CN112724710A - Plasma graphene powder surface modification process - Google Patents
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- CN112724710A CN112724710A CN202110057566.8A CN202110057566A CN112724710A CN 112724710 A CN112724710 A CN 112724710A CN 202110057566 A CN202110057566 A CN 202110057566A CN 112724710 A CN112724710 A CN 112724710A
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
Abstract
The invention discloses a plasma graphene powder surface modification process, which comprises the following steps: s1: weighing graphene powder, placing the graphene powder in a reaction chamber of equipment, starting the equipment, and vacuumizing a reactor; s2: rotating the reactor, and heating and baking the graphene powder; s3, introducing reaction gas into the reaction chamber, carrying out plasma treatment, and modifying the graphene powder; s4: the modified graphene powder is annealed, and the surface of the graphene powder is modified, so that the conductivity, the dispersibility, the stability and the compatibility of the obtained graphene powder are improved.
Description
Technical Field
The invention relates to the field of graphene, in particular to a plasma graphene powder surface modification process.
Background
The fourth state of the plasma, i.e., the substance, is an ionized gaseous substance composed of atoms from which some electrons have been deprived and positive and negative electrons generated by ionization of the atoms. The ionized gas is composed of atoms, molecules, atomic groups, ions and electrons. The surface modification agent is acted on the surface of an object to realize ultra-clean cleaning, surface activation, etching, finishing and plasma surface coating of the object, thereby achieving the effect of surface modification. The principle of specifically realizing object treatment is different according to different elements and components in the plasma, and diversification of object treatment is realized by the difference of input gas and control power. Because the intensity of low-temperature plasma on the surface of an object is small, the protection effect on the surface of the object to be processed can be realized, and low-temperature plasma is mostly used in application. And the effects exhibited by the various particles in the treatment of the object are also different,
the method comprises the following steps of performing low-temperature plasma surface treatment, wherein the surface of a material is subjected to various physical and chemical changes, or is etched to be rough, or a compact cross-linking layer is formed, or an oxygen-containing polar group is introduced, so that the hydrophilicity, the cohesiveness, the dyeability, the biocompatibility and the electrical property are respectively improved, especially the improvement on the graphene conductivity is incomparable to other methods. The wet process is complex in process, mostly requires high baking temperature, is difficult to ensure uniform and firm coating, and has great influence on the environment. CVD, PVD, etc. are difficult to mass produce due to equipment, materials, throughput, and consistency limitations.
Disclosure of Invention
Aiming at the defects in the technology, the invention provides the plasma graphene surface modification process, which improves the conductivity, the dispersibility, the stability and the compatibility of the obtained graphene powder by modifying the surface of the graphene powder.
In order to achieve the purpose, the invention provides a plasma graphene powder surface modification process, which comprises the following steps:
s1: weighing graphene powder, placing the graphene powder in a reaction chamber of equipment, starting the equipment, and vacuumizing a reactor;
s2: rotating the reactor, and heating and baking the graphene powder;
s3, introducing reaction gas into the reaction chamber, carrying out plasma treatment, and modifying the graphene powder;
s4: and carrying out annealing treatment on the modified graphene powder.
Preferably, in step S1, the powder is placed in a reaction chamber of the apparatus, and the ratio of the total volume of the powder to the volume of the reaction chamber is not more than 1: 10, the reaction chamber adopts a cylindrical horizontal design, and a channel for gas circulation is arranged on the side wall of the reaction type.
Preferably, the graphene powder is single-layer graphene, double-layer graphene or a mixture thereof.
Preferably, in step S2, the reaction chamber is rotated to rotate the graphene powder, and the temperature is raised to heat and bake the graphene powder, wherein the heating temperature is controlled to be 50-80 ℃.
Preferably, in step S3, different gases are introduced into the reaction chamber according to requirements, the introduced gases are introduced continuously, and the plasma device in the reaction chamber is turned on to modify the graphene powder.
