CN115196605A - Preparation method and application of graphite phase carbon nitride nanosheet - Google Patents
Preparation method and application of graphite phase carbon nitride nanosheet Download PDFInfo
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000002135 nanosheet Substances 0.000 title claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 17
- 239000010439 graphite Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000002243 precursor Substances 0.000 claims abstract description 39
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 230000020477 pH reduction Effects 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000000967 suction filtration Methods 0.000 claims abstract description 3
- 239000006228 supernatant Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- 239000005416 organic matter Substances 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 239000002055 nanoplate Substances 0.000 claims 4
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 description 14
- 239000000047 product Substances 0.000 description 12
- 238000001027 hydrothermal synthesis Methods 0.000 description 7
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- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000004005 microsphere Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000002071 nanotube Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000005036 potential barrier Methods 0.000 description 2
- OWYWGLHRNBIFJP-UHFFFAOYSA-N Ipazine Chemical group CCN(CC)C1=NC(Cl)=NC(NC(C)C)=N1 OWYWGLHRNBIFJP-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
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- 230000031700 light absorption Effects 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000012360 testing method Methods 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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/30—Cold cathodes, e.g. field-emissive cathode
- H01J1/304—Field-emissive cathodes
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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Abstract
The invention discloses a preparation method and application of a graphite phase carbon nitride nanosheet, wherein the preparation process comprises the following steps: nitrogen-rich organic matters are used as raw materials, hydrochloric acid acidification and hydrothermal treatment are carried out on the nitrogen-rich organic matters to obtain a mixed solution which is dispersed in a supermolecule precursor, the mixed solution of the supermolecule precursor is subjected to suction filtration, washing, drying and grinding into powder, the powder is placed into an aluminum oxide crucible with a cover, the aluminum oxide crucible with the cover is placed in the center of a muffle furnace chamber, and graphite-phase carbon nitride nanosheets are obtained through high-temperature treatment. The method has the advantages that hydrochloric acid is adopted to carry out acidification treatment on the nitrogen-rich compound to obtain the single pure graphite phase carbon nitride which has regular nanosheet morphology, excellent and stable field emission performance, can meet the actual production and application requirements, is simple in preparation process and easy to operate, does not relate to expensive raw materials, and has a very wide application prospect.
Description
Technical Field
The invention belongs to the technical field of carbon nitride nano material preparation, and particularly relates to a preparation method and application of a graphite phase carbon nitride nanosheet.
Background
Electron emission, one of the most common physical phenomena, has been widely used in many fields. The electron source of many apparatus is manufactured by using electron emission principle, such as the common display in life, in which the cathode ray tube is manufactured by using thermionic emission principle; in the testing characterization of materials, the most commonly used electron microscope, which provides a device electron gun of high-energy electrons, relies on the field electron emission (field emission) principle to realize. Compared with thermionic emission which can be realized under the condition of high temperature, the field emission can realize electron emission under the condition of very low temperature, so the energy consumption is correspondingly very low. In addition, the field emission electron source has many advantages such as stable current, easy integration, small volume, and the like. Therefore, research and application of field emission functional characteristics are also important fields of interest. Currently, field emission technology has wide application prospects in many fields, such as electron sources, microwave vacuum devices, scanning electron microscopes, flat panel displays, and the like. The graphite phase carbon nitride has many excellent properties such as excellent thermal stability and the like, and can meet the use requirements of a field emission device under some extreme conditions; with a large forbidden band width, wide forbidden band semiconductors tend to have small or even negative electron affinities, which are favorable for electron emission. However, the bulk-phase carbon nitride prepared by conventional thermal polycondensation has small specific surface area and few electron emission sites, so that the field emission performance of the material is poor. The field emission performance can be improved by constructing the nano structure. Compared with structures such as graphite-phase carbon nitride nanorods and graphite-phase carbon nitride nanospheres, the graphite-phase carbon nitride nanosheets with the graphene-like structures have the advantages of large specific surface area, large length-diameter ratio and the like of other nanostructure, and meanwhile, the edges of the nanosheets can help weaken the surface potential barrier of the material, improve the escape probability of internal electrons and promote the density of field emission current, which is not possessed by other structures, so that the graphite-phase carbon nitride nanosheets can be used as the best choice for preparing field emission cathode materials in several structures.
