CN113104838A - Preparation method of plasma fluorine-doped modified gamma-type graphite single alkyne carbon material - Google Patents
Preparation method of plasma fluorine-doped modified gamma-type graphite single alkyne carbon material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 59
- 239000010439 graphite Substances 0.000 title claims abstract description 59
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- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000003575 carbonaceous material Substances 0.000 title description 7
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001301 oxygen Substances 0.000 claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 11
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 9
- CAYGQBVSOZLICD-UHFFFAOYSA-N hexabromobenzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1Br CAYGQBVSOZLICD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000009832 plasma treatment Methods 0.000 claims description 13
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 12
- 229910052731 fluorine Inorganic materials 0.000 claims description 12
- 239000011737 fluorine Substances 0.000 claims description 12
- 238000005516 engineering process Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
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- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000010189 synthetic method Methods 0.000 abstract 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000001237 Raman spectrum Methods 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
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- 238000004458 analytical method Methods 0.000 description 6
- 125000004432 carbon atom Chemical group C* 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
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- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229920000557 Nafion® Polymers 0.000 description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
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- 229910004014 SiF4 Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000000370 acceptor Substances 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910021387 carbon allotrope Inorganic materials 0.000 description 1
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- 239000002041 carbon nanotube Substances 0.000 description 1
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- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
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- 125000005842 heteroatom Chemical group 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
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- 229910052726 zirconium Inorganic materials 0.000 description 1
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/96—Carbon-based electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a plasma modified graphite monoalkyne, a preparation method and an application of a fuel cell cathode oxygen reduction catalyst thereof, wherein calcium carbide and hexabromobenzene are mixed and added into a ball mill, the ball milling reaction is carried out under the protection of vacuum or normal-temperature inert gas to obtain graphite monoalkyne, and then graphite monoalkyne powder is put into a microwave plasma device; the system adopts a vacuum system less than 10Pa, and CF is introduced4The gas is processed for 300-1200s under the condition of the power of 150W with the flow rate of 5sccm, and the gamma-type graphite monoalkyne with different F doping concentrations is prepared. The invention dopes F atoms into gamma-type graphite monoalkyne, provides an active site for reduction reaction, and expands the application of the gamma-type graphite monoalkyne to the field of electrocatalytic reduction; the doped F atoms can improve the conductivity of the gamma-type graphite single alkyne semiconductor and improve the dynamic performance of the gamma-type graphite single alkyne semiconductor in catalysis. Compared with the existing synthetic method of the F-doped graphite diyne material, the method has the advantages of simple process and low requirements on instruments and equipmentAnd the production is easy. The prepared product is used for electrocatalytic reduction of O2The catalyst material has application prospect in the field.
Description
Technical Field
The invention belongs to the technical field of carbon material modification, and particularly relates to a preparation method of a plasma fluorine-doped modified gamma-type graphite single alkyne carbon material.
Background
The graphdiyne has a two-dimensional planar network structure, is a novel carbon allotrope consisting of a benzene ring and the graphdiyne, has an orderly-distributed pore channel structure, a rich and adjustable electronic structure and unique semiconductor transport property, and has important application prospects in the field of energy storage and conversion. However, experiments and theoretical researches on the synthesis of gamma-type graphite monoalkyne by a mechanochemical method show that the oxygen permeation energy barrier is large in the electrocatalytic oxygen reduction process, and the method is not suitable for application in the field of oxygen reduction catalysis. Previous researches prove that the carbon material is doped with other elements to further regulate and control charge distribution, and the doping position can be used as an active site of reduction reaction, so that the performance of the carbon material in electrocatalytic reduction reaction, such as oxygen reduction reaction in a fuel cell and carbon dioxide reduction reaction in carbon-based fuel synthesis, is improved. See: gao X, Liu H, Wang D, et al graphdiyne: chem Soc Rev, 2019, 48 (3): 908 and 936.; kang B, Lee J Y. Graphynes as formulating Cathode Material of Fuel Cell: improvement of Oxygen Reduction efficiency, the Journal of physical Chemistry C, 2014, 118 (22): 12035-12040.
