CN111453733A - Nano β -silicon carbide and preparation method thereof - Google Patents
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Abstract
The invention relates to the technical field of silicon carbide preparation, in particular to nano β -silicon carbide and a preparation method thereof, wherein the preparation method of the nano β -silicon carbide comprises the following steps of carrying out heat treatment on a mixture of a carbon-coated silicon dioxide nano material and magnesium powder in a carbon dioxide atmosphere, and carrying out acid treatment and carbon removal treatment on the heat-treated substance.
Description
Technical Field
The invention relates to the technical field of silicon carbide preparation, and particularly relates to nano β -silicon carbide and a preparation method thereof.
Background
Silicon carbide is also known as carbo-silica, corundum or refractory sand, and has the chemical formula: SiC is a refractory material which is prepared by high-temperature smelting of quartz sand, petroleum coke (or coal coke) and wood dust as raw materials through a resistance furnace. The hardness of silicon carbide is very high, the Mohs hardness is 9.5 grade, which is next to the hardest diamond (10 grade) in the world, the silicon carbide has excellent heat-conducting property, is a semiconductor and has excellent oxidation resistance at high temperature.
The silicon carbide crystal structure is divided into hexagonal or rhombohedral α -SiC and cubic β -SiC (called cubic silicon carbide), α -SiC forms many different variants because of different stacking sequences of carbon and silicon atoms in the crystal structure, more than 70 kinds of β -SiC are found to be converted into α -SiC at the temperature of more than 2100 ℃, and the industrial preparation method of the silicon carbide is to use high-quality quartz sand and petroleum coke to refine in a resistance furnace, refine the obtained silicon carbide blocks, and prepare products with various particle sizes through crushing, acid-alkali washing, magnetic separation, sieving or water separation.
Silicon carbide has at least 70 crystal types, α -silicon carbide is the most common one of the isomorphous substances, and is formed at high temperature higher than 2000 ℃, has hexagonal crystal structure (like wurtzite), β -silicon carbide, cubic structure, similar to diamond, and is formed at temperature lower than 2000 ℃.
The silicon carbide is industrially produced by utilizing a carbothermic method, namely, high-temperature heat treatment of carbon and silicon dioxide to obtain silicon carbide, and then crushing and ball-milling to obtain micron-grade silicon carbide, so that the energy consumption is high, α -silicon carbide is mostly obtained, and β -silicon carbide with a specified crystal form cannot be synthesized.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a preparation method of nano β -silicon carbide, which aims to solve the problems that most of micron-level silicon carbide is obtained in the prior art, the energy consumption in the preparation process is high, most of the micron-level silicon carbide is α -silicon carbide, and β -silicon carbide with a specified crystal form cannot be synthesized.
The invention also aims to provide the nano β -silicon carbide prepared by the method for preparing the nano β -silicon carbide, and the nano β -silicon carbide has higher purity.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a preparation method of nano β -silicon carbide comprises the following steps:
and (3) carrying out heat treatment on the mixture of the carbon-coated silicon dioxide nano material and the magnesium powder in a carbon dioxide atmosphere, and carrying out acid treatment and decarbonization on the heat-treated substance.
Preferably, the silica nanomaterial is a silica nanoparticle and/or a silica nanotube.
Preferably, the diameter of the silica nanoparticles is 50-300 nm.
Preferably, the molar ratio of the magnesium powder to the silicon dioxide is (6-16): 1;
preferably, the molar ratio of the magnesium powder to the silicon dioxide is (7.5-12): 1.
preferably, the heat treatment temperature is 655-820 ℃ and the time is 2-5 h.
Preferably, the heat treatment temperature is 670-750 ℃ and the time is 2-4 h.
Preferably, the acid comprises nitric acid and/or hydrochloric acid;
preferably, the concentration of the acid is 0.9-3.2 mol/L.
Preferably, the method further comprises the steps of centrifuging, drying and grinding the mixture after the acid treatment.
