CN106082227A - A kind of fluidized-bed chemical vapor deposition preparation method of nanometer silicon carbide granule - Google Patents
A kind of fluidized-bed chemical vapor deposition preparation method of nanometer silicon carbide granule Download PDFInfo
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Abstract
The present invention relates to the fluidized-bed chemical vapor deposition preparation method of a kind of nanometer silicon carbide granule, including using fluidized-bed chemical vapor deposition method, the heating of precursor material hexamethyldisilane is produced steam, by the way of gas carries, enters fluidized-bed reactor；There is pyrolytic reaction in precursor steam, form nanometer silicon carbide granule in high-temperature region；Nano-particle is transported to reactor top under the effect of fluidizing gas, by negative pressure device sucking-off, collects and obtains nano-sized SiC powder；High-temperature heat treatment under an inert atmosphere, obtains the nanometer silicon carbide granule of well-crystallized.Gained nanometer silicon carbide granule is cubic-phase silicon carbide, and grain shape is spherical, narrow diameter distribution, and particle size is adjustable in 5～300 nanometers.By regulation reaction atmosphere, obtain pure carborundum, Silicon-rich or the nanometer silicon carbide granule of rich carbon.Present invention process flow process is simple, and technological operation is convenient, low cost, is advantageously implemented industrialized production.
Description
Technical field
The present invention relates to carbofrax material preparing technical field, specifically, relate to the stream of a kind of nanometer silicon carbide granule
Fluidized-bed chemical gas-phase deposition process for preparing.
Background technology
Carbofrax material is due to its wide electronic band gap, excellent mechanical behavior under high temperature, low thermal coefficient of expansion, high warm
Conductance, and resistance to irradiation, corrosion-resistant, antioxidation, as high-temperature structural components and novel sub-components and parts be widely used in Aero-Space,
The fields such as chemical industry, the energy, electronics.By the particle size of reduction silicon carbide nano material to nanoscale, due to dimensional effect, carbon
Silicon nitride material can show the numerous novel performance being different from block materials, widens its application further.There is nanometer chi
Very little silicon-carbide particle also shows the high temperature sintering performance of excellence, overcomes current carborundum to be difficult to the difficulty of sinter molding, and
Significantly reduce sintering temperature, be expected to be answered in fields such as carborundum chained technology and novel silicon carbide base nuclear fuel elements
With.
The method preparing nanometer silicon carbide granule at present mainly has: (1) passes through carbon, silicon mixture pyroreaction method；(2) change
Learn vapour deposition process；(3) sol-gal process；(4) microwave or plasma high-temperature synthetic method etc..Use carbon synthesized by these methods
SiClx nano-particle, on the one hand the control relative difficulty of product pattern and size, and prepare good sphericity, particle size distribution
Narrow, the challenge especially of the single dispersing nanometer silicon carbide granule of size adjustable；On the other hand, gained nanometer silicon carbide granule is often
Containing other element impurity, and the stoichiometric proportion of carborundum cannot be carried out programmable Effective Regulation.Additionally, part side
Method needs higher energy input, and equipment proposes the highest requirement, and the continuous metaplasia of high-volume that product cannot be realized
Produce.
Summary of the invention
In order to solve problems of the prior art, it is an object of the invention to provide a kind of size adjustable, composition is controlled
The preparation method of spherical carbide nano silicon particles, and be capable of industrialized production.
In order to realize the object of the invention, the present invention provides the fluidized-bed chemical vapor deposition system of a kind of nanometer silicon carbide granule
Preparation Method, described preparation method specifically includes following steps:
1) fluidized-bed reactor is heated to uniform temperature, is passed through a certain amount of fluidizing gas simultaneously, and adds a certain amount of
Non-reactive fluidizing granule；
2) heating of precursor material hexamethyldisilane being produced steam, steam enters fluidized-bed reaction by gas carrier band
Device；
3) there is pyrolytic reaction in precursor material steam in fluidized-bed reactor high-temperature region, forms nanometer silicon carbide granule；
4) described nanometer silicon carbide granule is transported to fluidized-bed reactor top under the effect of fluidizing gas, passes through negative pressure
Device sucking-off, collects and obtains nano-sized SiC powder；
5) gained nano-sized SiC powder is carried out under an argon atmosphere heat treatment, obtain the nanometer silicon carbide of well-crystallized
Granule.
