CN110090604A - The technique for preparing graphene coated inorganic non-metallic micro-/ nano particle - Google Patents
The technique for preparing graphene coated inorganic non-metallic micro-/ nano particle Download PDFInfo
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- CN110090604A CN110090604A CN201910333441.6A CN201910333441A CN110090604A CN 110090604 A CN110090604 A CN 110090604A CN 201910333441 A CN201910333441 A CN 201910333441A CN 110090604 A CN110090604 A CN 110090604A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
Abstract
The present invention provides a kind of technique for preparing graphene coated inorganic non-metallic micro-/ nano particle conducive to plasma fluidisation bed powder treatment device, it is passed through the mixed gas of carbon source and other gases into plasma fluidisation bed powder treatment device first during the preparation process, adjusts air velocity and pressure makes the powder of micro-/ nano particle form fluidisation；Then, microwave is introduced by the region of powder fluidisation by microwave generator and coupling device and gas ionization is made to generate plasma；The power for finally adjusting microwave makes gas in fluidized bed reach predetermined temperature, and graphene coated powder micro-/ nano granular materials can be obtained.
Description
Technical field
The present invention relates to powder handling technical fields, prepare graphene coated inorganic non-metallic in particular to a kind of
The technique of micro-/ nano particle.
Background technique
Inorganic powder materials are carried out with surface is modified, regulates and controls the electric conductivity on its surface, thermal conductivity, refractive index, wellability, hard
Degree, chemical activity etc. can obviously improve the performances such as dispersion, stabilization, enhancing, electricity, calorifics, optics, the catalysis of dusty material, open up
Open up its application range.
Since heat and mass is high-efficient, uniform feature is handled, the processing of powder has been obtained in fluidization
It is widely applied.And gas molecule free radical is generated by electric discharge, the reaction that plasma technique can greatly improve gas is living
Property, it is a kind of efficient process for treating surface.
Summary of the invention
It is conducive to plasma fluidisation bed powder treatment device it is an object of that present invention to provide one kind and prepares graphene coated powder
The technique of last micro-/ nano granular materials, realization are fast and efficiently prepared.
To reach above-mentioned purpose, the following technical solutions are proposed by the present invention:
The work of graphene coated inorganic non-metallic micro-/ nano particle is prepared conducive to plasma fluidisation bed powder treatment device
Skill, plasma fluidisation bed powder treatment device are that can be carried out based on microwave coupling and using microwave the powder of heating automatically
Body processing unit, in which:
Plasma fluidisation bed powder treatment device has the variable diameter fluidized bed body being uprightly arranged, microwave generator, coupling
Device, feedback gas system and cyclone separator, wherein the variable diameter fluidized bed body being uprightly arranged, by the circle of at least two sections different inner diameters
Pipe composition, the caliber of round tube are incremented by successively from the bottom to top；Gas outlet, bottom setting are provided at the top of the variable diameter fluidized bed body
There is air inlet；Microwave generator generates microwave by microwave magnetron；Coupling device is configured to open the rectangular wave of circular hole up and down
It leads, the variable diameter fluidized bed body passes through the circular hole；The microwave that the microwave magnetron generates is coupled by rectangular waveguide
Variable diameter fluidized bed body, generates plasma inside bed body；Gas system is presented, air delivering pipeline is provided through and is fluidized to the variable diameter
The air inlet of bed body fills into single or mixed gas；Cyclone separator is arranged to recycling powder and is re-circulated into
Variable diameter fluidized bed body；Gas outlet at the top of the variable diameter fluidized bed body via a four-way pipe respectively with vacuum meter, vent valve and rotation
The air inlet of wind separator connects, and the gas outlet of cyclone separator is connected to vacuum by angle valve and accuracy controlling valve in parallel
Pump；The meal outlet of cyclone separator is connected to by circulation conduit with the side of variable diameter fluidized bed body, so that passing through cyclone separator