Preferably, the flow rate of the carbon dioxide is 15-25 m L/min.
The nanometer β -silicon carbide is prepared by the preparation method of the nanometer β -silicon carbide.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts the heat generated by the magnesiothermic reduction reaction to prepare the silicon carbide, adopts the carbon-coated nano silicon dioxide to obtain the nano β -silicon carbide and carbon composite material by one step of magnesiothermic reaction, and removes the carbon to obtain the nano β -silicon carbide, and the method has low energy consumption and can generate the high-purity β -silicon carbide.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a TEM image of a nano β -silicon carbide and carbon composite in example 1 of the present invention;
fig. 2 is an XRD pattern of the nano β -silicon carbide and carbon composite in example 1 of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
According to one aspect of the invention, the invention relates to a preparation method of nano β -silicon carbide, which comprises the following steps:
and (3) carrying out heat treatment on the mixture of the carbon-coated silicon dioxide nano material and the magnesium powder in a carbon dioxide atmosphere, and carrying out acid treatment and decarbonization on the heat-treated substance.
The simultaneous existence of the silicon dioxide and the carbon dioxide is one of the key points, the magnesium thermal reaction can generate silicon and carbon nano materials in situ in the silicon dioxide, and then the silicon and the carbon nano materials are synchronously converted into β -silicon carbide under the condition of a large amount of heat released by the reaction, the carbon-coated silicon dioxide is one of the key points for preparing high-purity β -silicon carbide, and the nano silicon dioxide spheres without carbon coating can not generate high-purity products under the same condition.
The carbon coating has the functions of 1) ensuring that high-purity β silicon carbide is generated, if a magnesium thermal experiment is directly carried out by using a silicon dioxide ball, the obtained silicon carbide is α silicon carbide, the peak is very miscellaneous and the silicon dioxide cannot be completely converted into the silicon carbide, and 2) ensuring that silicon dioxide nano-particles exist independently, so that the generated silicon carbide is also nano-particles and is independent particles.
Preferably, the silica nanomaterial is a silica nanoparticle and/or a silica nanotube.
The carbon-coated silicon dioxide nano material can be a core-shell structure nano material of carbon-coated silicon dioxide, and the preparation method comprises the following steps:
25.32mmol of ammonia water was added to an aqueous ethanol solution (27.3g of ethanol, 17.4g of water) and stirred uniformly, and stirred uniformly and kept at a constant temperature of 30 ℃, 7.94mmol of tetrabutyl silicate (TEOS) was added dropwise, after stirring uniformly, 2.23mmol of resorcinol and 4.46mmol of formaldehyde were added, respectively, stirred at 30 ℃ for 24 hours, and then left to stand at 100 ℃ for 24 hours. Centrifugally separating, cleaning and drying to obtain SiO2@ Resin, heat treatment in inert atmosphere to obtain SiO2@C。
The carbon-coated silicon dioxide nano material can be a carbon-coated one-dimensional silicon dioxide nano material, and the preparation method comprises the following steps:
adding 1m L tetrabutyl silicate (TEOS) dropwise into 20m L anhydrous ethanol, continuously ultrasonically stirring for uniform dispersion, then adding dropwise into 20m L anhydrous ethanol in which 100mg of Carbon Nano Tube (CNT) is dispersed, ultrasonically dispersing for 5min, adding 1m L ammonia (25% -28%) and stirring for 30min, continuing adding 1.37mmol of resorcinol and 2.74mmol of formaldehyde (36% -38%), stirring for 1h at 50 ℃, filtering, cleaning and thermally treating for 2h at 500 ℃ in nitrogen atmosphere to obtain CNT @ SiO2@C。
Preferably, the diameter of the silica nanoparticles is 135-155 nm.
