CN208964552U - A kind of normal pressure microwave plasma reduction removing graphene oxide device - Google Patents
A kind of normal pressure microwave plasma reduction removing graphene oxide device Download PDFInfo
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- CN208964552U CN208964552U CN201821114283.2U CN201821114283U CN208964552U CN 208964552 U CN208964552 U CN 208964552U CN 201821114283 U CN201821114283 U CN 201821114283U CN 208964552 U CN208964552 U CN 208964552U
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Abstract
The utility model discloses a kind of normal pressure microwave plasma reductions to remove graphene oxide device, including microwave excitation cavity, the top and bottom side of microwave excitation cavity is equipped with microwave source, microwave excitation is intracavitary to be equipped with boiler tube, the top of boiler tube is connect with the discharge port being located above microwave excitation cavity, ignition electrode is equipped in boiler tube, the bottom of boiler tube is connect with the expects pipe that is mixed into being located at below microwave excitation cavity, is mixed into expects pipe and is successively arranged feeding mechanism, reduction mixing gas source and ion excitation gas source.The utility model has the advantages that by opening microwave source, at this point, microwave establishes high-voltage electromagnetic field in microwave excitation cavity, puncture ion excitation gas, generate plasma, graphene oxide is by heating region, and removing is reduced to graphene rapidly, and process flow is simple, the chemical substance for needing to carry out subsequent environmental protection treatment is not added, speed is fast, and yield is high, and quality is good.
Description
Technical field
The utility model relates to oxidation-reduction methodes, and graphene powder field is made, it particularly relates to a kind of normal pressure microwave
Plasma reduction removes graphene oxide device.
Background technique
Graphene (Graphene) be one kind by carbon atom with sp2Hybridized orbit forms the two dimension that hexangle type is in honeycomb lattice
Carbon nanomaterial.Graphene has excellent optics, electricity, mechanical characteristic, in materialogy, micro-nano technology, the energy, biomedicine
It is with important application prospects with drug delivery etc., it is considered to be a kind of future revolutionary material.Graphene at this stage
Main production method have mechanical stripping method, oxidation-reduction method, SiC epitaxial growth method and chemical vapour deposition technique (CVD).
Oxidation-reduction method is by using the oxidants such as the chemical reagent such as sulfuric acid, nitric acid and potassium permanganate, hydrogen peroxide by day
Right graphite oxidation increases the spacing between graphite linings, is inserted into oxide between layers in graphite, and graphite oxide is made
(Graphite Oxide).Then reactant is washed, and low temperature drying is carried out to the solid after cleaning, oxidation stone is made
Ink powder body.Graphite oxide powder is removed by the methods of physics removing, high-temperature expansion, graphene oxide is made.Finally
Graphene oxide is restored by chemical method, obtains graphene (RGO).This method and process is mature, available single layer or few
Layer graphene.
At this stage after graphite oxide powder is made in oxidizing process, ultrasonic wave removing is carried out in hydrazine hydrate solution, obtains oxygen
Graphite alkene dispersion liquid is freeze-dried in freeze drier to prevent graphene oxide powder in drying process from reuniting；
The graphene oxide obtained after freeze-drying reduction in reduction furnace (general hydrogen furnace), removes oxygen-containing functional group, generates graphite
Alkene powder.Oxidizing process at this stage is made graphite oxide powder and still remains many puzzlements, such as: hydrazine hydrate have strong basicity and
Hygroscopicity, its energy attack glass, rubber, leather, cork etc., resolves into N2, NH3 and H2 at high temperature；Hydrazine hydrate solution has
Toxicity is harmful to the human body, and not environmentally, subsequent treatment cost is high；Ultrasonic wave splitting time is long, low efficiency；Peeling effect is poor, can reach
Content to single layer or few layer graphene is low；Graphene oxide solution after removing is easy to reunite in the drying process, to prevent
The reunion of graphene oxide powder, using freeze-drying, freeze-drying is so that solution is directly distilled dry under the conditions of cryogenic vacuum
Dry, drying cost is high, and drying time is long, low output, and the graphene oxide being freeze-dried contains a large amount of oxygen-containing functional group,
It need to be reacted through high temperature reduction, remove oxygen-containing functional group, typically now use high-temperature hydrogen reduction furnace, energy consumption height, anti-explosion safety etc.
Grade is high；Entirely long from graphite oxide powder to graphene process flow, control node is more, and graphene Manufacture quality control guarantees work
Make complicated.So that graphite oxide powder, which is made, in oxidizing process has certain limitation.
For the problems in the relevant technologies, currently no effective solution has been proposed.
Utility model content
The problems in view of the above technology, the purpose of this utility model is to propose a kind of normal pressure microwave plasma reduction removing
Graphene oxide device, to overcome above-mentioned technical problem present in existing the relevant technologies.
The technical solution of the utility model is achieved in that
A kind of normal pressure microwave plasma reduction removing graphene oxide device, including microwave excitation cavity, the microwave excitation
Microwave source is equipped with outside chamber, the microwave excitation is intracavitary equipped with boiler tube pipe, the top of the boiler tube and positioned at the microwave excitation
Discharge port connection above chamber, the boiler tube are interior equipped with ignition electrode, the bottom of the boiler tube and under the microwave excitation cavity
Side is mixed into expects pipe connection, and described be mixed into expects pipe is successively arranged feeding mechanism, reduction mixing gas source and ion excitation gas
Body gas source.
Further, the boiler tube is cavity structure, and material is high temperature resistant, microwave penetration ability strong quartz glass or pottery
Porcelain.
Further, the bottom of the ignition electrode is elongated sharp structure, is refractory metal material.
Further, the expects pipe that is mixed into is L-type.
The utility model has the beneficial effects that by opening microwave source, at this point, microwave establishes high-voltage electricity in microwave excitation cavity
Magnetic field, the igniting needle tip in boiler tube generate electric arc, open ion excitation gas source, ion excitation gas is passed through into quartz ampoule
Body, the ion excitation gas in boiler tube are broken down by high-voltage, and plasma is generated under the induction of electric arc, open reduction gaseous mixture
Source, feeding mechanism are continuously conveyed graphite oxide powder and are transported in boiler tube to expects pipe, mixed gas is mixed into, and graphite oxide is through micro-
Removing is reduced to graphene to wave plasma rapidly under the double action of microwave and plasma.Use microwave energy for plasma
Body excitation provides the energy, and high-voltage electromagnetic field is established in microwave excitation cavity, uses low breakdown voltage gas for plasma exciatiaon
Gas is warming up to graphite oxide flash degree Celsius in the high coupling of microwave field and the high temperature of plasma using graphite oxide
2000 or more, reduction reaction occurs with oxygen atom in oxygen-containing functional group in graphite oxide at high temperature, replaces the oxygen in functional group
Atom, after flash heating, the intercalator of reduction reaction and graphite oxide interlayer decomposes generated gas, and graphite oxide is exploded
For graphene film, reducing gas restores the protective gas in mixed gas as current-carrying gas, graphene film is prevented to go back in removing
Reunion during original forms Multi-layer graphite, in addition, the protective atmosphere as reduction reaction, reduces the content of reducing atmosphere, mention
Graphite oxide powder is directly reduced to graphene, work by normal pressure microwave plasma spy removing by the safety of high equipment, device
Skill process is simple, does not add the chemical substance for needing to carry out subsequent environmental protection treatment, and speed is fast, and yield is high, and quality is good.
Detailed description of the invention
In order to illustrate the embodiment of the utility model or the technical proposal in the existing technology more clearly, below will be to embodiment
Needed in attached drawing be briefly described, it should be apparent that, the accompanying drawings in the following description is only the utility model
Some embodiments for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other attached drawings.
Fig. 1 is to remove graphene oxide device according to a kind of normal pressure microwave plasma reduction of the utility model embodiment
Structural schematic diagram.
In figure:
1, microwave source；2, microwave excitation cavity；3, boiler tube；4, ignition electrode；5, discharge port；6, it is mixed into expects pipe；7, charger
Structure；8, reduction mixing gas source；9, ion excitation gas source.
Specific embodiment
The following will be combined with the drawings in the embodiments of the present invention, carries out the technical scheme in the embodiment of the utility model
Clearly and completely describe, it is clear that the described embodiments are only a part of the embodiments of the utility model, rather than whole
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art's every other embodiment obtained, all belongs to
In the range of the utility model protection.
Embodiment according to the present utility model provides a kind of normal pressure microwave plasma reduction removing graphene oxide dress
It sets.
As shown in Figure 1, removing graphene oxide according to a kind of normal pressure microwave plasma reduction of the utility model embodiment
Device, including microwave excitation cavity 2, the outer wall of microwave excitation cavity 2 are equipped with microwave source 1, are equipped with boiler tube 3, stone furnace in microwave excitation cavity 2
The top of pipe 3 is connect with the discharge port 5 for being located at 2 top of microwave excitation cavity, and ignition electrode 4, the bottom of quartz ampoule 3 are equipped in quartz ampoule 3
Portion is connect with the expects pipe 6 that is mixed into for being located at 2 lower section of microwave excitation cavity, and being mixed into expects pipe 6 is L-type, is successively arranged charger thereon
Structure 7, reduction mixing gas source 8 and ion excitation gas source 9.
In addition, in one embodiment, for above-mentioned boiler tube 3, boiler tube 3 is the sky of the strong material of high temperature resistant microwave penetration
Cavity configuration, such as quartz glass, ceramics.
In addition, in one embodiment, for above-mentioned ignition electrode 4, the bottom of ignition electrode 4 is elongated sharp structure,
Material is refractory metal.
To sum up, by means of the above-mentioned technical proposal of the utility model, by opening microwave source 1, at this point, microwave swashs in microwave
It encourages in chamber 2 and establishes high-voltage electromagnetic field, 4 tip of ignition electrode in quartz ampoule 3 generates electric arc, opens ion excitation gas source
9, ion excitation gas is passed through into boiler tube 3, the ion excitation gas in boiler tube pipe 3 is broken down by high-voltage, under the induction of electric arc
Plasma is generated, reduction mixing gas source 8 is opened, feeding mechanism 7 is continuously conveyed graphite oxide powder to expects pipe 6 is mixed into, is gone back
In former mixed gas delivery to boiler tube 3, graphite oxide is fast under the double action of microwave and plasma through microwave plasma
Speed removing is reduced to graphene.It uses microwave energy to provide the energy for plasma exciatiaon, high-voltage electricity is established in microwave excitation cavity
Magnetic field uses low breakdown voltage gas for plasma excitation gas, in the high coupling of microwave field and is waited using graphite oxide
The high temperature of gas ions makes graphite oxide flash be warming up to 2000 degrees Celsius or more, reducing gas at high temperature with contain in graphite oxide
Reduction reaction occurs for oxygen atom in oxygen functional group, replaces the oxygen atom in functional group, after flash heating, reduction reaction and oxidation stone
Intercalator between layer of ink decompose caused by gas, graphite oxide explode for graphene film, the protection in reduction mixed gas
Gas prevents reunion of the graphene film in removing reduction process, forms Multi-layer graphite, in addition, reduction is mixed as current-carrying gas
The protective atmosphere for closing gas, reduces the content of reducing atmosphere, improves the safety of equipment, device directly leads to graphite oxide powder
It crosses normal pressure microwave plasma spy removing and is reduced to graphene, process flow is simple, does not add and needs to carry out subsequent environmental protection treatment
Chemical substance, speed is fast, and yield is high, and quality is good.
The above is only the preferred embodiments of the present utility model only, is not intended to limit the utility model, all practical at this
Within novel spirit and principle, any modification, equivalent replacement, improvement and so on should be included in the guarantor of the utility model
Within the scope of shield.
Claims (5)
1. a kind of normal pressure microwave plasma reduction removes graphene oxide device, which is characterized in that including microwave excitation cavity (2),
The outside of the microwave excitation cavity (2) is equipped with microwave source (1), is equipped with boiler tube (3) in the microwave excitation cavity (2), the boiler tube
(3) top is connect with the discharge port (5) being located above the microwave excitation cavity (2), and ignition electrode is equipped in the boiler tube (3)
(4), the bottom of the boiler tube (3) is connect with the expects pipe (6) that is mixed into being located at below the microwave excitation cavity (2), the mixing
Feeding mechanism (7), reduction mixing gas source (8) and ion excitation gas source (9) are successively arranged on feed pipe (6).
2. a kind of normal pressure microwave plasma reduction according to claim 1 removes graphene oxide device, which is characterized in that
The boiler tube (3) is cavity structure, and material is the strong material of microwave penetration resistant to high temperature.
3. a kind of normal pressure microwave plasma reduction according to claim 1 removes graphene oxide device, which is characterized in that
The bottom of the ignition electrode (4) is elongate tip shape structure, and material is refractory metal material.
4. a kind of normal pressure microwave plasma reduction according to claim 1 removes graphene oxide device, which is characterized in that
Stable plasma is quickly established easily by electromagnetism field breakdown in the present apparatus using ion excitation gas.
5. normal pressure microwave plasma reduction according to claim 1-4 removes graphene oxide device, feature
It is, described be mixed into expects pipe (6) are L-type.
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| CN201821114283.2U CN208964552U (en) | 2018-07-14 | 2018-07-14 | A kind of normal pressure microwave plasma reduction removing graphene oxide device |
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| CN201821114283.2U CN208964552U (en) | 2018-07-14 | 2018-07-14 | A kind of normal pressure microwave plasma reduction removing graphene oxide device |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453719A (en) * | 2020-04-24 | 2020-07-28 | 湖北航天化学技术研究所 | High-quality graphene and preparation method thereof |
| CN113727508A (en) * | 2020-05-26 | 2021-11-30 | 上海大学 | Novel vacuum microwave plasma ion source |
| CN114031071A (en) * | 2021-09-28 | 2022-02-11 | 云南华谱量子材料有限公司 | Method and equipment for preparing graphene by microwave excitation catalysis self-propagating |
| CN115196621A (en) * | 2021-09-28 | 2022-10-18 | 云南华谱量子材料有限公司 | Method and device for preparing graphene by catalyst-assisted microwave excitation metal discharge |
-
2018
- 2018-07-14 CN CN201821114283.2U patent/CN208964552U/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453719A (en) * | 2020-04-24 | 2020-07-28 | 湖北航天化学技术研究所 | High-quality graphene and preparation method thereof |
| CN111453719B (en) * | 2020-04-24 | 2022-05-24 | 湖北航天化学技术研究所 | High-quality graphene and preparation method thereof |
| CN113727508A (en) * | 2020-05-26 | 2021-11-30 | 上海大学 | Novel vacuum microwave plasma ion source |
| CN114031071A (en) * | 2021-09-28 | 2022-02-11 | 云南华谱量子材料有限公司 | Method and equipment for preparing graphene by microwave excitation catalysis self-propagating |
| CN115196621A (en) * | 2021-09-28 | 2022-10-18 | 云南华谱量子材料有限公司 | Method and device for preparing graphene by catalyst-assisted microwave excitation metal discharge |
| CN115196621B (en) * | 2021-09-28 | 2023-09-19 | 云南华谱量子材料有限公司 | Method and device for preparing graphene by catalyst-assisted microwave excitation metal discharge |
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