Further, described non-reactive fluidizing granule is the granule not reacted with described presoma under described preparation temperature,
It is preferably metal or ceramic particle；More preferably zirconia particles, alumina particle, metallic cobalt granule or metallic iron
Grain.
Further, the mode of heating of described precursor is water-bath or electrical heating, and heating-up temperature is 30～110 DEG C.
Further, described fluidizing gas is hydrogen or argon or the mixed gas of the two.
Further, described carrier band gas is hydrogen or argon.
Further, described carrier band gas is 0.1%～50% with the volume ratio of fluidizing gas.
Further, step 3) described fluidized-bed reactor high-temperature region temperature is 750～1450 DEG C.
Further, rate-determining steps 3) hydrogen is 30%～70% with the ratio of argon in described reaction system, described stream
Fluidized bed reactor high-temperature region temperature is 750～1300 DEG C, and reaction obtains pure phase silicon carbide nano-particle.
Further, rate-determining steps 3) ratio of hydrogen and argon is 70% to infinity in described reaction system, described
Fluidized-bed reactor high-temperature region temperature is 750～1200 DEG C, obtains the nanometer silicon carbide granule of Silicon-rich, and the mass fraction of silicon is 0
～8%.
Further, rate-determining steps 3) hydrogen is 0 to 30% with the ratio of argon in described reaction system, high-temperature region is reacted
Temperature is 750～1450 DEG C, obtains the nanometer silicon carbide granule of rich carbon, and the mass fraction of carbon is 0～10%.
Further, step 5) described heat treatment temperature is 1300～1500 DEG C, heat treatment time is 1～4 hour.
The present invention also provides for nanometer silicon carbide granule prepared by said method.Described nanometer silicon carbide granule is Emission in Cubic carbon
SiClx, grain shape is spherical, and particle size is adjustable in 5～300 nanometers.
Present invention also offers a kind of fluidized reaction equipment for preparing above-mentioned nanometer silicon carbide granule, it is hollow circle
Column jecket body, described its bottom is precursor steam inlet, and body top is provided with product discharge mouth, and connects to have and can form negative pressure
Device.This equipment is particularly suited for preparing single dispersing nanometer silicon carbide granule.
The beneficial effects of the present invention is:
Nanometer silicon carbide granule prepared by the present invention is cubic-phase silicon carbide, and grain shape is monodisperse spherical, has
The narrowest particle diameter distribution, particle size is adjustable in 5～300 nanometers.By controlling reaction system gas mixing ratio, obtain pure carbonization
Silicon, Silicon-rich or the nanometer silicon carbide granule of rich carbon.Pure nanometer silicon carbide granule can enrich answering of existing silicon carbide nano material
With scope and can as raw material reduce compact silicon carbide ceramic material sintering temperature.Carbon containing or siliceous nanometer silicon carbide granule
New coupling performance can be obtained as composite, and there is as template preparation the carbon silicon system material of meso-hole structure.
The present invention passes through reactor design structure, and nanometer silicon carbide granular product can utilize negative pressure from the product discharge mouth on fluidisation pipe top
Sucking-off, it is achieved prepared by serialization.Present invention process flow process is simple, and technological operation is convenient, low cost, can accomplish scale production.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the embodiment of the present invention 1 gained nanometer silicon carbide granule；
Fig. 2 is the XRD spectra of the embodiment of the present invention 1 gained nanometer silicon carbide granule；
Fig. 3 is the transmission electron microscope photo of the embodiment of the present invention 2 gained nanometer silicon carbide granule；
Fig. 4 is the stereoscan photograph of the embodiment of the present invention 5 gained nanometer silicon carbide granule；
Fig. 5 is the XRD spectra of the embodiment of the present invention 5 gained nanometer silicon carbide granule；
Fig. 6 is the XRD spectra of the embodiment of the present invention 7 gained nanometer silicon carbide granule.
Detailed description of the invention
Following example are used for illustrating the present invention, but are not limited to the scope of the present invention.