Preferably, the molar ratio of the magnesium powder to the silicon dioxide is (6-16): 1.
in one embodiment, the molar ratio of the magnesium powder to the silicon dioxide is (6-16): 1, alternatively 6.5:1, 7:1, 7.5:1, 8:1, 8.5:1, 9:1, 9.5:1, 10:1, 10.5:1, 11:1, 11.5:1, 12:1, 12.5:1, 13:1, 13.5:1, 14:1, 14.5:1, 15:1 or 15.5: 1.
β -silicon carbide with higher purity can be obtained by the specific molar ratio of magnesium powder to silicon dioxide.
Preferably, the molar ratio of the magnesium powder to the silicon dioxide is (7.5-12): 1.
preferably, the heat treatment temperature is 655-820 ℃ and the time is 1-5 h.
In one embodiment, the heat treatment temperature is 655 to 820 ℃, and 660 ℃, 670 ℃, 680 ℃, 690 ℃, 700 ℃, 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃, 800 ℃ or 810 ℃ can be selected.
In an embodiment, the time of the heat treatment is 2 to 5 hours, and 2 hours, 2.5 hours, 2.6 hours, 2.7 hours, 2.8 hours, 2.9 hours, 3.0 hours, 3.1 hours, 3.2 hours, 3.3 hours, 3.4 hours, 3.5 hours, 3.6 hours, 3.7 hours, 3.8 hours, 3.9 hours, 4.0 hours, 4.1 hours, 4.2 hours, 4.3 hours, 4.4 hours, and 4.5 hours can be selected.
The thermal treatment is carried out at a specific temperature and for a specific time, so as to meet the condition of the magnesiothermic reduction reaction and further obtain β -silicon carbide with higher purity.
Preferably, the heat treatment temperature is 670-750 ℃ and the time is 2-4 h.
Preferably, the acid comprises hydrochloric acid and/or nitric acid.
Preferably, the concentration of the acid is 1 to 3 mol/L.
Preferably, the method further comprises the steps of centrifuging, drying and grinding the mixture after the acid treatment.
Preferably, the rotating speed of the centrifugation is 9000-11000 rpm, and the time is 25-35 min.
More preferably, the centrifugation is performed at 10000rpm for 30 min.
Preferably, the drying temperature is 55-65 ℃ and the drying time is 20-25 h.
More preferably, the drying temperature is 60 ℃ and the drying time is 24 h.
Furthermore, the invention adopts hydrochloric acid or nitric acid solution with certain concentration to remove magnesium oxide and unreacted substrates.
In one embodiment, the concentration of the acid is 1 to 3 mol/L, and may also be 1.1 mol/L, 1.2 mol/L0, 1.3 mol/L1, 1.4 mol/L2, 1.5 mol/L3, 1.6 mol/L4, 1.7 mol/L5, 1.8 mol/L6, 1.9 mol/L7, 2.0 mol/L8, 2.1 mol/L9, 2.2 mol/L, 2.3 mol/L, 2.4 mol/L, 2.5 mol/L, 2.6 mol/L, 2.7 mol/L, 2.8 mol/L, or 2.9 mol/L.
Preferably, the flow rate of the carbon dioxide is 15-25 m L/min.
In an embodiment, the flow rate of the carbon dioxide is 15-25 m L/min, and may further be 15.5m L/min, 16m L0/min, 16.5m L1/min, 17m L2/min, 17.5m L3/min, 18m L4/min, 18.5m L5/min, 19m L6/min, 19.5m L7/min, 20m L8/min, 20.5m L9/min, 21m L/min, 21.5m L/min, 22m L/min, 22.5m L/min, 23m L/min, 23.5m L/min, 24m L/min, or 24.5m L/min.
By controlling the flow of carbon dioxide to be 15-25 m L/min, the synthesis of the nano β -silicon carbide with the specified crystal form is facilitated.
