CN115092919A - Production process of plasma graphene powder - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 98
- 239000000843 powder Substances 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 210000002381 plasma Anatomy 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 23
- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 16
- -1 boron ions Chemical class 0.000 claims description 12
- 229910052796 boron Inorganic materials 0.000 claims description 11
- 229910052731 fluorine Inorganic materials 0.000 claims description 11
- 239000002356 single layer Substances 0.000 claims description 6
- 239000011737 fluorine Substances 0.000 claims description 5
- 238000011065 in-situ storage Methods 0.000 claims description 5
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 238000004299 exfoliation Methods 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 150000002500 ions Chemical class 0.000 description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 8
- 230000007547 defect Effects 0.000 description 8
- 125000004429 atom Chemical group 0.000 description 7
- 150000001721 carbon Chemical group 0.000 description 7
- 125000004432 carbon atom Chemical group C* 0.000 description 7
- 230000006378 damage Effects 0.000 description 7
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
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- 239000012535 impurity Substances 0.000 description 5
- 125000004430 oxygen atom Chemical group O* 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 125000005842 heteroatom Chemical group 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
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- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
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- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 2
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- AAMATCKFMHVIDO-UHFFFAOYSA-N azane;1h-pyrrole Chemical compound N.C=1C=CNC=1 AAMATCKFMHVIDO-UHFFFAOYSA-N 0.000 description 1
- DLGYNVMUCSTYDQ-UHFFFAOYSA-N azane;pyridine Chemical compound N.C1=CC=NC=C1 DLGYNVMUCSTYDQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 230000002925 chemical effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
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- 125000001033 ether group Chemical group 0.000 description 1
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- 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
- C01B32/194—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C01B2204/22—Electronic properties
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- 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
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Abstract
The invention discloses a production process of plasma graphene powder, which comprises the following steps: s1, weighing graphene powder, placing the graphene powder in a reaction chamber of equipment, and starting the equipment to vacuumize the reactor; s2: rotating the reactor, and heating and baking the graphene powder; s3: introducing plasma into the reaction chamber, wherein the incident ion beam energy of the plasma is 20eV-50eV, and the dosage is 10 eV 14 cm ‑2 ‑10 16 cm ‑2 Modifying the graphene powder; according to the invention, different plasmas are used for modifying graphene, 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 materials, in particular to a production process of plasma graphene powder.
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 treatment of an object is low, the protection effect on the surface of the object to be treated can be realized, and low-temperature plasma is mostly used in application. And the effects of various particles on the object treatment process are 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 higher baking temperature, is difficult to ensure uniform and firm coating, and has larger 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 production process of the plasma graphene powder, and the graphene is modified by using different plasmas, so that the conductivity, the dispersibility, the stability and the compatibility of the obtained graphene powder are improved.
In order to achieve the purpose, the invention provides a production process of plasma graphene powder, which comprises the following steps:
s1, weighing graphene powder, placing the graphene powder in a reaction chamber of equipment, and starting the equipment to vacuumize the reactor;
s2: rotating the reactor, and heating and baking the graphene powder;
s3: introducing plasma into the reaction chamber, wherein the plasma adopts ion beam energy of 20eV-50eV, and the dosage is 10 14 cm -2 -10 16 cm -2 And modifying the 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: and 5, the reaction chamber is designed in a cylindrical horizontal mode, and a generating unit for generating ion beams and an air hole are formed in the side wall of the reaction chamber.
Preferably, the graphene powder is single-layer graphene obtained by an in-situ exfoliation method.
Preferably, in step S2, the temperature of the reaction chamber is controlled at 200-300 ℃ during the rotation, and the temperature is decreased to 10 ℃ or less after the temperature is increased for 5-10 minutes.
Preferably, in step S3, different plasmas are used according to requirements, and the plasmas include one or more of boron ions, oxygen ions and fluorine ions.
