CN110090604B - Process for preparing graphene-coated inorganic nonmetal micro/nanoparticles - Google Patents
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- CN110090604B CN110090604B CN201910333441.6A CN201910333441A CN110090604B CN 110090604 B CN110090604 B CN 110090604B CN 201910333441 A CN201910333441 A CN 201910333441A CN 110090604 B CN110090604 B CN 110090604B
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- 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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- 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 invention provides a process for preparing graphene coated inorganic nonmetal micro/nano particles by using a plasma fluidized bed powder processing device, which comprises the steps of firstly introducing mixed gas of a carbon source and other gases into the plasma fluidized bed powder processing device in the preparation process, and adjusting the gas flow speed and pressure to ensure that the powder of the micro/nano particles is fluidized; then, introducing microwaves into the powder fluidization area through a microwave generator and a coupling device, and ionizing the gas to generate plasma; finally, adjusting the power of the microwave to enable the gas in the fluidized bed to reach a preset temperature, and obtaining the graphene coated powder micro/nano particle material.
Description
Technical Field
The invention relates to the technical field of powder treatment, in particular to a process for preparing graphene-coated inorganic nonmetal micro/nanoparticles.
Background
The inorganic powder material is subjected to surface modification, the electrical conductivity, the thermal conductivity, the refractive index, the wettability, the hardness, the chemical activity and the like of the surface of the inorganic powder material are regulated and controlled, the dispersion, the stability, the enhancement, the electrical property, the thermal property, the optical property, the catalysis and other properties of the powder material can be obviously improved, and the application range of the inorganic powder material is expanded.
Because of the characteristics of high heat and mass transfer efficiency and uniform treatment, the fluidized bed technology has been widely applied to the treatment of powder. The plasma technology can greatly improve the reactivity of the gas by generating gas molecular free radicals through discharge, and is an efficient surface treatment technology.
Disclosure of Invention
The invention aims to provide a process for preparing a graphene coated powder micro/nano particle material by using a plasma fluidized bed powder treatment device, and the process can be used for realizing rapid and efficient preparation.
In order to achieve the above purpose, the invention provides the following technical scheme:
do benefit to plasma fluidized bed powder processing apparatus and prepare graphite alkene cladding inorganic nonmetal micron/nano-particle's technology, plasma fluidized bed powder processing apparatus is based on microwave coupling and can utilize the powder processing apparatus that microwave energy carries out the heating automatically, wherein:
the plasma fluidized bed powder processing device is provided with a vertically arranged reducing fluidized bed body, a microwave generator, a coupling device, a gas feeding system and a cyclone separator, wherein the vertically arranged reducing fluidized bed body consists of at least two sections of circular tubes with different inner diameters, and the tube diameters of the circular tubes are sequentially increased from bottom to top; the top of the reducing fluidized bed body is provided with an air outlet, and the bottom of the reducing fluidized bed body is provided with an air inlet; a microwave generator for generating microwaves through a microwave magnetron; the coupling device is constructed as a rectangular waveguide with a circular hole at the upper part and the lower part, and the reducing fluidized bed body penetrates through the circular hole; the microwave generated by the microwave magnetron enters the reducing fluidized bed body through rectangular waveguide coupling, and plasma is generated in the bed body; the air feeding system is arranged to supplement single or mixed air to the air inlet of the reducing fluidized bed body through an air conveying pipeline; the cyclone separator is arranged for recovering the powder and recycling the powder into the reducing fluidized bed body; the gas outlet at the top of the reducing fluidized bed body is respectively connected with a vacuum gauge, a gas release valve and a gas inlet of a cyclone separator through a four-way pipe, and the gas outlet of the cyclone separator is connected to a vacuum pump through an angle valve and an accurate regulating valve