CN114735704B - Method for synthesizing nano silicon carbide at low temperature - Google Patents
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- CN114735704B CN114735704B CN202210579171.9A CN202210579171A CN114735704B CN 114735704 B CN114735704 B CN 114735704B CN 202210579171 A CN202210579171 A CN 202210579171A CN 114735704 B CN114735704 B CN 114735704B
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- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 55
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 37
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 70
- 241000209094 Oryza Species 0.000 claims abstract description 39
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 39
- 235000009566 rice Nutrition 0.000 claims abstract description 39
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 27
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000012298 atmosphere Substances 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 239000011780 sodium chloride Substances 0.000 claims abstract description 12
- 238000001291 vacuum drying Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 150000003839 salts Chemical class 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 239000012798 spherical particle Substances 0.000 claims 1
- 239000011777 magnesium Substances 0.000 abstract description 21
- 239000000463 material Substances 0.000 abstract description 8
- 239000001103 potassium chloride Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000002154 agricultural waste Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 235000013339 cereals Nutrition 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000010903 husk Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000010574 gas phase reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/977—Preparation from organic compounds containing silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/984—Preparation from elemental silicon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of material preparation, and particularly relates to a method for synthesizing nano silicon carbide at low temperature, which mainly comprises the following steps: heat-treating clean rice hulls in an air atmosphere, mixing the heat-treated product with a proper amount of NaCl, KCl and Mg powder, carrying out reduction heat treatment in an inert atmosphere, and carrying out acid washing and drying on the product to obtain nano silicon powder containing trace oxygen and carbon; mixing silicon powder, magnesium powder and a carbon source, performing heat treatment at 550-750 ℃ in an inert atmosphere, and performing acid soaking, cleaning and vacuum drying on a heat treatment product to obtain a pure nano silicon carbide material, wherein the yield is more than 96%. According to the invention, rice hulls are used as main raw materials to prepare the nano silicon carbide material, so that the recycling of agricultural wastes is realized; meanwhile, the preparation process is simple, high in efficiency, low in synthesis temperature and low in cost, and can be directly used for industrial production.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a method for synthesizing nano silicon carbide at a low temperature.
Background
Silicon carbide has unique physicochemical properties such as wide band gap, high mechanical strength, high thermal conductivity, good oxidation resistance and chemical stability, and wide application prospect. The unique physical and chemical properties lead the polymer to have wide application prospects in the aspects of electric field emission, electronic equipment, microwave absorbers, catalysts, capacitors, sensors, biological probes and the like. The preparation method of the nano silicon carbide generally adopts a sol-gel method, a thermochemical gas phase reaction method, a carbothermal reduction method and the like. The sol-gel method for preparing the nano silicon carbide material is influenced by a plurality of factors, such as hydrolysis time, pH value of solution, heat treatment temperature and the like, so that the microstructure of the silicon carbide material cannot be precisely controlled, and nano silicon carbide with good crystallization, high purity and controllable shape and particle size is difficult to generate; in addition, mass production is difficult. The thermochemical gas phase reaction method is to heat reactants to a gas phase state for reaction, and has high energy consumption and low yield. Therefore, the method has high cost for producing the nano silicon carbide. The carbothermal reduction method is a method in which an oxidation-reduction reaction is performed at a certain temperature by using inorganic carbon as a reducing agent. When silicon carbide is prepared by a carbothermal reduction method, the reaction temperature generally reaches 1300 ℃, and the silicon carbide with higher purity can be obtained; therefore, silicon carbide tends to form large grains at high temperatures, and the product size is not easily controlled.
The rice hulls contain a large amount of carbon and silicon, and patent document publication No. CN103803982B discloses that silicon carbide is synthesized by directly utilizing the carbon and silicon in the rice hulls, but after the rice hulls are carbonized, the silicon exists in a silicon dioxide form, and the silicon carbide synthesized by the carbon and the silicon dioxide is required to be synthesized at more than 1400 ℃. Patent document CN109748282B discloses that nano silicon dioxide and organic matter are used as raw materials, carbonized and then heated with metal magnesium powder in a closed container, and silicon carbide is synthesized at low temperature, but the process is carried out under high pressure.
In view of this, it is desirable to provide a method for synthesizing nano silicon carbide at low temperatures.
Disclosure of Invention
The present invention has been made to solve the above-mentioned problems occurring in the conventional art, and an object of the present invention is to provide a method for synthesizing nano silicon carbide at a low temperature, which can increase a reaction area to reduce a reaction of a silicon carbide synthesis reaction by using ultrafine nano silicon particle powder prepared from a biomass material and graphene oxide as raw materials, and can synthesize silicon carbide at a low temperature.