Embodiment 1
The mode that precursor hexamethyldisilane uses heating in water bath is heated to 80 DEG C, and using argon is carrier band gas,
Carrier band gas flow is 0.3L/min, and the mixed gas using hydrogen and argon is fluidizing gas, H2Flow be 1.2L/min,
The flow of Ar is 1.5L/min.Fluidized-bed reactor is heated to 900 DEG C add zirconium oxide fluidized particles and be passed through carrier band gas,
Powder body is collected by the powder body collection system of reactor top.By gained powder body 1300 DEG C of argon gas atmosphere heat treatments 1 hour.
The transmission electron microscope photo of products therefrom is as shown in Figure 1, it is seen that products therefrom is monodisperse spherical granule, grain diameter
Being distributed the narrowest, the average particle size particle size of product is 120 nanometers, and the XRD spectra of product is as in figure 2 it is shown, pass through comparison standard card
Can be seen that the carborundum that product is Emission in Cubic, there is no other dephasign.
Embodiment 2
The mode that precursor hexamethyldisilane uses heating in water bath is heated to 80 DEG C, and using argon is carrier band gas,
Carrier band gas flow is 0.1L/min, and the mixed gas using hydrogen and argon is fluidizing gas, H2Flow be 1.5L/min,
The flow of Ar is 0.9L/min.Fluidized-bed reactor is heated to 900 DEG C add zirconium oxide fluidized particles and be passed through carrier band gas,
Powder body is collected by the powder body collection system of reactor top.By gained powder body 1300 DEG C of argon gas atmosphere heat treatments 1 hour.
The transmission electron microscope photo of products therefrom is as shown in Figure 3, it is seen that products therefrom is monodisperse spherical granule, putting down of product
All particle sizes are 15 nanometers, product is carried out XRD test, is the carborundum of Emission in Cubic by comparison standard card product, and
Without other dephasign.
Embodiment 3
The mode that precursor hexamethyldisilane uses electric heating heating is heated to 100 DEG C, and using hydrogen is carrier band gas,
Carrier band gas flow is 2.0L/min, and the mixed gas using hydrogen and argon is fluidizing gas, H2Flow be 1.0L/min,
The flow of Ar is 1.5L/min.Fluidized-bed reactor is heated to 800 DEG C add metallic cobalt fluidized particles and be passed through carrier band gas,
Powder body is collected by the powder body collection system of reactor top.By gained powder body 1400 DEG C of argon gas atmosphere heat treatments 2 hours.
Products therefrom is monodisperse spherical granule, and particle size distribution is the narrowest, and the average particle size particle size of product is 280 to receive
Rice, carries out XRD test to product, is the carborundum of Emission in Cubic by comparison standard card product, there is no other dephasign.
Embodiment 4
The mode that precursor hexamethyldisilane uses electric heating heating is heated to 75 DEG C, and using hydrogen is carrier band gas,
Carrier band gas flow is 1.0L/min, and the mixed gas using hydrogen and argon is fluidizing gas, H2Flow be 1.0L/min,
The flow of Ar is 4.0L/min.Fluidized-bed reactor is heated to 1100 DEG C add aluminium oxide fluidized particles and be passed through carrier band gas
Body, collects powder body by the powder body collection system of reactor top.Gained powder body is little at 1450 DEG C of argon gas atmosphere heat treatments 3
Time.
Products therefrom is monodisperse spherical granule, and particle size distribution is the narrowest, and the average particle size particle size of product is 50 nanometers,
Product is carried out XRD test, is the carborundum of Emission in Cubic by comparison standard card product, there is no other dephasign.
Embodiment 5
The mode that precursor hexamethyldisilane uses heating in water bath is heated to 80 DEG C, and using argon is carrier band gas,
Carrier band gas flow is 0.3L/min, and employing argon is fluidizing gas, and the flow of Ar is 3.7L/min.Fluidized-bed reactor is added
Heat adds zirconium oxide fluidized particles to 1000 DEG C and is passed through carrier band gas, collects powder by the powder body collection system of reactor top
Body.By gained powder body 1300 DEG C of argon gas atmosphere heat treatments 1 hour.
The stereoscan photograph of products therefrom is as shown in Figure 4, it is seen that products therefrom is monodisperse spherical granule, grain diameter
Being distributed the narrowest, the average particle size particle size of product is 50 nanometers, and the XRD spectra of product is as it is shown in figure 5, can by comparison standard card
To find out the product carborundum as Emission in Cubic and a small amount of carbon, the mass fraction of carbon is 4.0%.