which are connected in parallel; the powder outlet of the cyclone separator is communicated with the side surface of the reducing fluidized bed body through a circulating conduit, so that the powder separated by the cyclone separator is recovered and enters the fluidized bed body again; a gas distributor is arranged between the bottom circular tube of the reducing fluidized bed body and the gas inlet so as to ensure that the gas flow is uniformly distributed and bear the powder; the microwave generator is also arranged for carrying out microwave heating on the reducing fluidized bed body, and the heating temperature of the reaction chamber in the reducing fluidized bed body reaches more than 500 ℃ through microwave heating; the reducing fluidized bed body is provided with a first round pipe and a second round pipe, the diameter of the first round pipe is larger than that of the second round pipe, and the joint of the first round pipe and the second round pipe is positioned at the round hole at the upper part of the rectangular waveguide;
the process comprises the following steps:
drying and dehydrating the sample, crushing the sample to obtain inorganic nonmetal micro/nano particles, and feeding the particles into a reducing fluidized bed body from the upper part of the plasma fluidized bed powder treatment device;
after the vacuum environment is maintained, introducing mixed gas of auxiliary gas B and gas A serving as a carbon source into a plasma fluidized bed powder treatment device, and adjusting the gas flow velocity to ensure that inorganic nonmetal micro/nanoparticles form fluidization;
controlling the pressure at 102～105In the Pa range, the plasma glow starting condition is met; introducing microwaves into the powder fluidization area by using a microwave generator and a coupling device, and ionizing the mixed gas to generate plasma;
adjusting the microwave power to enable the mixed gas in the fluidized bed to reach the predetermined temperature of 300-950 ℃ to obtain the graphene coated powder micro/nano particle material.
Preferably, the gas A is one or a combination of several of methane, ethane, propane, ethylene, propylene, acetylene, methanol, ethanol, propanol, benzene and toluene.
Preferably, the gas B as the gas for assisting fluidization and adjusting the gas pressure can be one or a mixture of several of nitrogen, argon, hydrogen and ammonia.
Preferably, the mass flow controller is used for controlling the flow of the mixed gas to achieve the purpose of adjusting the gas flow speed, and the gas flow speed and the pressure are matched to achieve the fluidization state of the powder.
Preferably, during the treatment, the ionized gas is the mixed gas, and the region where the gas is ionized to generate plasma coincides with the region where the powder is fluidized.
Preferably, in the gas ionization treatment process, the microwave power can be adjusted to be 200-1300W, and the preset temperature for heating the gas is 300-950 ℃.
Preferably, the power of the microwave magnetron is 1 KW.
Preferably, the inorganic non-metallic micro/nanoparticles include particles of silicon, silicon dioxide, iron oxide, tin dioxide and titanium dioxide materials.
According to the technical scheme, the invention provides the plasma fluidized bed powder treatment and the specific process flow for coating inorganic nonmetal micro/nano particles with graphene, and the preparation device is characterized in that after the original powder is subjected to chemical vapor deposition treatment, a transparent film uniformly grows along the surface of the particles, wraps silicon particles and extends out of the surface of the particles; the graphene is completely and uniformly coated on the silicon particles to form a clear core/shell structure.
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The drawings are not intended to be drawn to scale. In the drawings, each identical or nearly identical component that is illustrated in various figures may be represented by a like numeral. For purposes of clarity, not every component may be labeled in every drawing. Embodiments of various aspects of the present invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is a transmission electron micrograph of a raw powder of a battery material (silica nanopowder).
FIG. 2 is a schematic view of a plasma fluidized bed powder processing apparatus according to the present invention.
Fig. 3 is a scanning electron microscope picture of the battery material (nano silicon powder) wrapped by graphene.
Fig. 4 is a transmission electron microscope picture of a battery material (nano silicon powder) coated by graphene.
Detailed Description
In order to better understand the technical content of the present invention, specific embodiments are described below with reference to the accompanying drawings.
