CN109879285A - A kind of silicon carbide nano material and preparation method thereof - Google Patents
A kind of silicon carbide nano material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of silicon carbide nano material and preparation method thereof, silicon carbide nano material is nanobelt shape structure.The preparation method of silicon carbide nano material includes the following steps: using silicon monoxide as silicon source, the mixed dispersion liquid of silicon monoxide and carbon nanotube, silicon source and carbon source are prepared using carbon nanotube as carbon source according to the molar ratio (0.5-3) of element silicon and carbon: 1, which feeds intake, mixes；Dispersion liquid is dried, presoma is obtained；By presoma vacuum degree be 0.03-0.1MPa, temperature be 1000-1400 DEG C under conditions of calcine, obtain crude product；Crude product is carried out handling to obtain silicon carbide/carbon nanotube complex except silicon; silicon carbide/carbon nanotube complex is roasted under air or oxygen atmosphere; obtain nanometer silicon carbide band; the carbofrax material prepared according to the method for the present invention by carbon source of carbon nanotube is nanometer silicon carbide band; and raw material is easy to get, simple process, equipment requirement is low; it is at low cost, it is advantageously implemented the large-scale production of nanometer silicon carbide band.
Description
Technical field
The present invention relates to field of nanometer material technology, and in particular to a kind of silicon carbide nano material and preparation method thereof.
Background technique
Silicon carbide (SiC) has some excellent performances as one of most important semiconductor material: such as tunable broadband
Gap, high intensity, high heat conductance, outstanding thermal-shock resistance, low thermal coefficient of expansion and excellent chemical inertness, in high temperature and respectively
It can keep stable under kind acid-base condition.These special performances make it use electronics in high-power electronic device, adverse circumstances
Device, blue light diode, sensor, catalyst and heterogeneous catalysis agent carrier etc. become ideal candidate materials.Because of nanometer
The nanoscale effect of silicon carbide makes it be expected to obtain application breakthrough in terms of photocatalysis hydrogen production, supercapacitor.One-dimensional carbonization
Silicon nano material is expected to be applied to as enhancing phase material multiple because of its anisotropic high-intensitive, high rigidity and high elastic modulus
In condensation material.In addition, the distinctive electronic structure of silicon carbide monodimension nanometer material, electron-transport feature make it have unique light, electricity
Performance can break through the object in conventional microelectronic using silicon carbide monodimension nanometer material as the basic construction unit of nano electron device
The limit is managed, there is huge potential application foreground in terms of constructing electronics nanometer device of new generation.Nanobelt is even more one kind special one
Dimension nanometer construction, there is also anisotropy in the dimension of two nanoscale.The namely width and thickness of one-dimentional structure
Direction is all nanoscale, but its width is bigger than thickness.Its electronic structure of the nano material of this structure is different from general
Isotropism nano wire has differences in wide, thick both direction electron transport mode, thus is expected to become a kind of unique quantum
Nano electric material, such as carbon nanobelts just show the entirely different electronic structure of carbon nano-fiber and electron transport mode
(Ezawa M.Peculiar width dependence of the electronic properties of carbon
nanoribbons[J].Physical Review B,2006,73(4):045432.).In addition, nanobelt is in enhanced film material
Because its anisotropy its performance is also superior to common nano wire in material, and obtain anisotropic mechanical property.It is published at present
The method of preparation nanostructure silicon carbide mainly has: sol-gal process, carbothermic method, chemical vapour deposition, chemical gaseous phase
The methods of deposition and laser cutting.It such as opens wave and is prepared for SiC nano-powder with sol-gal process, and miscellaneous have 1-dimention nano knot
Structure silicon carbide (Zhang Bo builds several influence factors [J] charcoal element technology for protecting sol-gel processing preparation nano carborundum powder,
