CN111441087B - Preparation method of 6H-silicon carbide two-dimensional single crystal nanosheet - Google Patents

Preparation method of 6H-silicon carbide two-dimensional single crystal nanosheet Download PDF

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CN111441087B
CN111441087B CN202010254990.7A CN202010254990A CN111441087B CN 111441087 B CN111441087 B CN 111441087B CN 202010254990 A CN202010254990 A CN 202010254990A CN 111441087 B CN111441087 B CN 111441087B
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CN111441087A (en
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尉国栋
段明娜
万宁
刘红梅
杜晓波
周密
纪媛
付成伟
韩炜
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Jilin University
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    • C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
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Abstract

The invention discloses a preparation method of a 6H-silicon carbide single crystal two-dimensional nanosheet, which comprises the following steps: ultrasonically pickling the silicon carbide nano-particles with 6H crystal phase subjected to neutron radiation by using mixed acid prepared by HF and HCl; washing sequentially by deionized water and absolute ethyl alcohol, and drying in vacuum; then uniformly mixing the silicon carbide nano particles subjected to acid treatment with ammonium chloride or a doping source, and sealing in a quartz tube; heating the quartz tube with the sample in a muffle furnace, naturally cooling the sample to room temperature along with the furnace after heating, taking out, ultrasonically cleaning the sample with absolute ethyl alcohol and deionized water in sequence, and drying in vacuum; the silicon carbide of the invention has the characteristics of low price of raw materials, wide sources, uniform nano-scale, good crystal quality, good monodispersity, large yield, simple preparation and synthesis process, short preparation time, no need of expensive equipment, safety and easy operation, is beneficial to realizing the rapid preparation of large-size two-dimensional silicon carbide materials, and can realize synchronous doping and uniform doping.

Description

Preparation method of 6H-silicon carbide two-dimensional single crystal nanosheet
Technical Field
The invention belongs to the technical field of preparation of silicon carbide nano materials, and particularly relates to a preparation method based on silicon carbide two-dimensional nanosheets.
Background
By two-dimensional material is meant a material with dimensions in two dimensions up to the nanometer scale (1-100nm), and its electrons are free to move (planar motion) only in the nanometer scale of two dimensions. Two-dimensional materials are confined to two-dimensional planes due to their carrier transport and thermal diffusion, making such materials exhibit many unique properties. So far, the two-dimensional materials mainly have structures such as nano-films, superlattices, quantum wells, nano-sheets and the like. Since the 2004 university of manchester, geom group successfully separated the two-dimensional graphene with a monoatomic layer, the two-dimensional nanomaterial has a unique nanosheet structure, a large surface area and extraordinary physicochemical properties, and has attracted great interest to researchers. Since then, many other types of two-dimensional nanomaterials, including black phosphorus, molybdenum disulfide, transition metal carbides, MXene, nitrides, carbonitrides, layered double hydroxides, MOF nanoplates, and the like, have become hot research points in the semiconductor nano field. The two-dimensional nanosheet material has a series of excellent physicochemical properties such as high mechanical flexibility, large specific surface area, rich active sites, stable chemical properties and the like, and is widely applied to various fields such as catalysis, biology, electrochemical energy storage and the like, such as photo/electro-catalysts, semiconductor photoelectric devices, lithium batteries, nuclear magnetic resonance imaging and the like.