In a preferred embodiment, the preparation method of the nano β -silicon carbide comprises the following steps:
the method comprises the following steps of carrying out heat treatment on a mixture of a carbon-coated silicon dioxide nano material and magnesium powder in a carbon dioxide atmosphere, wherein the carbon-coated silicon dioxide nano material comprises a carbon-coated core-shell structure nano material and/or a carbon-coated one-dimensional silicon dioxide nano tube, the molar ratio of the magnesium powder to the silicon dioxide is (6-15): 1, the heat treatment temperature is 680-700 ℃, the time is 3.5-4.5 h, treating the obtained mixture with 1-3 mol/L hydrochloric acid/nitric acid solution, centrifuging and drying to remove carbon, and thus obtaining the nano β -silicon carbide.
According to another aspect of the invention, the invention also relates to the nano β -silicon carbide prepared by the preparation method of the nano β -silicon carbide.
The high-purity β -silicon carbide of the present invention has stable chemical performance, high heat conductivity, small heat expansion coefficient, good wear resistance, and may be used as abrasive material in many other applications, such as coating silicon carbide powder onto the inner wall of turbine vane wheel or cylinder body to raise its wear resistance and prolong its service life by 1-2 times, and the high-grade refractory material has high heat shock resistance, small size, light weight, high strength and good energy saving effect.
The invention will now be further illustrated with reference to specific examples.
Example 1
A preparation method of nano β -silicon carbide comprises the following steps:
50mg of SiO with a core-shell structure2@ C, the diameter of the silicon dioxide ball is 150nm, the silicon dioxide ball is uniformly mixed with 300mg magnesium powder and then placed in a porcelain boat, heat treatment is carried out under the atmosphere of 20m L/min of carbon dioxide, the heat treatment temperature is 680 ℃, the treatment time is 3h, the product obtained by cooling is treated by hydrochloric acid of 2 mol/L, and the black solid mixture is obtained by centrifugation, drying and grinding, namely the β -silicon carbide and carbon nano composite material, and carbon is removed to obtain the nano β -silicon carbide.
β -TEM image of the silicon carbide and carbon composite material is shown in FIG. 1, and XRD image is shown in FIG. 2.
The purity of the nano β -silicon carbide obtained in the embodiment is more than 99%.
Example 2
A preparation method of nano β -silicon carbide comprises the following steps:
50mg of SiO with a core-shell structure2@ C, uniformly mixing the silica spheres with the diameter of 145nm with 300mg of magnesium powder, then placing the mixture into a porcelain boat, carrying out heat treatment in the atmosphere of 18m L/min of carbon dioxide at the heat treatment temperature of 670 ℃ for 2h, treating the cooled product with 1 mol/L of hydrochloric acid, centrifuging, drying and grinding the treated product to obtain a black solid mixture, namely the β -silicon carbide and carbon nano composite material, and removing carbon to obtain the nano β -silicon carbide.
The purity of the nano β -silicon carbide obtained in the embodiment is more than 98%.
Example 3
A preparation method of nano β -silicon carbide comprises the following steps:
50mg of SiO with a core-shell structure2@ C, the diameter of the silicon dioxide ball is 150nm, the silicon dioxide ball is uniformly mixed with 300mg magnesium powder and then placed in a porcelain boat for heat treatment under the atmosphere of carbon dioxide of 21m L/min, the heat treatment temperature is 750 ℃, the treatment time is 4 hours, the product obtained by cooling is treated by hydrochloric acid of 3 mol/L, and the product is obtained by centrifugation, drying and grindingThe black solid mixture is β -silicon carbide and carbon nano composite material, and the carbon is removed to obtain the nano β -silicon carbide.
The purity of the nano β -silicon carbide obtained in the embodiment is more than 98%.
Example 4
A preparation method of nano β -silicon carbide comprises the following steps:
50mg of SiO with a core-shell structure2@ C, uniformly mixing the silica spheres with the diameter of 155nm and 300mg of magnesium powder, then placing the mixture into a porcelain boat, carrying out heat treatment in the atmosphere of 25m L/min of carbon dioxide at the temperature of 655 ℃ for 2h, treating the cooled product with 2.5 mol/L of hydrochloric acid, centrifuging, drying and grinding the treated product to obtain a black solid mixture, namely the β -silicon carbide and carbon nano composite material, and removing carbon to obtain the nano β -silicon carbide.