Preferably, in step S3, when the gas is filled into the reaction chamber, the rare gas and the reaction gas are mixed and filled, and the volume ratio of the rare gas to the reaction gas is 1: (2-4), and before the reaction gas is filled, oxygen and hydrogen are filled in advance.
Preferably, in step S3, the plasma source in the plasma device is: a dielectric barrier discharge plasma source, a surface discharge plasma source, a bulk discharge plasma source, a sliding arc plasma torch, a cold plasma torch, a direct current plasma source, a pulsed plasma source, a magnetron plasma source, an inductively coupled plasma source, a helical tube plasma source, a helical resonator plasma source, a microwave plasma source, an atmospheric pressure plasma jet source, a corona discharge plasma source, a microplasma source, a low pressure plasma source, or a high pressure plasma source.
Preferably, the gas to be charged is one or a mixture of more of hydrogen, oxygen, nitrogen, argon, SF6, NH3 and SO 2.
Preferably, in step S4, a vacuum tube furnace is used for annealing, the annealing temperature is controlled at 300-500 ℃, the annealing time is 15-20 minutes, and the vacuum degree of the vacuum tube furnace is maintained at 0.1-0.5 Pa;
the invention has the beneficial effects that: compared with the existing method for modifying graphene, the plasma graphene powder surface improvement process provided by the invention has the following advantages:
1. the environmental protection technology comprises the following steps: the plasma reaction process is a gas-solid phase dry reaction, so that water resources are not consumed, and chemical agents are not required to be added;
2. the efficiency is high: the whole process can be completed in a short time;
3. the cost is low: the device is simple, easy to operate and maintain, a small amount of gas replaces expensive cleaning solution, and meanwhile, no waste liquid is treated;
4. the treatment is more precise: can penetrate into the inside of the micropores and the pits and complete the cleaning or activating task.
Drawings
FIG. 1 is a flow chart of the steps of the present invention.
Detailed Description
In order to more clearly describe the present invention, the present invention will be further described with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, 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 some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. 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 present invention discloses a plasma graphene powder surface modification process, which includes the following steps:
s1: weighing graphene powder, placing the graphene powder in a reaction chamber of equipment, starting the equipment, and vacuumizing a reactor;
s2: rotating the reactor, and heating and baking the graphene powder;
s3, introducing reaction gas into the reaction chamber, carrying out plasma treatment, and modifying the graphene powder;
s4: and carrying out annealing treatment on the modified graphene powder.
In order to achieve the above object, in step S1, the powder is placed in a reaction chamber of the apparatus, and the ratio of the total volume of the powder to the volume of the reaction chamber is not more than 1: 10, the reaction chamber adopts a cylindrical horizontal design, a channel for gas circulation is formed in the side wall of the reaction chamber, and the graphene powder is single-layer graphene, double-layer graphene or a mixture of the single-layer graphene and the double-layer graphene. In a specific embodiment, firstly, graphene powder is placed in a reaction chamber, micropores are formed in the side wall of the reaction chamber, and the size of each micropore is smaller than that of the graphene powder, so that the graphene powder can be effectively ensured to be located in the reaction chamber without leakage, the amount of the graphene powder placed in the reaction chamber cannot be too large, if the amount of the graphene powder is too large, modification treatment cannot be performed on all surfaces of the graphene powder in a subsequent process, treatment is not comprehensive, and therefore the whole modification process is influenced.
In step S2, the reaction chamber is rotated to rotate the graphene powder, and the graphene powder is heated and baked at 50-80 ℃. In this embodiment, rotate the reacting chamber to drive graphite alkene powder and rotate together, carrying out the processing procedure like this, can both carry out the thermal treatment to all faces of graphite alkene powder, evaporate the moisture content in the graphite alkene powder, thereby avoid the influence that moisture content caused in the modification process, carrying out the drying process in, the temperature of heating chooses for use 70 degrees centigrade best.