2000(4):50-53.)；Zhang Haojie disclose a kind of carbothermic method prepare nanometer silicon carbide method (Zhang Haojie,
CN201711321349.5 nanometer silicon carbide and preparation method thereof), carbothermic method (Hao Yajuan, Jin Guoqiang, Guo Xiangyun carbon heat
Reduction prepares silicon carbide nanometer line [J] Chinese Journal of Inorganic Chemistry of different-shape, 2006,10:017.), gas-phase chemical reaction (Korea Spro
Big strong, Yu great Peng studies [J] Journal of Inorganic Materials using the SiC Nanometer Whiskers of carbon nanotube preparation, 1997,12 (6):
774-778.), (Luo Fang, Lu Xiaoxiao, Wang Weibin wait a kind of SiC nano fiber of .CN201710463059 to laser cutting method
Preparation method), (Li Binbin, Yuan little Sen, Mao Bangxiao wait a kind of nanometer silicon carbide of .CN201810086069 to chemical vapour deposition technique
Line aeroge and preparation method thereof), microwave process for synthesizing etc..From current published nano silicon carbide silicon preparation method it is found that these
Method synthesis technology is complicated, raw material costly, and to the more demanding of synthesis device.In addition, these methods mainly synthesize
Silicon carbide nanometer line, nano whisker etc., do not find the synthetic method introduction in relation to nanometer silicon carbide carrying material.
Summary of the invention
Technical problem solved by the present invention is providing a kind of silicon carbide nano material, the nano material has unique
One-dimensional banded structure has huge potential application foreground.Silicon carbide can be prepared in the preparation method provided according to the present invention
Nanobelt, and raw material needed for preparing nanometer silicon carbide band is easy to get, simple process, equipment requirement are low, at low cost, is advantageously implemented
The large-scale production of nanometer silicon carbide band.
To solve the above-mentioned problems, the main technical schemes that the present invention uses include:
The present invention provides a kind of silicon carbide nano material, the silicon carbide nano material is nanobelt shape structure.
On the basis of above scheme, silicon carbide nano material of the invention can also be improved as follows:
Further, the nanobelt is provided with nanoscale on thickness and width direction, and the nanometer bandwidth is 1-
40nm。
The silicon carbide nano material has unique one-dimensional banded structure, exists in the dimension of two nanoscale
Anisotropy.This unique structure makes silicon carbide nano material electronic structure be different from general isotropism nano wire,
It is had differences in wide, thick both direction electron transport mode, thus is expected to become a kind of unique quantum nanoparticles electronic material.
The present invention also provides a kind of silicon carbide nano material preparation methods, are prepared into carbon nanotube (CNTs) for carbon source
To nanometer silicon carbide band, raw material needed for preparing nanometer silicon carbide band is easy to get, simple process, equipment requirement are low, at low cost, favorably
In the large-scale production for realizing nanometer silicon carbide band.
Silicon carbide nano material preparation method provided by the invention includes the following steps:
1) with silicon monoxide (SiO) for silicon source, silicon monoxide and carbon nanotube is prepared by carbon source of carbon nanotube
Mixed dispersion liquid, the silicon source and carbon source according to element silicon and carbon molar ratio (0.5-3): 1, which feeds intake, mixes；
2) dispersion liquid is dried, obtains presoma；
It 3) is 0.03-0.1MPa in vacuum degree by the presoma, temperature is calcined under conditions of being 1000-1400 DEG C, obtained
To crude product；
4) crude product handle except silicon, silicon carbide/carbon nanotube complex is obtained, in air or oxygen atmosphere
Lower roasting, obtains nanometer silicon carbide band.
Specifically, the carbon nanotube, silicon monoxide powder are commercial product.
By CNTs and SiO through high-temperature calcination, except silicon processing and the charcoal processing of the row of roasting, SiC nanobelt has been synthesized.Due to reaction
It persistently vacuumizes in the process and temperature control, leads to calcining and except silicon treated product is that SiC gives birth in situ on CNTs
Long obtained SiC/CNTs composite material, pattern is consistent with CNTs, because of the rupture of tubular structure after row's charcoal processing, obtains SiC
Nanobelt.