The invention has the beneficial effects that: compared with the prior art, the production process of the plasma graphene powder is improved in the prior art, and the graphene with the thickness of only a single-layer carbon atom is modified by changing various parameters, so that the finally obtained graphene powder is doped, the electrical property of the graphene is changed from metallic to a semiconductor, and the subsequent production requirements are met.
Drawings
FIG. 1 is a flow chart of the steps of the present invention;
fig. 2 is a raman spectrum of graphene.
Detailed Description
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.
In the prior art, nitrogen is frequently used as a doping element of graphene, but in the actual production process, nitrogen-doped graphene usually contains impurity nitrogen, the impurity nitrogen mainly comprises graphite nitrogen, pyridine nitrogen and pyrrole nitrogen, and the content of the impurity nitrogen is high and can reach 8.9% at most.
Referring to fig. 1 and 2, the invention discloses a production process of plasma graphene powder, which includes the following steps:
s1, weighing graphene powder, placing the graphene powder in a reaction chamber of equipment, and starting the equipment to vacuumize the reactor;
s2: rotating the reactor, and heating and baking the graphene powder;
s3: introducing plasma into the reaction chamber, wherein the plasma adopts ion beam energy of 20eV-50eV, and the dosage is 10 14 cm -2 -10 16 cm -2 And modifying the 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: and 5, the reaction chamber is designed in a cylindrical horizontal mode, and a generating unit for generating ion beams and an air hole are formed in the side wall of the reaction chamber. 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 much, if the amount of the graphene powder is too much, all surfaces of the graphene powder cannot be modified in a subsequent process, treatment is incomplete, and the whole modification process is influenced.
The graphene powder is single-layer graphene obtained by adopting an in-situ stripping method; in step S2, the temperature of the reaction chamber is controlled at 200-300 ℃ during the rotation, and the temperature is decreased to 10 ℃ or below after the temperature is increased for 5-10 minutes. In the implementation process, as the graphene surface has huge specific surface area and large adsorption and load capacity to impurities, numerous molecules such as hydrogen, oxygen, ammonia gas and nitrogen dioxide can be adsorbed on the graphene surface in a large amount, surface doping can be formed under the condition of catalytic reaction, the existing catalytic reaction is high temperature, and annealing treatment is realized by utilizing the high temperature, so that the doping purpose is realized, but in the operation process, the required temperature is higher and is generally not lower than 700 ℃, the high temperature resistance of instrument and equipment is higher, and in the temperature rise process, impurity molecules (hydrogen, oxygen, ammonia gas, nitrogen dioxide and the like) can be desorbed in a large amount, so that loss can be lost under the condition that the reaction temperature is not reached, while the in-situ doping effect of the single-layer graphene obtained by adopting the in-situ stripping method is generally higher than that of the graphene obtained by adopting the chemical vapor deposition method, meanwhile, in order to make the reaction irreversible, a substitution doping mode is adopted, the lattice position of carbon atoms in graphene is substituted by heteroatoms to generate heterocycles, the structure and charge distribution of the graphene are changed, the influence on the energy band structure and the conductivity of the graphene is larger, plasma modification is adopted, defects can be introduced into the graphene by utilizing the etching effect of the plasma to provide more active vacancies for the heteroatoms to enter, the defects around the heteroatoms can also provide larger specific surface area to improve the catalytic performance of the heteroatoms, in the specific implementation process, high temperature is adopted to carry out drying treatment on moisture in graphene powder, the influence of the moisture on the subsequent modification process of the graphene is avoided, temperature reduction treatment is carried out after high temperature, the temperature is reduced because the high temperature is not required when the plasma is adopted to modify the graphene, can directly carry out work under the low temperature condition, avoid the waste of resource, in addition, the temperature rise can accelerate the etching to graphite alkene to a certain extent to make graphite alkene produce the defect, consequently need with temperature control at lower level, generally be less than 10 degrees centigrade.