The purity of the nano β -silicon carbide obtained in the embodiment is more than 98%.
Example 5
A preparation method of nano β -silicon carbide comprises the following steps:
50mg of SiO2@ C with a core-shell structure and the diameter of a silicon dioxide sphere of 150nm is uniformly mixed with 300mg of magnesium powder and then placed in a porcelain boat for heat treatment under the atmosphere of carbon dioxide of 16m L/min, the heat treatment temperature is 820 ℃, the treatment time is 2 hours, the product obtained by cooling is treated by nitric acid of 0.9 mol/L, and the mixture is centrifuged, dried and ground to obtain a black solid mixture, namely the β -silicon carbide and carbon nano composite material, and the carbon is removed to obtain the nano β -silicon carbide.
The purity of the nano β -silicon carbide obtained in the embodiment is more than 99%.
Comparative example 1
A method for preparing nano β -silicon carbide, which is carried out under the same conditions as example 1 except that the silica nanospheres are not carbon-coated.
The obtained silicon carbide is detected to be α silicon carbide, the peak is very miscellaneous, and the complete conversion of silicon dioxide into silicon carbide cannot be ensured.
Comparative example 2
A process for preparing nanometer β -silicon carbide is carried out at 500 deg.C, and the other operations are the same as in example 1.
The comparative example can only obtain nano silicon material, and cannot prepare silicon carbide.
Comparative example 3
A method for preparing nano β -silicon carbide comprises the same steps as example 1 except that acid treatment and decarbonization are not performed.
The purity of the nano β -silicon carbide obtained by the comparative example is less than 50%.
The invention adopts the heat generated by the magnesiothermic reduction reaction to prepare the silicon carbide, adopts the carbon-coated nano silicon dioxide to obtain the nano β -silicon carbide and carbon composite material by one step of magnesiothermic reaction, and removes the carbon to obtain the nano β -silicon carbide, and the method has low energy consumption and can generate the high-purity β -silicon carbide.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of nanometer β -silicon carbide is characterized by comprising the following steps:
and (3) carrying out heat treatment on the mixture of the carbon-coated silicon dioxide nano material and the magnesium powder in a carbon dioxide atmosphere, and carrying out acid treatment and decarbonization on the heat-treated substance.
2. The method of claim 1, wherein the silica nanomaterial is silica nanoparticles and/or silica nanotubes.
3. The method of claim 1, wherein the silica nanoparticles have a diameter of 50-300 nm.
4. The method for preparing nano β -silicon carbide according to any one of claims 1 to 3, wherein the molar ratio of the magnesium powder to the silicon dioxide is (6-16): 1;
preferably, the molar ratio of the magnesium powder to the silicon dioxide is (7.5-12): 1.
5. the method for preparing nanometer β -silicon carbide of claim 1, wherein the heat treatment temperature is 655-820 ℃ and the time is 2-5 h.
6. The method for preparing nanometer β -silicon carbide of claim 5, wherein the heat treatment temperature is 670-750 ℃ and the time is 2-4 h.
7. The method of claim 1, wherein the acid comprises nitric acid and/or hydrochloric acid;
preferably, the concentration of the acid is 0.9-3.2 mol/L.
8. The method of claim 7, wherein the acid-treated mixture is centrifuged, dried and ground after the acid treatment and before the carbon removal treatment.
9. The method for preparing nano β -SiC of claim 1, wherein the flow rate of the carbon dioxide is 15-25 m L/min.
10. The nano β -silicon carbide prepared by the method for preparing nano β -silicon carbide according to any one of claims 1 to 9.
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| CN114132928A (en) * | 2021-12-24 | 2022-03-04 | 江苏理工学院 | Method for preparing silicon carbide nano material by using waste silicon dioxide |
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