Embodiment 6
The mode that precursor hexamethyldisilane uses heating in water bath is heated to 90 DEG C, and using argon is carrier band gas,
Carrier band gas flow is 0.6L/min, and the mixed gas using hydrogen and argon is fluidizing gas, H2Flow be 1.0L/min,
The flow of Ar is 3.4L/min.Fluidized-bed reactor is heated to 1250 DEG C add aluminium oxide fluidized particles and be passed through carrier band gas
Body, collects powder body by the powder body collection system of reactor top.Gained powder body is little at 1400 DEG C of argon gas atmosphere heat treatments 4
Time.
Products therefrom is monodisperse spherical granule, and particle size distribution is the narrowest, and the average particle size particle size of product is 30 nanometers,
Product is carried out XRD test, can be seen that, by comparison standard card, the carborundum and a small amount of carbon that product is Emission in Cubic, carbon
Mass fraction is 5.6%.
Embodiment 7
The mode that precursor hexamethyldisilane uses heating in water bath is heated to 80 DEG C, and using hydrogen is carrier band gas,
Carrier band gas flow is 2.0L/min, and the mixed gas using hydrogen and argon is fluidizing gas, H2Flow be 4.0L/min,
The flow of Ar is 0.6L/min.Fluidized-bed reactor is heated to 850 DEG C add metallic iron fluidized particles and be passed through carrier band gas,
Powder body is collected by the powder body collection system of reactor top.By gained powder body 1350 DEG C of argon gas atmosphere heat treatments 1 hour.
Products therefrom is monodisperse spherical granule, and particle size distribution is the narrowest, and the average particle size particle size of product is 150 to receive
Rice, the XRD spectra of product as shown in Figure 6, can be seen that carborundum that product is Emission in Cubic and a small amount of by comparison standard card
Silicon, the mass fraction of silicon is 3.5%.
Embodiment 8
The mode that precursor hexamethyldisilane uses heating in water bath is heated to 70 DEG C, and using argon is carrier band gas,
Carrier band gas flow is 0.4L/min, and employing hydrogen is fluidizing gas, H2Flow be 6.0L/min,.By fluidized-bed reactor
It is heated to 1100 DEG C add zirconium oxide fluidized particles and be passed through carrier band gas, is collected by the powder body collection system of reactor top
Powder body.By gained powder body 1400 DEG C of argon gas atmosphere heat treatments 2 hours.
Products therefrom is monodisperse spherical granule, and particle size distribution is the narrowest, and the average particle size particle size of product is 40 nanometers,
Product is carried out XRD test, can be seen that, by comparison standard card, the carborundum and a small amount of silicon that product is Emission in Cubic, silicon
Mass fraction is 4.8%.
Embodiment 9
The mode that precursor hexamethyldisilane uses heating in water bath is heated to 90 DEG C, and using argon is carrier band gas,
Carrier band gas flow is 5.4L/min, and the mixed gas using hydrogen and argon is fluidizing gas, H2Flow be 120.0L/
The flow of min, Ar is 50.0L/min.Fluidized-bed reactor is heated to 1150 DEG C add aluminium oxide fluidized particles and be passed through load
Band gas, collects powder body by the powder body collection system of reactor top.By gained powder body at 1400 DEG C of argon gas atmosphere heat treatments 4
Hour.
Products therefrom is monodisperse spherical granule, and particle size distribution is the narrowest, and the average particle size particle size of product is 35 nanometers,
Product is carried out XRD test, can be seen that, by comparison standard card, the carborundum that product is Emission in Cubic.
Although, the present invention is described in detail the most with a general description of the specific embodiments, but
On the basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.
