CN114735704A - Method for synthesizing nano silicon carbide at low temperature - Google Patents
Method for synthesizing nano silicon carbide at low temperature Download PDFInfo
- Publication number
- CN114735704A CN114735704A CN202210579171.9A CN202210579171A CN114735704A CN 114735704 A CN114735704 A CN 114735704A CN 202210579171 A CN202210579171 A CN 202210579171A CN 114735704 A CN114735704 A CN 114735704A
- Authority
- CN
- China
- Prior art keywords
- heat treatment
- nano silicon
- silicon carbide
- powder
- low temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 58
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 48
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 68
- 241000209094 Oryza Species 0.000 claims abstract description 37
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 37
- 235000009566 rice Nutrition 0.000 claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 27
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 25
- 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 19
- 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
- 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
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 229910021389 graphene Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 abstract description 21
- 239000000463 material Substances 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000001103 potassium chloride Substances 0.000 abstract description 4
- 239000002154 agricultural waste Substances 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
- 239000011863 silicon-based powder Substances 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 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000010903 husk Substances 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
- 235000013339 cereals Nutrition 0.000 description 2
- 238000010574 gas phase reaction Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000007669 thermal treatment Methods 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
- 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
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Images
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: carrying out heat treatment on clean rice hulls in air atmosphere, mixing the heat-treated product with a proper amount of NaCl, KCl and Mg powder, carrying out reduction heat treatment in 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, carrying out heat treatment at 550-750 ℃ in an inert atmosphere, and carrying out acid soaking, cleaning and vacuum drying on a heat treatment product to obtain a pure nano silicon carbide material, wherein the yield reaches over 96%. The invention takes rice hulls as main raw materials to prepare the nano silicon carbide material, thereby realizing the recycling of agricultural wastes; meanwhile, the preparation method disclosed by the invention is simple in preparation process, 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 low temperature.
Background
The silicon carbide has unique physical and chemical 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 make it have wide application prospect 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 carbothermic reduction method and the like. The sol-gel method for preparing the nano silicon carbide material is influenced by many 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 accurately controlled, and the nano silicon carbide with good crystallization, high purity and controllable shape and grain size is difficult to generate; in addition, it is also difficult to mass-produce. The thermochemical gas phase reaction method is to heat the reactants to react in a gas phase state, and has high energy consumption and low yield. Therefore, the method has high cost for producing the nano silicon carbide. The carbothermic process is a process in which an oxidation-reduction reaction is carried out at a certain temperature using inorganic carbon as a reducing agent. When the carbothermic method is used for preparing the silicon carbide, the reaction temperature generally reaches 1300 ℃, and the silicon carbide with higher purity can be obtained; therefore, silicon carbide tends to produce large grains at high temperatures, and the product size is not easily controlled.
Although rice hulls contain a large amount of carbon and silicon, and patent document CN103803982B discloses that silicon carbide is synthesized by directly using carbon and silicon in rice hulls, silicon exists in the form of silica after the rice hulls are carbonized, and the synthesis of silicon carbide from carbon and silica must be above 1400 ℃. Patent publication No. CN109748282B discloses that silicon carbide is synthesized from nanosilicon dioxide and an organic substance as raw materials, and then the raw materials are carbonized and heated with magnesium powder in a closed container at a low temperature.
In view of the above, there is a need to provide a method for synthesizing nano silicon carbide at low temperature.
Disclosure of Invention
The present invention has been made to overcome the above 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 ultra-fine nano silicon particle powder prepared from a biomass material and graphene oxide as raw materials, thereby synthesizing silicon carbide at a low temperature.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a method for synthesizing nano silicon carbide at low temperature comprises the following steps:
1) carrying out constant-temperature heat treatment on the clean rice hulls in the 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 performing 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 carrying out 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 hours, 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 hours.
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 the inert atmosphere is 550-750 ℃, and the constant-temperature heat treatment time is 0.5-3 hours.
