CN106784667B - A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof - Google Patents
A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof Download PDFInfo
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- CN106784667B CN106784667B CN201611138624.5A CN201611138624A CN106784667B CN 106784667 B CN106784667 B CN 106784667B CN 201611138624 A CN201611138624 A CN 201611138624A CN 106784667 B CN106784667 B CN 106784667B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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 present invention relates to a kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof.Its technical solution is: by silicon powder: the molar ratio of silicon dioxide powder is 1: silicon powder and silicon dioxide powder are mixed, obtain silicon source by (0.3 ~ 4)；Pitch based carbon fiber or Carbon fibe felt are placed in high temperature graphitization furnace, 0.5 ~ 1h is heat-treated under the conditions of 1000 ~ 2800 DEG C in argon atmosphere, obtains carbon source.By silicon source: the molar ratio of carbon source is 1: silicon source and carbon source are sequentially placed into graphite crucible, then graphite crucible are put into high temperature carbonization furnace, be evacuated to 5 ~ 20Pa by (0.25 ~ 4), then are passed through argon gas to normal pressure；Under the conditions of argon atmosphere, high temperature carbonization furnace is warming up to 1200 ~ 1500 DEG C with the rate of 10 ~ 20 DEG C/min, keeps the temperature 0.5 ~ 3h, charcoal material surface SiC Nanometer Whiskers are made in cooled to room temperature.Present invention process is simple, reaction condition is mild, environmentally friendly, made product optical property and electrochemical performance.
Description
Technical field
The invention belongs to SiC Nanometer Whiskers technical fields.More particularly to a kind of charcoal material surface SiC Nanometer Whiskers
And preparation method thereof.
Background technique
SiC Nanometer Whiskers (SiCw) it be a kind of diameter is nanometer to micron-sized high purity single crystal material.Based on its perfection
Crystal structure, silicon carbide whisker has high-melting-point (> 2700 DEG C), low-density, tensile strength, and excellent (tensile strength is
2100MPa) and good specific strength and the mechanical property than elasticity modulus, it is widely used as the reinforcement of various high performance materials
Flexibilizer additive.Meanwhile one-dimensional SiC Nanometer Whiskers have excellent optically and electrically performance, it can be in high temperature, high energy and height
It works under the harsh environments such as frequency, therefore there is tempting application prospect in terms of preparing advanced nano photoelectronic devices.Another party
Face, Carbon fibe and SiC Nanometer Whiskers it is compound can particle effectively in filtered fuel, be a kind of novel cheap, lightweight filtering
Equipment has biggish industrial application value；In electrochemical field, SiC Nanometer Whiskers and Carbon Materials it is compound after, become performance
The electrode material of excellent lithium cell cathode material and supercapacitor, shows excellent chemical property.
Currently, the preparation process of SiC whisker mainly includes that chemical vapour deposition technique (CVD), carbothermic method, presoma are split
Solution and carbon nano carbon tube limited reactions method etc..
Chemical vapour deposition technique (CVD) is using wide method, and this method utilizes carbon containing and silicon gas or utilization
Carbon containing and siliceous gas organic matter can be decomposed to form as raw material, prepare SiC whisker.
Chemical vapor deposition process needs strict control reactant and carrier gas flux, the high requirements on the equipment, process cycle
It is longer, thus silicon carbide whisker preparation cost is higher, and with a large amount of harmful poisonous gas in the preparation process of silicon carbide whisker
Body generates, larger to environmental hazard.
The higher reaction temperature of carbothermic method process requirement (> 1500 DEG C) generally requires catalyst in the technical process
Participation, this preparation cost is higher, catalyst participation largely effect on silicon carbide whisker purity and performance, limit silicon carbide whisker
A large amount of preparations and application.
Presoma cracking process generally uses Polycarbosilane for raw material, obtains that purity is higher, draw ratio is taught by Pintsch process
Big silicon carbide whisker, but Polycarbosilane presoma is expensive, is not suitable for as the raw material for largely preparing silicon carbide whisker.
Carbon nanotube lambda limiting process simple process, reaction condition is mild, and no toxic and harmful gas generates, and the technique does not need
Catalyst participates in, and can prepare the SiC Nanometer Whiskers of high quality high-purity.But using nano carbon tube as carbon source in the technique, valence
Lattice are expensive, and preparation cost is higher.
Summary of the invention
The present invention is directed to overcome the deficiencies of existing technologies, it is therefore an objective to provide that a kind of simple process, reaction condition be mild and ring
The preparation method of the charcoal material surface SiC Nanometer Whiskers of border close friend；The charcoal material surface nanometer silicon carbide of this method preparation is brilliant
Must have excellent optical property and chemical property.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that:
Step 1: pressing silicon powder: the molar ratio of silicon dioxide powder is 1: (0.25 ~ 4) mixes silicon powder and silicon dioxide powder equal
It is even, obtain silicon source.
Step 2: pitch based carbon fiber or pitch based carbon fiber felt are placed in high temperature graphitization furnace, it is passed through argon gas progress
High temperature carbonization processing, the temperature of high temperature carbonization processing are 1000 ~ 2800 DEG C, and the time of high temperature carbonization processing is 0.5 ~ 1h, are obtained
Carbon source.
Step 3: pressing the silicon source: the molar ratio of the carbon source is 1: (0.25 ~ 4), by the silicon source and the carbon source according to
It is secondary to be placed in graphite crucible, then the graphite crucible is put into high temperature carbonization furnace, is evacuated to 5 ~ 20Pa, then be passed through argon gas
To normal pressure.
Step 4: the high temperature carbonization furnace is warming up to 1200 with the rate of 10 ~ 20 DEG C/min under the conditions of argon atmosphere
~ 1500 DEG C, 0.5 ~ 3h is kept the temperature, charcoal material surface SiC Nanometer Whiskers are made in cooled to room temperature.
The granularity of the silicon powder is 20 ~ 80 μm.
The granularity of the SiO 2 powder is 20 ~ 80 μm.
Due to using the technology described above, the present invention has following good effect compared with prior art:
(1) present invention uses solid phase inorganic silicon source and carbon source, and charcoal is participated in and be made when at 1200 ~ 1500 DEG C in no catalyst
Material surface silicon carbide whisker, simple process to equipment without particular/special requirement, and discharge in preparation process without toxic and harmful gas.
(2) SiC Nanometer Whiskers of big L/D ratio are made in charcoal material surface in the present invention, and silicon carbide whisker diameter is 30 ~
120nm, length are 30 ~ 150um.Prepared charcoal material surface SiC Nanometer Whiskers are shown through laser excitation at room temperature
Obvious blue-shifted phenomenon, emission wavelength are 420 ~ 460nm, have excellent photoluminescence performance；As negative electrode of lithium ion battery material
Capacity is 550 ~ 700mAh/g when material, shows excellent electrochemical performance.
Therefore, the present invention has the characteristics that simple process, reaction condition are mild and environmental-friendly, the charcoal material surface of preparation
The optical property and electrochemical performance of SiC Nanometer Whiskers.
Detailed description of the invention
Fig. 1 is a kind of optical photograph of charcoal material surface SiC Nanometer Whiskers of the invention；
Fig. 2 is the XRD spectra of charcoal material surface SiC Nanometer Whiskers shown in Fig. 1；
Fig. 3 is the low power SEM photograph of charcoal material surface SiC Nanometer Whiskers shown in Fig. 1；
Fig. 4 is the high power SEM photograph of charcoal material surface SiC Nanometer Whiskers shown in Fig. 1.
Specific embodiment
For a better understanding of the present invention, present invention will be further described below with reference to the accompanying drawings and specific embodiments,
Not to the limitation of its protection scope.
It is first that the raw material Unify legislation of silicon source described in present embodiment is as follows to avoid repeating, in embodiment no longer
It repeats:
The granularity of the silicon powder is 20 ~ 80 μm.
The granularity of the SiO 2 powder is 20 ~ 80 μm.
Embodiment 1
A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof.The present embodiment comprises the concrete steps that:
Step 1: pressing silicon powder: the molar ratio of silicon dioxide powder is 1: (0.25 ~ 1) mixes silicon powder and silicon dioxide powder equal
It is even, obtain silicon source.
Step 2: pitch based carbon fiber is placed in high temperature graphitization furnace, it is passed through argon gas and carries out high temperature carbonization processing, high temperature
The temperature of charing process is 1000 ~ 1600 DEG C, and the time of high temperature carbonization processing is 0.5 ~ 1h, obtains carbon source.
Step 3: pressing the silicon source: the molar ratio of the carbon source is 1: (0.25 ~ 1), by the silicon source and the carbon source according to
It is secondary to be placed in graphite crucible, then the graphite crucible is put into high temperature carbonization furnace, is evacuated to 5 ~ 20Pa, then be passed through argon gas
To normal pressure.
Step 4: the high temperature carbonization furnace is warming up to 1200 with the rate of 10 ~ 20 DEG C/min under the conditions of argon atmosphere
~ 1300 DEG C, 0.5 ~ 1h is kept the temperature, charcoal material surface SiC Nanometer Whiskers are made in cooled to room temperature.
Charcoal material surface SiC Nanometer Whiskers manufactured in the present embodiment: diameter is 30 ~ 70nm；Length is 30 ~ 70um.
Embodiment 2
A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof.The present embodiment comprises the concrete steps that:
Step 1: pressing silicon powder: the molar ratio of silicon dioxide powder is 1: silicon powder and silicon dioxide powder are uniformly mixed by (1 ~ 2),
Obtain silicon source.
Step 2: pitch based carbon fiber felt is placed in high temperature graphitization furnace, it is passed through argon gas and carries out high temperature carbonization processing, it is high
The temperature of warm charing process is 1600 ~ 2200 DEG C, and the time of high temperature carbonization processing is 0.5 ~ 1h, obtains carbon source.
Step 3: pressing the silicon source: the molar ratio of the carbon source is 1: (1 ~ 2), successively by the silicon source and the carbon source
It is placed in graphite crucible, then the graphite crucible is put into high temperature carbonization furnace, be evacuated to 5 ~ 20Pa, then be passed through argon gas extremely
Normal pressure.
Step 4: the high temperature carbonization furnace is warming up to 1300 with the rate of 10 ~ 20 DEG C/min under the conditions of argon atmosphere
~ 1400 DEG C, 1 ~ 2h is kept the temperature, charcoal material surface SiC Nanometer Whiskers are made in cooled to room temperature.
Charcoal material surface SiC Nanometer Whiskers manufactured in the present embodiment: diameter is 50 ~ 100nm；Length is 80 ~ 150um.
Embodiment 3
A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof.The present embodiment comprises the concrete steps that:
Step 1: pressing silicon powder: the molar ratio of silicon dioxide powder is 1: silicon powder and silicon dioxide powder are uniformly mixed by (2 ~ 3),
Obtain silicon source.
Step 2: pitch based carbon fiber is placed in high temperature graphitization furnace, it is passed through argon gas and carries out high temperature carbonization processing, high temperature
The temperature of charing process is 2200 ~ 2800 DEG C, and the time of high temperature carbonization processing is 0.5 ~ 1h, obtains carbon source.
Step 3: pressing the silicon source: the molar ratio of the carbon source is 1: (3 ~ 4), successively by the silicon source and the carbon source
It is placed in graphite crucible, then the graphite crucible is put into high temperature carbonization furnace, be evacuated to 5 ~ 20Pa, then be passed through argon gas extremely
Normal pressure.
Step 4: the high temperature carbonization furnace is warming up to 1400 with the rate of 10 ~ 20 DEG C/min under the conditions of argon atmosphere
~ 1500 DEG C, 2 ~ 3h is kept the temperature, charcoal material surface SiC Nanometer Whiskers are made in cooled to room temperature.
Charcoal material surface SiC Nanometer Whiskers manufactured in the present embodiment: diameter is 80 ~ 120nm；Length is 50 ~ 100um.
Embodiment 4
A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof.The present embodiment comprises the concrete steps that:
Step 1: pressing silicon powder: the molar ratio of silicon dioxide powder is 1: silicon powder and silicon dioxide powder are uniformly mixed by (3 ~ 4),
Obtain silicon source.
Step 2: pitch based carbon fiber felt is placed in high temperature graphitization furnace, it is passed through argon gas and carries out high temperature carbonization processing, it is high
The temperature of warm charing process is 1600 ~ 2200 DEG C, and the time of high temperature carbonization processing is 0.5 ~ 1h, obtains carbon source.
Step 3: pressing the silicon source: the molar ratio of the carbon source is 1: (2 ~ 3), successively by the silicon source and the carbon source
It is placed in graphite crucible, then the graphite crucible is put into high temperature carbonization furnace, be evacuated to 5 ~ 20Pa, then be passed through argon gas extremely
Normal pressure.
Step 4: the high temperature carbonization furnace is warming up to 1300 with the rate of 10 ~ 20 DEG C/min under the conditions of argon atmosphere
~ 1400 DEG C, 1 ~ 2h is kept the temperature, charcoal material surface SiC Nanometer Whiskers are made in cooled to room temperature.
Charcoal material surface SiC Nanometer Whiskers manufactured in the present embodiment: diameter is 60 ~ 110nm；Length is 70 ~ 130um.
Present embodiment has following good effect compared with prior art:
(1) present embodiment uses solid phase inorganic silicon source and carbon source, participates in no catalyst and at 1200 ~ 1500 DEG C
When be made charcoal material surface silicon carbide whisker, simple process, to equipment without particular/special requirement, and without poisonous and harmful gas in preparation process
Body release.
(2) SiC Nanometer Whiskers of big L/D ratio are made in charcoal material surface for present embodiment.Fig. 1 is embodiment
A kind of optical photograph of charcoal material surface SiC Nanometer Whiskers of 2 preparations；Fig. 2 is that charcoal material surface silicon carbide shown in Fig. 1 is received
The XRD spectra of meter Jing Xu；Fig. 3 is the low power SEM photograph of charcoal material surface SiC Nanometer Whiskers shown in Fig. 1；Fig. 4 is Fig. 1 institute
Show the high power SEM photograph of charcoal material surface SiC Nanometer Whiskers.As seen from Figure 1, Carbon fibe felt becomes greyish white from black
Color shows that the growth of carbon fiber surface silicon carbide whisker is intensive；As seen from Figure 2, the phase composition of SiC Nanometer Whiskers is main
For β-SiC, the diffraction maximum near 36 °, 60 °, 72 ° is corresponding in turn to (111), (220), (311) crystal face of β-SiC, wherein
26 ° or so of diffraction maximum corresponds to Carbon fibe matrix, shows to grow a large amount of SiC Nanometer Whiskers in charcoal material surface；From Fig. 3
As can be seen that Carbon fibe is carbonized silicon wafer completely to be wrapped up, silicon carbide whisker length is 100-150 μm；From fig. 4, it can be seen that
SiC Nanometer Whiskers are relatively uniform, it is smooth, without obvious fault of construction, silicon carbide whisker diameter is 80-120nm.Therefore, this tool
Charcoal material surface silicon carbide whisker purity is high, better crystallinity degree and draw ratio prepared by body embodiment is big, silicon carbide whisker diameter
For 30 ~ 120nm, length is 30 ~ 150um.
The charcoal material surface SiC Nanometer Whiskers of present embodiment preparation are at room temperature through laser excitation table
Reveal obvious blue-shifted phenomenon, emission wavelength is 420 ~ 460nm, has excellent photoluminescence performance；Product conduct as shown in Figure 1
Capacity is 550 ~ 700mAh/g when lithium ion battery negative material, shows excellent electrochemical performance.
Therefore, present embodiment has the characteristics that simple process, reaction condition are mild and environmental-friendly, the charcoal of preparation
The optical property and electrochemical performance of material surface SiC Nanometer Whiskers.
Claims (4)
1. a kind of preparation method of charcoal material surface SiC Nanometer Whiskers, it is characterised in that the following steps are included:
Step 1: pressing silicon powder: the molar ratio of silicon dioxide powder is 1: silicon powder and silicon dioxide powder are uniformly mixed by (0.25 ~ 4),
Obtain silicon source；
Step 2: pitch based carbon fiber or pitch based carbon fiber felt are placed in high temperature graphitization furnace, it is passed through argon gas and carries out high temperature
Charing process, the temperature of high temperature carbonization processing are 1000 ~ 2800 DEG C, and the time of high temperature carbonization processing is 0.5 ~ 1h, obtain carbon source；
Step 3: pressing the silicon source: the molar ratio of the carbon source is 1: (0.25 ~ 4) successively sets the silicon source and the carbon source
In graphite crucible, then the graphite crucible is put into high temperature carbonization furnace, is evacuated to 5 ~ 20Pa, then is passed through argon gas to normal
Pressure；
Step 4: under the conditions of argon atmosphere, the high temperature carbonization furnace is warming up to 1200 with the rate of 10 ~ 20 DEG C/min ~
1500 DEG C, 0.5 ~ 3h is kept the temperature, charcoal material surface SiC Nanometer Whiskers are made in cooled to room temperature.
2. the preparation method of charcoal material surface SiC Nanometer Whiskers according to claim 1, it is characterised in that the silicon powder
Granularity be 20 ~ 80 μm.
3. the preparation method of charcoal material surface SiC Nanometer Whiskers according to claim 1, it is characterised in that the dioxy
The granularity of SiClx powder is 20 ~ 80 μm.
4. a kind of charcoal material surface SiC Nanometer Whiskers, it is characterised in that the charcoal material surface SiC Nanometer Whiskers are roots
According to Carbon Materials table prepared by the preparation method of charcoal material surface SiC Nanometer Whiskers described in any one of claim 1 ~ 3
Face SiC Nanometer Whiskers.
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| CN107128926B (en) * | 2017-06-28 | 2020-01-24 | 湖南大学 | Preparation method of self-supporting carbide derived carbon nanowire |
| CN108560058B (en) * | 2018-05-18 | 2020-10-23 | 湖南东映碳材料科技有限公司 | Preparation method of zirconium carbide whisker |
| CN108502886A (en) * | 2018-06-15 | 2018-09-07 | 天津工业大学 | A kind of preparation method of nano-sheet silicon carbide |
| CN111392730B (en) * | 2020-04-22 | 2022-08-30 | 扬州市汀月科技有限公司 | Method for preparing silicon carbide whisker by combining fluidized bed with carbothermic reduction reaction and application thereof |
| CN114477185B (en) * | 2020-10-28 | 2023-07-07 | 中国科学院理化技术研究所 | beta-SiC with lamellar structure and preparation method thereof |
| CN112608156B (en) * | 2020-12-29 | 2021-12-03 | 内蒙古海特华材科技有限公司 | Preparation method of micro-nano mixed SiC chopped fibers |
| CN113185327B (en) * | 2021-04-28 | 2022-05-31 | 大连理工大学 | Silicon carbide whisker obtained on surface of carbon fiber reinforced composite material rapidly and efficiently and preparation method thereof |
| CN114032607B (en) * | 2021-11-02 | 2024-01-09 | 西北工业大学 | Method for preparing zirconium carbide whisker by adopting zirconium carbide seed crystal |
| CN114959905A (en) * | 2022-03-07 | 2022-08-30 | 西北工业大学 | Catalyst-free synthesized tantalum carbide nano whisker and preparation method thereof |
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| CN1281910A (en) * | 1999-07-21 | 2001-01-31 | 中国科学院山西煤炭化学研究所 | Preparation method of nanometer silicon carbide whiskers |
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