Currently, the research on the gamma-type graphite monoalkyne element doping mainly focuses on nitrogen atoms, for example, invention CN 109626368 discloses a method for using pyridine as the source of pyridine N and pyridine and benzene/hexahalogenobenzene as sp2Synthesizing pyridine N-doped gamma-type graphite monoalkyne by a precursor hybridized with carbon atoms through the mechanochemical action of the precursor and calcium carbide and a subsequent heat treatment process; the invention of the invention, CN 111137875, discloses a method for preparing a calcium carbide ball, which comprises mixing a polyhalogenated hydrocarbon containing hetero atoms as a nitrogen source with calcium carbide, and adding the mixture into a ball mill one or more timesAnd carrying out ball milling reaction under the protection of vacuum or normal pressure inert gas to obtain a reaction product. In addition, CN 108455591 discloses a method for synthesizing hydrogen substituted graphite monoalkyne by using trihalobenzene and calcium carbide as raw materials and mechanically ball milling with a planetary ball mill. The invention introduces other impurities in the preparation process, needs washing for many times, is difficult to remove, is difficult to obtain a pure product, and has great influence on the improvement of the catalytic performance by the impurities.
The invention utilizes the microwave plasma technology to dope fluorine into the graphite monoacyne, which is applied to the field of electrocatalysis, and on one hand, the introduction of impurities in the conventional ball milling doping process is avoided. On the other hand, the plasma modification process can generate an etching effect and introduce defects, and fluorine atoms have the highest electronegativity and extremely strong electron-withdrawing capability, which are beneficial to the improvement of the electrocatalytic activity.
Disclosure of Invention
The invention mainly aims at the problem that gamma-type graphite monoalkyne is not suitable for fuel cell catalysis, and provides an improved method for promoting the electrochemical performance of the gamma-type graphite monoalkyne by regulating and controlling the electronic structure of plasma fluorine-doped graphite monoalkyne; the method has simple process, no need of high temperature and high doping efficiency.
The technical scheme of the invention is as follows: the preparation method and the application of the plasma modified gamma graphite monoalkyne are provided, and the preparation method is characterized by comprising the following specific preparation steps:
(1) adding calcium carbide and hexahalobenzene into a ball milling tank, and preparing gamma-type graphite monoalkyne by using a ball milling method;
(2) adopting a microwave plasma technology, and putting the gamma-type graphite single alkyne sample prepared in the step (1) into a microwave plasma device for modification treatment in a vacuum state;
and after the reaction is finished, performing structural characterization and electrochemical performance test on the sample before and after the microwave plasma treatment.
In the invention, the modified graphite alkyne is gamma-type graphite monoalkyne prepared by a ball milling method, ball milling beads adopt 2-5mm small-size zirconium beads, the ball milling time is 8-16 hours, and the ball milling is carried out for 30-200min under the inert atmosphere.
In the invention, the plasma processing device is a quartz tube type, a quartz bell jar, a stainless steel cavity type or a water-cooling jacket stainless steel cavity type microwave plasma powder processing device.
In the invention, the vacuum pressure of the system is 0-1 Pa.
In the invention, the gas introduced in the reaction is CF4、F2、SF6、HF、PFs、SiF4、SF6Or WF6The fluorine-containing gas has a working power of 100-.
In the present invention, the plasma treatment time is 1 to 1200 seconds.
The microwave plasma is utilized to prepare the fluorine-doped gamma-type graphite monoalkyne, the reaction quantity of the fluorine plasma and the gamma-type graphite monoalkyne can be regulated and controlled by regulating the processing time of the microwave fluorine plasma, the fluorine doping of the gamma-type graphite monoalkyne is realized, and the carbon-fluorine semi-ionic bond is introduced.
