CN106784667A - 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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- 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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Abstract
The present invention relates to a kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof.Its technical scheme is：By silica flour: the mol ratio of silicon dioxide powder is 1:（0.3~4）, silica flour and silicon dioxide powder are mixed, obtain silicon source；Pitch based carbon fiber or Carbon fibe felt are placed in high temperature graphitization stove, 0.5 ~ 1h is heat-treated under the conditions of 1000 ~ 2800 DEG C in argon gas atmosphere, carbon source is obtained.By silicon source: the mol ratio of carbon source is 1:（0.25~4）, silicon source and carbon source are sequentially placed into graphite crucible, then graphite crucible is put into high temperature carbonization furnace, 5 ~ 20Pa is evacuated to, then be passed through argon gas to normal pressure；Under the conditions of argon gas atmosphere, high temperature carbonization furnace is warming up to 1200 ~ 1500 DEG C with the speed of 10 ~ 20 DEG C/min, is incubated 0.5 ~ 3h, naturally cool to room temperature, charcoal material surface SiC Nanometer Whiskers are obtained.Present invention process is simple, reaction condition is gentle, environmentally friendly, made product optical property and electrochemical performance.
Description
Technical field
The invention belongs to SiC Nanometer Whiskers technical field.More particularly to a kind of charcoal material surface SiC Nanometer Whiskers
And preparation method thereof.
Background technology
SiC Nanometer Whiskers（SiCw）It is a kind of a diameter of nanometer to micron-sized high purity single crystal material.It is perfect based on it
Crystal structure, silicon carbide whisker has high-melting-point（>2700℃）, low-density, tensile strength it is excellent（Tensile strength is
2100MPa）And good specific strength and the mechanical property than elastic modelling quantity, 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, can be in high temperature, high energy and height
Worked under the harsh environments such as frequency, therefore there is tempting application prospect in terms of advanced nano photoelectronic devices are prepared.The opposing party
Face, Carbon fibe and SiC Nanometer Whiskers it is compound can particulate effectively in filtered fuel, be it is a kind of it is new inexpensively, the filtering of lightweight
Equipment, there is larger industrial application value；In electrochemical field, after SiC Nanometer Whiskers are compound with Carbon Materials, as performance
Excellent lithium cell cathode material and the electrode material of ultracapacitor, show excellent chemical property.
At present, the preparation technology of SiC whiskers mainly includes that chemical vapour deposition technique (CVD), carbothermic method, presoma split
Solution and carbon nano carbon tube limited reactions method etc..
Chemical vapour deposition technique (CVD) is gas or utilization of the method using carbon containing and silicon using wide method
Carbon containing and siliceous gas organic matter can be decomposed to form as raw material, SiC whiskers are prepared.
Chemical vapor deposition method needs strict control reactant and carrier gas flux, process cycle higher to equipment requirement
It is more long, 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 is produced, larger to environmental hazard.
Carbothermic method technique needs reaction temperature higher（>1500℃）, catalyst is generally required in the technical process
Participation, this preparation cost is higher, and catalyst participates in largely effecting on silicon carbide whisker purity and performance, limitation silicon carbide whisker
It is a large amount of to prepare and apply.
It is raw material that presoma cracking process typically use Polycarbosilane, 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.
CNT lambda limiting process process is simple, reaction condition is gentle, is produced without toxic and harmful, and the technique need not
Catalyst is participated in, and can prepare the SiC Nanometer Whiskers of high-quality high-purity.But with nano carbon tube as carbon source in the technique, valency
Lattice are expensive, and preparation cost is higher.
The content of the invention
It is contemplated that overcoming the defect of prior art, it is therefore an objective to provide a kind of process is simple, reaction condition gently and ring
The preparation method of the friendly charcoal material surface SiC Nanometer Whiskers in border；Charcoal material surface nanometer silicon carbide prepared by the method is brilliant
Must have excellent optical property and chemical property.
To achieve the above object, the technical solution adopted by the present invention is comprised the concrete steps that：
Step one, by silica flour: the mol ratio of silicon dioxide powder be 1:（0.25~4）, silica flour and silicon dioxide powder are well mixed,
Obtain silicon source.