The 6H silicon carbide, as the third-generation semiconductor which is the most mature and commercial in research and has the most commercial application value, has the characteristics of wide band gap, low price, wide source, strong thermal stability, high thermal conductivity carrier, large saturation input rate, excellent radiation resistance and the like, and becomes a research hotspot in the field of novel semiconductor materials, so the 6H polytype is the most common semiconductor in industrial application. However, almost all the SiC nanomaterials reported at present are focused on 3C-SiC thin film materials, and 6H-SiC two-dimensional nanosheets are still rarely reported, for example, document 1(ACS appl.mater.interfaces,2019,11,42, 39109-. So that the following disadvantages exist in the process of preparing the two-dimensional silicon carbide nanosheet: (1) the catalyst is epitaxially grown, so that the sample yield is small, and the method is not suitable for industrial mass production; (2) because the raw material adopts silicon dioxide, the product has low purity and is easy to be polluted by silicon oxide; (3) effective doping and simultaneous doping cannot be achieved. In the prior invention patent 1 (patent name: preparation method and flow of two-dimensional flaky SiC material), a microwave method is reported to synthesize a two-dimensional flaky SiC product, but the prepared two-dimensional flaky crystal structure is poor, and the sheets are mutually glued and assembled into a large-size irregular granular product. In the prior invention patent 2 (patent name: synthesis of two-dimensional SiC ultrathin nano structure by using graphene as template molten salt method and preparation method thereof), SiC ultrathin nanosheets are prepared by using graphene as template high-temperature molten salt, but the pictures given in the patent show that the SiC crystal prepared by the method has poor crystallinity. Document 2(Journal of Alloys and Compounds,5,345-. According to the reported invention patents and literature reports, the following defects exist in the process of preparing the two-dimensional silicon carbide nanosheet: (1) epitaxial growth on a substrate by means of a catalyst is required. By means of the catalyst epitaxial growth, not only the sample yield is small and easy to be polluted by doping of metal, but also an expensive single crystal substrate is required, and the method is obviously not suitable for industrial mass production; (2) the product is impure and has poor crystallinity. Because most of the raw materials in the carbothermic reduction technology adopt silicon dioxide, the self property of the silicon dioxide easily causes low purity of the product and is easily polluted by amorphous silicon oxide; (3) effective doping and simultaneous doping cannot be achieved. (4) The product cost is high. Most reports require expensive equipment such as chemical vapor deposition systems, precise temperature control and gas routing systems, and cumbersome manufacturing processes. Therefore, the preparation of the high-quality 6H-SiC two-dimensional single crystal nanosheet still faces a plurality of problems, and a universal, low-cost and high-quality preparation method is urgently needed to be developed.
Disclosure of Invention
The invention aims to solve the problem of research and development of a preparation method based on a synchronously-doped 6H-SiC two-dimensional single crystal nanosheet.
Specifically, silicon carbide nanoparticles treated by neutron radiation and mixed acid of HF and HCl are used as a precursor, ammonium chloride is used as an etching agent and a doping source (or aluminum chloride and an n-type or p-type doping source), and a high-temperature heating method is adopted to dissociate a single-crystal nanowire into two-dimensional nanosheets along a specific crystal orientation direction under the combined action of high-pressure chloride ions and doping ions, so that the uniformly-doped silicon carbide two-dimensional single-crystal nanosheets are finally obtained. The invention provides a preparation method of a SiC two-dimensional nanosheet, which has the advantages of high crystal quality, high yield, no need of expensive equipment, an accurate gas control system and a doping system, safety and easiness in operation. The invention is expected to solve the bottleneck problems that the 6H-silicon carbide two-dimensional nano material is difficult to prepare with high quality and synchronous doping and uniform doping cannot be effectively realized based on the traditional carbothermic reduction technology and the single crystal substrate epitaxy technology at present.