In order to achieve the technical purpose and the technical effect, the invention is realized by the following technical scheme:
a method for synthesizing nano silicon carbide at low temperature, which comprises the following steps:
1) Performing constant-temperature heat treatment on clean rice hulls in an air atmosphere to obtain rice hull heat treatment products containing trace carbon;
2) Mixing the obtained rice hull heat treatment product with mixed salt and Mg powder, and carrying out constant-temperature heat treatment in an inert atmosphere to obtain a heat treatment product A;
3) Continuously stirring the obtained heat treatment product A in hydrochloric acid for 3-6 hours, separating, washing and vacuum drying to obtain nano silicon powder containing trace oxygen and carbon;
4) Mixing the obtained nano silicon powder with a carbon source, and ball milling for a period of time to obtain a Si/C composite material;
5) Mixing the obtained Si/C composite material with Mg powder, and performing constant-temperature heat treatment in an inert atmosphere to obtain a heat treatment product B;
6) And continuously stirring the obtained heat treatment product B in hydrochloric acid for 2-8 h, and then separating, washing and vacuum drying to obtain the nano silicon carbide.
Further, in the method for synthesizing the nano silicon carbide at the low temperature, in the step 1), the constant temperature heat treatment temperature in the air atmosphere is 450-600 ℃, and the constant temperature heat treatment time is 3-7 h.
Further, in the method for synthesizing the nano silicon carbide at the low temperature, in the step 2), the constant temperature heat treatment temperature in an inert atmosphere is 550-750 ℃, and the constant temperature heat treatment time is 0.5-3 h.
Further, in the step 2) of the method for synthesizing the nano silicon carbide at the low temperature, the mixed salt consists of NaCl and KCl according to the mol ratio of 1:1, the mass ratio of Mg powder to rice hull heat treatment products is 1:0.9-1.1, and the mass ratio of the total mass of the rice hull heat treatment products and the Mg powder to the mixed salt is 1:2.2 to 2.8.
Further, in the method for synthesizing nano silicon carbide at low temperature as described above, in the steps 2) and 5), the particle size of the Mg powder is 50 to 300 mesh.
Further, in the method for synthesizing nano silicon carbide at low temperature as described above, the concentration of hydrochloric acid is 5 to 15wt% in the steps 3) and 6).
Further, in the method for synthesizing nano silicon carbide at low temperature as described above, in step 4), the carbon source is graphene oxide.
Further, in the method for synthesizing nano silicon carbide at low temperature as described above, in the step 4), the molar ratio of the nano silicon powder to the carbon source is 1:1.1 to 2.0.
Further, in the method for synthesizing the nano silicon carbide at the low temperature, in the step 4), the mass ratio of the total mass of the nano silicon powder and the carbon source to the grinding ball is 1:10-15, and the working conditions of the ball mill are as follows: the rotating speed is 400-450 rpm, and the total ball milling time is 10-12 h.
Further, in the method for synthesizing the nano silicon carbide at the low temperature, in the step 5), the constant temperature heat treatment temperature in an inert atmosphere is 550-750 ℃, and the constant temperature heat treatment time is 1-5 hours.
The beneficial effects of the invention are as follows:
the invention provides a method for synthesizing nano silicon carbide at low temperature, which is scientific and reasonable in design, and on one hand, the rice husk of agricultural waste is subjected to carbon removal treatment and then used as a silicon source of silicon carbide, so that the waste of agricultural waste is changed into valuable; on the other hand, compared with the prior art, the method can prepare the silicon carbide powder with the spherical shape and the particle size smaller than 100nm at the ultralow temperature, and has higher yield.
Of course, it is not necessary for any one product to practice the invention to achieve all of the advantages set forth above at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an XRD pattern of rice husk reduced product in example 1 according to the invention;
FIG. 2 is an SEM of rice husk reduced product of example 1 according to the invention;
FIG. 3 is a graph showing nitrogen desorption curves and pore size distribution of rice husk reduction products in example 1 of the present invention;
FIG. 4 is an X-ray diffraction pattern of nano-silicon carbide prepared in example 1 of the present invention;
fig. 5 is a field emission scanning electron microscope (sem) image of nano silicon carbide prepared in example 1 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a method for synthesizing nano silicon carbide at low temperature, which is characterized in that in the research process of using rice hulls as raw materials for preparing nano silicon carbide, the inventor finds that in the process of directly using the rice hulls as a main carbon source and a silicon source, the low-temperature synthesis can not be realized, even the nano silicon carbide can not be synthesized, and the inventor finds that the problem occurs at the point of using the rice hulls as the carbon source through long-term research, therefore, the technical scheme of using the rice hulls as the main silicon source after heat treatment carbon removal is correspondingly designed, and then realizing the low-temperature synthesis of the nano silicon carbide with the added carbon source.