Step 2, pitch based carbon fiber or pitch based carbon fiber felt are placed in high temperature graphitization stove, being passed through argon gas is carried out
High temperature carbonization treatment, the temperature of high temperature carbonization treatment is 1000 ~ 2800 DEG C, and the time of high temperature carbonization treatment is 0.5 ~ 1h, is obtained
Carbon source.
Step 3, by the silicon source: the mol ratio of the carbon source be 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, 5 ~ 20Pa is evacuated to, then be passed through argon gas
To normal pressure.
Step 4, under the conditions of argon gas atmosphere, the high temperature carbonization furnace is warming up to 1200 with the speed of 10 ~ 20 DEG C/min
~ 1500 DEG C, 0.5 ~ 3h is incubated, naturally cools to room temperature, charcoal material surface SiC Nanometer Whiskers are obtained.
The granularity of the silica flour is 20 ~ 80 μm.
The granularity of the SiO 2 powder is 20 ~ 80 μm.
There is following good effect compared with prior art due to using above technical scheme, the present invention：
(1) present invention uses solid phase inorganic silicon source and carbon source, and Carbon Materials are obtained when being participated in without catalyst and at 1200 ~ 1500 DEG C
Surface carborundum whisker, process is simple, to equipment without in particular/special requirement, and preparation process without toxic and harmful discharge.
(2) SiC Nanometer Whiskers that big L/D ratio is obtained in charcoal material surface of the invention, silicon carbide whisker a diameter of 30 ~
120nm, length is 30 ~ 150um.Prepared charcoal material surface SiC Nanometer Whiskers show through laser excitation at room temperature
Obvious blue-shifted phenomenon, emission wavelength is 420 ~ 460nm, with excellent photoluminescence performance；As lithium ion battery negative material
Capacity is 550 ~ 700mAh/g during material, shows excellent electrochemical performance.
Therefore, the characteristics of present invention has process is simple, reaction condition is gentle and environment-friendly, the charcoal material surface of preparation
The optical property and electrochemical performance of SiC Nanometer Whiskers.
Brief description of the drawings
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, the invention will be further described with reference to the accompanying drawings and detailed description,
Not to the limitation of its protection domain.
It is first that the raw material Unify legislation of silicon source described in this specific embodiment is as follows to avoid repeating, in embodiment no longer
Repeat：
The granularity of the silica flour 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 is comprised the concrete steps that：
Step one, by silica flour: the mol ratio of silicon dioxide powder be 1:（0.25~1）, silica flour and silicon dioxide powder are well mixed,
Obtain silicon source.
Step 2, pitch based carbon fiber is placed in high temperature graphitization stove, being passed through argon gas carries out high temperature carbonization treatment, high temperature
The temperature of charing process is 1000 ~ 1600 DEG C, and the time of high temperature carbonization treatment is 0.5 ~ 1h, obtains carbon source.
Step 3, by the silicon source: the mol ratio of the carbon source be 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, 5 ~ 20Pa is evacuated to, then be passed through argon gas
To normal pressure.
Step 4, under the conditions of argon gas atmosphere, the high temperature carbonization furnace is warming up to 1200 with the speed of 10 ~ 20 DEG C/min
~ 1300 DEG C, 0.5 ~ 1h is incubated, naturally cools to room temperature, charcoal material surface SiC Nanometer Whiskers are obtained.
Charcoal material surface SiC Nanometer Whiskers manufactured in the present embodiment：A diameter of 30 ~ 70nm；Length is 30 ~ 70um.
Embodiment 2
A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof.The present embodiment is comprised the concrete steps that：
Step one, by silica flour: the mol ratio of silicon dioxide powder be 1:（1~2）, silica flour and silicon dioxide powder are well mixed, obtain
Silicon source.
Step 2, pitch based carbon fiber felt is placed in high temperature graphitization stove, being passed through argon gas carries out high temperature carbonization treatment, it is high
The temperature of warm charing process is 1600 ~ 2200 DEG C, and the time of high temperature carbonization treatment is 0.5 ~ 1h, obtains carbon source.
