CN113979439B - Si 5 C 3 Micro-nano material and preparation method thereof - Google Patents

Si 5 C 3 Micro-nano material and preparation method thereof Download PDF

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Publication number
CN113979439B
CN113979439B CN202111453275.7A CN202111453275A CN113979439B CN 113979439 B CN113979439 B CN 113979439B CN 202111453275 A CN202111453275 A CN 202111453275A CN 113979439 B CN113979439 B CN 113979439B
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micro
nano material
preparation
sodium chloride
mass ratio
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CN113979439A (en
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张利锋
阮欢
胡越
白嘉玺
郭守武
刘毅
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • 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
    • C01B32/97—Preparation from SiO or SiO2
    • 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
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • 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
    • C01P2004/45—Aggregated particles or particles with an intergrown morphology
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Abstract

The invention provides Si 5 C 3 A micro-nano material and a preparation method thereof belong to the field of micro-nano material synthesis. Silicon oxide powder as silicon sourceHumic acid carbon source is added with sodium chloride and other auxiliary reagents and heated to 500-700 ℃ in a tube furnace, then directly cooled or cooled to room temperature after heat preservation, and finally Si is prepared by impurity removal and drying 5 C 3 Nanoparticle assembled microsheet. The method has the advantages of high yield, low reaction temperature, short reaction time, energy conservation, good repeatability, simple operation, no pollution, easy removal of the reactants and products of the auxiliary reaction, and favorability for Si 5 C 3 And (4) mass production of micro-nano materials.

Description

Si 5 C 3 Micro-nano material and preparation method thereof
Technical Field
The invention belongs to the field of micro-nano material synthesis, and particularly relates to Si 5 C 3 Micro-nano material and a preparation method thereof.
Background
Silicon carbide, which is a wide band gap semiconductor material, is receiving attention because of its excellent physical properties such as high thermal conductivity, high electron saturation rate, high breakdown voltage, etc., and is considered as a potential candidate material for high-temperature high-power electronic device applications. In addition, under the action of the strong carbon-silicon covalent bond, the ceramic prepared by taking silicon carbide as a raw material has the characteristics of high mechanical strength, good acid-base corrosion resistance and thermal shock resistance and the like, and has wide application prospects in the aspects of high-temperature flue gas dust removal, water treatment, gas separation and the like. However, silicon carbide materials are typically prepared at higher temperatures.
For example, chinese patent CN200910256515.7 discloses a silicon carbide superfine powder and a production method thereof, the silicon carbide superfine powder with the particle size D50 of less than or equal to 0.45 micron is subjected to steps of slurry mixing, grading, dehydration and drying to obtain the superfine powder with the particle size D50 value of 0.1-0.3 mu m and the BET specific surface area of 30-50m 2 The purity is more than or equal to 98 weight percent, the sintering temperature is 1860-2000 ℃, and the sintering density is more than 3.15g/m 3 Silicon carbide superfine powder. Chinese patent CN201811307639.9 relates to a preparation method of solid-phase sintered silicon carbide ceramics, which comprises the following steps: preparing a main material and preparing water-based silicon carbide slurryAnd (3) feeding, performing spray granulation to obtain a silicon carbide biscuit, and sintering to obtain the solid-phase sintered silicon carbide ceramic, wherein the sintering temperature of the solid-phase sintered silicon carbide ceramic is reduced to 1750 ℃ at the lowest and is relatively low.
Disclosure of Invention
The object of the present invention is to overcome the disadvantages of the prior art mentioned above and to provide Si 5 C 3 A micro-nano material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
si 5 C 3 The preparation method of the micro-nano material comprises the following steps:
1) Grinding and mixing a silicon source and a carbon source to obtain a mixture;
2) Adding sodium chloride and aluminum powder into the mixture, adding absolute ethyl alcohol, grinding, and drying in vacuum to obtain a precursor;
3) Calcining the precursor at 500-700 ℃ for 1-2 hours, and then carrying out acid washing, water washing and vacuum drying to obtain Si 5 C 3 And (3) micro-nano materials.
Further, in the step 1), the silicon source is industrial-grade silicon oxide powder, and the carbon source is humic acid.
Further, in the step 1), the mass ratio of the silicon source to the carbon source is 1 (0.5 to 1).
Further, in step 1), the grinding time is 10 to 20 minutes.
Further, in the step 2), the mass ratio of the sodium chloride to the aluminum powder is 1 (0.2-1), and the mass ratio of the sodium chloride to the silicon source is 2:1.
Further, in the step 2), the grinding time is 0.5 to 1 hour.
Further, in the step 3), the calcining atmosphere is argon or nitrogen.
Si prepared by the method of the invention 5 C 3 And (3) micro-nano materials.
Further, is made of Si 5 C 3 Si assembled by nano particles 5 C 3 Micron sheet.
Compared with the prior art, the invention has the following beneficial effects:
si provided by the invention 5 C 3 The preparation method of the micro-nano material adopts common and easily-obtained industrial products as raw materials, has simple equipment, simple and convenient preparation process, strong repeatability, lower preparation temperature and smaller overall energy consumption, and is beneficial to industrial large-scale production.
Si provided by the invention 5 C 3 The micro-nano material has a structure and a component which are obviously different from common silicon carbide materials, and the crystal structure is cubic Si 5 C 3 The corresponding standard card number is PDF #50-1349. The product appearance is Si 5 C 3 The nanometer particles are assembled into micron sheets.
Drawings
FIG. 1 shows Si in example 1 5 C 3 XRD (X-ray diffraction) pattern of micro-nano material;
FIG. 2 shows Si in example 1 5 C 3 Scanning electron microscope images of the micro-nano materials.
Detailed Description
In order to make the technical solutions of the present invention better understood, 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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
example 1
Mixing silicon oxide powder and humic acid according to the mass ratio of 1:0.5, and grinding for 20 minutes. And adding sodium chloride and aluminum powder into the mixture, wherein the mass ratio of the sodium chloride to the aluminum oxide powder is 1.2, 2:1, adding 5ml of absolute ethyl alcohol, grinding for 1 hour, and drying in vacuum to obtain the precursor. Calcining the precursor at 700 ℃, acid washing, water washing and vacuum drying to obtain Si 5 C 3 And (3) micro-nano materials.
Referring to FIG. 1, FIG. 1 shows Si prepared according to the present invention 5 C 3 The XRD pattern of the micro-nano material can determine that the phase composition is cubic Si 5 C 3 The corresponding standard card number is PDF #50-1349.
Referring to FIG. 2, FIG. 2 is a scanning electron micrograph of the product of example 1, wherein Si is obtained 5 C 3 The micro-nano material has bright appearance characteristic and is in a micron sheet shape assembled by nano particles, and the size of the nano particles is about 100nm.
Example 2
Mixing silicon oxide powder and humic acid according to the mass ratio of 1.8, and grinding for 10 minutes. And adding sodium chloride and aluminum powder into the mixture, wherein the mass ratio of the sodium chloride to the aluminum oxide powder is 1.5, 2:1, adding 5ml of absolute ethyl alcohol, grinding for 0.5 hour, and drying in vacuum to obtain the precursor. Calcining the precursor at 500 ℃, acid washing, water washing and vacuum drying to obtain Si 5 C 3 And (3) micro-nano materials.
Example 3
Mixing silicon oxide powder and humic acid according to the mass ratio of 1:1, and grinding for 15 minutes. Adding sodium chloride and aluminum powder into the mixture, wherein the mass ratio of the sodium chloride to the aluminum powder is 1:1, and the mass ratio of the sodium chloride to the silicon oxide powder is2:1, adding 5ml absolute ethyl alcohol, grinding for 1 hour, and vacuum drying to obtain a precursor. Calcining the precursor at 600 ℃, acid washing, water washing and vacuum drying to obtain Si 5 C 3 And (3) micro-nano materials.
Example 4
Mixing silicon oxide powder and humic acid according to the mass ratio of 1. And adding sodium chloride and aluminum powder into the mixture according to the mass ratio of 1.2 to 2:1, adding 5ml of absolute ethyl alcohol, grinding for 1 hour, and drying in vacuum to obtain the precursor. Calcining the precursor at 500-700 ℃, acid washing, water washing and vacuum drying to obtain Si 5 C 3 And (3) micro-nano materials.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (6)