By treating the nitrogen-rich organic with an acid to obtain supramolecular precursor structures, the structural, optical and electronic properties of the resulting carbon nitride can be altered without introducing additional templates. For example, the task group Wang Jigang of southeast university uses phosphoric acid to acidify and treat melamine, and then obtains carbon nitride nanotubes through high-temperature treatment (a preparation method of porous carbon nitride nanotubes, publication number: CN 110002414B). In addition, wang Jigang, a group of subjects used nitrogen-containing organic powders as raw materials, and they were acidified with sulfuric acid, subjected to hydrothermal treatment, and then subjected to high-temperature treatment to obtain fluffy microspheres of carbon nitride (a method for preparing fluffy microspheres of carbon nitride having high catalytic activity, publication No. CN 109772404B). However, the obtained graphite-phase carbon nitride structures are respectively of a nanotube structure and a microsphere structure, the edge of the nanosheet can help weaken the surface potential barrier of the material, the internal electron escape probability is improved, and the field emission current density is improved. In addition, the graphite phase carbon nitride obtained by the two methods is inevitably doped with phosphorus and sulfur elements, so that the obtained carbon nitride is not single carbon nitride, and the subsequent field emission is influenced by the doping of external elements.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method and application of a graphite-phase carbon nitride nanosheet, which can obtain single pure graphite-phase carbon nitride without doping of external elements and has more excellent field emission performance when applied to the fields of field emission and the like.
In order to achieve the purpose and achieve the technical effect, the invention adopts the following technical scheme:
a preparation method of graphite phase carbon nitride nanosheets is characterized by comprising the following preparation processes: taking a nitrogen-rich organic matter as a raw material, acidifying by hydrochloric acid and carrying out hydrothermal treatment to obtain a mixed liquid dispersed in a supramolecular precursor, carrying out suction filtration, washing, drying and grinding on the supramolecular precursor mixed liquid into powder, then placing the powder into an aluminum oxide crucible with a cover, then placing the aluminum oxide crucible with the cover at the central position of a furnace chamber of a muffle furnace, and carrying out high-temperature treatment to obtain graphite-phase carbon nitride nanosheets;
the hydrochloric acid acidification is to put the nitrogen-rich organic matter into hydrochloric acid and magnetically stir until the nitrogen-rich organic matter is uniformly mixed;
the hydrothermal treatment is to transfer the hydrochloric acid acidification mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and perform hydrothermal treatment for 9 to 12 hours at the temperature of between 140 and 160 ℃;
the high-temperature treatment is to place the alumina crucible with the cover in a muffle furnace, heat up to 500-520 ℃ at the heating rate of 3-5 ℃/min, and then keep the temperature for 4-6 h.
The nitrogen-rich organic matter is one of melamine, dicyandiamide and urea.
The concentration of the hydrochloric acid is 0.5-0.75 mol/L, the dosage is 70mL, and the hydrochloric acid of 0.5-0.75 mol/L is obtained by diluting concentrated hydrochloric acid.
The mass of the nitrogen-rich organic matter is 3-5 g.
The washing is to use a centrifugal machine to centrifuge the supermolecule precursor solution for many times until a glass rod is used for obtaining supernatant, the pH value is measured to be neutral, and then the supernatant is poured out; the drying is to dry the supermolecule precursor in a vacuum drying oven for 12 hours at the temperature of 80 ℃.
The invention also aims to provide application of the graphite-phase carbon nitride prepared by the preparation method of the graphite-phase carbon nitride nanosheet in the field emission field.
Compared with the prior art, the invention has the following beneficial effects: the hydrochloric acid is adopted to carry out acidification treatment on the nitrogen-rich compound to obtain the single pure graphite phase carbon nitride which has regular nanosheet morphology, excellent and stable field emission performance, can meet the actual production and application requirements, is simple in preparation process, easy to operate, does not relate to expensive raw materials, and has a very wide application prospect.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a Scanning Electron Microscope (SEM) image of the product prepared in example 1.
FIG. 2 is an X-ray diffraction (XRD) pattern of the product prepared in example 1.
FIG. 3 is an ultraviolet-visible diffuse reflectance spectrum (UV-Vis-DRS) of the product prepared in example 1 compared to bulk-phase carbon nitride.
FIG. 4 is a field emission performance graph of the product prepared in example 1 and the turn-on electric field of some common field emission cathodes.
Detailed Description
The following provides a detailed description of the preparation method of graphite phase carbon nitride nanosheets of the present invention by way of specific examples.
Example 1
Weighing 3g of melamine and 70mL of hydrochloric acid solution with the concentration of 0.5mol/L, uniformly mixing, transferring to a 100mL high-temperature reaction kettle, carrying out hydrothermal reaction at 160 ℃ for 9h, naturally cooling to room temperature to obtain a supramolecular precursor mixed solution, centrifuging the supramolecular precursor solution for multiple times by using a centrifugal machine until a glass rod is used for obtaining a supernatant, measuring the pH to be neutral, pouring out the supernatant, and drying the supramolecular precursor in a vacuum drying oven at 80 ℃ for 12h. And (3) putting the dried supermolecule precursor into an alumina crucible with a cover, placing the crucible at the center of a muffle furnace chamber, heating to 520 ℃ at a heating speed of 3 ℃/min, preserving heat for 4 hours, and taking out a sample after naturally cooling to room temperature to obtain the graphite-phase carbon nitride nanosheet.
Fig. 1 is an SEM image of the resultant product, and it can be seen that the graphite-phase carbon nitride in the product has a sheet-like morphology with warped edges.
Figure 2 is the XRD pattern of the resulting product. The diffraction peak located in the vicinity of 13.1 ° corresponds to the (100) crystal plane in carbon nitride, and corresponds to the distance between adjacent nitrogen holes in the repeating heptazine ring unit of carbon nitride in the same plane. The diffraction peak located in the vicinity of 27.3 ° corresponds to the (002) crystal face in carbon nitride, and is attributable to the interplane stacking peak of the aromatic hydrocarbon system. Thus demonstrating that graphite phase carbon nitride is successfully prepared.
The graphite-phase carbon nitride nanosheet in example 1 was subjected to a field emission performance test, and the field intensity at the turn-on was found to be 0.59V/μm.
As shown in fig. 4, the morphology of the prepared sample was analyzed by SEM, confirming that the graphite-phase carbon nitride nanosheets were successfully prepared; the crystal structure of the prepared sample is analyzed by XRD, which proves that the graphite phase carbon nitride is successfully prepared and the product is pure; fig. 4 is a comparison of the field emission performance of the prepared product and the turn-on field strength of some common field emission cathodes, demonstrating that the prepared product has more excellent field emission performance.
As shown in fig. 3, the electron affinity of the material was studied by UV-Vis-DRS and the field emission performance test was performed. FIG. 3 is a comparison graph of the UV-Vis-DRS of the obtained product and bulk-phase carbon nitride, and it can be seen that compared with bulk-phase carbon nitride, the carbon nitride nanosheet has a narrow light absorption range, a large forbidden band width and a small electron affinity, and is beneficial to improving the field enhancement factor of the product and further improving the field emission performance of the material.
Example 2
Weighing 3g of urea and 70mL of hydrochloric acid solution with the concentration of 0.53mol/L, uniformly mixing, transferring to a 100mL high-temperature reaction kettle, carrying out hydrothermal reaction at 143 ℃ for 9.5h, naturally cooling to room temperature to obtain a supramolecular precursor mixed solution, centrifuging the supramolecular precursor solution for multiple times by using a centrifugal machine until a glass rod is used for obtaining a supernatant, measuring the pH to be neutral, pouring out the supernatant, and drying the supramolecular precursor in a vacuum drying oven at 80 ℃ for 12h. And (3) putting the dried supermolecule precursor into an alumina crucible with a cover, placing the crucible at the center of a muffle furnace chamber, heating to 505 ℃ at a heating speed of 3.5 ℃/min, preserving heat for 4.5 hours, and taking out a sample after naturally cooling to room temperature to obtain the graphite-phase carbon nitride nanosheet.
Example 3
Weighing 3.5g of dicyandiamide and 70mL of hydrochloric acid solution with the concentration of 0.56mol/L, uniformly mixing, transferring to a 100mL high-temperature reaction kettle, carrying out hydrothermal reaction at 146 ℃ for 10 hours, naturally cooling to room temperature to obtain a supramolecular precursor mixed solution, centrifuging the supramolecular precursor solution for multiple times by using a centrifuge until a glass rod is used for obtaining a supernatant, measuring the pH value to be neutral, then pouring out the supernatant, and placing the supramolecular precursor in a vacuum drying oven for drying at 80 ℃ for 12 hours. And (3) putting the dried supermolecule precursor into an alumina crucible with a cover, placing the crucible at the center of a muffle furnace chamber, heating to 508 ℃ at a heating speed of 4 ℃/min, preserving heat for 4.5 hours, and taking out a sample after naturally cooling to room temperature to obtain the graphite-phase carbon nitride nanosheet.
Example 4
Weighing 4g of dicyandiamide and 70mL of hydrochloric acid solution with the concentration of 0.6mol/L, uniformly mixing, transferring to a 100mL high-temperature reaction kettle, carrying out hydrothermal reaction at 150 ℃ for 10.5h, naturally cooling to room temperature to obtain a supramolecular precursor mixed solution, centrifuging the supramolecular precursor solution for multiple times by using a centrifugal machine until a glass rod is used for obtaining a supernatant, measuring the pH value to be neutral, pouring out the supernatant, and drying the supramolecular precursor in a vacuum drying oven at 80 ℃ for 12h. And (3) putting the dried supramolecular precursor into an alumina crucible with a cover, placing the crucible at the center of a muffle furnace chamber, heating to 513 ℃ at a heating speed of 4.5 ℃/min, preserving heat for 5 hours, and taking out a sample after naturally cooling to room temperature to obtain the graphite-phase carbon nitride nanosheet.
Example 5
Weighing 4.5g of urea and 70mL of hydrochloric acid solution with the concentration of 0.65mol/L, uniformly mixing, transferring to a 100mL high-temperature reaction kettle, carrying out hydrothermal reaction at 155 ℃ for 11h, naturally cooling to room temperature to obtain a supramolecular precursor mixed solution, centrifuging the supramolecular precursor solution for multiple times by using a centrifugal machine until a glass rod is used for obtaining a supernatant, measuring the pH to be neutral, pouring out the supernatant, and drying the supramolecular precursor in a vacuum drying oven at 80 ℃ for 12h. And (3) putting the dried supermolecule precursor into an alumina crucible with a cover, placing the crucible at the center of a muffle furnace chamber, heating to 515 ℃ at a heating speed of 5 ℃/min, preserving heat for 5.5 hours, and taking out a sample after naturally cooling to room temperature to obtain the graphite-phase carbon nitride nanosheet.
Example 6
Weighing 5g of urea and 70mL of hydrochloric acid solution with the concentration of 0.68mol/L, uniformly mixing, transferring to a 100mL high-temperature reaction kettle, carrying out hydrothermal reaction at 158 ℃ for 11.5h, naturally cooling to room temperature to obtain a supramolecular precursor mixed solution, centrifuging the supramolecular precursor solution for multiple times by using a centrifugal machine until a glass rod is used for obtaining a supernatant, measuring the pH to be neutral, pouring out the supernatant, and drying the supramolecular precursor in a vacuum drying oven at 80 ℃ for 12h. And (3) putting the dried supermolecule precursor into an alumina crucible with a cover, putting the crucible at the center of a muffle furnace chamber, heating to 518 ℃ at a heating speed of 4.7 ℃/min, preserving heat for 6 hours, and taking out a sample after naturally cooling to room temperature to obtain the graphite-phase carbon nitride nanosheet.
Example 7
Weighing 5g of melamine and 70mL of hydrochloric acid solution with the concentration of 0.7mol/L, uniformly mixing, then transferring to a 100mL high-temperature reaction kettle, carrying out hydrothermal reaction at 160 ℃ for 12 hours, naturally cooling to room temperature to obtain a supramolecular precursor mixed solution, centrifuging the supramolecular precursor solution for multiple times by using a centrifuge until a glass rod is used to obtain a supernatant, measuring the pH value to be neutral, then pouring out the supernatant, and placing the supramolecular precursor in a vacuum drying oven to be dried at 80 ℃ for 12 hours. And (3) putting the dried supermolecule precursor into an alumina crucible with a cover, placing the crucible at the center of a muffle furnace chamber, heating to 520 ℃ at a heating speed of 5 ℃/min, preserving heat for 6 hours, and taking out a sample after naturally cooling to room temperature to obtain the graphite-phase carbon nitride nanosheet.
The above-mentioned embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be used, not restrictive; it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications belong to the protection scope of the present invention.
Claims (6)
1. A preparation method of graphite phase carbon nitride nanosheets is characterized by comprising the following preparation processes: taking a nitrogen-rich organic matter as a raw material, acidifying by hydrochloric acid and carrying out hydrothermal treatment to obtain a mixed liquid dispersed in a supramolecular precursor, carrying out suction filtration, washing, drying and grinding on the supramolecular precursor mixed liquid into powder, then placing the powder into an aluminum oxide crucible with a cover, then placing the aluminum oxide crucible with the cover at the central position of a furnace chamber of a muffle furnace, and carrying out high-temperature treatment to obtain graphite-phase carbon nitride nanosheets;
the hydrochloric acid acidification is to put the nitrogen-rich organic matter into hydrochloric acid and magnetically stir until the nitrogen-rich organic matter is uniformly mixed;
the hydrothermal treatment is to transfer the hydrochloric acid acidification mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and perform hydrothermal treatment for 9 to 12 hours at the temperature of between 140 and 160 ℃;
the high-temperature treatment is to place the alumina crucible with the cover in a muffle furnace, heat up to 500-520 ℃ at the heating rate of 3-5 ℃/min, and then keep the temperature for 4-6 h.
2. A method of preparing graphite phase carbon nitride nanosheets as defined in claim 1, wherein: the nitrogen-rich organic matter is one of melamine, dicyandiamide and urea.
3. A method of preparing graphite phase carbon nitride nanoplates as defined in claim 1, wherein: the concentration of the hydrochloric acid is 0.5-0.75 mol/L, the dosage is 70mL, and the hydrochloric acid of 0.5-0.75 mol/L is obtained by diluting concentrated hydrochloric acid.
4. A method of preparing graphite phase carbon nitride nanoplates as defined in claim 1, wherein: the mass of the nitrogen-rich organic matter is 3-5 g.
5. A method of preparing graphite phase carbon nitride nanoplates as defined in claim 1, wherein: the washing is to use a centrifugal machine to centrifuge the supermolecule precursor solution for many times until a glass rod is used for obtaining supernatant, the pH value is measured to be neutral, and then the supernatant is poured out; the drying is to dry the supermolecule precursor in a vacuum drying oven for 12 hours at the temperature of 80 ℃.
6. Use of graphite-phase carbon nitride prepared by a method of preparing graphite-phase carbon nitride nanoplates as described in any of claims 1-5 in the field of field emission.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115636984A (en) * | 2022-10-31 | 2023-01-24 | 嘉兴学院 | Application of oxidized carbon nitride nanosheet in tough heat-resistant epoxy resin composite material |
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