Step 3, by the silicon source: the mol ratio of the carbon source be 1:（1~2）, by the silicon source and the carbon source successively
It is 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 extremely
Normal pressure.
Step 4, under the conditions of argon gas atmosphere, the high temperature carbonization furnace is warming up to 1300 with the speed of 10 ~ 20 DEG C/min
~ 1400 DEG C, 1 ~ 2h is incubated, naturally cools to room temperature, charcoal material surface SiC Nanometer Whiskers are obtained.
Charcoal material surface SiC Nanometer Whiskers manufactured in the present embodiment：A diameter of 50 ~ 100nm；Length is 80 ~ 150um.
Embodiment 3
A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof.The present embodiment is comprised the concrete steps that：
Step one, by silica flour: the mol ratio of silicon dioxide powder be 1:（2~3）, silica flour and silicon dioxide powder are well mixed, obtain
Silicon source.
Step 2, pitch based carbon fiber is placed in high temperature graphitization stove, being passed through argon gas carries out high temperature carbonization treatment, high temperature
The temperature of charing process is 2200 ~ 2800 DEG C, and the time of high temperature carbonization treatment is 0.5 ~ 1h, obtains carbon source.
Step 3, by the silicon source: the mol ratio of the carbon source be 1:（3~4）, by the silicon source and the carbon source successively
It is 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 extremely
Normal pressure.
Step 4, under the conditions of argon gas atmosphere, the high temperature carbonization furnace is warming up to 1400 with the speed of 10 ~ 20 DEG C/min
~ 1500 DEG C, 2 ~ 3h is incubated, naturally cools to room temperature, charcoal material surface SiC Nanometer Whiskers are obtained.
Charcoal material surface SiC Nanometer Whiskers manufactured in the present embodiment：A diameter of 80 ~ 120nm；Length is 50 ~ 100um.
Embodiment 4
A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof.The present embodiment is comprised the concrete steps that：
Step one, by silica flour: the mol ratio of silicon dioxide powder be 1:（3~4）, silica flour and silicon dioxide powder are well mixed, obtain
Silicon source.
Step 2, pitch based carbon fiber felt is placed in high temperature graphitization stove, being passed through argon gas carries out high temperature carbonization treatment, it is high
The temperature of warm charing process is 1600 ~ 2200 DEG C, and the time of high temperature carbonization treatment is 0.5 ~ 1h, obtains carbon source.
Step 3, by the silicon source: the mol ratio of the carbon source be 1:（2~3）, by the silicon source and the carbon source successively
It is 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 extremely
Normal pressure.
Step 4, under the conditions of argon gas atmosphere, the high temperature carbonization furnace is warming up to 1300 with the speed of 10 ~ 20 DEG C/min
~ 1400 DEG C, 1 ~ 2h is incubated, naturally cools to room temperature, charcoal material surface SiC Nanometer Whiskers are obtained.
Charcoal material surface SiC Nanometer Whiskers manufactured in the present embodiment：A diameter of 60 ~ 110nm；Length is 70 ~ 130um.
This specific embodiment has following good effect compared with prior art：
(1) this specific embodiment uses solid phase inorganic silicon source and carbon source, is being participated in and in 1200 ~ 1500 DEG C of when systems without catalyst
Charcoal material surface silicon carbide whisker, process is simple, to equipment without being released without toxic and harmful in particular/special requirement, and preparation process
Put.
(2) SiC Nanometer Whiskers of big L/D ratio are obtained in charcoal material surface for this specific embodiment.Fig. 1 is embodiment
A kind of optical photograph of the 2 charcoal material surface SiC Nanometer Whiskers for preparing；Fig. 2 receives for charcoal material surface carborundum shown in Fig. 1
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 institutes
Show the high power SEM photograph of charcoal material surface SiC Nanometer Whiskers.As seen from Figure 1, Carbon fibe felt is changed into 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
It is β-SiC, the diffraction maximum near 36 °, 60 °, 72 ° is corresponding in turn to β-SiC's（111）、（220）、（311）Crystal face, wherein
26 ° or so of diffraction maximum correspondence 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 must wrap up, silicon carbide whisker length is 100-150 μm；From fig. 4, it can be seen that
SiC Nanometer Whiskers than it is more uniform, smooth, without obvious fault of construction, a diameter of 80-120nm of silicon carbide whisker.Therefore, this tool
Body implementation method prepare charcoal material surface silicon carbide whisker purity is high, better crystallinity degree and draw ratio are big, silicon carbide whisker diameter
It is 30 ~ 120nm, length is 30 ~ 150um.