The invention discloses a preparation method of uniformly doped 6H-silicon carbide single crystal two-dimensional nanosheets, which comprises the following steps:
(1) weighing 10 g of 6H-SiC nanoparticles prepared by a chemical vapor deposition method, putting the nanoparticles into a lead box, and putting the lead box into a neutron activation chamber. Irradiating the nanoparticles in fast neutron source for 70-85min (irradiation range of 10k-10M eV), with equivalent fast neutron fluence of 1 × 1013-1×1015n/cm2Total dose of gamma radiation of 1X 105-3×105And (7) rad. The 6H-SiC nanoparticles are prepared by chemical vapor deposition method and have a density of 3.21g/cc, a diameter of about 0.1-0.6 μm and a thickness of about 0.35-0.7mm
(2) And putting the 6H-SiC nano-particles subjected to radiation treatment into mixed acid for acid etching, wherein the mixed acid is prepared by mixing the following components in a volume ratio of 1: 1 HF and HCl, containing 0.05g of sodium dodecylbenzenesulfonate per hundred milliliters of solution. The 6H-SiC nanoparticle acid treatment process is carried out in the environment of an ultrasonic bath, and the whole solution is placed in a polytetrafluoroethylene container, wherein the ultrasonic power of the ultrasonic bath is 150W, and the temperature of the solution is 40 ℃. And ultrasonically dispersing the silicon carbide nano-particles in the mixed acid solution for 5-20 minutes, and etching for 60-120 minutes by using ethanol and ferric chloride solution, wherein the ethanol and the ferric chloride solution are prepared by dissolving 1-5g of ferric chloride in one hundred milliliters of ethanol solution. Then adding deionized water for dilution, repeating the process for 5-8 times, and after the pH value of the solution is greater than 4, washing and centrifuging the silicon carbide sample by 50-100mL of deionized water and 50-100mL of absolute ethyl alcohol in sequence, wherein the centrifugation conditions are as follows: 4000 and 5000r/min, and centrifuging for 5-10 min. Then the mixture is put into an oven with the temperature of 60-80 ℃ for vacuum drying for 24-36 hours for standby.
(3) Doping silicon carbide nanoparticles: 0.05-0.2g of silicon carbide obtained in the step (2) and 0.005-0.02g of ammonium chloride (or aluminum chloride, n-type or p-type doping source) are weighed respectively, and the mass ratio of the silicon carbide to the ammonium chloride (or aluminum chloride, n-type or p-type doping source) is 10: 1. And then the samples are uniformly mixed and then are put into a quartz tube with the length of 15cm, the inner diameter of the tube of 1cm and the wall thickness of the tube of 2mm, and the pressure in the quartz tube is sealed by 1 mTorr after the tube is sealed. And (3) putting the sealed quartz tube into a muffle furnace for heating, wherein the heating rate is 3-10 ℃ per minute, the heating temperature is 1000-1200 ℃, the heat preservation time is 60-600 minutes, and the sample is naturally cooled to room temperature along with the furnace and then taken out after the heating is finished.
(4) Cleaning a sample: putting the reactant obtained in the step (3) into 50-100mL of absolute ethyl alcohol solution for ultrasonic dispersion for 10-20 minutes, and then centrifuging under the following conditions: 4000 and 5000r/min, and centrifuging for 5-10 min. In the same way, the sample was purified again by being put into deionized water. Repeating the operation for 3-6 times to remove impurities such as silicon dioxide on the surface of the sample, and drying in vacuum to obtain the final product.
According to the scheme, silicon carbide nano particles treated by HF and HCl mixed acid are used as templates of two-dimensional nano sheets, ammonium chloride is used as an etching agent and a doping source (or aluminum chloride and an n-type or p-type doping source), and the nano particles are dissociated into the two-dimensional nano sheets along a specific crystal orientation direction under the combined action of high-pressure chloride ions and doping ions by a high-temperature heating method, so that synchronous doping and uniform doping of the silicon carbide two-dimensional single crystal nano sheets are promoted.
Has the advantages that: compared with the reported silicon carbide two-dimensional nanosheet
1) The preparation method has the main advantages that the raw material 6H-SiC nano particles are low in price, wide in source and large in forbidden bandwidth, and the prepared SiC two-dimensional single crystal nano sheet is high in crystal quality, good in crystallinity, uniform in nano sheet thickness and good in monodispersity and can realize the preparation of a single-atom layer two-dimensional nano sheet and triangular, hexagonal and wafer two-dimensional nano sheets.
2) The preparation method for preparing the SiC two-dimensional nanosheet is simple in preparation process, high in yield, low in preparation cost, safe and easy to operate.