The invention has the beneficial effects that:
(1) the method is different from ball milling doping and a common hydrothermal doping method in that after reaction, post-treatment such as washing is not needed, impurities are not introduced, and the doping process is simple and efficient;
(2) the invention is different from other microwave plasma fluorine-doped carbon materials (graphene, carbon nano tubes and the like) in that sp hybridized fluorine atoms are doped at acetyl sites, and an excellent catalytic effect is shown.
(3) The microwave plasma fluorine-doped gamma-type graphite monoalkyne prepared by the method can generate a little plasma etching on the surface of the material, and the improvement of the catalytic performance can be promoted by increasing a proper amount of surface defect positions;
(4) the fluorine atoms serve as electron acceptors to promote charge transfer between the fluorine atoms and the carbon atoms, improve the conductivity of the gamma-type graphite single alkyne semiconductor and change the electronic property of the original carbon atoms, and meanwhile, the introduction of the fluorine atoms can improve the wettability of the surface of the catalyst, thereby promoting the transmission of electrolyte and oxygen in a carbon skeleton;
(5) the fluorine-doped gamma-type graphite monoalkyne prepared by the method can realize fluorine doping with different concentrations by adjusting the fluorine doping time of the microwave plasma, and can realize continuous regulation and control of the electronic structure of the gamma-type graphite monoalkyne;
(6) the fluorine-doped gamma-type graphite monoalkyne prepared by the method disclosed by the invention adopts a microwave plasma method, requires simple equipment, is suitable for the existing electronic industrial production, and is low in cost and easy to control the preparation process. The preparation method can realize large-scale doping of the gamma-type graphite monoacyne and batch surface doping treatment of the gamma-type graphite monoacyne.
The salient features and significant improvements of the present invention can be seen from the following examples, but are not limited thereto.
Drawings
(1) FIG. 1 is a diagram of a microwave plasma reaction process;
(2) FIG. 2a is a Scanning Electron Micrograph (SEM) of untreated gamma-form graphitic monoalkyne and FIG. 2b example 1;
(3) FIG. 3 is a Raman spectrum (Raman) of untreated gamma-form graphitic monoalkyne and examples 1-3;
(4) FIG. 4 is an X-ray photoelectron spectroscopy C spectrum of untreated gamma-type graphitic monoalkyne and examples 1-3;
(5) FIG. 5 is an electrochemical Cyclic Voltammogram (CV) for untreated gamma graphite monoalkyne and examples 1-3;
(6) FIG. 6a is an electrochemical Linear Sweep Voltammogram (LSV) of untreated gamma-type graphitic monoalkyne and FIG. 6b example 1;
(7) FIG. 7a is a Tafel plot (Tafel) for untreated gamma-type graphitic monoalkyne and FIG. 7b is example 1;
Detailed Description
The following describes in detail the preparation method of a modified graphite monoalkyne material using a quartz tube type microwave plasma powder processing device according to the present invention with reference to specific examples. It should be understood that the specific examples are included merely for purposes of explanation and description and are not intended to limit the scope of the invention. Any modification and variation of the present invention can be made without departing from the object and scope of the present invention.
In the embodiment, a microwave plasma powder processing apparatus developed by combined-fertilizer positive plasma technology ltd is used.
Example 1:
firstly, putting calcium carbide and hexabromobenzene into a ball milling tank, and preparing gamma graphite monoalkyne by adopting a ball milling technology. And performing Raman spectrum and SEM characterization on the prepared gamma-type graphite monoalkyne, preparing catalyst ink, and testing the initial catalytic activity of the catalyst.
And secondly, putting the gamma-type graphite monoalkyne prepared by the ball mill into a quartz tube type microwave plasma powder processing device, opening a vacuumizing device, opening a flow meter after reaching a required vacuum state (less than 1Pa) for about 5-20min, introducing CF4 gas, slowly adjusting to the flow rate (5sccm) required by the experiment, opening a microwave power supply, adjusting to the power (100W) required by the experiment, and processing for 300 s.
And thirdly, carrying out X-ray photoelectron spectroscopy analysis on the fluorine-doped gamma-type graphite monoalkyne sample after the plasma treatment to prove that the fluorine element is successfully introduced and the doping concentration is 8.87 at.%. (FIG. 4b)
And fourthly, after plasma treatment, physical damage or surface etching effect is caused to the sample, and Raman spectrum analysis proves that the defects of the sample are increased. (FIG. 3b)
Fifthly, dispersing the obtained fluorine-doped gamma-type graphite monoalkyne powder in an ethanol solution of Nafion, ultrasonically preparing uniformly dispersed catalyst ink, dripping the uniformly dispersed catalyst ink on a clean glassy carbon electrode, naturally airing, carrying out an electrochemical performance test, carrying out plasma treatment, wherein the CV peak position is from 645 (figure 5a) to 704mV (figure 5b), the initial potential of LSV is from 735 to 769mV, and the limiting current density is from 2.41 to 3.42mA/cm2(FIG. 6b), the tafel slope was from 114 to 83 mV/dec. This shows that fluorine-doped gamma-type graphite monoalkyne can significantly improve the structural characteristics thereof, reduce the oxygen permeability barrier, and fluorine atoms have extremely strong electronegativity and an electron-withdrawing effect, so that adjacent carbon atoms are positively charged and are easy to attract electrons, and the catalytic reaction is promoted to proceed.
Example 2:
firstly, putting calcium carbide and hexabromobenzene into a ball milling tank, and preparing gamma graphite monoalkyne by adopting a ball milling technology. And performing Raman spectrum and SEM characterization on the prepared gamma-type graphite monoalkyne, preparing catalyst ink, and testing the initial catalytic activity of the catalyst.
Secondly, putting the gamma-type graphite monoalkyne prepared by the ball mill into a quartz tube type microwave plasma powder processing device, opening a vacuumizing device, opening a flowmeter after the required vacuum state (less than 1Pa) is reached within about 5-20min, and introducing CF4After the gas is slowly adjusted to the flow rate (10sccm) required by the experiment, the microwave power supply is turned on, the power (150W) required by the experiment is adjusted, and the treatment is carried out for 600 s.
And thirdly, carrying out X-ray photoelectron spectroscopy analysis on the fluorine-doped gamma-type graphite monoalkyne sample after the plasma treatment to prove that the fluorine element is successfully introduced, and the doping concentration is 16.59 at.%. (FIG. 4 c).
And fourthly, after plasma treatment, physical damage or surface etching effect is caused to the sample, and Raman spectrum analysis proves that the defects of the sample are increased. (FIG. 3c)
And fifthly, dispersing the obtained fluorine-doped gamma-type graphite mono-alkyne powder in an ethanol solution of Nafion, ultrasonically preparing uniformly dispersed catalyst ink, dripping the uniformly dispersed catalyst ink on a clean glassy carbon electrode, naturally airing, carrying out an electrochemical performance test, and carrying out plasma treatment to obtain a CV peak position of 645mV (shown in figure 5a) to 679mV (shown in figure 5 d). This shows that fluorine-doped gamma-type graphite monoalkyne can significantly improve the structural characteristics thereof, reduce the oxygen permeability barrier, and fluorine atoms have extremely strong electronegativity and an electron-withdrawing effect, so that adjacent carbon atoms are positively charged and are easy to attract electrons, and the catalytic reaction is promoted to proceed.
Example 3
Firstly, putting calcium carbide and hexabromobenzene into a ball milling tank, and preparing gamma graphite monoalkyne by adopting a ball milling technology. And performing Raman spectrum and SEM characterization on the prepared gamma-type graphite monoalkyne, preparing catalyst ink, and testing the initial catalytic activity of the catalyst.
And secondly, putting the gamma-type graphite monoalkyne prepared by the ball mill into a quartz tube type microwave plasma powder processing device, opening a vacuumizing device, opening a flow meter after reaching a required vacuum state (less than 1Pa) for about 5-20min, introducing CF4 gas, slowly adjusting to the flow rate (2sccm) required by the experiment, opening a microwave power supply, adjusting to the power (200W) required by the experiment, and processing for 1200 s.
And thirdly, carrying out X-ray photoelectron spectroscopy analysis on the fluorine-doped gamma-type graphite monoalkyne sample after the plasma treatment to prove that the fluorine element is successfully introduced and the doping concentration is 9.21 at.%. (FIG. 4d)
And fourthly, after plasma treatment, physical damage or surface etching effect is caused to the sample, and Raman spectrum analysis proves that the defects of the sample are increased. (FIG. 3d)
And fifthly, dispersing the supported fluorine-doped gamma-type graphite mono-alkyne powder in an ethanol solution of Nafion, ultrasonically preparing uniformly dispersed catalyst ink, dripping the uniformly dispersed catalyst ink on a clean glassy carbon electrode, naturally airing, carrying out an electrochemical performance test, and carrying out plasma treatment to obtain the CV peak position of from 645 (figure 5a) to 687mV (figure 5 c). This shows that fluorine-doped gamma-type graphite monoalkyne can significantly improve the structural characteristics thereof, reduce the oxygen permeability barrier, and fluorine atoms have extremely strong electronegativity and an electron-withdrawing effect, so that adjacent carbon atoms are positively charged and are easy to attract electrons, and the catalytic reaction is promoted to proceed.
TABLE 1 examples 1-3 variation of microwave plasma treatment conditions
TABLE 2 change in electrocatalytic properties and fluorine incorporation ratio of unmodified gamma-type graphite monoalkynes and examples 1-3
Claims (4)
1. In order to apply the graphite monoalkyne to the field of electrocatalysis and carry out modification treatment on gamma-type graphite monoalkyne, the technical scheme is as follows: a method for doping graphite single alkyne by fluorine plasma comprises the following steps:
(1) adding calcium carbide and hexabromobenzene into a ball milling tank, and preparing gamma-type graphite monoalkyne by using a ball milling method;
(2) a vacuum system and a microwave plasma technology are adopted; putting a gamma-type graphite single alkyne sample prepared by ball milling into a three-dimensional device such as a microwave device; the system is in a vacuum state, the pressure is less than 1Pa, and the influence of impurities such as oxygen contained in the system is reduced; introducing CF in the reaction process4Gas, the machine power is 140-
2. The method of claim 1, wherein: the modified graphite alkyne is gamma type graphite monoalkyne prepared by a ball milling method.
3. The method of claim 1, wherein: the gas introduced in the reaction is CF4The working power is 140-160W, and the gas flow rate is 5 sccm.
4. The method of claim 1, wherein: and adjusting the plasma treatment time according to the required requirements to obtain the required sample.
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| CN115133045A (en) * | 2022-06-28 | 2022-09-30 | 天津工业大学 | Preparation method of iron and nitrogen co-doped gamma-graphite single alkyne carbon material |
| US11590568B2 (en) | 2019-12-19 | 2023-02-28 | 6K Inc. | Process for producing spheroidized powder from feedstock materials |
| US11633785B2 (en) | 2019-04-30 | 2023-04-25 | 6K Inc. | Mechanically alloyed powder feedstock |
| CN116081778A (en) * | 2023-03-09 | 2023-05-09 | 石河子大学 | Method for recovering fluorine element in perfluoro or polyfluoroalkyl compound from aqueous solution |
| US11717886B2 (en) | 2019-11-18 | 2023-08-08 | 6K Inc. | Unique feedstocks for spherical powders and methods of manufacturing |
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