CN112225197A - Preparation method of heteroatom doped carbon material with framework structure - Google Patents
Preparation method of heteroatom doped carbon material with framework structure Download PDFInfo
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- CN112225197A CN112225197A CN202011149060.1A CN202011149060A CN112225197A CN 112225197 A CN112225197 A CN 112225197A CN 202011149060 A CN202011149060 A CN 202011149060A CN 112225197 A CN112225197 A CN 112225197A
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 38
- 125000005842 heteroatom Chemical group 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 229960003638 dopamine Drugs 0.000 claims abstract description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 3
- 238000011144 upstream manufacturing Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052755 nonmetal Inorganic materials 0.000 claims description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 3
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 2
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- 229940068041 phytic acid Drugs 0.000 claims description 2
- 235000002949 phytic acid Nutrition 0.000 claims description 2
- 239000000467 phytic acid Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- -1 dicyanodiamine Chemical compound 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/33—
-
- B01J35/61—
-
- 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
Abstract
The invention provides a preparation method of a heteroatom doped carbon material with a framework structure. The method comprises the following steps: adding silicon dioxide spheres into deionized water, and performing ultrasonic dispersion to form silicon dioxide sphere dispersion liquid; adding dopamine directly under stirring, dissolving, and then adding tris-HCl solution for polymerization reaction; washing and drying the filter residue to obtain a sample; putting the sample in a porcelain boat, putting the porcelain boat in the middle of a tubular furnace, and putting a compound containing non-metallic heteroatom at the upstream of the flow of the tubular furnace for heating and doping; and adding the doped sample into a mixed solution of deionized water and hydrofluoric acid, ultrasonically stirring, washing with deionized water, and drying to obtain the heteroatom doped carbon material. The preparation method has the advantages of low requirement on equipment, convenience, high efficiency, strong controllability of reaction conditions, adjustable frame structure, adjustable heteroatom proportion and content of the prepared material and wide application range. The synthesized heteroatom doped carbon material with the framework structure can be used as a carrier or a catalyst and can be directly applied to various catalytic and electrocatalytic fields.
Description
Technical Field
The invention relates to a preparation method of a heteroatom doped carbon material with a framework structure, belonging to the technical field of material synthesis.
Background
In order to solve the energy and environmental problems in China and worldwide and to develop sustainable economy and society, the development of clean energy technology is urgent. The new energy technology such as lithium air battery, fuel cell, electrochemical nitrogen/carbon dioxide reduction and the like has the advantages of high energy density, environmental protection, greenness and the like, is regarded as an important key technology for efficiently utilizing clean energy such as electric energy converted from solar energy and wind energy, and represents an important direction for converting and storing the novel electrochemical energy. In these new energy conversion technologies, the catalyst is the core and is one of the key determinants of the performance and cost of the whole device. And a carbon-based catalytic material is the first choice to develop a green and environment-friendly catalyst. The carbon material has the advantages of good conductivity, high porosity, strong plastic structure, adjustable atomic structure, good mechanical property, stable chemical property and the like, and plays an extremely important role in electrocatalysts of various new energy devices. In the electrocatalysis process, reactants and products need to be rapidly transferred in a catalyst to reach an active site and carry out electrocatalysis reaction. Thus, high-flux pore structure carbon materials are critical to electrochemical activity. On one hand, the high-flux pore structure can improve the active surface area and the number of active sites of the material, thereby improving the overall activity; on the other hand, the high-flux pore structure can be provided with a three-dimensional communicating pore channel, and can realize multi-directional rapid ion transmission, thereby accelerating the surface/interface electro-catalytic reaction kinetics. For decades, a series of efforts have been made through the design of carbon materials, yet the preparation of high-throughput pore-structured carbon materials remains a great challenge.
The invention prepares the heteroatom doped carbon material with a frame structure by utilizing the processes of self-polymerization, carbonization, silica ball template removal and the like of dopamine on the surface of the silica ball template. The method has the advantages of definite and simple preparation process, low requirement on equipment, unique frame structure heteroatom doped carbon material prepared by the method, application to various electrocatalysis fields and good benefit.
Disclosure of Invention
The invention aims to overcome the defects of low activity of active sites of carbon-based materials and limited mass transmission in electrocatalysis reaction, prepare high-activity heteroatom doped carbon materials with a framework structure by a silicon dioxide template method, and realize the application of the heteroatom doped carbon materials in electrochemical reaction. The invention provides a heteroatom doped carbon material with a frame structure and a preparation method thereof, wherein the typical preparation process is characterized in that dopamine is self-polymerized to the surface of a silicon dioxide template and a heteroatom doping process is carried out, and the typical structural characteristic is that the synthesized carbon material has a frame structure and is doped with single elements or multiple elements.
The technical scheme adopted for realizing the purpose of the invention is as follows:
(1) adding silicon dioxide spheres into deionized water, and performing ultrasonic dispersion for a period of time to form silicon dioxide sphere dispersion liquid;
the size of the silicon dioxide spheres is 2 nm-200 nm.
(2) Under the condition of keeping 200-2000 rpm magnetic stirring, directly adding dopamine into the silicon dioxide sphere dispersion liquid, after complete dissolution, adding tris-HCl solution, controlling the pH value to be 7-14, and carrying out polymerization reaction for 1-72 hours;
the dosage of the silicon dioxide spheres, the dopamine, the tris-HC and the deionized water is respectively as follows: 1-20 g, 0.1-10 g, 2-80 g: 1000 ml.
