CN113979439A - Si5C3Micro-nano material and preparation method thereof - Google Patents

Si5C3Micro-nano material and preparation method thereof Download PDF

Info

Publication number
CN113979439A
CN113979439A CN202111453275.7A CN202111453275A CN113979439A CN 113979439 A CN113979439 A CN 113979439A CN 202111453275 A CN202111453275 A CN 202111453275A CN 113979439 A CN113979439 A CN 113979439A
Authority
CN
China
Prior art keywords
micro
nano material
preparation
nano
sodium chloride
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
Application number
CN202111453275.7A
Other languages
Chinese (zh)
Other versions
CN113979439B (en
Inventor
张利锋
阮欢
胡越
白嘉玺
郭守武
刘毅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN202111453275.7A priority Critical patent/CN113979439B/en
Publication of CN113979439A publication Critical patent/CN113979439A/en
Application granted granted Critical
Publication of CN113979439B publication Critical patent/CN113979439B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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
    • C01B32/97—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 Si5C3A micro-nano material and a preparation method thereof belong to the field of micro-nano material synthesis. Silicon oxide powder is taken as a silicon source, humic acid carbon source and auxiliary reagents such as sodium chloride are added into a tube furnace to be heated to the temperature of 500-700 ℃, then the mixture is directly cooled or cooled to the room temperature after heat preservation, and finally the Si is prepared by impurity removal and drying5C3Nanoparticle 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 reactants and products of auxiliary reaction, and contribution to the Si-like5C3And (4) mass production of micro-nano materials.

Description

Si5C3Micro-nano material and preparation method thereof
Technical Field
The invention belongs to the field of micro-nano material synthesis, and particularly relates to Si5C3Micro-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 granularity D50 being less than or equal to 0.45 micron is subjected to the steps of slurry mixing, classification, dehydration and drying to obtain the powder with the granularity D50 value of 0.1-0.3 micron and the BET specific surface area of 30-50m2The 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/m3Silicon carbide superfine powder. Chinese patent CN201811307639.9 relates to a preparation method of solid-phase sintered silicon carbide ceramic, which comprises the following steps: preparing a main material, preparing water-based silicon carbide slurry, performing spray granulation to obtain a silicon carbide biscuit, and sintering to obtain 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 present invention is directed to overcoming the above-mentioned disadvantages of the prior art and providing Si5C3Micro-nano material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
si5C3The 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 ℃, and calciningBurning for 1-2 hours, and then carrying out acid washing, water washing and vacuum drying to obtain Si5C3And (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.
Furthermore, in the step 1), the mass ratio of the silicon source to the carbon source is 1 (0.5-1).
Further, in the step 1), the grinding time is 10-20 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 0.5-1 hour.
Further, in the step 3), the calcining atmosphere is argon or nitrogen.
Si prepared by the method of the invention5C3And (3) micro-nano materials.
Further, is made of Si5C3Si assembled by nano particles5C3Micron sheet.
Compared with the prior art, the invention has the following beneficial effects:
si provided by the invention5C3The 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 invention5C3The micro-nano material has a structure and a component which are obviously different from common silicon carbide materials, and the crystal structure is cubic Si5C3The corresponding standard card number is PDF # 50-1349. The product appearance is Si5C3The nanometer particles are assembled into micron sheets.
Drawings
FIG. 1 shows Si in example 15C3XRD (X-ray diffraction) pattern of micro-nano material;
FIG. 2 shows Si in example 15C3Scanning electron microscope for micro-nano materialFigure (a).
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 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.
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 according to the mass ratio of 1:0.2 and the mass ratio of the sodium chloride to the silicon oxide powder of 2:1, adding 5ml of absolute ethyl alcohol, grinding for 1 hour, and drying in vacuum to obtain a precursor. Calcining the precursor at 700 ℃, acid washing, water washing and vacuum drying to obtain Si5C3And (3) micro-nano materials.
Referring to FIG. 1, FIG. 1 shows Si prepared according to the present invention5C3XRD pattern of micro-nano material, which can be obtained byTo determine the composition of the phase as cubic Si5C3The 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 was obtained5C3The micro-nano material has distinct morphology and features, is in a micron sheet shape assembled by nano particles, and has the size of about 100 nm.
Example 2
Mixing silicon oxide powder and humic acid according to the mass ratio of 1:0.8, and grinding for 10 minutes. And adding sodium chloride and aluminum powder into the mixture according to the mass ratio of 1:0.5 and the mass ratio of the sodium chloride to the silicon oxide powder of 2:1, adding 5ml of absolute ethyl alcohol, grinding for 0.5 hour, and drying in vacuum to obtain a precursor. Calcining the precursor at 500 ℃, acid washing, water washing and vacuum drying to obtain Si5C3And (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. And adding sodium chloride and aluminum powder into the mixture according to the mass ratio of 1:1 and the mass ratio of the sodium chloride to the silicon oxide powder of 2:1, adding 5ml of absolute ethyl alcohol, grinding for 1 hour, and drying in vacuum to obtain a precursor. Calcining the precursor at 600 ℃, acid washing, water washing and vacuum drying to obtain Si5C3And (3) micro-nano materials.
Example 4
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 according to the mass ratio of 1:0.2 and the mass ratio of the sodium chloride to the silicon oxide powder of 2:1, adding 5ml of absolute ethyl alcohol, grinding for 1 hour, and drying in vacuum to obtain a precursor. Calcining the precursor at 500-700 ℃, pickling, washing with water, and vacuum drying to obtain Si5C3And (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 (9)