1. Si 5 C 3 The preparation method of the micro-nano material is characterized by comprising the following steps:
1) Grinding and mixing a silicon source and a carbon source to obtain a mixture;
2) Adding sodium chloride and aluminum powder into the mixture, adding absolute ethyl alcohol, grinding, and drying in vacuum to obtain a precursor;
in the step 2), the mass ratio of the sodium chloride to the aluminum powder is 1 (0.2-1), and the mass ratio of the sodium chloride to the silicon source is 2:1;
3) Calcining the precursor at 500-700 ℃ for 1-2 hours, and then carrying out acid washing, water washing and vacuum drying to obtain Si 5 C 3 Micro-nano materials;
the silicon source is industrial grade silicon oxide powder, and the carbon source is humic acid.
2. The Si according to claim 1 5 C 3 The preparation method of the micro-nano material is characterized in that in the step 1), a silicon source and a carbon sourceThe mass ratio of (1) to (0.5-1).
3. Si according to claim 1 5 C 3 The preparation method of the micro-nano material is characterized in that in the step 1), the grinding time is 10-20 minutes.
4. Si according to claim 1 5 C 3 The preparation method of the micro-nano material is characterized in that in the step 2), the grinding time is 0.5-1 hour.
5. Si according to claim 1 5 C 3 The preparation method of the micro-nano material is characterized in that in the step 3), the calcining atmosphere is argon or nitrogen.
6. Si produced by the method according to any one of claims 1 to 5 5 C 3 The micro-nano material is characterized in that the crystal structure is cubic Si 5 C 3 The product appearance is Si 5 C 3 The nanometer particles are assembled into micron sheets.
CN202111453275.7A 2021-11-30 2021-11-30 Si 5 C 3 Micro-nano material and preparation method thereof Active CN113979439B (en)

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* Cited by examiner, † Cited by third party
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CN105692622A (en) * 2016-03-18 2016-06-22 宁夏大学 Preparation method of nanoscale silicon carbide particles and product of nanoscale silicon carbide particles
WO2017180083A1 (en) * 2016-04-15 2017-10-19 Андрей ЦЫБА A method for the industrial production of sic nanopowders and high quality sio-c nanocomposite material and equipment for implementing said method
CN110639515B (en) * 2016-12-28 2022-04-15 苏州大学 Hollow mesoporous carbon nanosphere composite material loaded with gold nanoparticles and application of composite material in continuous CO treatment
CN109128149A (en) * 2018-08-22 2019-01-04 天津大学 The method for preparing three-dimensional carbon nanomaterial in aluminium powder surface in situ using sodium chloride template
CN109879285B (en) * 2019-03-21 2022-03-22 武汉工程大学 Silicon carbide nano material and preparation method thereof
CN110921651A (en) * 2019-11-18 2020-03-27 天津大学 Preparation of three-dimensional carbon-based composite material by metal-assisted salt template method

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