In step S3, different gases are introduced into the reaction chamber as required, the introduced gases are introduced uninterruptedly, and the plasma device in the reaction chamber is turned on to modify the graphene powder, in step S3, when the gases are introduced into the reaction chamber, the gases are mixed with the reaction gases to be introduced, and the volume ratio of the rare gases to the reaction gases is 1: (2-4), before the reaction gas is filled, oxygen and hydrogen are filled in advance, and the plasma source in the plasma device is as follows: a dielectric barrier discharge plasma source, a surface discharge plasma source, a bulk discharge plasma source, a sliding arc plasma torch, a cold plasma torch, a direct current plasma source, a pulsed plasma source, a magnetron plasma source, an inductively coupled plasma source, a helical tube plasma source, a helical resonator plasma source, a microwave plasma source, an atmospheric pressure plasma jet source, a corona discharge plasma source, a microplasma source, a low pressure plasma source, or a high pressure plasma source; the gas filled is one or more of hydrogen, oxygen, nitrogen, argon, SF6, NH3 and SO 2. In this embodiment, after the gas is introduced, the gas drives the graphene powder to move together and act on the surface of the graphene powder, and more specifically, under the driving of a plasma device, oxygen is introduced first to remove organic matters on the surface of the graphene powder, and hydrogen is introduced for a period of time to remove oxides on the surface of the graphene powder and oxygen remaining in a reaction chamber (the remaining oxygen and the introduced hydrogen are changed into oxygen ions and hydrogen ions under the action of the plasma device and combined together to produce water molecules, and the whole device is in a heating state, so that the produced water molecules are discharged from micropores on the side wall of the reaction chamber, thereby ensuring that the graphene powder is not interfered by moisture in the heating process, and ensuring that the surface modification of the graphene powder in the subsequent process is not interfered by oxygen; then filling corresponding gas into the reaction chamber according to modification requirements, for example, when functional groups in NH3 need to be introduced to the surface of graphene powder, performing volume ratio of NH3 to nitrogen and argon to be 2.5: 0.5:0.5, mixing, then putting into a reaction chamber, fixing NH3 on the surface of graphene powder under the drive of a plasma device, and arranging a rare gas to mix with an introduced gas, so that on one hand, the rare gas is used for protecting the modification process to ensure the stability and uniformity of plasma in the discharge process, and on the other hand, the mixture can also be used for other purposes, for example, nitrogen can be converted into two free nitrogen atoms under the drive of the plasma device to be matched with NH3 so as to modify the graphene powder; the argon can remove residues on the surface of the graphene powder on a plasma platform; in a specific working process, gas continuously acts on graphene powder to drive the graphene powder to continuously rotate in a reaction chamber, so that all surfaces of the graphene powder can collide with the gas treated by a plasma device, the graphene powder is modified, the gas containing any carbon source is not particularly adopted, and the graphene powder is bonded and adsorbed together under the action of the carbon element to cause the growth of the graphene if the element containing the carbon element is adopted; although the conductivity will be further enhanced, it does not meet the actual use requirements; in addition, the plasma device works with the power of 100-160w, if the power is lower than 100w, the diameter of the ions is large, so that the ions continuously bombard the surface of the graphene powder to damage the surface of the graphene powder, and if the power is higher than 160w, the density of the ions is low, so that the ions cannot act on the surface of the graphene powder, and the graphene powder is modified.