1. Si5C3The 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;
3) calcining the precursor at 500-700 ℃, calcining for 1-2 hours, and then carrying out acid washing, water washing and vacuum drying to obtain Si5C3And (3) micro-nano materials.
2. Si according to claim 15C3The preparation method of the micro-nano material is characterized in that in the step 1), the silicon source is industrial-grade silicon oxide powder, and the carbon source is humic acid.
3. Si according to claim 25C3The preparation method of the micro-nano material is characterized in that in the step 1), the mass ratio of the silicon source to the carbon source is 1 (0.5-1).
4. Si according to claim 15C3The preparation method of the micro-nano material is characterized in that in the step 1), the grinding time is 10-20 minutes.
5. Si according to claim 15C3The preparation method of the micro-nano material is characterized in that in the step 2), the mass ratio of sodium chloride to aluminum powder is 1 (0.2-1), and the mass ratio of sodium chloride to a silicon source is 2: 1.
6. Si according to claim 15C3The preparation method of the micro-nano material is characterized in that in the step 2), the grinding time is 0.5-1 hour.
7. Si according to claim 15C3The preparation method of the micro-nano material is characterized in that in the step 3), the calcining atmosphere is argon or nitrogen.
8. Si prepared by the method of any one of claims 1 to 75C3And (3) micro-nano materials.
9. Si according to claim 85C3The micro-nano material is characterized in that the micro-nano material is made of Si5C3Si assembled by nano particles5C3Micron sheet.
CN202111453275.7A 2021-11-30 2021-11-30 Si 5 C 3 Micro-nano material and preparation method thereof Active CN113979439B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111453275.7A CN113979439B (en) 2021-11-30 2021-11-30 Si 5 C 3 Micro-nano material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111453275.7A CN113979439B (en) 2021-11-30 2021-11-30 Si 5 C 3 Micro-nano material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN113979439A true CN113979439A (en) 2022-01-28
CN113979439B CN113979439B (en) 2022-12-20

Family

ID=79732882

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111453275.7A Active CN113979439B (en) 2021-11-30 2021-11-30 Si 5 C 3 Micro-nano material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113979439B (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
US20180178197A1 (en) * 2016-12-28 2018-06-28 Soochow University Hollow mesoporous carbon nanosphere composite material loaded with gold nanoparticles, and preparation method thereof and application in continuous processing of co
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
CN109879285A (en) * 2019-03-21 2019-06-14 武汉工程大学 A kind of 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

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
US20180178197A1 (en) * 2016-12-28 2018-06-28 Soochow University Hollow mesoporous carbon nanosphere composite material loaded with gold nanoparticles, and preparation method thereof and application in continuous processing of co
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
CN109879285A (en) * 2019-03-21 2019-06-14 武汉工程大学 A kind of 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

Also Published As

Publication number Publication date
CN113979439B (en) 2022-12-20

Similar Documents

Publication Publication Date Title
CN103539088B (en) A kind of synthetic method of aluminum nitride nanometer particle
CN110980664B (en) Porous few-layer h-BN nanosheet and preparation method thereof
CN103553002A (en) Method for preparation of high purity alpha phase silicon nitride powder from recovered silicon chip cut sawdust
CN102009993A (en) Method for preparing submicron aluminium oxide by two-stage roasting method
CN103553647B (en) Method for preparation of silicon nitride bonded silicon carbide refractory material by using silicon cutting waste mortar
CN110577403A (en) high-purity aluminum nitride powder and preparation method thereof
CN109264680A (en) The method for preparing high-purity ultra-fine aluminum nitride powder based on aluminium alcoholates Hydrolyze method
CN112159234A (en) High-entropy ceramic powder and preparation method and application thereof
CN103265291A (en) Preparation method of nanometer calcium hexaboride powder
CN100560487C (en) A kind of method of low-temperature preparation of cubic silicon carbide nano wire
Liu et al. Fabrication of β-sialon powder from kaolin
CN100480438C (en) Monocrystal AIN nano chain
CN113979439B (en) Si 5 C 3 Micro-nano material and preparation method thereof
CN109650896B (en) Synthesis method of LiAlON transparent ceramic powder
CN114538913B (en) Pure-phase nano MgAl with high sintering activity 2 O 4 Powder and preparation method and application thereof
CN107188181B (en) A kind of low temperature synthesizes the method and silicon carbide products of high-specific-surface mesoporous silicon carbide
US11623210B2 (en) Method for preparing silicate/carbon composite from attapulgite, and use of silicate/carbon composite
CN113213968B (en) Micron-sized metastable phase epsilon-Fe 2 O 3 Preparation method of (1)
CN108502886A (en) A kind of preparation method of nano-sheet silicon carbide
Ishihara et al. Synthesis of silicon carbide powders from fumed silica powder and phenolic resin
CN101318638B (en) Novel method for preparing nano-carbon titanium nitride powder with precursors
CN114180560A (en) Preparation method of coal-based graphene in molten salt system
CN112919891A (en) Environment-friendly high-new powder material for ceramic roller and preparation method thereof
CN112760703A (en) Method for preparing mullite whisker from dedusting ash of electric melting alpha-beta alumina brick
KR102509020B1 (en) SiC Powder For Pressureless Sintering From Wasted Solar Panel And Manufacturing Metholds Thereof

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