The chemical reaction being related in the preparation process are as follows:
2C (s)+SiO (g)=SiC (s)+CO (g) formula (1)
2SiO (g)=Si (s)+SiO2(s) formula (2)
Si (s)+C (s)=SiC (s) formula (3)
SiO2(s)+2C (s)=SiC (s)+CO2(g) formula (4)
C(s)+CO2(g)=2CO (g) formula (5)
SiO (g)+3CO (g)=SiC (s)+2CO2(g) formula (6)
4CO(g)+SiO2(s)=SiC (s)+3CO2(g) formula (7)
3C (s)+2SiO (g)=2SiC (s)+CO2(g) formula (8)
Wherein reaction (1) and (6) is to generate the key reaction of SiC, reacts SiO (s) distillation under (1) high temperature and forms SiO
(g), carbothermic reduction reaction occurs with the surface CNTs；Since disproportionated reaction (reaction (2)) can occur for SiO itself under high temperature, generate
Si (s) and SiO2(s) surface CNTs and surrounding are deposited in, due to solid phase reaction mainly by diffusion carry out, so reaction (3) and
(4) only few part carries out；Theoretically reaction (8) is likely to occur, but can not become main reaction from activation energy consideration；Though
So reaction (6) either all take advantage in thermodynamics or dynamics, but in order to make main reaction (1) towards positive reaction direction into
Row, needs to control the temperature and pressure of reaction.It is lasting during the experiment to vacuumize, while for unnecessary original
The abundant progress of material loss and reaction (1), can the tapped bulk density of seal degree and raw material to reactor be adjusted and make
The mixed gas that reaction generates can overflow in time, improve the yield of SiC nanobelt.Temperature is higher, various side reactions such as (2),
(5) (7) and (8) reaction aggravation, with SiC in-situ preparation 1) response competition, it will be unable to obtain with CNTs shape after calcination processing
The SiC/CNTs composite material of looks is also unable to get SiC nanobelt after row's carbon processing.
There are various side reactions for the reaction (reaction (1)) of in-situ preparation SiC on CNTs, and due in calcination process not
Disconnected to vacuumize, the actual consumption amount of SiO is much higher than above-mentioned theory reaction ratio.It is found through experiments that if working as mole of SiO and C
Than being lower than 0.5, the SiC content of the SiC/CNTs composite material obtained after calcining is very low；If molar ratio be greater than 3, high-temperature calcination,
Except silicon processing and the row's of roasting charcoal treated final product are Sic nanotube, SiC nanobelt cannot be obtained.
Beneficial effect using the above scheme is:
(1) one-dimensional nanometer silicon carbide band has been prepared by carbon source of carbon nanotube.
(2) raw material needed for preparing nanometer silicon carbide band is easy to get, and preparation process is simple, and equipment requirement is low, is expected to realize carbon
The large-scale production of SiClx nanobelt.
Based on the above technical solution, the preparation method of silicon carbide nano material of the invention can also be done changes as follows
Into:
Further, the dispersion solvent in the dispersion liquid is deionized water, the deionized water and the silicon monoxide and
The mass ratio of carbon nanotube mixture is (9-1): 1.
As a result, using deionized water as dispersion solvent, raw material is easy to get, price is low.
Further, the silicon source and carbon source according to element silicon and carbon molar ratio (1-2): 1, which feeds intake, mixes.
High yield, regular appearance, the SiC nanobelt of size uniformity can be obtained as a result,.
Further, the calcination temperature of step 3) is 1050-1350 DEG C, and heating rate is 3-8 DEG C/min, calcination time 1-
24h。
Preferably, the calcination temperature is 1150-1200 DEG C, and heating rate is 4-6 DEG C, calcination time 6-18h.