In step S4, a vacuum tube furnace is used for annealing, the annealing temperature is controlled at 300-500 ℃ for 15-20 minutes, and the vacuum degree of the vacuum tube furnace is maintained at 0.1-0.5 Pa. In this embodiment, if annealing is not performed, the degree of lattice defects is large after the graphene powder is modified, so that the overall strength is reduced, and thus annealing is particularly performed, so that carbon atoms in the graphene powder are rearranged, gaps are filled, and lattice errors are repaired, so that the graphene hexagonal primitive cells are restored to the original structure; meanwhile, microscopic measurement shows that after annealing treatment, the size of the graphene powder is increased from 60nm to 109.35nm, so that the crystal size of the graphene powder is increased, and the conductivity is further improved, and further shows that when a sample is annealed at 300 ℃, the particle size is increased, the particle size is further increased along with the further increase of the annealing temperature, when the annealing temperature reaches 500 ℃, the surface of the graphene powder is covered by large-size particles, and the covered particles, such as amino groups, have weaker conductivity, so that the conductivity of the whole crystal is reduced, and the stability is reduced, so that 400 ℃ is selected as the optimal annealing temperature, and the size of the whole graphene powder is increased while the conductivity is ensured.
The invention is illustrated below by means of specific examples:
the first embodiment is as follows:
according to the volume ratio of the graphene powder to the reaction chamber of 1: 5 add corresponding graphite alkene powder in the reacting chamber, close the hatch door of reacting chamber, carry out vacuum heat treatment, after heating 20 minutes with the temperature of 60 degrees centigrade, treat the drying back, open plasma device, work with 150W's power, at first let in oxygen, let in 5 minutes after the rethread hydrogen is handled graphite alkene powder surface, carry out the volume ratio with NH3 and nitrogen gas and argon gas after 5 minutes and be 2.5: and (3) mixing 0.5:0.5, introducing the mixture into a reaction chamber for reaction, closing a plasma device after 10 minutes, transferring the graphene powder into a vacuum tube furnace for annealing treatment, annealing at the temperature of 400 ℃ for 15 minutes, keeping the vacuum degree of the vacuum tube furnace at 0.1Pa, and obtaining the modified graphene plasma powder after the treatment is finished.
Example two:
according to the volume ratio of the graphene powder to the reaction chamber of 1: 5 add corresponding graphite alkene powder in the reacting chamber, close the hatch door of reacting chamber, carry out vacuum heat treatment, after heating 20 minutes with the temperature of 60 degrees centigrade, treat the drying back, open plasma device, work with 130W's power, at first let in oxygen, let in 5 minutes after the rethread hydrogen is handled graphite alkene powder surface, carry out the volume ratio with NH3 and nitrogen gas and argon gas after 5 minutes and be 2.5: and (3) mixing 0.5:0.5, introducing the mixture into a reaction chamber for reaction, closing a plasma device after 10 minutes, transferring the graphene powder into a vacuum tube furnace for annealing treatment, annealing at the temperature of 400 ℃ for 15 minutes, keeping the vacuum degree of the vacuum tube furnace at 0.1Pa, and obtaining the modified graphene plasma powder after the treatment is finished.
Example three:
according to the volume ratio of the graphene powder to the reaction chamber of 1: 5 add corresponding graphite alkene powder in the reacting chamber, close the hatch door of reacting chamber, carry out vacuum heat treatment, after heating 20 minutes with the temperature of 60 degrees centigrade, treat the drying back, open plasma device, work with 110W's power, at first let in oxygen, let in 5 minutes after the rethread hydrogen is handled graphite alkene powder surface, carry out the volume ratio with NH3 and nitrogen gas and argon gas after 5 minutes and be 2.5: and (3) mixing 0.5:0.5, introducing the mixture into a reaction chamber for reaction, closing a plasma device after 10 minutes, transferring the graphene powder into a vacuum tube furnace for annealing treatment, annealing at the temperature of 400 ℃ for 15 minutes, keeping the vacuum degree of the vacuum tube furnace at 0.1Pa, and obtaining the modified graphene plasma powder after the treatment is finished.