Specific embodiments of the invention are as follows:
example 1
A method for synthesizing nano silicon carbide at low temperature, comprising the following steps:
1) Keeping the temperature of the clean rice hulls at 500 ℃ in an air atmosphere for 4 hours to obtain rice hull heat treatment products;
2) Mixing the rice hull heat treatment product with mixed salt consisting of NaCl and KCl and Mg powder, and carrying out constant temperature heat treatment for 0.5h at 750 ℃ in Ar gas atmosphere to obtain a heat treatment product A. Wherein the mole ratio of NaCl to KCl is 1:1; the mass ratio of the Mg powder to the rice hull heat treatment product is 1:1; the grain diameter of Mg powder is 150 meshes; the total mass ratio of the rice hull heat treatment product to the Mg powder to the total mass ratio of the NaCl and KCl mixed salt is 1:2.5;
3) Placing the obtained heat treatment product A in hydrochloric acid with the concentration of 15wt% for continuous stirring for 3 hours, and then washing, separating and vacuum drying to obtain nano silicon powder containing trace oxygen and carbon;
4) Mixing the obtained nano silicon powder with graphene oxide according to the molar ratio of silicon to carbon of 1:1.5, and ball milling for 12 hours to obtain a Si/C composite material;
5) Uniformly mixing the obtained Si/C composite material with Mg powder, and keeping the temperature at 700 ℃ and Ar gas atmosphere for 1.5 hours to obtain a heat treatment product B;
6) And continuously stirring the obtained heat treatment product B in hydrochloric acid with the concentration of 15wt% for 3 hours, and washing, separating and vacuum drying to obtain the nano silicon carbide powder. Yield (in terms of SiO after calcination) 2 Calculated) was 96.5%.
Example 2:
a method for synthesizing nano silicon carbide at low temperature, comprising the following steps:
1) Placing clean and dried rice hulls in a high-temperature furnace, and keeping the temperature for 7 hours in an air atmosphere at 450 ℃ to obtain a rice hull heat treatment product;
2) Mixing the obtained rice hull heat treatment product with mixed salt composed of NaCl and KCl and Mg powder, and carrying out constant temperature heat treatment for 1.5h at 700 ℃ in Ar gas atmosphere to obtain a heat treatment product A. Wherein the mole ratio of NaCl to KCl is 1:1; the mass ratio of the Mg powder to the rice hull heat treatment product is 1:1.1; the grain diameter of Mg powder is 50 meshes; the total mass ratio of the rice hull heat treatment product to the Mg powder to the total mass ratio of the NaCl and KCl mixed salt is 1:2.2;
3) Taking out the heat treatment product A, placing the heat treatment product A in hydrochloric acid with the concentration of 15wt% for continuous stirring for 3 hours, and obtaining nano silicon powder containing trace oxygen and carbon through separation, washing and vacuum drying;
4) The molar ratio of the obtained nanometer silicon powder to graphene oxide is 1:1.3, mixing, namely placing the mixture into a sealed ball milling tank, wherein the mass ratio of the material to the grinding balls is 1:15; the rotating speed of the ball mill is 400-450 rpm, and the total ball milling time is 10 hours;
5) Mixing the obtained mixture with 150-mesh Mg powder in a mass ratio of 1:1.1, and performing heat treatment for 1h in an argon atmosphere at 650 ℃ to obtain a heat treatment product B;
6) And placing the obtained heat treatment product B into hydrochloric acid with the concentration of 15wt% for continuous stirring for 4 hours, and then separating, washing and vacuum drying to obtain the nano silicon carbide powder. Yield (in terms of SiO after calcination) 2 Calculated) was 97.2%.
Example 3
A method for synthesizing nano silicon carbide at low temperature, comprising the following steps:
1) Removing impurities from rice hulls, cleaning, drying, placing the obtained clean rice hulls in a muffle furnace, heating to 600 ℃ at 5 ℃/min in air atmosphere, and performing heat treatment for 3 hours to obtain rice hull heat treatment products;
2) Mixing the obtained rice hull heat treatment product with mixed salt composed of NaCl and KCl and Mg powder, and carrying out constant temperature heat treatment for 3 hours at 550 ℃ in Ar gas atmosphere to obtain a heat treatment product A. Wherein the mole ratio of NaCl to KCl is 1:1; the mass ratio of Mg powder to the rice hull heat treatment product is 1:0.9; the grain diameter of Mg powder is 300 meshes; the total mass ratio of the rice hull heat treatment product to the Mg powder to the total mass ratio of the NaCl and KCl mixed salt is 1:2.8;
3) Placing the obtained heat treatment product A in hydrochloric acid with the concentration of 10wt% for continuous stirring for 5 hours, and then washing, separating and vacuum drying to obtain nano silicon powder containing trace oxygen and carbon;
4) Mixing the obtained nano silicon powder with graphene oxide according to the molar ratio of silicon to carbon of 1:1.5, and ball milling for 12 hours to obtain a Si/C composite material;
5) Uniformly mixing the obtained Si/C composite material with 300-mesh Mg powder, and keeping the temperature at 550 ℃ and Ar gas atmosphere for 5 hours to obtain a heat treatment product B;
6) And continuously stirring the obtained heat treatment product B in hydrochloric acid with the concentration of 15wt% for 3 hours, and washing, separating and vacuum drying to obtain the nano silicon carbide powder. Yield (in terms of SiO after calcination) 2 Calculated) was 97.9%.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (7)
1. A method for synthesizing nano silicon carbide at low temperature, which is characterized by comprising the following steps:
1) Performing constant-temperature heat treatment on clean rice hulls in an air atmosphere to obtain rice hull heat treatment products containing trace carbon;
2) Mixing the obtained rice hull heat treatment product with mixed salt and Mg powder, and carrying out constant-temperature heat treatment in an inert atmosphere to obtain a heat treatment product A;
3) Continuously stirring the obtained heat treatment product A in hydrochloric acid for 3-6 hours, separating, washing and vacuum drying to obtain nano silicon powder containing trace oxygen and carbon;
4) Mixing the obtained nano silicon powder with graphene oxide, and ball milling for a period of time to obtain a Si/C composite material; wherein, the molar ratio of the nanometer silicon powder to the graphene oxide is 1:1.1 to 2.0;
5) Mixing the obtained Si/C composite material with Mg powder, and performing constant-temperature heat treatment in an inert atmosphere to obtain a heat treatment product B; wherein the constant temperature heat treatment temperature in inert atmosphere is 550-750 ℃, and the constant temperature heat treatment time is 1-5 h;
6) And continuously stirring the obtained heat treatment product B in hydrochloric acid for 2-8 h, and then separating, washing and vacuum drying to obtain the silicon carbide powder with the spherical particle size of less than 100 nanometers.
2. The method for synthesizing nano silicon carbide at low temperature according to claim 1, wherein: in the step 1), the constant temperature heat treatment temperature in the air atmosphere is 450-600 ℃, and the constant temperature heat treatment time is 3-7 h.
3. The method for synthesizing nano silicon carbide at low temperature according to claim 1, wherein: in the step 2), the constant temperature heat treatment temperature in inert atmosphere is 550-750 ℃, and the constant temperature heat treatment time is 0.5-3 h.
4. The method for synthesizing nano silicon carbide at low temperature according to claim 1, wherein: in the step 2), the mixed salt consists of NaCl and KCl according to the mol ratio of 1:1, the mass ratio of Mg powder to rice hull heat treatment products is 1:0.9-1.1, and the mass ratio of the total mass of the rice hull heat treatment products and the Mg powder to the mixed salt is 1:2.2 to 2.8.
5. The method for synthesizing nano silicon carbide at low temperature according to claim 1, wherein: in the step 2) and the step 5), the particle size of the Mg powder is 50-300 meshes.
6. The method for synthesizing nano silicon carbide at low temperature according to claim 1, wherein: in the steps 3) and 6), the concentration of the hydrochloric acid is 5-15 wt%.
7. The method for synthesizing nano silicon carbide at low temperature according to claim 1, wherein: in the step 4), the mass ratio of the total mass of the nano silicon powder and the graphene oxide to the grinding ball is 1:10-15, and the working conditions of the ball mill are as follows: the rotating speed is 400-450 rpm, and the total ball milling time is 10-12 h.
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| CN110943211A (en) * | 2019-12-16 | 2020-03-31 | 安徽工业大学 | Preparation method of high-performance Si/C negative electrode material |
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| CN101525135A (en) * | 2009-04-10 | 2009-09-09 | 山东大学 | Method for inducing and synthesizing carborundum or carborundum nano tube by low-temperature auxiliary reaction |
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| CN108285145A (en) * | 2018-04-27 | 2018-07-17 | 中国人民解放军国防科技大学 | Three-dimensional multi-level structure nano silicon carbide, preparation method and application thereof |
| CN108610051A (en) * | 2018-07-18 | 2018-10-02 | 东北林业大学 | A kind of preparation method being modified wooden base silicon carbide ceramic material |
| CN110943211A (en) * | 2019-12-16 | 2020-03-31 | 安徽工业大学 | Preparation method of high-performance Si/C negative electrode material |
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