In step S3, different plasmas are used according to requirements, and the plasmas include one or more of hydrogen ions, boron ions, oxygen ions and fluorine ions. In a specific implementation process, boron (B) has one less electron than carbon atom (C), the atomic size of boron is close to that of carbon atom, B-doped graphene has P-type semiconductor properties, and fluorine atom (F) has the similar size to that of carbon atom and is easily doped into graphene; for the oxygen atom, the surface of the graphene with a complete structure is covered with pi electron cloud to play a role of blocking foreign particles from being close to the carbon atom, only enough high-energy active particles can be close to and react with the surface of the graphene, particularly, the plasma state oxygen particle is a strong oxidation factor with super electronegativity and reactivity, under the strong oxidation action of the plasma state oxygen, the surface of the graphene is subjected to oxidation grafting reaction, the oxygen atom can form an epoxy bond on the surface of the graphene, namely, the bridge type configuration of the epoxy is the configuration which is most easily formed by the oxygen atom on the surface of the graphene, so that the carbon atom is enabled to be from sp 2 Conversion of hybridization to sp 3 Hybridization, followed by transformation of the epoxy group into other types of oxygen-containing groups, such as carboxyl, hydroxyl, carbonyl, etc., destroys the integrity and planarity of the pi-pi conjugated structure of graphene, so that the band gap of graphene is opened to exhibit semiconductor properties.
It is based on these characteristics that the energy of the incident ion beam is controlled to be 20eV-50eV, and if the energy is too largeIf the amount of the graphene is too small, the graphene cannot approach the surface of the graphene to react with the graphene; and at lower doses, e.g. at doses less than 10 14 cm -2 The doping amount is too low, and it is difficult to analyze the doping condition by general testing methods, so it is very necessary to select proper ion beam parameters.
Firstly, carrying out Raman spectrum analysis on graphene at 1350cm -1 ，1585cm -1 And 2720cm -1 Three obvious peaks are respectively a D peak, a G peak and a 2D peak, wherein the D peak is a reaction of the disorder degree of a crystal structure and is caused by the excitation of defects in a hexagonal carbon ring of the graphene, and the G peak represents the scattering E of the Brillouin zone 2g The vibro-magic is a two-fold degeneracy, used to characterize the SP of carbon 2 The bond structure and the 2D peak are derived from the second-order Raman scattering of a Brillouin zone boundary phonon and are sharp single peaks in single-layer graphene, and the intensity ratio (ID/IG) of the D peak to the G peak can quantitatively research the lattice defect degree of the graphene.
The experiments were carried out according to the experimental parameters of the following table:
| examples | Ion species | Ion energy (eV) | Ion beam dose (cm) -2 ) |
| 1 | Boron (B) | 20 | 2*10 14 |
| 2 | Boron (B) | 50 | 1*10 15 |
| 3 | Fluorine (F) | 35 | 1*10 14 |
| 4 | Fluorine (F) | 30 | 2*10 15 |
| 5 | Oxygen (O) | 30 | 4*10 15 |
| 6 | Oxygen (O) | 40 | 1*10 14 |
| 7 | Nitrogen (N) | 35 | 6*10 15 |
| 8 | Nitrogen (N) | 45 | 1*10 14 |
Simultaneously using nitrogen element for phase separationIn contrast experiments, two groups of experiments are carried out on each element to ensure the accuracy of experimental results, and after the experiments, it is found that under the low-energy condition, B and F ions can be doped into graphene, but certain damage is caused to the graphene, the damage degree is related to ion species, energy and dosage, and when the dosage is 10 14 cm -2 The ID/IG of B, F and N ion beam irradiated graphene were 0.55,0.69, and 1.27, respectively; if the dosage is increased to 10 15 cm -2 The ID/IG of the B and F ion beam irradiated samples increased to 3.3 and 4.96, respectively, while the N ion beam irradiated graphene became amorphous. Among the three ions, B ion beam irradiation causes the least damage to graphene because B atoms are lighter than C atoms in mass, and when B ions perpendicularly irradiate a graphene film, there is a possibility that the B ions are scattered by carbon atoms and move along a direction parallel to the plane of the carbon atoms, collide with another carbon atom and are scattered, and most of the carbon atoms in graphene still remain in the original lattice position, so that the B ion beam irradiation causes less damage to graphene. While F and N are heavier than C, if considering atomic mass, since F is larger than N, the damage of graphene by F ion irradiation should be larger than that of N ion, but the experimental result is contrary thereto. It is inferred that the reason for this may be related to the chemical bond energy. For high energy ion beam irradiation, since the kinetic energy of the foreign ions is very large, the physical collision effect between the foreign ions and the irradiated atoms is much larger than the chemical reaction effect, so the chemical effect may be disregarded. However, for low energy ion beam irradiation, the chemical reaction between the ions and the irradiated atoms is very important because the bond energy of the C-N bond is 293kJ/mol, which is smaller than the C-C bond (348kJ/mol) and the C-F bond (485kJ/mol), so the C-N bond is less stable than the C-C bond and the C-F bond, which means that the C-N bond is most easily broken, thereby causing more destruction of graphene. Therefore, the damage degree of graphene caused by N ion beam irradiation is larger than that caused by F ion beam irradiation.
The oxygen content increase and the temperature rise on the surface of the graphene promote the diffusion of oxygen atoms on the surface of the graphene, and the oxygen atomsThe atoms diffuse rather than hopping between six-membered rings, but rather diffuse more readily along the tops of the carbon atoms until a stable structure or other oxygen-containing group is formed, the lowest energy structure being the formation of two opposing epoxy groups in one six-membered carbon ring, the other two carbon atoms remaining sp 2 Because the process is a self-sustaining exothermic reaction, domino effect is initiated to break and decompose the epoxy chain, graphene sheets are broken, more edge parts with dangling bonds, defect sites or vacancies are exposed, and the graphene sheets are more easily attacked by the oxygen atoms, and the oxidation process is accelerated; the C-C bond in the epoxy group can also be broken to form a C-O-C ether group, and then converted into other oxidation groups, and the oxidation groups can also be active sites of reaction besides changing the inherent properties of graphene.
The surface of the graphene treated by the plasma is grafted with polar oxygen-containing groups, such as carboxyl, carbonyl, hydroxyl and the like, or a large number of microstructures such as surface defects, holes and the like are formed, the change of the surface microtopography endows the graphene material with a plurality of new macroscopic properties, different graphene functional modifications are realized, and the eight embodiments are subjected to the periscopic observation and conductivity test, and the results are as follows:
tests show that the particle diameters are increased to a certain extent, the conductivity is further improved, the conductivity of F and B is obviously higher than that of N, the N forms an amorphous structure, the conductivity of the amorphous structure is obviously weaker than that of the crystal structure, O ions initiate surface branch action, main oxygen-containing groups are converted from carboxyl to carbonyl and hydroxyl, and meanwhile, the increase of the hydroxyl has an obvious effect on the improvement of the conductivity, so that the conductivity is improved more obviously.
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 (5)
1. A production process of plasma graphene powder is characterized by comprising the following steps:
s1, weighing graphene powder, placing the graphene powder in a reaction chamber of equipment, and starting the equipment to vacuumize the reactor;
s2: rotating the reactor, and heating and baking the graphene powder;
s3: introducing plasma into the reaction chamber, wherein the incident ion beam energy of the plasma is 20eV-50eV, and the dosage is 10 eV 14 cm -2 -10 16 cm -2 And modifying the graphene powder.
2. The process for producing plasma graphene powder according to 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: and 5, the reaction chamber is designed in a cylindrical horizontal mode, and a generating unit for generating ion beams and an air hole are formed in the side wall of the reaction chamber.
3. The production process of the plasma graphene powder according to claim 1, wherein the graphene powder is single-layer graphene obtained by an in-situ exfoliation method.
4. The process for producing plasma graphene powder according to claim 1, wherein in step S2, the temperature of the reaction chamber is controlled at 200-300 ℃ during the rotation, and the temperature is decreased to below 10 ℃ after the temperature is increased for 5-10 minutes.
5. The process of claim 1, wherein in step S3, different plasmas are used as required, and the plasmas include one or more of boron ions, oxygen ions, and fluorine ions.
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