3) The 6H-SiC two-dimensional nanosheet prepared by the invention can realize synchronous doping, n-type doping and p-type doping in the nanosheet forming process, and has the characteristics of simple doping process, uniform doping, various doping types, capability of realizing synchronous doping of two dopants, no need of expensive growth equipment and doping equipment and the like.
Drawings
FIG. 1 is an XRD pattern of a silicon carbide two-dimensional single-crystal nanosheet prepared according to a first embodiment of the present invention;
FIG. 2 is a TEM image of a prepared silicon carbide two-dimensional single-crystal nanosheet according to an embodiment of the present invention;
FIG. 3 is a transmission electron microscope Selected Area Electron Diffraction (SAED) diagram of the prepared silicon carbide two-dimensional single crystal nanosheet in one embodiment of the present invention
Detailed Description
In order to make the technical solution of the present invention clear, the technical solution of the present invention is fully described in detail below.
The first embodiment is as follows: preparation of nitrogen-doped n-type 6H-SiC two-dimensional single crystal nanosheet
(1) Weighing 10 g of ultra-long 6H-SiC nano-particles prepared by a chemical vapor deposition method, putting the nano-particles into a lead box, and putting the lead box into a neutron activation chamber. Placing into fast neutron source for radiation (radiation range is 10k-10MeV), radiation time is 70-85min, and equivalent fast neutron fluence is 1 × 1013-1×1015n/cm2The total dose of gamma radiation is about 1X 105-3×105rad。
(2) Placing the 6H-SiC nano-particles subjected to radiation treatment into 10mL of mixed acid of HF and HCl for acid etching, placing a solution of silicon carbide and the mixed acid into a polytetrafluoroethylene container, adding 0.01g of sodium dodecyl benzene sulfonate for ultrasonic dispersion for 10 minutes, then etching for 60-120 minutes by using the mixed acid and an iron chloride solution, adding deionized water for dilution, stirring uniformly, performing ultrasonic dispersion for 20 minutes, standing for 2 hours, pouring out a supernatant, and adding 20mL of deionized water for dilution. Repeating the steps for 5 times until the pH value of the solution is more than 4. Then centrifuged at 4500r/min for 10 min. Drying for 24h in an oven at 60 ℃, and grinding to obtain the acid-treated standby nanoparticles.
(3) 0.1g of the 6H-SiC nanoparticles obtained in step 2 and 0.02g of ammonium chloride are weighed, and the weighed materials are put into a quartz tube with the length of 15cm, the inner diameter of the tube of 1cm, the wall thickness of the tube of 2mm and the pressure of 1 mTorr, then the quartz tube is sealed, and the quartz tube is shaken back and forth to mix the materials uniformly as much as possible. And then, the quartz tube filled with the sample is arranged in a muffle furnace, the heating temperature is 1000 ℃, the heating rate is 4 ℃ per minute, the temperature is kept for 360 minutes, and the sample is naturally cooled to the room temperature along with the furnace after the heating is finished and then taken out.
(4) And ultrasonically dispersing the taken sample in 80mL of deionized water for 10 minutes, centrifuging the sample for 8 minutes at the speed of 4500r/min by using a centrifuge, ultrasonically cleaning the obtained sample for 10 minutes by using 100mL of absolute ethyl alcohol, centrifuging the sample under the same parameters, drying the sample in an oven at 60 ℃ for 120 minutes, naturally cooling the sample to room temperature along with the oven after heating, and taking out the sample to obtain the nitrogen-doped n-type silicon carbide two-dimensional single crystal nanosheet.
Example two: preparation of nitrogen and phosphorus double-doped n-type 6H-SiC two-dimensional single crystal nanosheet
(1) The same as the step (1) in the first embodiment;
(2) the same as the step (2) in the first embodiment;
(3) weighing 0.1g of 6H-SiC nano-particles obtained in the step (2), 0.01g of a mixture of ammonium chloride and 0.01g of red phosphorus, uniformly mixing, filling into a quartz tube with the length of 15cm, the inner diameter of the tube of 1cm, the wall thickness of the tube of 2mm and the pressure of 1 mTorr, and sealing. And then, the quartz tube filled with the sample is arranged in a muffle furnace, the heating temperature is 1000 ℃, the heating rate is 4 ℃ per minute, the temperature is kept for 360 minutes, and the sample is naturally cooled to the room temperature along with the furnace after the heating is finished and then taken out.