Further, in the method for synthesizing nano silicon carbide at low temperature, in the step 2), the mixed salt is composed of NaCl and KCl according to the molar ratio of 1:1, the mass ratio of Mg powder to the rice hull heat treatment product is 1: 0.9-1.1, and the mass ratio of the total mass of the rice hull heat treatment product and the Mg powder to the mixed salt is 1: 2.2 to 2.8.
Further, in the method for synthesizing the nano silicon carbide at the low temperature, in the step 2) and the step 5), the particle size of the Mg powder is 50-300 meshes.
Further, in the method for synthesizing the nano silicon carbide at the low temperature, in the step 3) and the step 6), the concentration of hydrochloric acid is 5-15 wt%.
Further, in the method for synthesizing nano silicon carbide at low temperature, in the step 4), the carbon source is graphene oxide.
Further, in the method for synthesizing nano silicon carbide at low temperature, in the step 4), the molar ratio of the nano silicon powder to the carbon source is 1: 1.1-2.0 mixing.
Further, in the method for synthesizing nano silicon carbide at 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 balls 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 the inert atmosphere is 550-750 ℃, and the constant-temperature heat treatment time is 1-5 hours.
The invention has the beneficial effects that:
the invention provides a method for synthesizing nano silicon carbide at low temperature, which has scientific and reasonable design, on one hand, the rice hull of agricultural wastes is decarbonized and then is used as a silicon source of silicon carbide, thereby changing the agricultural wastes into valuables; on the other hand, compared with the prior art, the method can prepare the silicon carbide powder with spherical shape and particle size less than 100nm at ultralow temperature, and has higher yield.
Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an XRD pattern of a rice husk reduced product in example 1 of the present invention;
FIG. 2 is an SEM of a rice husk reduced product in example 1 of the present invention;
FIG. 3 is a graph showing a nitrogen desorption curve and a pore size distribution of a rice husk reduced product in example 1 of the present invention;
FIG. 4 is an X-ray diffraction pattern of nano-sized silicon carbide produced in example 1 of the present invention;
FIG. 5 is a field emission scanning electron microscope image of nano-SiC prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for synthesizing nano silicon carbide at low temperature, and the inventor finds that the low-temperature synthesis even the synthesis of nano silicon carbide cannot be realized in the process of directly utilizing rice hulls as a main carbon source and a silicon source in the research process of utilizing the rice hulls as raw materials for preparing the nano silicon carbide.
The specific embodiment of the invention is as follows:
example 1
A method for synthesizing nano silicon carbide at low temperature comprises the following steps:
1) keeping the temperature of the clean rice hulls at 500 ℃ in the air atmosphere for 4 hours to obtain a rice hull heat treatment product;
2) and (3) 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 molar ratio of NaCl to KCl is 1: 1; the mass ratio of Mg powder to the rice hull heat treatment product is 1: 1; the particle size of Mg powder is 150 meshes; the ratio of the total mass of the rice hull heat treatment product and the Mg powder to the total mass 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 15 wt% to be continuously stirred for 3 hours, and then washing, separating and vacuum drying the product 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 carrying out 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 of the mixture constant at 700 ℃ for 1.5 hours in an Ar gas atmosphere to obtain a heat treatment product B;
6) and continuously stirring the obtained heat treatment product B in hydrochloric acid with the concentration of 15 wt% for 3 hours, washing, separating and vacuum drying to obtain the nano silicon carbide powder. Yield (as SiO after calcination)2Calculated) was 96.5%.