In this disclosure, aspects of the present invention are described with reference to the accompanying drawings, in which a number of illustrative embodiments are shown. Embodiments of the present disclosure are not necessarily intended to include all aspects of the invention. It should be appreciated that the various concepts and embodiments described above, as well as those described in greater detail below, may be implemented in any of numerous ways, as the disclosed concepts and embodiments are not limited to any one implementation. In addition, some aspects of the present disclosure may be used alone, or in any suitable combination with other aspects of the present disclosure.
Referring to fig. 2 to 4, a preferred embodiment of the present invention discloses a process for preparing graphene coated inorganic non-metallic micro/nanoparticles by using a plasma fluidized bed powder processing apparatus, wherein during the preparation process, a mixed gas of a carbon source and other gases is introduced into the plasma fluidized bed powder processing apparatus, and the gas flow velocity and pressure are adjusted to fluidize the micro/nanoparticles; then, introducing microwaves into the powder fluidization area through a microwave generator and a coupling device, and ionizing the gas to generate plasma; finally, adjusting the power of the microwave to enable the gas in the fluidized bed to reach a preset temperature, and obtaining the graphene coated powder micro/nano particle material.
Referring to fig. 2, the plasma fluidized bed powder processing apparatus of the present invention is a plasma fluidized bed processing method with innovative design, and includes a plasma fluidized bed powder processing apparatus having a vertically arranged variable diameter fluidized bed body, a microwave generator, a coupling device, a gas feeding system, and a cyclone separator.
The vertically arranged reducing fluidized bed body 1 consists of at least two sections of circular tubes (4A and 4B) with different inner diameters, and the diameters of the circular tubes are sequentially increased from bottom to top. In fig. 2, the top of the reducing fluidized bed body 1 is provided with an air outlet 7, and the bottom is provided with an air inlet 14.
The air feeding system is connected to the air inlet 14 through an air transmission pipeline, and single or mixed air is supplemented to the air inlet of the reducing fluidized bed body 1 to the reaction chamber in the reducing fluidized bed body 1.
As shown in fig. 2, the gas feed system has a plurality of gas cylinders 20 for providing a supply of gas. At least one device for controlling the gas flow is also arranged between the gas cylinder and the gas inlet, which is a mass flow controller MFC, particularly preferably a digital mass flow controller, for precise measurement and control of the gas mass flow.
Referring to fig. 2, a microwave generator 2 serves as a microwave source for generating microwaves through a microwave magnetron. Preferably, the microwave generator is arranged at the side of the reducing fluidized bed body 1. The power of the microwave magnetron is 1 KW.
A coupling device is matched with the microwave generator 2 to realize microwave power transmission and distribution. In the embodiment shown in fig. 2, the coupling device is arranged on one side of the reducing fluidized bed body 1, is on the same side as the microwave generator, and is a rectangular waveguide 4 with an upper circular hole and a lower circular hole, and the reducing fluidized bed body 1 penetrates through the upper circular hole and the lower circular hole. The microwave generated by the microwave magnetron 2 is coupled into the reducing fluidized bed body through the rectangular waveguide 4, and plasma is generated in the bed body to fluidize the powder.
In the example shown in figure 2, the microwave generator is also arranged to apply microwave heating to the bed of reduced diameter fluidised bed to cause an increase in temperature within the bed.
And the cyclone separator 3 is arranged above the other side of the reducing fluidized bed body 1 and is used for recovering the powder and recycling the powder into the reducing fluidized bed body 1.
Referring to fig. 2, an air outlet 7 at the top of the reducing fluidized bed body 1 is respectively connected with a vacuum gauge 8, a release valve 9 and an air inlet 16 of the cyclone separator 3 through a four-way pipe, and an air outlet 10 of the cyclone separator is connected to a vacuum pump 13 through an angle valve 11 and a precise regulating valve 12 which are connected in parallel, so as to realize the maintenance of a vacuum environment and the regulation of the vacuum degree. The precision regulating valve 12 is a needle valve or a metering valve.