(4) The same as the step (4) in the first embodiment, the nitrogen-phosphorus double-doped n-type 6H-SiC two-dimensional nanosheet can be obtained.
Example three: preparation of aluminum-doped p-type 6H-SiC two-dimensional single crystal nanosheet
(1) The same as the step (1) in the first embodiment;
(2) the same as the step (2) in the first embodiment;
(3) weighing 0.1g of the 3C-SiC nanoparticles obtained in the step (2) and 0.01g of aluminum chloride, uniformly mixing, filling into a quartz tube with the length of 15cm, the inner diameter of the tube of 1cm, the wall thickness of the tube of 2mm and the pressure of 1 mTorr, and sealing. And then, the quartz tube filled with the sample is arranged in a muffle furnace, the heating temperature is 1000 ℃, the heating rate is 4 ℃ per minute, the temperature is kept for 360 minutes, and the sample is naturally cooled to the room temperature along with the furnace after the heating is finished and then taken out.
(4) The same as the step (4) in the first embodiment, the aluminum-doped p-type 6H-SiC two-dimensional nanosheet can be obtained.
Example four: preparation of boron-doped p-type 6H-SiC two-dimensional single crystal nanosheet
(1) The same as the step (1) in the first embodiment;
(2) the same as the step (2) in the first embodiment;
(3) weighing 0.1g of the 6H-SiC nanoparticles obtained in the step 2 and 0.01g of boron chloride, uniformly mixing, filling into a quartz tube with the length of 15cm, the inner diameter of the tube of 1cm, the wall thickness of the tube of 2mm and the pressure of 1 mTorr, and sealing. And then, the quartz tube filled with the sample is arranged in a muffle furnace, the heating temperature is 1000 ℃, the heating rate is 4 ℃ per minute, the temperature is kept for 360 minutes, and the sample is naturally cooled to the room temperature along with the furnace after the heating is finished and then taken out.
(4) The same as the step (4) in the first embodiment, the boron-doped p-type 6H-SiC two-dimensional nanosheet can be obtained.
Example five: preparation of boron-aluminum double-doped p-type 6H-SiC two-dimensional single crystal nanosheet
(1) The same as the step (1) in the first embodiment;
(2) the same as the step (2) in the first embodiment;
(3) weighing 0.1g of the 6H-SiC nanoparticles obtained in the step 2, 0.01g of a mixture of aluminum chloride and 0.01g of boron chloride, uniformly mixing, filling into a quartz tube with the length of 15cm, the inner diameter of the tube of 1cm, the wall thickness of the tube of 2mm and the pressure of 1 mTorr, and sealing. And then, the quartz tube filled with the sample is arranged in a muffle furnace, the heating temperature is 1000 ℃, the heating rate is 4 ℃ per minute, the temperature is kept for 360 minutes, and the sample is naturally cooled to the room temperature along with the furnace after the heating is finished and then taken out.
(4) The same as the step (4) in the first embodiment, the boron-aluminum double-doped p-type 6H-SiC two-dimensional nanosheet can be obtained.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present 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 solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (8)

1. A preparation method of a 6H-silicon carbide two-dimensional single crystal nanosheet is characterized by comprising the following steps:
(1) neutron irradiation treatment of silicon carbide nanoparticles: the 6H-SiC nano particles prepared by the chemical vapor deposition method are put into a fast neutron source to be radiated, the radiation range is 10k-10M eV, the radiation time is 70-85min, the equivalent fast neutron fluence is 1 multiplied by 1013-1×1015n/cm2Total dose of gamma radiation of 1X 105-3×105rad；
(2) Acid treatment of silicon carbide nanoparticles: placing the 6H-SiC nano-particles subjected to radiation treatment into a mixed acid solution of HF and HCl for ultrasonic dispersion for 5-20 minutes, then etching for 60-120 minutes by using ethanol and a ferric chloride solution, adding deionized water for dilution, repeating the steps for 5-8 times, washing a silicon carbide sample by using the deionized water and absolute ethanol in sequence after the pH value of the solution is greater than 4, centrifuging, and placing the silicon carbide sample into a 60-80 ℃ oven for vacuum drying for 24-36 hours for later use;
(3) doping silicon carbide nanoparticles: respectively weighing a certain amount of the sample obtained in the step (2) and ammonium chloride or aluminum chloride or an n-type doping source or a p-type doping source, uniformly mixing, and then filling into a quartz tube for sealing; placing the sealed quartz tube into a muffle furnace for heating, wherein the heating rate of the muffle furnace is 3-10 ℃/min, the heating temperature is 1000-1200 ℃, the heat preservation time is 60-600 minutes, and the sample is taken out after being naturally cooled to room temperature along with the furnace after the heating is finished;
(4) cleaning a sample: and (4) putting the sample obtained in the step (3) into 50-100mL of absolute ethyl alcohol solution for ultrasonic dispersion for 10-20 minutes, putting the sample after centrifugation and filtration into 50-100mL of deionized water for ultrasonic dispersion for 10-20 minutes, and drying in vacuum to obtain the final product.
2. The preparation method of 6H-silicon carbide two-dimensional single crystal nanosheets according to claim 1, wherein: the 6H-SiC nanoparticles described in step (1) are 6H-SiC nanoparticles prepared by a chemical vapor deposition method, having a density of 3.21g/cc, a diameter of 0.1 to 0.6 μm, and a thickness of 0.35 to 0.7 mm.
3. The preparation method of 6H-silicon carbide two-dimensional single crystal nanosheets according to claim 1, wherein: the mixed acid in the step (2) is mainly prepared from the following components in a volume ratio of 1: 1 HF and HCl and contains 0.05g of sodium dodecylbenzenesulfonate per hundred milliliters of mixed acid.
4. The preparation method of 6H-silicon carbide two-dimensional single crystal nanosheets according to claim 1, wherein: the ethanol and ferric chloride solution in the step (2) is prepared by dissolving 1-5g of ferric chloride in one hundred milliliters of ethanol solution.
5. The preparation method of 6H-silicon carbide two-dimensional single crystal nanosheets according to claim 1, wherein: the acid treatment process of the nanoparticles in the step (2) is carried out in an ultrasonic bath environment, the whole solution is placed in a polytetrafluoroethylene container, the ultrasonic power of the ultrasonic bath is 150W, and the temperature of the solution is 40 ℃.
6. The preparation method of 6H-silicon carbide two-dimensional single crystal nanosheets according to claim 1, wherein: the sample raw materials contained in the sealed quartz tube in the step (3) are as follows: 0.05-0.2g of the silicon carbide raw material obtained in the step (2), and 0.005-0.02g of ammonium chloride or aluminum chloride or an n-type doping source or a p-type doping source; the mass ratio of the silicon carbide sample to the ammonium chloride or aluminum chloride or the n-type doping source or the p-type doping source is 10: 1.
7. The preparation method of 6H-silicon carbide two-dimensional single crystal nanosheets according to claim 1, wherein: the n-type doping sources in the step (3) are ammonium chloride and red phosphorus; the P-type doping source is aluminum chloride and boron chloride.
8. The preparation method of 6H-silicon carbide two-dimensional single crystal nanosheets according to claim 1, wherein: the quartz tube in the step (3) is as follows: the length of the tube is 15cm, the inner diameter of the tube is 1cm, the wall thickness of the tube is 2mm, and the pressure in the quartz tube is 1 mTorr after the tube is sealed.
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