Example four:
according to the volume ratio of the graphene powder to the reaction chamber of 1: 5 add corresponding graphite alkene powder in the reacting chamber, close the hatch door of reacting chamber, carry out vacuum heat treatment, after heating 20 minutes with the temperature of 60 degrees centigrade, treat the drying back, open plasma device, work with 100W's power, at first let in oxygen, let in 5 minutes after the rethread hydrogen is handled graphite alkene powder surface, carry out the volume ratio with NH3 and nitrogen gas and argon gas after 5 minutes and be 2.5: and (3) mixing 0.5:0.5, introducing the mixture into a reaction chamber for reaction, closing a plasma device after 10 minutes, transferring the graphene powder into a vacuum tube furnace for annealing treatment, annealing at the temperature of 300 ℃ for 15 minutes, keeping the vacuum degree of the vacuum tube furnace at 0.1Pa, and obtaining the modified graphene plasma powder after the treatment is finished.
Relevant tests are carried out on the modified graphene powder obtained in the above embodiments, it is found that the diameter of the particles is obviously increased, the conductivity is further improved, and through screening, the conductivity of the second embodiment is excellent, and the use requirement is met.
The above disclosure is only for a few specific embodiments of the present invention, but the present invention is not limited thereto, and any variations that can be made by those skilled in the art are intended to fall within the scope of the present invention.
Claims (9)
1. A plasma graphene powder surface modification process is characterized by comprising the following steps:
s1: weighing graphene powder, placing the graphene powder in a reaction chamber of equipment, starting the equipment, and vacuumizing a reactor;
s2: rotating the reactor, and heating and baking the graphene powder;
s3, introducing reaction gas into the reaction chamber, carrying out plasma treatment, and modifying the graphene powder;
s4: and carrying out annealing treatment on the modified graphene powder.
2. The plasma graphene powder surface modification process of claim 1, wherein in step S1, the powder is placed in a reaction chamber of a device, and the ratio of the total volume of the powder to the volume of the reaction chamber is not more than 1: 10, the reaction chamber adopts a cylindrical horizontal design, and a channel for gas circulation is arranged on the side wall of the reaction type.
3. The plasma graphene powder surface modification process of claim 1, wherein the graphene powder is single-layer graphene, double-layer graphene or a mixture thereof.
4. The plasma graphene powder surface modification process of claim 1, wherein in step S2, the reaction chamber is rotated to drive the graphene powder to rotate, and the graphene powder is heated and baked, wherein the heating temperature is controlled at 50-80 ℃.
5. The plasma graphene powder surface modification process according to claim 1, wherein in step S3, different gases are introduced into the reaction chamber according to requirements, the introduced gases are introduced uninterruptedly, and a plasma device in the reaction chamber is turned on to modify the graphene powder.
6. The plasma graphene powder surface modification process of claim 5, wherein in step S3, when gas is filled into the reaction chamber, a rare gas and a reaction gas are mixed and filled, and the volume ratio of the rare gas to the reaction gas is 1: (2-4), and before the reaction gas is filled, oxygen and hydrogen are filled in advance.
7. The plasma graphene powder surface modification process according to claim 5, wherein in step S3, the plasma source in the plasma device is: a dielectric barrier discharge plasma source, a surface discharge plasma source, a bulk discharge plasma source, a sliding arc plasma torch, a cold plasma torch, a direct current plasma source, a pulsed plasma source, a magnetron plasma source, an inductively coupled plasma source, a helical tube plasma source, a helical resonator plasma source, a microwave plasma source, an atmospheric pressure plasma jet source, a corona discharge plasma source, a microplasma source, a low pressure plasma source, or a high pressure plasma source.
8. The plasma graphene powder surface modification process of claim 5, wherein the charged gas is one or more of hydrogen, oxygen, nitrogen, argon, SF6, NH3 and SO 2.
9. The plasma graphene powder surface modification process of claim 1, wherein in step S4, a vacuum tube furnace is used for annealing, the annealing temperature is controlled at 300-500 ℃, the annealing time is 15-20 minutes, and the vacuum degree of the vacuum tube furnace is maintained at 0.1-0.5 Pa.
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| CN115092919A (en) * | 2022-06-21 | 2022-09-23 | 贵州玖碳科技有限公司 | Production process of plasma graphene powder |
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Application publication date: 20210430 |