Claims (10)
1. the fluidized-bed chemical vapor deposition preparation method of a nanometer silicon carbide granule, it is characterised in that described preparation method
Specifically include following steps:
1) fluidized-bed reactor is heated to uniform temperature, is passed through a certain amount of fluidizing gas simultaneously, and adds a certain amount of lazy
Property fluidized particles；
2) heating of precursor material hexamethyldisilane being produced steam, steam enters fluidized-bed reactor by gas carrier band；
3) there is pyrolytic reaction in precursor material steam in fluidized-bed reactor high-temperature region, forms nanometer silicon carbide granule；
4) described nanometer silicon carbide granule is transported to reactor top under the effect of fluidizing gas, by negative pressure device sucking-off,
Collection obtains nano-sized SiC powder；
5) gained nano-sized SiC powder is carried out under an argon atmosphere heat treatment, obtain the nanometer silicon carbide of well-crystallized
Grain.
Preparation method the most according to claim 1 and 2, it is characterised in that described non-reactive fluidizing granule is in described preparation
At a temperature of the granule that do not reacts with described presoma, preferably metal or ceramic particle；More preferably zirconia particles, oxygen
Change alumina particles, metallic cobalt granule or iron granule.
Preparation method the most according to claim 1 and 2, it is characterised in that the mode of heating of described precursor be water-bath or
Electrical heating, heating-up temperature is 30～110 DEG C.
Preparation method the most according to claim 1 and 2, it is characterised in that described fluidizing gas is hydrogen or argon or two
The mixed gas of person；Described carrier band gas is hydrogen or argon；Preferably, described carrier band gas and the volume ratio of fluidizing gas
It is 0.1%～50%.
Preparation method the most according to claim 1 and 2, it is characterised in that step 3) described fluidized-bed reactor high-temperature region
Temperature is 750～1450 DEG C.
Preparation method the most according to claim 1 and 2, it is characterised in that step 5) described heat treatment temperature be 1300～
1500 DEG C, heat treatment time is 1～4 hour.
7. according to the preparation method described in any one of claim 1-6, it is characterised in that rate-determining steps 3) in described reaction system
Hydrogen is 30%～70% with the ratio of argon, and described fluidized-bed reactor high-temperature region temperature is 750～1300 DEG C, and reaction obtains
Pure phase silicon carbide nano-particle；Or
Rate-determining steps 3) ratio of hydrogen and argon is 70% to infinity in described reaction system, described fluidized-bed reactor is high
Warm area temperature is 750～1200 DEG C, obtains the nanometer silicon carbide granule of Silicon-rich, and the mass fraction of silicon is 0～8%；Or
Rate-determining steps 3) hydrogen is 0 to 30% with the ratio of argon in described reaction system, high-temperature region reaction temperature be 750～
1450 DEG C, obtaining the nanometer silicon carbide granule of rich carbon, the mass fraction of carbon is 0～10%.
8. the nanometer silicon carbide granule that prepared by method described in any one of claim 1-7.
Nanometer silicon carbide granule the most according to claim 8, it is characterised in that described nanometer silicon carbide granule is Emission in Cubic
Carborundum, grain shape is spherical, and particle size is adjustable in 5～300 nanometers.
10. the fluid bed reaction apparatus being used for preparing nanometer silicon carbide granule, it is characterised in that it is hollow cylindrical tube
Body, described its bottom is precursor steam inlet, and body top is provided with product discharge mouth, and connection has the dress that can form negative pressure
Put.
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| CN108059166A (en) * | 2017-12-27 | 2018-05-22 | 江苏乐园新材料集团有限公司 | A kind of fluctuation-type carbonization silicon preparation method and its heating unit |
| CN108128777A (en) * | 2017-12-27 | 2018-06-08 | 江苏乐园新材料集团有限公司 | A kind of dynamic suspension is frictionally carbonized silicon preparation method and its heating unit |
| CN108423635A (en) * | 2018-03-22 | 2018-08-21 | 清华大学 | A kind of three-dimensional spherical nanometer silicon carbide assembled material and its preparation method and application |
| CN108675300A (en) * | 2018-06-15 | 2018-10-19 | 清华大学 | A kind of nuclear shell structure nano composite particles and preparation method thereof, its preparation facilities |
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| CN114220561A (en) * | 2021-11-10 | 2022-03-22 | 华能核能技术研究院有限公司 | Preparation method and equipment of surface coating of high-temperature gas cooled reactor absorption ball |
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| CN108128777A (en) * | 2017-12-27 | 2018-06-08 | 江苏乐园新材料集团有限公司 | A kind of dynamic suspension is frictionally carbonized silicon preparation method and its heating unit |
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