Example 2:
a method for synthesizing nano silicon carbide at low temperature comprises the following steps:
1) putting the clean and dry rice hulls in a high-temperature furnace, and keeping the temperature for 7 hours at 450 ℃ in the air atmosphere to obtain a rice hull heat treatment product;
2) mixing the obtained rice hull heat treatment product with mixed salt consisting 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 molar ratio of NaCl to KCl is 1: 1; the mass ratio of Mg powder to the rice hull heat treatment product is 1: 1.1; the particle size of Mg powder is 50 meshes; the ratio of the total mass of the thermal treatment product of the rice hull and the Mg powder to the total mass 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 15 wt% to be continuously stirred for 3 hours, and obtaining the nano silicon powder containing trace oxygen and carbon through separation, washing and vacuum drying;
4) and mixing the obtained nano silicon powder and graphene oxide according to the molar ratio of silicon to carbon of 1: 1.3, mixing, and placing the mixture in a sealed ball milling tank, wherein the mass ratio of the materials 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 at a mass ratio of 1:1.1, and carrying out constant-temperature heat treatment for 1 hour at 650 ℃ in an argon atmosphere to obtain a heat treatment product B;
6) and placing the obtained heat treatment product B in hydrochloric acid with the concentration of 15 wt% to continuously stir for 4 hours, and then separating, washing and vacuum drying to obtain the nano silicon carbide powder. Yield (as SiO after calcination)2Calculated) was 97.2%.
Example 3
A method for synthesizing nano silicon carbide at low temperature comprises the following steps:
1) removing impurities from rice hulls, cleaning and drying, placing the obtained clean rice hulls in a muffle furnace, heating to 600 ℃ at the speed of 5 ℃/min in the air atmosphere, and carrying out constant-temperature heat treatment for 3h to obtain rice hull heat treatment products;
2) and mixing the obtained rice hull heat treatment product with mixed salt consisting 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 molar 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 particle size of Mg powder is 300 meshes; the ratio of the total mass of the thermal treatment product of the rice hull and the Mg powder to the total mass of the NaCl and KCl mixed salt is 1: 2.8 of;
3) placing the obtained heat treatment product A in hydrochloric acid with the concentration of 10 wt% to be continuously stirred for 5 hours, and then washing, separating and vacuum drying the product 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 carrying out 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 of the mixture at 550 ℃ for 5 hours in Ar atmosphere to obtain a heat treatment product B;
6) and continuously stirring the obtained heat treatment product B in hydrochloric acid with the concentration of 15 wt% for 3 hours, washing, separating and vacuum drying to obtain the nano silicon carbide powder. Yield (as SiO after calcination)2Calculated) was 97.9%.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments 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 utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. A method for synthesizing nano silicon carbide at low temperature is characterized by comprising the following steps:
1) carrying out constant-temperature heat treatment on the clean rice hulls in the 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 performing 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 carrying out 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 hours, and then separating, washing and vacuum drying to obtain the nano silicon carbide.
2. The method for synthesizing nano silicon carbide at low temperature according to claim 1, wherein the method comprises the following steps: 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 hours.
3. The method for synthesizing nano silicon carbide at low temperature according to claim 1, wherein the method comprises the following steps: in the step 2), the constant-temperature heat treatment temperature in the 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 the method comprises the following steps: in the step 2), the mixed salt consists of NaCl and KCl according to a molar ratio of 1:1, the mass ratio of Mg powder to the rice hull heat treatment product is 1: 0.9-1.1, and the mass ratio of the total mass of the rice hull heat treatment product 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 the method comprises the following steps: 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 the method comprises the following steps: in the step 3) and the step 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 the method comprises the following steps: in the step 4), the carbon source is graphene oxide.
8. The method for synthesizing nano silicon carbide at low temperature according to claim 1, wherein the method comprises the following steps: in the step 4), the molar ratio of the nano silicon powder to the carbon source is 1: 1.1-2.0.
9. The method for synthesizing nano silicon carbide at low temperature according to claim 1, wherein the method comprises the following steps: in the step 4), the mass ratio of the total mass of the nano silicon powder and the carbon source to the grinding balls 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.