The powder isolated, which is recovered, reenters fluidized bed body；It is arranged between the bottom circular tube and air inlet of the variable diameter fluidized bed body
There is gas distributor, to make air flow method uniformly and carry powder；Wherein, the microwave generator is also arranged for change
Diameter fluidized bed body carries out microwave heating, makes the heating temperature of reaction chamber in variable diameter fluidized bed body reach 500 by microwave heating
DEG C or more；Variable diameter fluidized bed body has the first round tube and the second round tube, and the diameter of the first round tube is greater than the diameter of the second round tube, and
The junction of first round tube and the second round tube is located at the circular hole on the rectangular waveguide top；
The technique includes the following steps:
Sample drying removes water, and is crushed to obtain inorganic non-metallic micro-/ nano particle, fluidizes from plasma above-mentioned
Particle is sent into variable diameter fluidized bed body by the top of bed powder treatment device；
After vacuum environment maintenance, in plasma fluidisation bed powder treatment device, it is passed through auxiliary gas B and as carbon
The mixed gas of the gas A in source adjusts air velocity and inorganic non-metallic micro-/ nano particle is made to form fluidisation；
Pressure is controlled 102~105Within the scope of Pa, to meet plasma starter condition；Utilize microwave generator and coupling
Microwave is introduced the region of powder fluidisation and mixed gas ionization is made to generate plasma by device；
Microwave power is adjusted, so that mixed gas in fluidized bed is reached 300-950 DEG C of predetermined temperature, obtains graphene coated
Powder micro-/ nano granular materials.
Preferably, the gas A is methane, ethane, propane, ethylene, propylene, acetylene, methanol, ethyl alcohol, propyl alcohol, benzene and first
The combination of one or more of benzene.
Preferably, the gas B can be nitrogen, argon gas, hydrogen, ammonia as auxiliary fluidisation and the gas of adjusting air pressure
One or more of mixtures of gas.
Preferably, mixed gas flow is controlled using mass flow controller, achievees the purpose that adjust air velocity, matching
Air velocity and pressure make powder reach the state of fluidisation.
Preferably, described ionized gas is the mixed gas during processing, and gas ionization generates plasma
The area coincidence in the region of body and powder fluidisation.
Preferably, in gas ionization treatment process, it can adjust microwave power, make 200~1300W of power bracket, add
The predetermined temperature that hot gas reaches is 300~950 DEG C.
Preferably, the power of the microwave magnetron is 1KW.
Preferably, the inorganic non-metallic micro-/ nano particle includes silicon, silica, iron oxide, stannic oxide and dioxy
Change the particle of titanium material.
From the above technical scheme, technical solution of the present invention provides preparation facilities graphene coated inorganic non-metallic
The concrete technology flow process that the plasma of micro-/ nano particle fluidizes bed powder handling and uses, original powder is by chemistry
After vapor deposition processing, transparent membrane wraps up silicon particle along particle surface homoepitaxial, extends particle surface；
Graphene is completely uniform for the cladding of silicon particle, forms clearly core/shell structure.
Detailed description of the invention
Attached drawing is not intended to drawn to scale.In the accompanying drawings, identical or nearly identical group each of is shown in each figure
It can be indicated by the same numeral at part.For clarity, in each figure, not each component part is labeled.
Now, example will be passed through and the embodiments of various aspects of the invention is described in reference to the drawings, in which:
Fig. 1 is the transmission electron microscope photo of battery material (nano silica fume) starting powder.
Fig. 2 is the schematic diagram of plasma fluidisation bed powder treatment device of the invention.
Fig. 3 is the scanning electron microscopic picture after battery material (nano silica fume) is wrapped up by graphene.
Fig. 4 is the transmission electron microscope picture after battery material (nano silica fume) is wrapped up by graphene.
Specific embodiment
In order to better understand the technical content of the present invention, special to lift specific embodiment and institute's accompanying drawings is cooperated to be described as follows.
Various aspects with reference to the accompanying drawings to describe the present invention in the disclosure, shown in the drawings of the embodiment of many explanations.
It is not intended to cover all aspects of the invention for embodiment of the disclosure.It should be appreciated that a variety of designs and reality presented hereinbefore
Those of apply example, and describe in more detail below design and embodiment can in many ways in any one come it is real
It applies, this is because conception and embodiment disclosed in this invention are not limited to any embodiment.In addition, disclosed by the invention one
A little aspects can be used alone, or otherwise any appropriately combined use with disclosed by the invention.
In conjunction with shown in Fig. 2-4, preferred embodiments of the present invention disclose a kind of conducive to plasma fluidisation bed powder handling dress
The technique for preparing graphene coated inorganic non-metallic micro-/ nano particle is set, fluidizes bed to plasma first during the preparation process
It is passed through the mixed gas of carbon source and other gases in powder treatment device, adjusts air velocity and pressure makes micro-/ nano particle
Powder formed fluidisation；Then, microwave is introduced by the region of powder fluidisation by microwave generator and coupling device and makes gas
Ionization generates plasma；The power for finally adjusting microwave makes gas in fluidized bed reach predetermined temperature, and graphene packet can be obtained
Whiting end micro-/ nano granular materials.
As shown in connection with fig. 2, the plasma fluidisation bed powder treatment device that the present invention uses is the plasma of innovative design
Body fluidized bed processing mode has the variable diameter fluidized bed body, micro- being uprightly arranged including plasma fluidisation bed powder treatment device
Wave producer, coupling device, feedback gas system and cyclone separator.
The variable diameter fluidized bed body 1 being uprightly arranged is made of, the pipe of round tube the round tube (4A, 4B) of at least two sections different inner diameters
Diameter is incremented by successively from the bottom to top.In Fig. 2, the top of variable diameter fluidized bed body 1 is provided with gas outlet 7, and bottom is provided with air inlet 14.
Present gas system and air inlet 14 be linked by air delivering pipeline, to the air inlet of variable diameter fluidized bed body 1 fill into it is single or
Reaction chamber inside person's mixed gas to variable diameter fluidized bed body 1.
As shown in Fig. 2, feedback gas system has multiple gas cylinders 20, for providing gas supply.Between gas cylinder and air inlet also
It is mass flow controller MFC that at least one, which is provided with, for controlling the device of gas flow, the device, is especially preferably counted
Font mass flow controller, for carrying out accurate measurement and control for gas mass flow.
In conjunction with Fig. 2, microwave generator 2, as microwave source, for generating microwave by microwave magnetron.Preferably, micro-
The side of variable diameter fluidized bed body 1 is arranged in wave producer.The power of microwave magnetron is 1KW.
Microwave Power Transmission and distribution are realized in one coupling device and the cooperation of microwave generator 2.In embodiment shown in Fig. 2,
The side of variable diameter fluidized bed body 1 is arranged in coupling device, and with microwave generator the same side, the rectangular wave of circular hole is opened for about one
4 are led, variable diameter fluidized bed body 1 passes through upper and lower two circular holes.The microwave that microwave magnetron 2 generates is coupled by rectangular waveguide 4
Variable diameter fluidized bed body, generates plasma inside bed body, fluidizes to powder.
In example shown in Fig. 2, microwave generator is also arranged for carrying out microwave heating to variable diameter fluidized bed body, so that
The intracorporal temperature of bed increases.
One cyclone separator 3, is arranged in the top of the other side of variable diameter fluidized bed body 1, to recycle powder and follow again
Ring enters variable diameter fluidized bed body 1.
In conjunction with Fig. 2, the gas outlet 7 at 1 top of variable diameter fluidized bed body via a four-way pipe respectively with vacuum meter 8, vent valve 9 and
The air inlet 16 of cyclone separator 3 connects, and the gas outlet 10 of cyclone separator passes through angle valve 11 and accuracy controlling valve 12 in parallel
It is connected to vacuum pump 13, to realize that holding and the vacuum degree of vacuum environment are adjusted.Accuracy controlling valve 12 is needle valve or metering valve.
The meal outlet 18 of cyclone separator 3 is connected to by circulation conduit 19 with the side of variable diameter fluidized bed body 1, so that passing through
The powder that cyclone separator 3 is isolated, which is recovered, reenters fluidized bed body, so that from the gas outlet at 1 top of variable diameter fluidized bed body
The powder being mingled in 7 escaping gas is recycled in recycling.
Such as Fig. 2, it is provided with gas distributor 5 between the bottom circular tube 4B and air inlet 14 of variable diameter fluidized bed body, to make
Air flow method is uniform and carries powder.
During realization of the invention, by the cooperation of the two-part round tube, and the round tube of bottom (compared with mini diameter tube)
Positioned at the space that rectangular waveguide is surrounded, microwave generator also pass through microwave heating make reaction chamber in variable diameter fluidized bed body plus
Hot temperature reaches 500 DEG C or more, realizes stably and controllable temperature-rise effect.It certainly, in an alternate embodiment of the invention, can be micro- by adjusting
The power of wave producer realizes that temperature rise and plasma occur.
In conjunction with Fig. 2, it is preferable that variable diameter fluidized bed body 1 has the first round tube 4A and the second round tube 4B, and the first round tube 4A's is straight
Diameter D is greater than the diameter d of the second round tube 4B, and the junction of the first round tube 4A and the second round tube 4B are located at 6 top of rectangular waveguide
At circular hole.
The junction of first round tube 4A and the second round tube 4B include a hollow round table 4C, larger-diameter one end and first
The edge of round tube 4A is fixed, and smaller direct one end and the edge of the second round tube 4B are fixed, so that the powder in the first round tube is logical
The sloped transition for crossing hollow round table is flowed into the second round tube.
In some preferred embodiments, the diameter d of the second round tube and the diameter D of the first round tube meet: D/3≤d≤D/
2.In example shown in Fig. 2, the diameter d of the second round tube 4B is 20-30mm.
As shown in connection with fig. 2, it during preparing particle, is passed through first into plasma fluidisation bed powder treatment device
The mixed gas of carbon source and other gases, adjusts air velocity and pressure makes the powder of micro-/ nano particle form fluidisation；So
Afterwards, microwave is introduced by the region of powder fluidisation by microwave generator and coupling device and gas ionization is made to generate plasma；
The power for finally adjusting microwave makes gas in fluidized bed reach predetermined temperature, obtains graphene coated powder micro-/ nano granular material
Material.
The exemplary realization of above-mentioned technique is described below with reference to specific example.
Step 1, sample drying remove water, and are crushed to obtain inorganic non-metallic micro-/ nano particle, from plasma above-mentioned
Particle is sent into variable diameter fluidized bed body by the top of body fluidized bed powder processing unit；
After vacuum environment maintenance, in plasma fluidisation bed powder treatment device, it is passed through auxiliary gas B and as carbon
The mixed gas of the gas A in source adjusts air velocity and inorganic non-metallic micro-/ nano particle is made to form fluidisation；
Pressure is controlled 102~105Within the scope of Pa, to meet plasma starter condition；Utilize microwave generator and coupling
Microwave is introduced the region of powder fluidisation and mixed gas ionization is made to generate plasma by device；
Microwave power is adjusted, so that mixed gas in fluidized bed is reached 300-950 DEG C of predetermined temperature, obtains graphene coated
Powder micro-/ nano granular materials.
Preferably, gas A is in methane, ethane, propane, ethylene, propylene, acetylene, methanol, ethyl alcohol, propyl alcohol, benzene and toluene
One or more of combinations.
Preferably, gas B can be nitrogen, argon gas, hydrogen, ammonia as auxiliary fluidisation and the gas of adjusting air pressure
One or more of mixtures.
Preferably, mixed gas flow is controlled using mass flow controller, achievees the purpose that adjust air velocity, matching
Air velocity and pressure make powder reach the state of fluidisation.
Preferably, during processing, the mixed gas that ionized gas is, gas ionization generate the region of plasma
With the area coincidence of powder fluidisation.
Preferably, in gas ionization treatment process, it can adjust microwave power, make 200~1300W of power bracket, add
The predetermined temperature that hot gas reaches is 300~950 DEG C.
Preferably, the power of microwave magnetron is 1KW.
Preferably, inorganic non-metallic micro-/ nano particle includes silicon, silica, stannic oxide and titanic oxide material
Particle.
The explanation of specific implementation step is carried out by taking nano silica fume as an example below.
(1) sample drying removes water
The silicon powder for weighing the 50nm of 2g is placed in crucible, 80 DEG C drying 12 hours in hot air drier.
(2) it is crushed agglomerated particle
The silicon powder of step (1) after dry is fitted into mortar and is ground 20 minutes, the bulky grain reunited is crushed.
(3) corona treatment
Silicon powder after step (2) drying and grinding is filled into plasma fluidisation bed from top, is evacuated to background to system
After vacuum, the mixed gas flow for being passed through argon gas, methane and hydrogen is respectively 10sccm, 5sccm and 5sccm, and system is true at this time
Null value is 86pa.Then, by adjusting vavuum pump valve, system vacuum value is made to reach 104pa, opens microwave plasma source,
So that microwave input power is remained 1000W, carry out chemical vapor deposition, reaction time 60min is surveyed by infrared measurement of temperature at this time
Obtaining reaction chamber temperature is 500 DEG C.
In other examples, microwave energy is carried out with microwave input power 1000W, passes through control MFC and adjusting
Heating temperature corresponding to vavuum pump valve, gas with various ratio and system air pressure is summarized as follows table:
Finally, we choose under 100Pa air pressure therein, assessed using the sample under 500 degrees Celsius of examples, it is original
Powder particle be in elliposoidal, partial size is mainly distributed between 30~80nm, and surface is smooth.By chemical gaseous phase of the invention
After deposition processes, transparent membrane wraps up silicon particle along particle surface homoepitaxial, extends particle surface；Graphite
Alkene is completely uniform for the cladding of silicon particle, forms clearly core/shell structure.
Although the present invention has been disclosed as a preferred embodiment, however, it is not to limit the invention.Skill belonging to the present invention
Has usually intellectual in art field, without departing from the spirit and scope of the present invention, when can be used for a variety of modifications and variations.Cause
This, the scope of protection of the present invention is defined by those of the claims.
Claims (9)
1. a kind of prepare graphene coated inorganic non-metallic micro-/ nano particle conducive to plasma fluidisation bed powder treatment device
Technique, which is characterized in that the plasma fluidisation bed powder treatment device is that can utilize based on microwave coupling and automatically microwave
It can be carried out the powder treatment device of heating, in which:
Plasma fluidisation bed powder treatment device have uprightly be arranged variable diameter fluidized bed body, microwave generator, coupling device,
Gas system and cyclone separator are presented, wherein the variable diameter fluidized bed body being uprightly arranged, by the round tube group of at least two sections different inner diameters
At the caliber of round tube is incremented by successively from the bottom to top；Be provided with gas outlet at the top of the variable diameter fluidized bed body, bottom be provided with into
Port；Microwave generator generates microwave by microwave magnetron；Coupling device is configured to open the rectangular waveguide of circular hole, institute up and down
Variable diameter fluidized bed body is stated across the circular hole；The microwave that the microwave magnetron generates is coupled into variable diameter stream by rectangular waveguide
Change bed body, plasma is generated inside bed body；Gas system is presented, is provided through air delivering pipeline to the variable diameter fluidized bed body
Air inlet fills into single or mixed gas；Cyclone separator is arranged to recycling powder and is re-circulated into variable diameter stream
Change bed body；Gas outlet at the top of the variable diameter fluidized bed body via a four-way pipe respectively with vacuum meter, vent valve and cyclonic separation
The air inlet of device connects, and the gas outlet of cyclone separator is connected to vacuum pump by angle valve and accuracy controlling valve in parallel；Whirlwind
The meal outlet of separator is connected to by circulation conduit with the side of variable diameter fluidized bed body, so that isolated by cyclone separator
Powder, which is recovered, reenters fluidized bed body；Gas point is provided between the bottom circular tube and air inlet of the variable diameter fluidized bed body
Cloth device, to make air flow method uniformly and carry powder；Wherein, the microwave generator is also arranged for variable diameter fluidized bed
Body carries out microwave heating, makes the heating temperature of reaction chamber in variable diameter fluidized bed body reach 500 DEG C or more by microwave heating；Become
Diameter fluidized bed body has the first round tube and the second round tube, and the diameter of the first round tube is greater than the diameter of the second round tube, and the first round tube
It is located at the circular hole on the rectangular waveguide top with the junction of the second round tube；
The technique includes the following steps:
Sample drying removes water, and is crushed to obtain inorganic non-metallic micro-/ nano particle, fluidizes bed powder from plasma above-mentioned
Particle is sent into variable diameter fluidized bed body by the top of body processing unit；
After vacuum environment maintenance, in plasma fluidisation bed powder treatment device, it is passed through auxiliary gas B and as carbon source
The mixed gas of gas A adjusts air velocity and inorganic non-metallic micro-/ nano particle is made to form fluidisation；
Pressure is controlled 102~105Within the scope of Pa, to meet plasma starter condition；Utilize microwave generator and coupling dress
It sets, microwave is introduced into the region of powder fluidisation and mixed gas ionization is made to generate plasma；
Microwave power is adjusted, so that mixed gas in fluidized bed is reached 300-950 DEG C of predetermined temperature, obtains graphene coated powder
Micro-/ nano granular materials.
2. the technique according to claim 1 for preparing graphene coated inorganic non-metallic micro-/ nano particle, feature exist
In, the gas A be one of methane, ethane, propane, ethylene, propylene, acetylene, methanol, ethyl alcohol, propyl alcohol, benzene and toluene or
Several combinations.
3. the technique according to claim 1 for preparing graphene coated inorganic non-metallic micro-/ nano particle, feature exist
In the gas B can be one kind or several of nitrogen, argon gas, hydrogen, ammonia as auxiliary fluidisation and the gas of adjusting air pressure
The mixture of kind.
4. the technique according to claim 1 for preparing graphene coated inorganic non-metallic micro-/ nano particle, feature exist
In controlling mixed gas flow using mass flow controller, achieve the purpose that adjust air velocity, match air velocity and pressure
Force powder reaches the state of fluidisation.
5. the technique according to claim 4 for preparing graphene coated inorganic non-metallic micro-/ nano particle, feature exist
In described ionized gas is the mixed gas during processing, and gas ionization generates region and the powder of plasma
The area coincidence of the later and decadent stage of a school of thought.
6. the technique according to claim 4 for preparing graphene coated inorganic non-metallic micro-/ nano particle, feature exist
In, in gas ionization treatment process, it can adjust microwave power, make 200~1300W of power bracket, what heat gas reached
Predetermined temperature is 300~950 DEG C.
7. the technique according to claim 1 for preparing graphene coated inorganic non-metallic micro-/ nano particle, feature exist
In the power of the microwave magnetron is 1KW.
8. the technique according to claim 1 for preparing graphene coated inorganic non-metallic micro-/ nano particle, feature exist
In the inorganic non-metallic micro-/ nano particle includes of silicon, silica, iron oxide, stannic oxide and titanic oxide material
Grain.
9. the technique according to claim 1 for preparing graphene coated inorganic non-metallic micro-/ nano particle, feature exist
In, during the preparation process, matched using following microwave powers with air velocity and pressure, carry out powder fluidization, plasma treatment
And microwave heating:
Wherein, microwave power 1000W.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112429720A (en) * | 2020-11-19 | 2021-03-02 | 航天特种材料及工艺技术研究所 | Graphene-titanium dioxide nano composite material and preparation method thereof |
| CN114408899A (en) * | 2022-01-26 | 2022-04-29 | 株洲科能新材料股份有限公司 | Preparation method of nano high-purity carbon |
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