Under this condition, regular appearance, high yield and pattern and the consistent SiC/CNTs of CNTs can be obtained, after row's carbon processing
The SiC nanobelt of size uniformity can be obtained.Temperature is too low, and SiO hardly gasifies, and reaction cannot carry out substantially.Temperature is excessively high, and one
Aspect, SiO gasification rate is fast, and gaseous state SiO can not react in time, and most reaction gas can escape, and reduces SiC nanobelt
Yield；On the other hand, temperature is high, and reaction is fast, is unfavorable for the realization of in-situ preparation SiC reaction, can not inherit CNTs pattern,
It is not readily available SiC nanobelt.Primary product further includes the same SiC nanowire of other many document reports at this time,
Reaction process is mainly previous reaction (6).As for low heating rate is taken, primarily to control SiO gasification rate.Heating speed
Rate is slower, and SiO gasification rate is slower, and generated SiO gas can chemically react in situ with the carbon on the CNTs of surrounding,
It is unlikely to make SiO gas in reaction system to reach saturation state fastly very much and various side reactions are aggravated.
Further, step 4) includes that hydrofluoric acid solution washing by soaking or aqueous slkali soaking are handled except silicon is handled.
Specifically, washing by soaking can remove unreacted silicon and silicon in hydrofluoric acid solution or aqueous slkali by crude product
Oxide, obtain silicon carbide/carbon nanotube complex.
Further, the mass fraction of the hydrofluoric acid solution is 10%-40%, soaking time 2h-24h.
Under this condition, the removal effect of impurity silicon and its oxide is good.
Further, aqueous slkali soaking processing includes potassium hydroxide or sodium hydroxide hot solution washing by soaking in step 4).
Under this condition, the removal effect of impurity silicon and its oxide is good.
Further, the maturing temperature in step 4) is 500-700 DEG C, calcining time 1h-10h.
Preferably, the maturing temperature in step 4) is 550-650 DEG C, calcining time 4h-6h.
The complete carbon nanotube of unreacted can be removed sufficiently as a result, so that silicon carbide/carbon nano tubular structure is broken
It is bad, obtain nanometer silicon carbide band.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Fig. 1 is nanometer silicon carbide band preparation flow figure；
Fig. 2 is the X ray diffracting spectrum of nanometer silicon carbide band prepared by embodiment of the present invention method 1；
Fig. 3 is nanometer silicon carbide band transmission electron microscope photo prepared by embodiment of the present invention method 1.
Specific embodiment
With reference to the accompanying drawings and examples, specific embodiments of the present invention will be described in further detail.Implement below
Example is not intended to limit the scope of the invention for illustrating the present invention.
Embodiment 1 (refering to fig. 1)
It (1) is that 2:1 mix with the molar ratio of carbon according to element silicon with carbon nanotube powder by silicon monoxide
To mixture, it is that 4:1 addition deionized water is uniformly mixed according to the mass ratio of deionized water and mixture, 2h is sanded in sand mill
After obtain mixed dispersion liquid, carried out in 100 DEG C of baking ovens drying forming presoma；
(2) presoma is placed in alumina crucible, under vacuum conditions, is calcined in tube furnace, calcination temperature
It is 1050 DEG C, calcination time 3h obtains crude product；
(3) crude product is impregnated in the HF solution that mass fraction is 15% to 4h and removes silicon, it will be except the crude product after silicon be 600
DEG C Muffle kiln roasting 6h, obtain nanometer silicon carbide band.
Embodiment 1 is characterized, Fig. 2 is the XRD spectrum of nanometer silicon carbide band, and each strong peak in figure shows resulting
Nanometer silicon carbide band is the good silicon B-carbide of crystallinity.Fig. 3 show the TEM photo of nanometer silicon carbide band, can from photo
To find out, the nanometer silicon carbide bandwidth prepared is 1.7-38nm.
Embodiment 2:
1) silicon monoxide and carbon nanotube powder be mixed to get according to the molar ratio 1:1 of element silicon and carbon mixed
Object is closed, is that 6:1 addition deionized water is uniformly mixed according to the mass ratio of deionized water and mixture, in sand mill after sand milling 2h
To mixed dispersion liquid, drying is carried out in 100 DEG C of baking ovens and forms presoma；
(2) presoma is placed in alumina crucible, under vacuum conditions, is calcined in tube furnace, calcination temperature
It is 1350 DEG C, calcination time 10h obtains crude product；
(3) crude product is impregnated for 24 hours except silicon in the HF solution that mass fraction is 40%, will be existed except the crude product after silicon
500 DEG C of Muffle kiln roasting 1h, obtains nanometer silicon carbide band.
Embodiment 3:
It 1) is that 3:1 is mixed to get according to the molar ratio of element silicon and carbon by silicon monoxide and carbon nanotube powder
Mixture is that 9:1 addition deionized water is uniformly mixed according to the mass ratio of deionized water and mixture, after 2h is sanded in sand mill
Mixed dispersion liquid is obtained, drying is carried out in 100 DEG C of baking ovens and forms presoma；
(2) presoma is placed in alumina crucible, under vacuum conditions, is calcined in tube furnace, calcination temperature
It is 1200 DEG C, calcination time is for 24 hours, to obtain crude product；
(3) crude product is impregnated in the HF solution that mass fraction is 10% to 14h and removes silicon, will existed except the crude product after silicon
700 DEG C of Muffle kiln roasting 6h, obtains nanometer silicon carbide band.
Embodiment 4:
It 1) is that 0.5:1 mix with the molar ratio of carbon according to element silicon with carbon nanotube powder by silicon monoxide
To mixture, it is that 5:1 addition deionized water is uniformly mixed according to the mass ratio of deionized water and mixture, 2h is sanded in sand mill
After obtain mixed dispersion liquid, carried out in 100 DEG C of baking ovens drying forming presoma；
(2) presoma is placed in alumina crucible, under vacuum conditions, is calcined in tube furnace, calcination temperature
It is 1400 DEG C, calcination time 1h obtains crude product；
(3) crude product is impregnated in the HF solution that mass fraction is 30% to 2h and removes silicon, it will be except the crude product after silicon be 500
DEG C Muffle kiln roasting 10h, obtain nanometer silicon carbide band.
Embodiment 5:
It 1) is that 2.5:1 mix with the molar ratio of carbon according to element silicon with carbon nanotube powder by silicon monoxide
To mixture, it is that 1:1 addition deionized water is uniformly mixed according to the mass ratio of deionized water and mixture, 2h is sanded in sand mill
After obtain mixed dispersion liquid, carried out in 100 DEG C of baking ovens drying forming presoma；
(2) presoma is placed in alumina crucible, under vacuum conditions, is calcined in tube furnace, calcination temperature
It is 1000 DEG C, calcination time 18h obtains crude product；
(3) crude product is impregnated in the HF solution that mass fraction is 30% to 12h and removes silicon, will existed except the crude product after silicon
550 DEG C of Muffle kiln roasting 4h, obtains nanometer silicon carbide band.
Comparative example 1:
It is same as Example 1, the difference is that, by silicon monoxide and carbon nanotube powder according to silicon member in step (1)
The molar ratio of element and carbon is that 4:1 carries out being mixed to get mixture.It by calcining, removes silicon and removes carbon, finally obtained carbonization
Nano-tube.
Comparative example 2:
It is same as Example 1, the difference is that, by silicon monoxide and carbon nanotube powder according to silicon member in step (1)
The molar ratio of element and carbon is that 0.2:1 carries out being mixed to get mixture.Random shape has been obtained by calcining, except silicon and except carbon
The nanometer silicon carbide particle of looks.
Comparative example 4-5
It is same as Example 1, the difference is that, 1550 DEG C and 1700 DEG C of calcination temperature in step (2) have obtained straight
Diameter is the silicon carbide nanometer line of 120-200nm.
Although the embodiment of the present invention is described in detail above, it will be understood by those skilled in the art that:
A variety of change, modification, replacement and modification can be carried out to these embodiments in the case where not departing from the principle of the present invention and objective,
The scope of the present invention is defined by the claims and their equivalents.
Claims (10)
1. a kind of silicon carbide nano material, which is characterized in that the silicon carbide nano material is nanobelt shape structure.
2. silicon carbide nano material according to claim 1, which is characterized in that the nanobelt is on thickness and width direction
It is provided with nanoscale, the nanobelt mean breadth is 1-40nm.
3. a kind of preparation method of silicon carbide nano material, which comprises the steps of:
1) using silicon monoxide as silicon source, dispersed using the mixing that silicon monoxide and carbon nanotube is prepared as carbon source in carbon nanotube
Liquid, the silicon source and carbon source according to element silicon and carbon molar ratio (0.5-3): 1, which feeds intake, mixes；
2) dispersion liquid is dried, obtains presoma；
It 3) is 0.03-0.1MPa in vacuum degree by the presoma, temperature is calcined under conditions of being 1000-1400 DEG C, is obtained thick
Product；
4) crude product is carried out handling to obtain silicon carbide/carbon nanotube complex except silicon, by the silicon carbide/carbon nanotube
Compound roasts under air or oxygen atmosphere, obtains nanometer silicon carbide band.
4. silicon carbide nano material preparation method according to claim 3, which is characterized in that the dispersion in the dispersion liquid
Solvent is deionized water, and the deionized water and the silicon monoxide and the mass ratio of carbon nanotube mixture are (9-1): 1.
5. silicon carbide nano material preparation method according to claim 3, which is characterized in that the silicon source and carbon source according to
The molar ratio (1-2) of element silicon and carbon: 1, which feeds intake, mixes.
6. silicon carbide nano material preparation method according to claim 3, which is characterized in that the calcination temperature of step 3) is
1050-1350 DEG C, heating rate is 3-8 DEG C/min, calcination time 1-24h.
7. silicon carbide nano material preparation method according to claim 3, which is characterized in that step 4) is wrapped except silicon is handled
Include hydrofluoric acid solution washing by soaking or aqueous slkali soaking processing.
8. silicon carbide nano material preparation method according to claim 7, which is characterized in that the hydrofluoric acid solution of step 4)
Mass fraction be 10%-40%, soaking time 2h-24h.
9. silicon carbide nano material preparation method according to claim 7, which is characterized in that the aqueous slkali soaking of step 4)
Processing includes sodium hydroxide or sodium hydroxide hot solution washing by soaking.
10. according to any silicon carbide nano material preparation method of claim 3-9, which is characterized in that in step 4)
Maturing temperature is 500-700 DEG C, calcining time 1h-10h.
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| CN116161962A (en) * | 2023-02-06 | 2023-05-26 | 中国科学院上海硅酸盐研究所 | Silicon carbide pressure-sensitive ceramic with anisotropic electrical property and preparation method thereof |
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| CN113968582A (en) * | 2021-11-12 | 2022-01-25 | 郑州大学 | Silicon carbide fiber aerogel and preparation method thereof |
| CN113979439A (en) * | 2021-11-30 | 2022-01-28 | 陕西科技大学 | Si5C3Micro-nano material and preparation method thereof |
| CN115403045A (en) * | 2022-07-11 | 2022-11-29 | 嘉庚创新实验室 | Carbide and method for producing same |
| CN115403045B (en) * | 2022-07-11 | 2023-09-29 | 嘉庚创新实验室 | Carbide and preparation method thereof |
| CN116161962A (en) * | 2023-02-06 | 2023-05-26 | 中国科学院上海硅酸盐研究所 | Silicon carbide pressure-sensitive ceramic with anisotropic electrical property and preparation method thereof |
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