Charcoal material surface SiC Nanometer Whiskers prepared by this specific embodiment are at ambient temperature through laser excitation table
Reveal obvious blue-shifted phenomenon, emission wavelength is 420 ~ 460nm, with excellent photoluminescence performance；Product conduct as shown in Figure 1
Capacity is 550 ~ 700mAh/g during lithium ion battery negative material, shows excellent electrochemical performance.
Therefore, the characteristics of this specific embodiment has process is simple, reaction condition gentle and environment-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 comprise the following steps：
Step one, by silica flour: the mol ratio of silicon dioxide powder be 1:（0.25~4）, silica flour and silicon dioxide powder are well mixed,
Obtain silicon source；
Step 2, pitch based carbon fiber or pitch based carbon fiber felt are placed in high temperature graphitization stove, being passed through argon gas carries out high temperature
Charing process, the temperature of high temperature carbonization treatment is 1000 ~ 2800 DEG C, and the time of high temperature carbonization treatment is 0.5 ~ 1h, obtains carbon source；
Step 3, by the silicon source: the mol ratio of the carbon source be 1:（0.25~4）, the silicon source and the carbon source are put successively
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, under the conditions of argon gas atmosphere, the high temperature carbonization furnace is warming up to 1200 with the speed of 10 ~ 20 DEG C/min ~
1500 DEG C, 0.5 ~ 3h is incubated, naturally cools to room temperature, charcoal material surface SiC Nanometer Whiskers are obtained.
2. the preparation method of charcoal material surface SiC Nanometer Whiskers according to claim 1, it is characterised in that the silica flour
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 the Carbon Materials table prepared by the preparation method of charcoal material surface SiC Nanometer Whiskers any one of claim 1 ~ 3
Face SiC Nanometer Whiskers.
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Cited By (9)
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| CN107128926A (en) * | 2017-06-28 | 2017-09-05 | 湖南大学 | A kind of preparation method of self-supporting Carbide-derived carbons nano wire |
| CN108502886A (en) * | 2018-06-15 | 2018-09-07 | 天津工业大学 | A kind of preparation method of nano-sheet silicon carbide |
| CN108560058A (en) * | 2018-05-18 | 2018-09-21 | 湖南东映碳材料科技有限公司 | A kind of preparation method of zirconium carbide whisker |
| CN111392730A (en) * | 2020-04-22 | 2020-07-10 | 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 |
| CN112608156A (en) * | 2020-12-29 | 2021-04-06 | 黑龙江冠瓷科技有限公司 | Preparation method of micro-nano mixed SiC chopped fibers |
| CN113185327A (en) * | 2021-04-28 | 2021-07-30 | 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 |
| CN114032607A (en) * | 2021-11-02 | 2022-02-11 | 西北工业大学 | Method for preparing zirconium carbide whisker by adopting zirconium carbide seed crystal |
| CN114477185A (en) * | 2020-10-28 | 2022-05-13 | 中国科学院理化技术研究所 | beta-SiC with lamellar structure and preparation method thereof |
| 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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| CN114477185A (en) * | 2020-10-28 | 2022-05-13 | 中国科学院理化技术研究所 | beta-SiC with lamellar structure and preparation method 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 |
| CN112608156A (en) * | 2020-12-29 | 2021-04-06 | 黑龙江冠瓷科技有限公司 | Preparation method of micro-nano mixed SiC chopped fibers |
| CN113185327A (en) * | 2021-04-28 | 2021-07-30 | 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 |
| CN114032607A (en) * | 2021-11-02 | 2022-02-11 | 西北工业大学 | Method for preparing zirconium carbide whisker by adopting zirconium carbide seed crystal |
| 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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