10. The method for synthesizing nano silicon carbide at low temperature according to claim 1, wherein the method comprises the following steps: in the step 5), the constant-temperature heat treatment temperature in the inert atmosphere is 550-750 ℃, and the constant-temperature heat treatment time is 1-5 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210579171.9A CN114735704B (en) | 2022-05-25 | 2022-05-25 | Method for synthesizing nano silicon carbide at low temperature |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210579171.9A CN114735704B (en) | 2022-05-25 | 2022-05-25 | Method for synthesizing nano silicon carbide at low temperature |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114735704A true CN114735704A (en) | 2022-07-12 |
| CN114735704B CN114735704B (en) | 2024-01-05 |
Family
ID=82287624
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210579171.9A Active CN114735704B (en) | 2022-05-25 | 2022-05-25 | Method for synthesizing nano silicon carbide at low temperature |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114735704B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104671247A (en) * | 2015-02-11 | 2015-06-03 | 武汉科技大学 | Method for preparing superfine nano-silicon by taking silicon-containing biomass as raw material as well as prepared superfine nano-silicon and application thereof |
| CN105932240A (en) * | 2016-05-11 | 2016-09-07 | 武汉科技大学 | Nano-silicon-carbon compound and preparation method and application thereof |
| 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 |
-
2022
- 2022-05-25 CN CN202210579171.9A patent/CN114735704B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104671247A (en) * | 2015-02-11 | 2015-06-03 | 武汉科技大学 | Method for preparing superfine nano-silicon by taking silicon-containing biomass as raw material as well as prepared superfine nano-silicon and application thereof |
| CN105932240A (en) * | 2016-05-11 | 2016-09-07 | 武汉科技大学 | Nano-silicon-carbon compound and preparation method and application thereof |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114735704B (en) | 2024-01-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101157373B1 (en) | Method for producing high purity porous silica and silicon from rice husk | |
| CN105347346B (en) | Air-assisted preparation method of porous nano silicon | |
| CN107150127B (en) | Preparation method of spherical cobalt powder | |
| CN102491328A (en) | Titanium carbide powder and preparation method thereof | |
| Azadeh et al. | Three-dimensional rice husk-originated mesoporous silicon and its electrical properties | |
| CN110707206B (en) | SnSe/rGO thermoelectric composite material and preparation method thereof | |
| CN113479934B (en) | BiOCl nano-sheet and preparation method and application thereof | |
| CN101863663B (en) | Combustion method for preparing submicron grade titanium carbide polycrystal powder | |
| CN113461054B (en) | BiOCl powder and preparation method and application thereof | |
| Ajeel et al. | New magnesio-thermal reduction technique to produce high-purity crystalline nano-silicon via semi-batch reactor | |
| CN113184870A (en) | Macro-particle-size-controllable LaB6Method for preparing powder | |
| CN114735704B (en) | Method for synthesizing nano silicon carbide at low temperature | |
| CN108735518B (en) | Hexagonal flaky manganese oxide @ nickel oxide composite material and preparation method thereof | |
| CN111196604A (en) | Method for preparing high-purity silicon by using waste micro-silicon powder as raw material | |
| CN110697776A (en) | Preparation method of spherical nano chromium sesquioxide | |
| CN113548898B (en) | (Mo) 0.2 W 0.2 V 0.2 Cr 0.2 Ni 0.2 ) B high-entropy ceramic powder and preparation method thereof | |
| CN101709508A (en) | Preparation method of bismuth-containing eulytite bismuth silicate crystals | |
| CN102060544B (en) | Quick crystallization method for realizing amorphous silicon nitride powder by taking silica powder as additive | |
| CN101780959B (en) | Preparation method of Bi4Si3O12 nanocrystals | |
| CN108039484B (en) | Spongy silicon powder, preparation method thereof and lithium ion battery | |
| CN113582701A (en) | Method for preparing high-purity single-phase AlON transparent ceramic powder by one-step rapid heating and carbon thermal reduction nitridation | |
| CN115340093B (en) | Method for preparing nano silicon or amorphous silicon dioxide by silicate | |
| CN112850716A (en) | Method for preparing nano-scale porous crystal Si by magnesiothermic reduction | |
| CN114751752B (en) | High-purity TiB 2 Ceramic nano-sheet and preparation method thereof | |
| CN113023714B (en) | Preparation method for self-propagating synthesis of porous graphene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |