CN112010292B - Preparation method and application of graphene material - Google Patents
Preparation method and application of graphene material Download PDFInfo
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- CN112010292B CN112010292B CN202010941283.5A CN202010941283A CN112010292B CN 112010292 B CN112010292 B CN 112010292B CN 202010941283 A CN202010941283 A CN 202010941283A CN 112010292 B CN112010292 B CN 112010292B
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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
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
- B01D39/2055—Carbonaceous material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
- B01D46/0028—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions provided with antibacterial or antifungal means
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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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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- 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
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The embodiment of the invention discloses a preparation method and application of a graphene material. The preparation method of the graphene material comprises the following steps: heating the reaction space to 3500-3800K by electric arc under the protective gas environment; introducing reaction gas into the reaction space, wherein the reaction gas comprises acetylene and/or methane; obtaining the graphene material with 2-5 layers. According to the embodiment of the invention, the high-quality graphene material is prepared by using the low-cost methane or acetylene as the reaction gas, the preparation process is simple, the production cost is low, and the method is suitable for large-scale production.
Description
Technical Field
The invention relates to the field of graphene, in particular to a preparation method and application of a graphene material.
Background
Graphene is a polymer made of carbon atoms in sp2The hexagonal honeycomb-lattice two-dimensional carbon nanomaterial composed of the hybrid tracks has excellent optical, electrical and mechanical properties, and has important development prospects in the fields of air purification, water purification, medical treatment and clothing.
Graphene has been considered as a hypothetical structure and cannot exist stably in nature alone. Until 2004, professor anderlich heim and professor comasten norworth schooff of manchester university, uk, finally peeled off the graphene from the graphite sheet by adhering both sides of the graphite sheet to a special adhesive tape, tearing the tape to divide the graphite sheet into two parts, and so forth. Thus, they also honor the 2010 nobel prize in physics.
Although graphene is confirmed to exist in nature, it is generally present in the form of graphite, and it is difficult to exfoliate a single-layer structure. The existing graphene preparation methods include a mechanical stripping method, a redox method, a SiC epitaxial growth method and a chemical vapor deposition method. The main industrial application is a redox method, which is to oxidize natural graphite by using chemical reagents such as sulfuric acid and nitric acid and oxidants such as potassium permanganate and hydrogen peroxide to prepare graphene oxide, and then reduce the graphene oxide by a chemical method to finally prepare graphene. The method is simple to operate and high in yield, but the quality of the prepared graphene is difficult to control, and strong acids such as sulfuric acid and nitric acid have great danger.
Disclosure of Invention
Therefore, the embodiment of the invention provides a preparation method of a graphene material and an application of the graphene material; the graphene material with 2-5 layers and high quality is prepared by taking methane or acetylene with low cost as reaction gas.
The preparation method of the graphene material provided by the embodiment of the invention comprises the following steps: heating the reaction space to 3500-3800K by electric arc under the protective gas environment; introducing reaction gas into the reaction space, wherein the reaction gas comprises acetylene and/or methane; obtaining the graphene material with 2-5 layers.
In one embodiment of the present invention, heating the reaction space to 3500-: the reaction space is in a magnetic field environment; introducing 70-130A of current into the reaction space to generate a plasma arc; the plasma arc heated the reaction space to 3500-.
Preferably, the protective gas is an inert gas; the preparation method further comprises the following steps: the inert gas is used to maintain the pressure of the reaction space between 1.2MP and 1.5 MP.
Preferably, the temperature of the protective gas atmosphere is maintained at 50-70 ℃.
On the other hand, an embodiment of the present invention provides a graphene material, which is the graphene material obtained by the graphene preparation method according to any one of the embodiments.
Further, the graphene material can be applied to the field of air purification.
Further, the graphene material can be applied to the field of water purification.
Further, the graphene material can be applied to the medical field.
Further, the graphene material can be applied to the field of clothing.
In summary, the above embodiments of the present application may have one or more of the following advantages or benefits: i) the high-quality graphene material is prepared by taking low-cost methane or acetylene as a reaction gas, and the preparation process is simple, the production cost is low, and the method is suitable for large-scale production; ii) the graphene material prepared by the method has strong bacteriostasis, and the bacteriostasis rate of the air purification filter core prepared by the graphene material is as high as 99%.
Drawings
Fig. 1 is a flowchart of a preparation method of a graphene material provided by the present invention.
Fig. 2 is a photograph of the complete graphene crystal phase prepared according to the first embodiment of the present invention.
Fig. 3 is a photomicrograph of an edge portion of the graphene material prepared according to the first embodiment of the invention.
Fig. 4 is a two-dimensional structure of graphene obtained by the first embodiment of the present invention, which is enlarged by 5 ten thousand times.
Fig. 5 is a sample to be inspected of the air purifier filter element made of the graphene material according to the first embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the preparation method of the graphene material provided by the invention comprises the following steps:
1) heating the reaction space to 3500-3800K by electric arc under the protective gas environment;
2) introducing reaction gas into the reaction space, wherein the reaction gas comprises acetylene and/or methane;
3) obtaining the graphene material with 2-5 layers.
The invention firstly introduces protective gas into the reaction space, and then heats the reaction space to a certain temperature by electric arc. The protective gas is introduced to extrude all air out of the reaction space, so that the reaction of the reaction gas and oxygen in the air under the conditions of high temperature and high pressure is avoided; on one hand, the phenomenon of combustion and even explosion generated in the reaction space in the preparation process is prevented, and accidents are prevented; on the one hand, the pressure in the reaction space can be controlled, so that the reaction can be carried out more thoroughly. Preferably, the protective gas is an inert gas. For example, the shielding gas may be helium or argon, which is not limited herein.
Wherein the decomposition reaction of the gaseous carbon source is a reversible reaction, and the conversion rate of the reaction gas is between 90 and 95 percent. Wherein the conversion of the reaction gas increases with an increase in the reaction temperature; at the same temperature, the higher the pressure, the lower the conversion. In order to make the decomposition reaction proceed as forward as possible and prepare more graphene materials, preferably, the pressure of the reaction space is 1.2MP-1.5, specifically 1.2MP, 1.3MP, 1.4MP, 1.5 MP; the reaction temperature is 3500K-3800K, specifically 3500K, 3600K, 3700K and 3800K.
Further, the pressure in the reaction space is controlled by a protective gas, and meanwhile, in order to improve the safety of the experiment, the temperature of the protective gas is controlled to be 50-70 ℃, specifically 50 ℃, 55 ℃, 60 ℃, 65 ℃ and 70 ℃.
Wherein heating the reaction space to 3500-3800K under the protective gas environment comprises: the reaction space is in a magnetic field environment; the plasma arc is generated by the current introduced into the reaction space, and the magnitude of the introduced current is preferably 70-130A, and specifically 70A, 80A, 90A, 100A, 110A, 120A and 130A.
Under the protective gas environment, the reaction space is heated to 3500K-3800K by electric arc, and then reaction gas is introduced into the reaction space. The reaction gas is a gaseous carbon source, and preferably, the reaction gas is acetylene and/or methane. Wherein, common civil liquefied natural gas is subjected to sulfur removal and purification, and methane with purity of 99% can be obtained. The preparation cost is low, the preparation process is simple, and the method is suitable for large-scale industrial production.
And finally, obtaining the graphene material with 2-5 layers. A detection report (report number: LHKJ-2008-23-1/1) of an antibacterial material detection center of the institute of physical and chemical technology of Chinese academy of sciences indicates that the antibacterial rate of the air purifier filter element made of the graphene material to detection bacteria can reach 99% and far exceeds a standard requirement value.
[ first embodiment ] A method for manufacturing a semiconductor device
Setting the reaction space to be a magnetic field environment; introducing argon to make the pressure of the reaction space be 1.2 MP; a current of 70A is introduced, and the reaction space is heated to 3500K by an electric arc; after the target temperature was reached, methane gas having a low amount of impurities and a purity of 99% was passed into the reaction space. To improve the safety of the experiment, the temperature of the argon gas is controlled between 50 and 70 ℃. Wherein the input amount of methane is 100 g; the yield of the graphene material was 67.50 g; at the same time, 22.50g of hydrogen were discharged.
[ second embodiment ] A
Setting the reaction space to be a magnetic field environment; introducing argon to make the pressure of the reaction space be 1.2 MP; the reaction space was heated to 3700K with an electric arc by passing a current of 110A; after the target temperature was reached, methane gas having a low amount of impurities and a purity of 99% was passed into the reaction space. In order to improve the safety of the experiment, the temperature of the argon gas is controlled between 50 ℃ and 70 ℃. Wherein the input amount of methane is 100 g; the yield of the graphene material was 70.50 g; at the same time, 23.50g of hydrogen was discharged.
[ third embodiment ]
Setting the reaction space to be a magnetic field environment; introducing helium to make the pressure of the reaction space be 1.2 MP; the reaction space is heated to 3800K by electric arc after the current of 130A is introduced; after the target temperature has been reached, methane gas having a low content of impurities and a purity of 99% is passed into the reaction space. In order to improve the safety of the experiment, the temperature of helium gas is controlled between 50 and 70 ℃. Wherein the input amount of methane is 100 g; the yield of the graphene material was 71.25 g; at the same time, 23.75g of hydrogen was discharged.
[ fourth example ] A
Setting the reaction space to be a magnetic field environment; introducing helium to make the pressure of the reaction space be 1.4 MP; the reaction space is heated to 3800K by electric arc after the current of 130A is introduced; after the target temperature was reached, acetylene gas having a small amount of impurities and a purity of 99% was introduced into the reaction space. In order to improve the safety of the experiment, the temperature of helium gas is controlled between 50 and 70 ℃. Wherein the input amount of methane is 100 g; the yield of the graphene material was 69.75 g; at the same time, 23.25g of hydrogen was discharged.
[ fifth embodiment ]
Setting the reaction space to be a magnetic field environment; introducing argon to make the pressure of the reaction space be 1.5 MP; introducing 80A current, and heating the reaction space to 3600K by using an electric arc; after the target temperature was reached, acetylene gas having a small amount of impurities and a purity of 99% was introduced into the reaction space. To improve the safety of the experiment, the temperature of the argon gas is controlled between 50 and 70 ℃. Wherein the input amount of acetylene is 100 g; the yield of graphene material was 84.92 g; at the same time, 7.08g of hydrogen were discharged.
[ sixth embodiment ]
Setting the reaction space to be a magnetic field environment; introducing argon to make the pressure of the reaction space be 1.5 MP; introducing 80A current, and heating the reaction space to 3600K by using an electric arc; after the target temperature was reached, a mixed gas of methane and acetylene having a small amount of impurities and a purity of 99% was introduced into the reaction space. In order to improve the safety of the experiment, the temperature of the argon gas is controlled between 50 ℃ and 70 ℃. Wherein the input amount of the mixed gas of methane and acetylene is 100 g; the yield of graphene material was 76.12 g; at the same time, 14.88g of hydrogen was discharged.
The experimental data of examples 1 to 6 are collated to give the following table:
| temperature (K) | Pressure intensity (MP) | Reaction gas input (g) | Graphene yield (g) | Hydrogen yield (g) |
| 3500 | 1.2 | CH4100 | 67.50 | 22.50 |
| 3700 | 1.2 | CH4 100 | 70.50 | 23.50 |
| 3800 | 1.2 | CH4 100 | 71.25 | 23.75 |
| 3800 | 1.4 | CH4 100 | 69.75 | 23.25 |
| 3700 | 1.5 | C2H2 100 | 84.92 | 7.08 |
| 3600 | 1.3 | CH450；C2H250 | 76.12 | 14.88 |
As can be seen from the above table, the yield of graphene increases with the increase of the reaction temperature; when the temperature is constant, the higher the reaction pressure is, the lower the yield of the graphene is; and the conversion rate of the reaction gas is as high as 90% -95%, so that the preparation method of the graphene material can greatly improve the yield of the graphene material, and the reaction gas can adopt methane gas and/or acetylene gas with lower cost, so that the production cost of the graphene is reduced.
Next, the 2-5 layers of graphene materials prepared in the first example were tested for their bacteriostatic properties. Observing the physical form of the graphene material through a microscope to obtain an electron microscope image shown in fig. 2-4. Specifically, as can be seen from fig. 2, in an enlarged view at a 2 nm level, the material prepared by the first embodiment is a graphene material having a honeycomb structure; as can be seen from fig. 3, in the enlarged view of the 10-20 nm scale, the edge of the graphene material is like a sharp knife; as can be seen from fig. 4, in an enlarged view of 5 ten thousand times, the graphene material has an irregular two-dimensional structure, and sharp points are distributed around the graphene material.
On one hand, the graphene material can be sterilized by means of mechanical cutting. The graphene material is a nano-scale material, the bacteria are in a micron scale, the viruses are in a 100-nano scale, and the volume of the graphene material is far smaller than that of the bacteria and the viruses, so that the graphene material is just like a sharp knife and can directly cut the bacteria and the viruses. Specifically, the sharp physical edge of the graphene material can cut the surfaces of bacteria and viruses, destroy the cell walls of the bacteria and the membrane structures of the viruses, and enable intracellular substances of the bacteria and the viruses to flow out and cause metabolic imbalance of the bacteria and the viruses, so that the bacteria and the viruses die, and the effect of physical disinfection and sterilization is achieved.
On the other hand, when bacteria contact with the graphene material, the surface defects and sharp edge structures of the graphene material can induce the bacteria to generate active oxygen components, and disturb the normal physiological metabolism of the bacteria, so that the bacteria die, and the physical disinfection and sterilization effects are achieved.
On the other hand, the graphene has a large specific surface area, and the specific surface area of 2-5 layers of graphene can reach more than 500M2/G through determination, so that the graphene can be used for killing viruses and bacteria in a mechanical wrapping mode when bacterial viruses pass. The graphene material can wrap bacteria, so that the bacteria are isolated from surrounding media, and the bacteria can die due to the fact that the bacteria cannot absorb nutrition from the outside, so that growth and proliferation of the bacteria are blocked, and the effect of physical disinfection and sterilization is achieved.
The sample material shown in fig. 5 was sent to the antibacterial material detection center of the institute of physical and chemical technology of academy of sciences of china for the detection of the bacteriostatic rate. Wherein, the sample material is the air purifier filter element made of the graphene material prepared in example 1, and the control sample is PBS. The detection item is the bacteriostasis rate. According to the standard, the samples to be tested are cut into 5mm square and 0.75 g/bottle is weighed. The detection basis is GB/T20944.3-2008 evaluation of antibacterial performance of textiles in part 3: an oscillation method. The strains of the bacteria for detection are Escherichia coli (Escherichia coli) ATCC 25922, Staphylococcus aureus (Staphylococcus aureus) ATCC 6538, and Candida albicans (Candida albicans) ATCC 10231.
Specific detection data of the detection report are as follows:
wherein, the concentration of the initial inoculation bacterial liquid is respectively as follows: escherichia coli 3.3X 105CFU/ml, Staphylococcus aureus 3.5X 105CFU/ml, Candida albicans 2.8X 105CFU/ml; after the sample to be detected and the inoculated bacterial liquid are mixed for 18 hours, the average value of the number of bacteria is respectively as follows: escherichia coli<1.0CFU/ml, Staphylococcus aureus<1.0CFU/ml, 3.5X 10 Candida albicans3CFU/ml. The detection data shows that the samples are subjected to colibacillus, staphylococcus aureus and candida albicansThe bacteriostasis rate of the pearl bacteria is more than 99 percent, and the pearl bacteria has good bacteriostasis performance.
The detection results are as follows:
the detection result shows that the bacteriostasis rates of the samples to be detected on escherichia coli, staphylococcus aureus and candida albicans are all more than 99 percent and far exceed 60 percent and 70 percent of the standard requirement value. From this, it can be confirmed that the graphene prepared in example 1 has a strong bacteriostatic effect.
Further, the 2-5 layers of graphene materials can be applied to the field of air purification. For example, the 2-5 layers of graphene materials can be made into an air purifier filter element, when the air purifier works, indoor air is sucked through the air inlet, the air purifier filter element can kill bacteria or viruses in the air, and after purification is completed, the purified air is discharged from the air purifier, so that the functions of virus killing and sterilization are achieved. Of course, the air purifier filter element can also be used on air conditioners, vehicle-mounted air conditioners and other equipment.
Further, the strong physical antibacterial performance of the 2-5 layers of graphene materials can also be applied to the field of water purification. For example, the 2-5 layers of graphene materials can be used as water purification filter elements of water dispensers and water purifiers, and the water purification filter elements with the graphene materials can purify water.
Furthermore, the strong physical antibacterial performance of the graphene material with 2-5 layers can also be applied to the fields of medical treatment and clothing. For example, medical instruments such as medical masks and medical protective clothing can be made of medical cloth made of the graphene material; the common cloth made of the graphene can be made into clothing articles such as underwear, socks, bedding and the like.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (1)
1. A preparation method of a graphene material is characterized by comprising the following steps:
heating the reaction space to 3500-3800K by electric arc under the protective gas environment;
introducing reaction gas into the reaction space, wherein the reaction gas comprises acetylene and/or methane;
obtaining 2-5 layers of graphene materials; heating the reaction space to 3500-3800K under the protective gas environment, comprising:
the reaction space is in a magnetic field environment;
introducing 70-130A of current into the reaction space to generate a plasma arc;
the plasma arc heats the reaction space to 3500-3800K; the protective gas is inert gas; the preparation method further comprises the following steps:
maintaining the pressure of the reaction space between 1.2MP and 1.5MP using the inert gas; the preparation method further comprises the following steps:
the temperature of the protective gas environment is maintained at 50-70 ℃.
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