The powder outlet 18 of the cyclone separator 3 is communicated with the side surface of the reducing fluidized bed body 1 through a circulating conduit 19, so that the powder separated by the cyclone separator 3 is recovered and enters the fluidized bed body again, and the powder mixed in the gas escaping from the gas outlet 7 at the top of the reducing fluidized bed body 1 is recovered and recycled.
As shown in fig. 2, a gas distributor 5 is disposed between the bottom circular tube 4B of the reducing fluidized bed body and the gas inlet 14 to make the gas flow distribution uniform and to carry the powder.
In the implementation process of the invention, the two-section type circular tube is matched, the circular tube (thinner circular tube) at the bottom is positioned in the space surrounded by the rectangular waveguide, and the microwave generator is used for heating by microwave to enable the heating temperature of the reaction chamber in the reducing fluidized bed to reach more than 500 ℃, thereby realizing the stable and controllable temperature rise effect. Of course, in alternative embodiments, temperature rise and plasma generation may be achieved by adjusting the power of the microwave generator.
With reference to fig. 2, preferably, the variable diameter fluidized bed 1 has a first circular tube 4A and a second circular tube 4B, the diameter D of the first circular tube 4A is larger than the diameter D of the second circular tube 4B, and the joint of the first circular tube 4A and the second circular tube 4B is located at the circular hole at the upper part of the rectangular waveguide 6.
The junction of the first round tube 4A and the second round tube 4B comprises a hollow round table 4C, one end with a larger diameter is fixed with the edge of the first round tube 4A, and the other end with a smaller diameter is fixed with the edge of the second round tube 4B, so that powder in the first round tube flows into the second round tube through the slope transition of the hollow round table.
In some preferred embodiments, the diameter D of the second tube and the diameter D of the first tube satisfy: d is more than or equal to D/3 and less than or equal to D/2. In the example shown in fig. 2, the diameter d of the second round tube 4B is 20-30 mm.
Referring to fig. 2, in the process of preparing particles, firstly, a mixed gas of a carbon source and other gases is introduced into a plasma fluidized bed powder processing device, and the gas flow rate and pressure are adjusted to fluidize the micro/nano particle powder; then, introducing microwaves into the powder fluidization area through a microwave generator and a coupling device, and ionizing the gas to generate plasma; and finally, adjusting the power of the microwave to enable the gas in the fluidized bed to reach a preset temperature, so as to obtain the graphene coated powder micro/nano particle material.
An exemplary implementation of the above process is described below in connection with specific examples.
Step 1, drying and dehydrating a sample, crushing the sample to obtain inorganic nonmetal micro/nano particles, and sending the particles into a reducing fluidized bed body from the upper part of the plasma fluidized bed powder treatment device;
after the vacuum environment is maintained, introducing mixed gas of auxiliary gas B and gas A serving as a carbon source into a plasma fluidized bed powder treatment device, and adjusting the gas flow velocity to ensure that inorganic nonmetal micro/nanoparticles form fluidization;
controlling the pressure at 102～105In the Pa range, the plasma glow starting condition is met; introducing microwaves into the powder fluidization area by using a microwave generator and a coupling device, and ionizing the mixed gas to generate plasma;
adjusting the microwave power to enable the mixed gas in the fluidized bed to reach the predetermined temperature of 300-950 ℃ to obtain the graphene coated powder micro/nano particle material.
Preferably, the gas A is one or a combination of several of methane, ethane, propane, ethylene, propylene, acetylene, methanol, ethanol, propanol, benzene and toluene.
Preferably, the gas B as the gas for assisting fluidization and adjusting the gas pressure can be one or a mixture of several of nitrogen, argon, hydrogen and ammonia.
Preferably, the mass flow controller is used for controlling the flow of the mixed gas to achieve the purpose of adjusting the gas flow speed, and the gas flow speed and the pressure are matched to achieve the fluidization state of the powder.
Preferably, during the treatment, the ionized gas is a mixed gas, and the region where the gas ionizes to generate plasma coincides with the region where the powder fluidizes.
Preferably, in the gas ionization treatment process, the microwave power can be adjusted to be 200-1300W, and the preset temperature for heating the gas is 300-950 ℃.
Preferably, the microwave magnetron has a power of 1 KW.
Preferably, the inorganic non-metallic micro/nanoparticles comprise particles of silicon, silicon dioxide, tin dioxide and titanium dioxide materials.
The following description will be made of specific embodiments using nano-silicon powder as an example.
(1) Drying and dewatering sample
2g of 50nm silicon powder was weighed into a crucible and dried in a hot air drying oven at 80 ℃ for 12 hours.
(2) Breaking up agglomerated particles
And (3) putting the dried silicon powder obtained in the step (1) into a mortar, grinding for 20 minutes, and crushing agglomerated large particles.
(3) Plasma treatment
And (3) filling the silicon powder dried and ground in the step (2) into a plasma fluidized bed from the upper part, and introducing mixed gas of argon, methane and hydrogen with the flow rates of 10sccm, 5sccm and 5sccm respectively after the system is pumped to the background vacuum, wherein the vacuum value of the system is 86 pa. Then, the vacuum value of the system is made to reach 104pa by adjusting a vacuum pump valve, the microwave plasma source is opened, the microwave input power is kept to be 1000W, chemical vapor deposition is carried out, the reaction time is 60min, and the temperature of the reaction chamber is measured to be 500 ℃ by infrared temperature measurement.
In another example, microwave energy generation is performed at a microwave input power of 1000W, and heating temperatures corresponding to different gas ratios and system pressures are summarized in the following table by controlling MFC and adjusting vacuum pump valves:
finally, the original powder particles are in an ellipsoid shape, the particle size is mainly distributed between 30 and 80nm, and the surface is smooth when the sample at 500 ℃ is selected for evaluation under the pressure of 100 Pa. After the chemical vapor deposition treatment, the transparent film uniformly grows along the particle surface, wraps the silicon particles and extends out of the particle surface; the graphene is completely and uniformly coated on the silicon particles to form a clear core/shell structure.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, the protection scope of the present invention should be determined by the appended claims.
Claims (9)
1. The process for preparing graphene coated inorganic nonmetal micro/nanoparticles by using the plasma fluidized bed powder processing device is characterized in that the plasma fluidized bed powder processing device is a powder processing device which is based on microwave coupling and can automatically utilize microwave energy for heating, wherein:
the plasma fluidized bed powder processing device is provided with a vertically arranged reducing fluidized bed body, a microwave generator, a coupling device, a gas feeding system and a cyclone separator, wherein the vertically arranged reducing fluidized bed body consists of at least two sections of circular tubes with different inner diameters, and the tube diameters of the circular tubes are sequentially increased from bottom to top; the top of the reducing fluidized bed body is provided with an air outlet, and the bottom of the reducing fluidized bed body is provided with an air inlet; a microwave generator for generating microwaves through a microwave magnetron; the coupling device is constructed as a rectangular waveguide with a circular hole at the upper part and the lower part, and the reducing fluidized bed body penetrates through the circular hole; the microwave generated by the microwave magnetron enters the reducing fluidized bed body through rectangular waveguide coupling, and plasma is generated in the bed body; the air feeding system is arranged to supplement single or mixed air to the air inlet of the reducing fluidized bed body through an air conveying pipeline; the cyclone separator is arranged for recovering the powder and recycling the powder into the reducing fluidized bed body; the gas outlet at the top of the reducing fluidized bed body is respectively connected with a vacuum gauge, a gas release valve and a gas inlet of a cyclone separator through a four-way pipe, and the gas outlet of the cyclone separator is connected to a vacuum pump through an angle valve and an accurate regulating valve which are connected in parallel; the powder outlet of the cyclone separator is communicated with the side surface of the reducing fluidized bed body through a circulating conduit, so that the powder separated by the cyclone separator is recovered and enters the fluidized bed body again; a gas distributor is arranged between the bottom circular tube of the reducing fluidized bed body and the gas inlet so as to ensure that the gas flow is uniformly distributed and bear the powder; the microwave generator is also arranged for carrying out microwave heating on the reducing fluidized bed body, and the heating temperature of the reaction chamber in the reducing fluidized bed body reaches more than 500 ℃ through microwave heating; the reducing fluidized bed body is provided with a first round pipe and a second round pipe, the diameter of the first round pipe is larger than that of the second round pipe, and the joint of the first round pipe and the second round pipe is positioned at the round hole at the upper part of the rectangular waveguide; the joint of the first round pipe and the second round pipe comprises a hollow round table, wherein one end with a larger diameter is fixed with the edge of the first round pipe, and one end with a smaller diameter is fixed with the edge of the second round pipe, so that the powder in the first round pipe transits through the slope of the hollow round table and flows into the second round pipe;
the process comprises the following steps:
drying and dehydrating the sample, crushing the sample to obtain inorganic nonmetal micro/nano particles, and feeding the particles into a reducing fluidized bed body from the upper part of the plasma fluidized bed powder treatment device;
after the vacuum environment is maintained, introducing mixed gas of auxiliary gas B and gas A serving as a carbon source into a plasma fluidized bed powder treatment device, and adjusting the gas flow velocity to ensure that inorganic nonmetal micro/nanoparticles form fluidization;
controlling the pressure at 102～105In the Pa range, the plasma glow starting condition is met; introducing microwaves into the powder fluidization area by using a microwave generator and a coupling device, and ionizing the mixed gas to generate plasma;
adjusting the microwave power to enable the mixed gas in the fluidized bed to reach the predetermined temperature of 300-950 ℃ to obtain the graphene coated powder micro/nano particle material.
2. The process for preparing graphene coated inorganic non-metallic micro/nanoparticles according to claim 1, wherein the gas A is one or more of methane, ethane, propane, ethylene, propylene, acetylene, methanol, ethanol, propanol, benzene and toluene.
3. The process for preparing graphene coated inorganic non-metallic micro/nanoparticles according to claim 1, wherein the gas B is one or a mixture of nitrogen, argon, hydrogen and ammonia as a gas for assisting fluidization and adjusting gas pressure.
4. The process for preparing graphene coated inorganic non-metallic micro/nanoparticles according to claim 1, wherein the gas flow rate is controlled by a mass flow controller to adjust the gas flow rate, and the gas flow rate and pressure are matched to make the powder in a fluidized state.
5. The process for preparing graphene coated inorganic non-metallic micro/nanoparticles according to claim 4, wherein the ionized gas is the mixed gas during the treatment process, and the region where the gas ionizes to generate plasma coincides with the region where the powder is fluidized.
6. The process for preparing graphene coated inorganic non-metallic micro/nanoparticles according to claim 4, wherein the microwave power is adjusted to 200-1300W and the predetermined temperature of the heated gas is 300-950 ℃ during the gas ionization treatment.
7. The process according to claim 1, wherein the microwave magnetron has a power of 1 KW.
8. The process for preparing graphene coated inorganic non-metallic micro/nanoparticles according to claim 1, wherein the inorganic non-metallic micro/nanoparticles comprise particles of silicon, silicon dioxide, iron oxide, tin dioxide and titanium dioxide materials.
9. The process for preparing graphene coated inorganic non-metallic micro/nanoparticles according to claim 1, wherein the following microwave power is adopted to match with the air flow velocity and pressure in the preparation process, and powder fluidization, plasma treatment and microwave heating are carried out:
wherein the microwave power is 1000W.
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