(3) And filtering the black suspension after the polymerization reaction, washing the black suspension for 3-5 times by using deionized water, and drying filter residues in a drying box to obtain a dried sample overnight.
(4) The dried sample was placed in a porcelain boat and placed in the middle of a tube furnace. A non-metallic heteroatom-containing compound is placed upstream of the tube furnace gas stream for doping. In inert gas Ar or N2Under protection (the flow rate is 5-100 sccm), the temperature of the tubular furnace is 300-1000 ℃, and the heating rate of the tubular furnace is 1-20 ℃ per min. After the temperature is raised to a specified temperature, keeping the heating time for 3-8 hours, and then naturally cooling;
the compound containing non-metal heteroatom is sodium hypophosphite, dicyanodiamine, melamine, thiourea, triphenyl phosphorus, phytic acid, diboron trioxide, ammonium chloride, ammonium fluoride or sulfur.
(5) Adding the sample obtained in the step (4) into a mixed solution of deionized water and hydrofluoric acid, ultrasonically stirring for 2-10 hours to remove silicon, filtering, washing with deionized water for 3-5 times, and drying filter residues in a drying oven overnight to prepare the heteroatom doped carbon material with the frame structure;
the dosage ratios of the sample, the deionized water and the hydrofluoric acid are respectively 1 mg: 0.1-3 ml: 0.1 to 0.3 ml.
Compared with the existing carbon material synthesis method and the synthesized carbon material, the preparation method of the heteroatom doped carbon material with the framework structure and the material have the following obvious synthesis and structure characteristics:
(1) in the preparation process of a common carbon material, effective and regular heteroatom doping is not introduced. The preparation process of the heteroatom doped carbon material with the framework structure, which is related in the patent, effectively introduces N doping or N and other elements such as P, B and the like codoping, can form active sites, and realizes the application of the active sites in electrocatalysis.
(2) In the general preparation process of the carbon material, effective control on the micro-nano structure of the carbon material is lacked. In the patent, the preparation method utilizes the dopamine autopolymerization process, and realizes effective control of the three-dimensional size of the synthesized carbon material through the conditions of the size of the silicon dioxide spheres, the dosage of dopamine, the pH value, the reaction temperature and the like.
(3) Compared with other reported carbon materials, the carbon material synthesized by the invention has a remarkable framework structure, and the application depending on the carbon material surface nano structure can be further realized.
The synthetic method can be used for synthesizing various types of doped and various sizes of heteroatom doped carbon materials with frame structures, the synthesized material can effectively increase the specific surface area (active site) and accelerate the mass transfer process, and the method has wide application in the field of electrocatalysis.
Drawings
Fig. 1 is a TEM image of N-doped carbon with a framework structure prepared in example 1;
FIG. 2 is a graph of N-doped carbon with a framework structure prepared in example 1 at saturation of O20.1M HClO of4Graph of the CV of the solution.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1
N-doped nano-frame with frame structure synthesis and oxygen reduction performance
(1) Preparation of a polymer precursor: 6g of 30nm diameter nanosilica spheres were dispersed in 1000ml of deionized water and sonicated for half an hour while maintaining magnetic stirring at a rate of 500 rpm. 1.5g of dopamine was dissolved in 150ml of deionized water and added directly to the silica sphere dispersion. After mixing well, 30g of tris-HCl solution was added dropwise to a pH of 8.5. The reaction system is kept stirring for 20 hours, filtered and washed with deionized water for 5 times to prepare the polymer precursor.
(2) Synthesis of N-doped carbon with framework structure: the obtained polymer precursor was placed in a dry pot and placed in the center of a tube furnace, evacuated, and the tube furnace was purged with Ar gas three times. Then, the Ar gas rate was maintained at 100sccm, the furnace was heated to 500 ℃ at 10 ℃/min, and the temperature was maintained for 4 hours, followed by natural cooling. 100mg of the heat-treated sample was dispersed in 50ml of deionized water (using a PTFE beaker), 10ml of a 40% hydrofluoric acid solution was added, ultrasonic treatment was performed, magnetic stirring was performed at 200rpm for 6 hours, filtration was performed, and drying was performed overnight in a vacuum oven, thereby obtaining an N-doped carbon material having a framework structure.
(3) And (3) structural performance characterization: the prepared N-doped carbon material with the frame structure is shown in figure 1, and the material has a square-like frame structure, the thickness of the frame is about 10nm, and the size of the square is about 30 nm. The performance of the material on electrochemical oxygen reduction is shown in figure 2, and the figure shows that the material has obvious downward current increase at about 0.7V in the cyclic voltammetry scanning process, which indicates that the material has good electrochemical oxygen reduction performance.
Example 2
Synthesis of N/P co-doped carbon material with frame structure
3.6g of nano-silica spheres with the diameter of 30nm are taken and dispersed into 1000ml of water, stirred by ultrasonic for half an hour, and the magnetic stirring speed is kept at 400 rpm. 900mg of dopamine was added, followed by 36g of tris-HCl solution, sonicated for 20min, and stirred at room temperature for 18 hours. After the polymerization reaction is finished, filtering, washing with deionized water for several times, and drying in a drying oven to obtain a polymer sample. