CN114522620A - Vacuum reactor for preparing graphene by electrifying carbon powder - Google Patents
Vacuum reactor for preparing graphene by electrifying carbon powder Download PDFInfo
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- CN114522620A CN114522620A CN202011321359.0A CN202011321359A CN114522620A CN 114522620 A CN114522620 A CN 114522620A CN 202011321359 A CN202011321359 A CN 202011321359A CN 114522620 A CN114522620 A CN 114522620A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 239000010453 quartz Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 8
- 239000004693 Polybenzimidazole Substances 0.000 claims description 8
- 239000004642 Polyimide Substances 0.000 claims description 8
- 229920000265 Polyparaphenylene Polymers 0.000 claims description 8
- -1 Polytetrafluoroethylene Polymers 0.000 claims description 8
- 229920002480 polybenzimidazole Polymers 0.000 claims description 8
- 229920002530 polyetherether ketone Polymers 0.000 claims description 8
- 229920001721 polyimide Polymers 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 4
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- 229920002312 polyamide-imide Polymers 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 230000000149 penetrating effect Effects 0.000 claims 1
- 238000007599 discharging Methods 0.000 abstract description 7
- 238000005086 pumping Methods 0.000 abstract description 3
- 239000000843 powder Substances 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 238000001237 Raman spectrum Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000010410 layer Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 1
- 239000003830 anthracite Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/006—Processes utilising sub-atmospheric pressure; Apparatus therefor
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
-
- 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
-
- 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
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/0605—Composition of the material to be processed
- B01J2203/061—Graphite
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
- B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
- B01J2219/0809—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes employing two or more electrodes
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
- B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
- B01J2219/0837—Details relating to the material of the electrodes
- B01J2219/0841—Metal
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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Abstract
When carbon powder is electrified to prepare graphene, the invention provides a vacuum reactor for preparing graphene, which consists of a vacuum cavity with an upper cover and a lower cover, a reaction tube in the vacuum cavity and two electrodes inserted into the reaction tube from the upper cover and the lower cover, so as to improve the vacuum-pumping efficiency and facilitate the automation of equipment. The reactor greatly reduces the volume of the vacuum cavity and improves the vacuum pumping efficiency; meanwhile, the feeding and discharging from the outside of the vacuum cavity are realized, and the automation of the equipment is convenient to realize.
Description
Technical Field
The invention belongs to the field of nano material preparation, and particularly relates to a vacuum reactor for preparing graphene by electrifying carbon powder.
Background
Graphene is a two-dimensional nano material composed of single-layer honeycomb-shaped carbon atoms, is the thinnest, lightest, strongest and hardest material, has excellent electric conduction and heat conduction performance, and is called as the king of materials. The current large-scale production of graphene is primarily a graphite redox process. In view of the problems of complex process technology, waste liquid treatment and the like, the production cost of the graphene is very high, the price of the graphene powder in the market is high, and the large-scale application of the graphene is limited.
WO2020/051000 (Flash Joule Heating Synthesis Method and Compositions theory) discloses a Method for preparing graphene by electric power through a Joule Heating Flash evaporation Method, wherein carbon powder such as carbon black, coke or anthracite is put in a quartz tube, large current is applied for less than 1 second, the temperature is as high as about 3000 ℃, and the carbon powder is instantly changed into graphene. For the estimation of the electric power cost, only 2 degrees of electricity are needed for producing 1 kg of graphene, and the electric power cost is as low as 1 yuan. As the temperature of the reactor rises by 10 times within 1 second, the gas in the tube also expands by 10 times rapidly, carbon powder is ejected out of the reactor along with the gas, and the reaction can not be carried out normally. Therefore, the electric flash evaporation method needs to place the quartz tube in a vacuum environment, and avoids the ejection of carbon powder by reducing the gas in the quartz tube.
However, when the whole reaction device is placed in a vacuum environment, the volume of the vacuum cavity is quite large, and the vacuumizing time is long and the efficiency is low. In addition, the reaction device is arranged in the vacuum chamber, so that the feeding and discharging of the quartz tube are very complicated, and the automation of the machine is not facilitated. Therefore, a small vacuum reactor which is convenient for feeding and discharging needs to be designed to meet the requirement of equipment automation.
Disclosure of Invention
The invention aims to provide a vacuum reactor for preparing graphene by electrifying carbon powder, which aims to reduce the size of a vacuum cavity and facilitate feeding and discharging when preparing graphene by electric flash evaporation.
In order to achieve the purpose, the invention adopts the technical scheme that:
a vacuum reactor for preparing graphene by electrifying carbon powder is a reactor which consists of a vacuum cavity with an upper cover and a lower cover, a reaction tube positioned between the upper cover and the lower cover and two electrodes respectively inserted into the reaction tube through the upper cover and the lower cover.
Furthermore, holes are formed in the upper cover and the lower cover of the vacuum cavity and are communicated with the reaction tube.
Further, the reaction tube is made of quartz, alumina ceramic, magnesia ceramic, boron nitride ceramic, Polytetrafluoroethylene (PTFE), polyparaphenylene (PPL), Polybenzimidazole (PBI), Polyetheretherketone (PEEK), Polyimide (PI), or Polyamideimide (PAI).
Furthermore, the tube wall of the reaction tube is provided with a vent hole, and the vacuum cavity and the inner cavity of the reaction tube are communicated at the upper electrode and the lower electrode.
Further, the electrode is copper, tungsten copper alloy, iron, stainless steel, or graphite.
Further, the electrode is provided with 1-5 sealing rings at the position of passing through the upper cover and the lower cover of the vacuum cavity.
The invention has the beneficial effects that: (1) the vacuum cavity of the vacuum reactor is only provided with one reaction tube, so that the volume can be greatly reduced, the vacuum reactor is easy to vacuumize, and the vacuum pumping efficiency is greatly improved. (2) The reaction tube of the vacuum reactor is directly communicated with the vacuum cavity, and can be directly fed and discharged to an external container from the outside, so that the automation of equipment is facilitated.
Drawings
FIG. 1 is a diagram of a vacuum reactor apparatus for preparing graphene by an electric flash method according to the present invention.
FIG. 2 is a scanning electron micrograph of graphene prepared according to the present invention.
Fig. 3 is a raman spectrum of graphene prepared according to the present invention.
Detailed Description
The invention is further described below with reference to the figures and examples.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the starting materials and materials used, if not specifically required, are commercially available. The power supply used was a 100 kilowatt dc power supply (maximum voltage 200V and maximum current 500A).
Example 1
As shown in fig. 1, the vacuum reactor for preparing graphene by electrifying carbon powder in this embodiment includes an insulating vacuum chamber, a quartz tube as a reaction tube, and two copper electrodes. The vacuum cavity is provided with an upper cover 1, a lower cover 2 and a cavity wall 3, and the upper cover is provided with a small vacuumizing hole 4. A quartz reaction tube 5 with the inner diameter of 8 mm is arranged in the vacuum cavity, and the upper part and the lower part of the reaction tube are respectively provided with a small hole 6 which is communicated with the vacuum cavity and the inner cavity of the reaction tube. Carbon powder 7 is placed in the middle of the reaction tube, and the upper and lower surfaces of the carbon powder are compressed by copper electrodes 8 and 9 with the diameter of 8 mm. In order to ensure the sealing of the vacuum chamber, two sealing rings 10 are used for sealing the electrode and the upper cover and the lower cover of the vacuum chamber, so as to ensure that air leakage cannot occur.
The use method of the vacuum reactor comprises the following steps: the lower electrode 9 was inserted below the reaction tube, 0.1 g of conductive carbon black was poured from above the reactor, and the upper electrode 8 was inserted from above and pressed, and the resistance was measured to be about 1 ohm. Then, a vacuum was drawn from the vacuum port 4 of the vacuum chamber to 0.1 atmosphere. A discharging circuit is connected, a power supply is switched on, the voltage is selected to be 200V, discharging is carried out for 200 milliseconds, and strong light is emitted from the quartz tube. Cutting off power supply, introducing gas into the vacuum cavity, withdrawing the lower electrode, pushing the reacted carbon powder out from the lower opening by the upper electrode, and grinding to obtain black powder. Scanning electron microscopy of these black powders (fig. 2) revealed that a lamellar structure had been produced. The black powders were examined by laser raman spectroscopy to obtain a raman spectrum (fig. 3), in which the G peak indicates the vibration of the graphite sheet, the D peak indicates the size and defect of the graphene sheet, and the 2D peak indicates the number of layers of the graphene. The black powder can be analyzed from a Raman spectrum, and is a graphene nano material with less than 5 layers.
Therefore, the vacuum reactor is not only small, but also can be externally fed and discharged, the operation is very convenient, and the automation of equipment is easy to realize.
Example 2
Using the vacuum reactor of example 1, reaction tubes were fabricated using alumina ceramic, magnesia ceramic, boron nitride ceramic, Polytetrafluoroethylene (PTFE), polyparaphenylene (PPL), Polybenzimidazole (PBI), Polyetheretherketone (PEEK), Polyimide (PI), or Polyamideimide (PAI), respectively, and the inner diameter and wall thickness thereof were the same as those of the quartz tube of example 1, and 0.1 g of conductive carbon black was charged into each of the fabricated reaction tubes to perform an electric flash evaporation reaction. The obtained black powder is tested to obtain a scanning electron micrograph and a Raman spectrogram, the two drawings are basically the same as the embodiment 1, and the prepared graphene material with less than 5 layers is shown.
Therefore, alumina ceramics, magnesia ceramics, boron nitride ceramics, Polytetrafluoroethylene (PTFE), polyparaphenylene (PPL), Polybenzimidazole (PBI), Polyetheretherketone (PEEK), Polyimide (PI), or Polyamideimide (PAI) can be used as materials for reaction tubes for preparing graphene by electric flash evaporation.
Example 3
In example 1, 5 types of vacuum reactors for electric flash preparation were fabricated by attaching 1, 2, 3, 4, and 5 seal rings to the contact portions between the electrodes and the upper and lower covers, respectively. 0.1 g of conductive carbon black was placed in each case. When the reactor is vacuumized, the vacuum degree of the 5 reactors can reach 0.1 atmospheric pressure normally, and the scanning electron microscope image and the Raman spectrum image of the black powder obtained by discharging are the same as or similar to those of the example 1. Therefore, the sealing methods can realize the preparation of graphene by electric flash evaporation and generate the graphene.
Example 4
The copper electrode in example 1 was changed to tungsten, tungsten-copper alloy, iron, stainless steel or graphite, and 5 vacuum reactors for preparing graphene by electrical flash evaporation were respectively fabricated. 0.1 g of conductive carbon black is put into the reactor each time, and the graphene is prepared by electrifying. The scanning electron micrograph and the raman spectrum of the obtained black powder were identical to those of example 1.
Therefore, the upper and lower electrodes may be made of copper, tungsten-copper alloy, iron, stainless steel, or graphite.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, or direct or indirect applications in other related fields, which are made by the contents of the present specification, are included in the scope of the present invention.
Claims (6)
1. A vacuum reactor for preparing graphene by electrifying carbon powder is characterized in that: it is a reactor which is composed of a vacuum cavity with an upper cover and a lower cover, a reaction tube positioned between the upper cover and the lower cover and two electrodes respectively inserted into the reaction tube through the upper cover and the lower cover.
2. The vacuum reactor for preparing graphene by electrifying carbon powder as claimed in claim 1, wherein: the upper cover and the lower cover of the vacuum cavity are provided with holes which are communicated with the reaction tube.
3. The vacuum reactor for preparing graphene by electrifying carbon powder as claimed in claim 1, wherein: the reaction tube is made of quartz, alumina ceramic, magnesia ceramic, boron nitride ceramic, Polytetrafluoroethylene (PTFE), polyparaphenylene (PPL), Polybenzimidazole (PBI), Polyetheretherketone (PEEK), Polyimide (PI) or polyamide-imide (PAI).
4. The vacuum reactor for preparing graphene by electrifying carbon powder as claimed in claim 1, wherein: the tube wall of the reaction tube is provided with a vent hole, and the upper electrode and the lower electrode are communicated with the vacuum cavity and the inner cavity of the reaction tube.
5. The vacuum reactor for preparing graphene by electrifying carbon powder as claimed in claim 1, wherein: the electrode is copper, tungsten copper alloy, iron, stainless steel or graphite.
6. The vacuum reactor for preparing graphene by electrifying carbon powder as claimed in claim 1, wherein: the electrode is provided with 1-5 sealing rings at the position of penetrating through the upper cover and the lower cover of the vacuum cavity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011321359.0A CN114522620A (en) | 2020-11-23 | 2020-11-23 | Vacuum reactor for preparing graphene by electrifying carbon powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011321359.0A CN114522620A (en) | 2020-11-23 | 2020-11-23 | Vacuum reactor for preparing graphene by electrifying carbon powder |
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| Publication Number | Publication Date |
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| CN114522620A true CN114522620A (en) | 2022-05-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011321359.0A Pending CN114522620A (en) | 2020-11-23 | 2020-11-23 | Vacuum reactor for preparing graphene by electrifying carbon powder |
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| Country | Link |
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| CN (1) | CN114522620A (en) |
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- 2020-11-23 CN CN202011321359.0A patent/CN114522620A/en active Pending
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Application publication date: 20220524 |