
刘雪冰
王紫暄
马馨宇
阳肖
杨兆滢
翟配郴
尉国栋
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Shenyang University
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Abstract

The invention discloses a preparation method of a silicon carbide nanowire functional film, which comprises the following steps: the substrate is used as a cathode electrode, and the platinum sheet is used as an anode electrode; placing an electrode in a silicon carbide nanowire suspension; and applying voltage and stirring the solution by using a magnetic stirrer, and combining chemical nickel plating, welding and transferring processes to finally obtain the uniform and compact silicon carbide nanowire film. The method has the advantages of simple process, low cost, high efficiency, safety, easy operation, contribution to commercial mass production, integration of the advantages of one-dimensional nanowires and films, large size, large specific surface area, flexibility, no microtubule defect, uniformity and compactness. In addition, the invention provides an effective bottom-up mode for assembling the nano structure, has universality for almost all low-dimensional nano structures, and can be used for referring to the preparation of other semiconductor nano films.

Description

Preparation method of SiC nanowire functional film
Technical Field
The invention belongs to the technical field of semiconductor nanowire material preparation, and particularly relates to a preparation method of a silicon carbide nanowire functional film.
Background
As a third generation wide band gap semiconductor, silicon carbide (SiC) is one of the most important candidate materials for high performance semiconductor devices, and when the size of SiC material is in nano scale, it shows many excellent properties different from bulk materials, especially a nano thin film material composed of self-assembled low dimensional nano structures from bottom to top is of great interest, and the nano thin film has the characteristics of high porosity, better flexibility, high specific surface area, and interconnected pore structures. The one-dimensional nano material, such as a nanowire, a nanotube and the like, is assembled into a macroscopic thin film material, is obviously different from the traditional thin film material (an epitaxial monocrystalline thin film or a thin film formed by nano particles), can retain the characteristics of the one-dimensional nano material, can be used as a macroscopic two-dimensional material, and has the characteristics of two-dimensional easy processing, compatibility with a semiconductor plane processing technology and the like.
In recent years, the preparation technology of nanowires has been well-established, but the technology of connecting nano devices made of nano materials is not needed, which is similar to the technology of welding industrial products, and how to connect the nanowires together, and meanwhile, the structure of the nanowires is not damaged, which is still in the exploration stage, and is a leading problem in the world. Nanometer manufacturing is the basis for realizing the mass production of nanometer structures, devices and systems, nanometer connection is a key technology of nanometer manufacturing, the problem of nanometer connection is solved, and nanometer devices made of nanometer wires (tubes) can be assembled into nanometer robots in the future, so that large-scale industrialized production of biomolecular motors, nanometer motors and the like is possible. Therefore, how to better realize the welding of the nanowires is always a focus of scientists in various countries, becomes a research direction of a plurality of scholars at home and abroad in recent years, and has high application value.
However, nanowire bonding reported so far is mostly focused on bonding between the same metal nanowire (thin film) or different metal nanowires (thin films), and silicon carbide nanowire thin film bonding is still freshly reported. As in document 1 (PHYSICAL REVIEW B, 80, 2009, 155403), an arc welding method is adopted, direct current is directly introduced after a nano Pt wire and a nano Au wire are lapped on a nano operation platform, so that the area at the crossing point of the nano wire in the film is joule heated to realize welding; document 2 (Small, 1, 2005, 1221-1229.) adopts an electron beam welding method, and uses a high-energy electron beam to weld three nano gold wires and gold nanowires and monocrystalline silicon nanowires, and the welding effect of the method is relatively good, and the method can be used for welding dissimilar materials, but has high cost and is unfavorable for large-area preparation; document 3 (APPLIED PHYSICS LETTERS, 86, 2005, 033112.) discloses a laser welding method for nanowelding gold nanoparticles, which is simple and efficient, but the heating easily breaks the structure of the film itself, and affects the performance of the film. Aiming at the defects or the existing demands of the prior art, the welding of the silicon carbide nanowire film still faces a plurality of problems, and a preparation method of the SiC nanowire film which is universal, large in area, high in efficiency, low in cost and good in welding point contact is urgently required to be developed.
Disclosure of Invention
The invention aims to solve the problem of realizing the research and development of a preparation method based on a silicon carbide nanowire functional film.
The invention discloses a preparation method of a silicon carbide nanowire functional film, which comprises the following steps:
(1) Preparation of silicon carbide aerogel: and dissolving polycarbosilane and vinyl compound in an organic solvent, carrying out catalytic reaction on the polycarbosilane and the vinyl compound under the anaerobic condition of 70-90 ℃ and under the Karstedt catalyst of 4-8 h to obtain polycarbosilane gel, drying the polycarbosilane gel to obtain polycarbosilane aerogel, carrying out heat treatment on the polycarbosilane aerogel to obtain silicon carbide/carbon precursor aerogel, mixing the silicon carbide/carbon precursor aerogel with rice husk carbon and silicon according to a certain proportion, and calcining the mixture at 1000-1800 ℃ under the anaerobic argon protection condition to obtain silicon carbide aerogel of 0.5-5 h. The vinyl compound contains two or more vinyl groups;
(2) Treatment of silicon carbide nanowires: weighing silicon carbide aerogel prepared by 5g, respectively ultrasonically cleaning 10-20 min in acetone, absolute ethyl alcohol and deionized water, immersing in 98% hydrofluoric acid solution of 100-500 mL, and ultrasonically dispersing under ultraviolet irradiation for 0.5-3 h. After the ultrasonic treatment is finished, standing for 30-500 min, pouring out supernatant (90-450 mL), and obtaining the solution A. Adding a certain amount of deionized water (90-450 mL) into the solution A, and performing ultrasonic dispersion treatment and separation by ultraviolet light. Repeating the steps for 5-8 times, putting the solution A into a centrifuge tube, centrifuging to obtain SiC nanowires, dispersing the SiC nanowires into deionized water, centrifuging the SiC nanowires until the PH value of the solution is 7, obtaining single crystal silicon carbide nanowires which are free of impurities, monodisperse, 3C in crystalline phase, 3.21 g/cc in density, 50-300 nm in diameter and 10-100 mu m in length and uniform in size distribution, drying and storing for later use. The silicon carbide nanowire treatment process is carried out in an ultrasonic bath environment, and parameters of the ultrasonic bath are as follows: the ultrasonic power is 150W, the solution temperature is 30-50 ℃, the ultraviolet light parameter is the wavelength 365-nm, and the optical power is 5-10W;
(3) Doping treatment of silicon carbide nanowires: weighing 0.05-0.2 g of silicon carbide nanowire obtained in the step (2) and n-type and p-type doping sources of 0.005-0.02 g respectively, wherein the mass ratio of the silicon carbide nanowire to the n-type and p-type doping sources is 10:1, uniformly mixing the samples, then filling the mixed samples into a platinum pipe with the pipe length of 15 cm, the pipe inner diameter of 1 cm and the pipe wall thickness of 2 mm, and sealing the platinum pipe with the pressure of 1 mTorr in the platinum pipe after pipe sealing. Heating the sealed platinum pipe in a muffle furnace at a heating rate of 3-10 ℃ per minute, a heating temperature of 1000-1400 ℃ and a heat preservation time of 60-600 min, naturally cooling the sample to room temperature along with the furnace after heating is completed, and taking out;
(4) Annealing treatment of the silicon carbide nanowires: annealing the sample by adopting a tube furnace, wherein the annealing treatment temperature is 500-1000 ℃ and the annealing time is 60-120 min;
(5) Preparing a silicon carbide-Si nanowire core-shell structure: adding Si powder of 0.005-0.008-g into the silicon carbide nanowire treated in the step (4) of 0.01-0.04 g, mixing uniformly, and then filling into a platinum tube for sealing. And (3) placing the sealed platinum pipe into a muffle furnace for heating, wherein the heating rate is 3-10 ℃ per minute, the heating temperature is 1400-1550 ℃, the heat preservation time is 60-600 min, and taking out the sample after the sample is naturally cooled to room temperature along with the furnace after the heating is completed. Wherein the grain size of Si powder is 30 nm, the purity is 99.9%, and the thickness of an epitaxial Si layer is 10-30 nm;
(6) Configuration of silicon carbide nanowire suspension: weighing 0.05-0.1 g silicon carbide-Si nanowire core-shell structure sample prepared in the step (5), adding the sample into 100 mL isopropanol or ethylene glycol solution, and adding 0.075 g sodium dodecyl benzene sulfonate and 0.0025 g aluminum nitrate as dispersing agents and conductive solutes respectively to realize the directional movement of the nanowire in an electrostatic field. Dispersing 30-50 min by ultraviolet and ultrasonic to form stable suspension, and storing the suspension at low temperature for later use after the ultrasonic treatment is finished;
(7) Substrate processing: cutting monocrystalline silicon wafers with the size of 1 multiplied by 1 to 10 multiplied by 10 cm 2, respectively carrying out ultrasonic cleaning on the monocrystalline silicon wafers in acetone, absolute ethyl alcohol and deionized water for 15 to 20 min, taking out the monocrystalline silicon wafers and placing the monocrystalline silicon wafers in an oven at the temperature of 60 to 80 ℃ for drying for 10 to 20 min and storing the monocrystalline silicon wafers for later use;
(8) And (3) electrophoretic deposition: taking the silicon carbide nanowire suspension prepared in the step (6) as an electrophoretic deposition solution, taking a substrate as a negative electrode, taking a platinum sheet as a positive electrode, placing the electrodes in the deposition solution, taking a direct current power supply as an electrophoresis apparatus, applying a constant voltage of 50-100V, and carrying out electrophoretic deposition of 6-15 min under the condition that a magnetic stirrer stirs the solution to obtain a uniformly deposited and compact silicon carbide nanowire film;
(9) Nanowire welding: and (3) placing the sample obtained in the step (8) into a plasma bonding machine for welding. Firstly, argon plasma is adopted to treat the surface of the silicon carbide film at 500-1000 ℃ for 5-60 min, then 5-10 MPa force is applied, and 30-60 min is welded in a high-temperature furnace at 1000-1500 ℃, so that large-area welding of the silicon carbide nanometer is realized, and the preparation of a nanowire network film is realized;
(10) Gao Wenjian, combination: and (3) carrying out surface bonding enhancement treatment on the nanowire film prepared in the step (9). Firstly, adopting NH 3 plasma to treat 5-60 min at 500-1000 ℃, and then bonding the materials at constant temperature in a high-temperature furnace under the protection of argon at 1000-1200 ℃ for 30-60 min;
(11) Peeling the nanowire film: and (3) placing the nanowire film prepared in the step (10) into a spin coater with the rotation speed of 500-900 rpm, uniformly coating 3-6 drops of PVA glue solution on the surface of the film, and physically stripping the film after drying each drop of PVA glue solution with 20-100 mu L. Finally, washing the PVA film on the surface of the film by deionized water;
(12) Vapor deposition electrode: evaporating a layer of ordered nickel electrode array on the surface of the prepared film by using a thermal electron beam, wherein the evaporating time is 5-20 min, the distance between two adjacent electrodes is 40-200 mu m, and the thickness of the electrodes is 100-300 nm;
(13) Annealing: and (3) putting the film evaporated with the electrode into a vacuum annealing furnace for annealing, wherein the annealing temperature is 800-1000 ℃, the heating rate is 10-60 ℃/min, and the annealing time is 60-200 min.
The beneficial effects are that: compared with the reported method for preparing the silicon carbide nanowire film
(1) The invention has the main advantages of being capable of preparing the silicon carbide nanowire film with high quality, good electric contact and application to electronic devices. Compared with the epitaxial film (prepared based on the CVD principle) commonly used in the industry at present, the film integrates all the advantages of a one-dimensional nanowire (electrons are transmitted along the axial direction of the nanowire, the electron is transmitted quickly), has no fatal micropipe defect, has the advantages of flexibility and film (large-scale device integration by means of a semiconductor plane process is convenient), and has the advantages of large size, large specific surface area, uniformity and compactness;
(2) The nanowire is formed by welding, the original linear structure of the nanowire is not damaged, ohmic contact is formed between the nanowire and the nanowire, and contact resistance between the nanowire is avoided (nickel and silicon form nickel-silicon intermetallic compound with good conductivity at high temperature). Electrons can be transported from one nanowire to another nanowire along a network without loss, the nano welding process is simple and feasible, time-saving and efficient, the equipment cost is low, large-scale processing can be realized, and the research and development of high-speed electronic devices are expected to be realized;
(3) The invention provides an effective bottom-up nano structure assembling mode for preparing the silicon carbide nanowire film for the electronic device, and the method has the advantages of simple process, low cost, large prepared film area, flexibility, high efficiency, safety and easy operation;
(4) The invention has universality to almost all low-dimensional nano structures, and can be used for preparing other semiconductor nano films.
Drawings
FIG. 1 is a diagram of a silicon carbide nanowire aerogel made in accordance with an embodiment of the present invention;
FIG. 2 is an XRD pattern of a silicon carbide nanowire aerogel prepared in accordance with an embodiment of the present invention;
FIG. 3 is a TEM image of an epitaxial carbon layer of silicon carbide nanowires produced in accordance with an example of the present invention;
FIG. 4 is a HRTEM diagram of an epitaxial carbon layer of a silicon carbide nanowire fabricated according to an embodiment of the present invention;
FIG. 5 is a schematic diagram of a mechanism of electrophoretic deposition according to an embodiment of the present invention;
FIG. 6 is an SEM image of a functional film of silicon carbide nanowires fabricated by soldering a carbon layer according to an embodiment of the present invention;
FIG. 7 is a schematic diagram of a functional thin film photodetector device with silicon carbide nanowires according to an embodiment of the present invention.
Detailed Description
In order to make the technical scheme of the invention clear, the technical scheme of the invention is fully and completely described below.
Embodiment one: preparation of silicon carbide nanowire functional film by means of carbon layer welding
(1) Preparation of silicon carbide aerogel: and dissolving polycarbosilane and vinyl compound in an organic solvent, carrying out catalytic reaction on the polycarbosilane and the vinyl compound under the anaerobic condition of 70-90 ℃ and under the Karstedt catalyst of 4-8 h to obtain polycarbosilane gel, drying the polycarbosilane gel to obtain polycarbosilane aerogel, carrying out heat treatment on the polycarbosilane aerogel to obtain silicon carbide/carbon precursor aerogel, mixing the silicon carbide/carbon precursor aerogel with rice husk carbon and silicon according to a certain proportion, and calcining the mixture at 1000-1800 ℃ under the anaerobic argon protection condition to obtain silicon carbide aerogel of 0.5-5 h. The vinyl compound contains two or more vinyl groups;
(2) Treatment of silicon carbide nanowires: weighing silicon carbide aerogel prepared by 5g, respectively ultrasonically cleaning 10-20 min in acetone, absolute ethyl alcohol and deionized water, immersing in 98% hydrofluoric acid solution of 100-500 mL, and ultrasonically dispersing under ultraviolet irradiation for 0.5-3 h. After the ultrasonic treatment is finished, standing for 30-500 min, pouring out supernatant (90-450 mL), and obtaining the solution A. Adding a certain amount of deionized water (90-450 mL) into the solution A, and performing ultrasonic dispersion treatment and separation by ultraviolet light. Repeating the steps for 5-8 times, putting the solution A into a centrifuge tube, centrifuging to obtain SiC nanowires, dispersing the SiC nanowires into deionized water, centrifuging the SiC nanowires until the PH value of the solution is 7, obtaining single crystal silicon carbide nanowires which are free of impurities, monodisperse, 3C in crystalline phase, 3.21 g/cc in density, 50-300 nm in diameter and 10-100 mu m in length and uniform in size distribution, drying and storing for later use. The silicon carbide nanowire treatment process is carried out in an ultrasonic bath environment, and parameters of the ultrasonic bath are as follows: the ultrasonic power is 150W, the solution temperature is 30-50 ℃, the ultraviolet light parameter is the wavelength 365-nm, and the optical power is 5-10W;
(3) Doping treatment of silicon carbide nanowires: weighing 0.05-0.2 g of silicon carbide nanowire obtained in the step (2) and n-type and p-type doping sources of 0.005-0.02 g respectively, wherein the mass ratio of the silicon carbide nanowire to the n-type and p-type doping sources is 10:1, uniformly mixing the samples, then filling the mixed samples into a platinum pipe with the pipe length of 15 cm, the pipe inner diameter of 1 cm and the pipe wall thickness of 2 mm, and sealing the platinum pipe with the pressure of 1 mTorr in the platinum pipe after pipe sealing. Heating the sealed platinum pipe in a muffle furnace at a heating rate of 3-10 ℃ per minute, a heating temperature of 1000-1400 ℃ and a heat preservation time of 60-600 min, naturally cooling the sample to room temperature along with the furnace after heating is completed, and taking out;
(4) Annealing treatment of the silicon carbide nanowires: annealing the sample by adopting a tube furnace, wherein the annealing treatment temperature is 500-1000 ℃ and the annealing time is 60-120 min;
(5) Silicon carbide nanowire epitaxial carbon layer: taking 0.01-0.04 g of doped silicon carbide raw material obtained in the step (4), uniformly mixing polystyrene of 0.0007-0.0028 g, and filling the mixture into a platinum pipe for sealing. Heating the sealed platinum pipe in a muffle furnace at a heating rate of 3-10 ℃ per minute, a heating temperature of 800-1000 ℃ and a heat preservation time of 60-600 min, naturally cooling the sample to room temperature along with the furnace after heating, and taking out the sample, wherein the thickness of an epitaxial carbon layer is 10-30 nm;
(6) Configuration of silicon carbide nanowire suspension: weighing the silicon carbide nano wire with the epitaxial carbon layer of 0.05-0.1 g prepared in the step (5), adding the silicon carbide nano wire into 100 mL isopropanol or ethylene glycol solution, and adding 0.075 g sodium dodecyl benzene sulfonate and 0.0025 g aluminum nitrate as dispersing agents and conductive solutes respectively to realize the directional movement of the nano wire in an electrostatic field. Dispersing 30-50 min by ultraviolet and ultrasonic to form stable suspension, and storing the suspension at low temperature for later use after the ultrasonic treatment is finished;
(7) Substrate processing: cutting the substrate with the size of 1 multiplied by 1 to 10 multiplied by 10 cm 2, respectively carrying out ultrasonic cleaning on the substrate in acetone, absolute ethyl alcohol and deionized water for 15 to 20min, taking out the substrate and placing the substrate in an oven at 60 to 80 ℃ for drying for 10 to 20min, and storing the substrate for later use;
(8) And (3) electrophoretic deposition: taking the silicon carbide nanowire suspension prepared in the step (6) as an electrophoretic deposition solution, taking a substrate as a negative electrode, taking a platinum sheet as a positive electrode, placing the electrodes in the deposition solution, taking a direct current power supply as an electrophoresis apparatus, applying a constant voltage of 50-100V, and carrying out electrophoretic deposition of 6-15 min under the condition that a magnetic stirrer stirs the solution to obtain a uniformly deposited and compact silicon carbide nanowire film;
(9) Nanowire welding: and (3) placing the sample obtained in the step (8) into a plasma bonding machine for welding. Firstly, argon plasma is adopted to treat the surface of the silicon carbide film at 500-1000 ℃ for 5-60 min, then 5-10 MPa force is applied, and 30-60 min is welded in a high-temperature furnace at 1000-1500 ℃, so that large-area welding of the silicon carbide nanometer is realized, and the preparation of a nanowire network film is realized;
(10) Gao Wenjian, combination: and (3) carrying out surface bonding enhancement treatment on the nanowire film prepared in the step (9). Firstly, adopting NH 3 plasma to treat 5-60 min at 500-1000 ℃, and then bonding the materials at constant temperature in a high-temperature furnace under the protection of argon at 1000-1200 ℃ for 30-60 min;
(11) Peeling the nanowire film: and (3) placing the nanowire film prepared in the step (10) into a spin coater with the rotation speed of 500-900 rpm, uniformly coating 3-6 drops of PVA glue solution on the surface of the film, and physically stripping the film after drying each drop of PVA glue solution with 20-100 mu L. Finally, washing the PVA film on the surface of the film by deionized water;
(12) Vapor deposition electrode: evaporating a layer of ordered nickel electrode array on the surface of the prepared film by using a thermal electron beam, wherein the evaporating time is 5-20 min, the distance between two adjacent electrodes is 40-200 mu m, and the thickness of the electrodes is 100-300 nm;
(13) Annealing: and (3) putting the film evaporated with the electrode into a vacuum annealing furnace for annealing, wherein the annealing temperature is 800-1000 ℃, the heating rate is 10-60 ℃/min, and the annealing time is 60-200 min.
Embodiment two: preparation of silicon carbide nanowire functional film by means of C60 welding
(1) The same as in step (1) of the first embodiment;
(2) The same as in step (2) of the first embodiment;
(3) The same as in step (3) of the first embodiment;
(4) The same as in step (4) of the first embodiment;
(5) C60 modified silicon carbide nanowires: adding a certain amount of the silicon carbide nanowire treated in the step (4) into a prepared C60 ethanol solution with a certain concentration of 250 mL, stirring and reacting at 60-90 ℃ for 30-60 min, and then filtering, cleaning and drying to obtain the C60 modified silicon carbide nanowire;
(6) Configuration of silicon carbide nanowire suspension: weighing 0.05-0.1 g C60 modified silicon carbide nano wire prepared in the step (5), adding the silicon carbide nano wire into 100mL isopropanol or glycol solution, and adding 0.075 g sodium dodecyl benzene sulfonate and 0.0025 g aluminum nitrate as dispersing agent and conductive solute respectively, so as to realize the directional movement of the nano wire in an electrostatic field. Dispersing 30-50 min by ultraviolet and ultrasonic to form stable suspension, and storing the suspension at low temperature for later use after the ultrasonic treatment is finished;
(7) The same as in step (7) of the first embodiment;
(8) The same as in step (8) of the first embodiment;
(9) The same as in step (9) of the first embodiment;
(10) The same as in step (10) of the first embodiment;
(11) The same as in step (11) of the first embodiment;
(12) The same as in step (12) of the first embodiment;
(13) The same as in step (13) of the first embodiment.
Embodiment III: preparation of silicon carbide nanowire functional film by means of graphene welding
(1) The same as in step (1) in embodiment one;
(2) The same as in step (2) of embodiment one;
(3) The same as in step (3) of embodiment one;
(4) The same as in step (4) of embodiment one;
(5) Preparing a silicon carbide nanowire epitaxial graphene core-shell structure: carrying out high-temperature pyrolysis on the SiC nanowires to obtain epitaxial graphene, adopting a high-temperature vacuum carbon tube furnace, modulating the vacuum degree to 10 -1 Pa, placing the cleaned SiC into a graphite crucible with a cover, heating in the vacuum carbon tube furnace, firstly, rapidly heating to 1200-1400 ℃ at a speed of 60 ℃/min, slowly heating to a required pyrolysis temperature (1350-1650 ℃) at a heating speed of 4-40 ℃/min, and finally, carrying out heat preservation at the required temperature for a certain time to recombine surface carbon atoms;
(6) Configuration of silicon carbide nanowire suspension: weighing 0.05-0.1 g silicon carbide nanowire epitaxial graphene core-shell structure sample prepared in the step (5), adding the sample into 100mL isopropanol or ethylene glycol solution, and adding 0.075 g sodium dodecyl benzene sulfonate and 0.0025 g aluminum nitrate as a dispersing agent and a conductive solute respectively to realize directional movement of the nanowire in an electrostatic field. Dispersing 30-50 min by ultraviolet and ultrasonic to form stable suspension, and storing the suspension at low temperature for later use after the ultrasonic treatment is finished;
(7) The same as in step (7) of embodiment one;
(8) The same as in step (8) of embodiment one;
(9) The same as in step (9) of embodiment one;
(10) The same as in step (10) of embodiment one;
(11) The same as in step (11) of embodiment one;
(12) The same as in step (12) of embodiment one;
(13) The same as in step (13) of embodiment one.
Embodiment four: preparation of silicon carbide nanowire functional film by means of silicon carbide-Si nanowire core-shell structure
(1) The same as in step (1) in embodiment one;
(2) The same as in step (2) of embodiment one;
(3) The same as in step (3) of embodiment one;
(4) The same as in step (4) of embodiment one;
(5) Preparing a silicon carbide-Si nanowire core-shell structure: adding Si powder of 0.005-0.008-g into the silicon carbide nanowire treated in the step (4) of 0.01-0.04 g, mixing uniformly, and then filling into a platinum tube for sealing. And (3) placing the sealed platinum pipe into a muffle furnace for heating, wherein the heating rate is 3-10 ℃ per minute, the heating temperature is 1400-1550 ℃, the heat preservation time is 60-600 min, and taking out the sample after the sample is naturally cooled to room temperature along with the furnace after the heating is completed. Wherein the grain size of Si powder is 30 nm, the purity is 99.9%, and the thickness of an epitaxial Si layer is 10-30 nm;
(6) Configuration of silicon carbide nanowire suspension: weighing 0.05-0.1 g silicon carbide-Si nanowire core-shell structure sample prepared in the step (5), adding the sample into 100 mL isopropanol or ethylene glycol solution, and adding 0.075 g sodium dodecyl benzene sulfonate and 0.0025 g aluminum nitrate as dispersing agents and conductive solutes respectively to realize the directional movement of the nanowire in an electrostatic field. Dispersing 30-50 min by ultraviolet and ultrasonic to form stable suspension, and storing the suspension at low temperature for later use after the ultrasonic treatment is finished;
(7) The same as in step (7) of embodiment one;
(8) The same as in step (8) of embodiment one;
(9) The same as in step (9) of embodiment one;
(10) The same as in step (10) of embodiment one;
(11) The same as in step (11) of embodiment one;
(12) The same as in step (12) of embodiment one;
(13) The same as in step (13) of embodiment one.
Fifth embodiment: preparation of silicon carbide nanowire functional film by means of nickel plating of silicon carbide nanowire
(1) The same as in step (1) in embodiment one;
(2) The same as in step (2) of embodiment one;
(3) The same as in step (3) of embodiment one;
(4) The same as in step (4) of embodiment one;
(5) Nickel plating of silicon carbide nanowires: adding a certain amount of the silicon carbide nanowire treated in the step (4) into the prepared chemical nickel plating solution of 250 mL, stirring at 60-90 ℃ for reaction for 30-60 min, and then filtering, cleaning and drying to obtain the nickel-coated silicon carbide nanowire;
(6) Configuration of silicon carbide nanowire suspension: weighing 0.05-0.1 g nickel-coated silicon carbide nanowire prepared in the step (5), adding the nickel-coated silicon carbide nanowire into 100 mL isopropanol or ethylene glycol solution, and adding 0.075 g sodium dodecyl benzene sulfonate and 0.0025 g aluminum nitrate to serve as a dispersing agent and a conductive solute respectively, so that the directional movement of the nanowire in an electrostatic field is realized. Dispersing 30-50 min by ultraviolet and ultrasonic to form stable suspension, and storing the suspension at low temperature for later use after the ultrasonic treatment is finished;
(7) The same as in step (7) of embodiment one;
(8) The same as in step (8) of embodiment one;
(9) The same as in step (9) of embodiment one;
(10) The same as in step (10) of embodiment one;
(11) The same as in step (11) of embodiment one;
(12) The same as in step (12) of embodiment one;
(13) The same as in step (13) of embodiment one.
The last points to be described are: while the invention has been described in detail in the foregoing general description and with reference to specific embodiments, the foregoing embodiments are merely illustrative of the technical aspects of the invention and are not limiting thereof; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. The preparation method of the silicon carbide nanowire functional film is characterized by comprising the following steps of:
(1) Preparation of silicon carbide aerogel: dissolving polycarbosilane and vinyl compound in an organic solvent, carrying out catalytic reaction on the polycarbosilane and the vinyl compound under the anaerobic condition of 70-90 ℃ and under the Karstedt catalyst of 4-8 h to obtain polycarbosilane gel, then drying the polycarbosilane gel to obtain polycarbosilane aerogel, carrying out heat treatment on the polycarbosilane aerogel to obtain silicon carbide/carbon precursor aerogel, mixing the silicon carbide/carbon precursor aerogel with rice husk carbon and silicon according to a certain proportion, and calcining the mixture at 1000-1800 ℃ under the anaerobic argon protection condition to obtain silicon carbide aerogel of 0.5-5 h;
(2) Treatment of silicon carbide nanowires: weighing 1-5 g silicon carbide aerogel prepared in the step (1), respectively ultrasonically cleaning 10-20 min in acetone and deionized water, immersing in 98% hydrofluoric acid solution of 100-500 mL, and ultrasonically dispersing under ultraviolet irradiation for 0.5-3 h; after the ultrasonic treatment is finished, standing for 30-500 min, pouring out supernatant (90-450 mL) into a beaker, and obtaining a solution A from the rest solution; adding a certain amount of deionized water (90-450 mL) into the solution A, and performing ultrasonic dispersion treatment and separation by ultraviolet light; repeating the steps for 5-8 times, putting the solution A into a centrifuge tube, centrifuging to obtain SiC nanowires, dispersing the SiC nanowires into deionized water, centrifuging, repeating the operation until the PH value of the solution is 7, obtaining single crystal silicon carbide nanowires which are free of impurities, monodisperse and uniform in size distribution, drying and storing for later use;
(3) Doping treatment of silicon carbide nanowires: weighing a certain amount of the sample obtained in the step (1) and an n-type and p-type doping source respectively, uniformly mixing, and then filling the mixture into a platinum pipe for sealing; heating the sealed platinum pipe in a muffle furnace at a heating rate of 3-10 ℃ per minute, a heating temperature of 1000-1400 ℃ and a heat preservation time of 60-600 min, naturally cooling the sample to room temperature along with the furnace after heating is completed, and taking out;
(4) Annealing treatment of the silicon carbide nanowires: annealing the sample prepared in the step (3) by adopting a tube furnace, wherein the annealing treatment temperature is 500-1000 ℃ and the annealing time is 60-120 min;
(5) Preparing a silicon carbide-Si nanowire core-shell structure: adding a certain amount of Si powder into a certain amount of the silicon carbide nanowire treated in the step (4), uniformly mixing, and then filling into a platinum pipe for sealing; heating the sealed platinum pipe in a muffle furnace at a heating rate of 3-10 ℃ per minute, a heating temperature of 1400-1550 ℃ and a heat preservation time of 60-600 min, naturally cooling the sample to room temperature along with the furnace after heating is completed, and taking out;
(6) Configuration of silicon carbide nanowire suspension: weighing a certain amount of silicon carbide-Si nanowire core-shell structure samples obtained in the step (5), adding sodium dodecyl benzene sulfonate and aluminum nitrate into isopropanol or ethylene glycol solution, performing ultraviolet ultrasonic dispersion for 30-50 min to form stable suspension, and storing the suspension at a low temperature for later use after ultrasonic treatment is completed;
(7) Substrate processing: cutting the substrate with the size of 1 multiplied by 1 to 10 multiplied by 10 cm 2, respectively carrying out ultrasonic cleaning on the substrate in acetone, absolute ethyl alcohol and deionized water for 15 to 20min, taking out the substrate and placing the substrate in an oven at 60 to 80 ℃ for drying for 10 to 20min, and storing the substrate for later use;
(8) And (3) electrophoretic deposition: taking the prepared silicon carbide nanowire suspension as an electrophoretic deposition solution, taking a substrate as a cathode electrode, taking a platinum sheet as an anode electrode, placing the electrode in the deposition solution, taking a direct current power supply as an electrophoresis apparatus, applying constant voltage, and carrying out electrophoretic deposition on the solution under the condition of stirring the solution by a magnetic stirrer to obtain a uniformly deposited and compact silicon carbide nanowire film;
(9) Nanowire welding: placing the sample obtained in the step (8) into a plasma bonding machine for welding; firstly, argon plasma is adopted to treat the surface of a film at 500-1000 ℃, then 5-60 min ℃ is applied, 5-10 MPa force is applied, 30-60 min is welded in a high-temperature furnace with the temperature of 1000-1500 ℃, the welding of large-area silicon carbide nanowires is realized, and the preparation of a nanowire network functional film is realized;
(10) Gao Wenjian, combination: carrying out surface bonding enhancement treatment on the nanowire film prepared in the step (9); firstly, adopting NH 3 plasma to treat 5-60 min at 500-1000 ℃, and then bonding the materials at constant temperature in a high-temperature furnace under the protection of argon at 1000-1200 ℃ for 30-60 min;
(11) Peeling the nanowire film: placing the nanowire film prepared in the step (10) into a spin coater with the rotation speed of 500-900 rpm, uniformly coating 3-6 drops of PVA glue solution on the surface of the film, wherein each drop is 20-100 mu L, and physically stripping the film after drying; finally, washing the PVA film on the surface of the film by deionized water;
(12) Vapor deposition electrode: evaporating a layer of ordered nickel electrode array on the surface of the prepared film by using a thermal electron beam, wherein the evaporating time is 5-20 min, the distance between two adjacent electrodes is 40-200 mu m, and the thickness of the electrodes is 100-300 nm;
(13) Annealing: and (3) putting the film evaporated with the electrode into a vacuum annealing furnace for annealing, wherein the annealing temperature is 800-1000 ℃, the heating rate is 10-60 ℃/min, and the annealing time is 60-200 min.
2. The vinyl compound according to claim 1, wherein the vinyl compound contains two or more vinyl groups, the total concentration of polycarbosilane and vinyl compound in the organic solvent is 0.03 to 0.3 g/mL, the organic solvent is one selected from cyclohexane, toluene, xylene and benzene, and the drying means supercritical drying or freeze drying.
3. The silicon carbide/carbon precursor aerogel, rice hull carbon and silicon according to claim 1, step (1), wherein the proportions are 1 to 0.5:0.8:0.1 to 0.3, wherein the rice hull carbon has commercial granularity of 200 meshes and purity of 99 percent.
4. The silicon carbide nanowire treatment process of claim 1, step (2), performed in an ultrasonic bath environment, parameters of the ultrasonic bath: the ultrasonic power is 150W, the solution temperature is 20-30 ℃, the ultraviolet light parameter is the wavelength 365-nm, and the optical power is 5-10W.
5. The sealed platinum pipe according to claim 1, wherein the sample materials contained in step (3) are: the silicon carbide raw material obtained by the step (2) is 0.05-0.2 g, the ammonium chloride (aluminum chloride) or the n-type and p-type doping source is 0.005-0.02 g, and the mass ratio of the silicon carbide to the ammonium chloride (aluminum chloride) or the n-type and p-type doping source is 10:1.
6. The n-type or p-type dopant source of claim 1 in step (3) is: the n-type doping sources are: the melamine, ammonium bicarbonate, ammonium nitrate, urea, oxalic acid, red phosphorus, black phosphorus, and P-type doping sources include boron, aluminum nitrate, aluminum chloride, boron chloride, and sealed platinum pipe parameters are as follows: the tube length is 15 cm, the tube inner diameter is 1 cm, the tube wall thickness is 2 mm, and the pressure in the platinum tube after tube sealing is 1 millitorr.
7. The silicon carbide-Si nanowire core-shell structure sample material of step (5) of claim 1 is: the doped silicon carbide raw material obtained in the step (3) is 0.01-0.04 g, si powder is 0.005-0.008 g, wherein the particle size of the Si powder is 30 nm, the purity is 99.9%, and the thickness of an epitaxial Si layer is 10-30 nm.
8. According to the method in the step (6) of claim 1, 0.05-0.1 g of 3C-silicon carbide nanowires are added into each hundred milliliters of isopropanol or ethylene glycol, and 0.075 g sodium dodecyl benzene sulfonate and 0.0025 g aluminum nitrate are respectively added into each hundred milliliters of solution to serve as dispersing agents and conductive solvents, so that the nanowires can move directionally in an electrostatic field.
9. The selection of the substrate in step (7) according to claim 1: cu, PET, GP, si, ITO.
10. The electrode spacing of step (8) of claim 1, wherein the constant current voltage is between 50 and 100V.
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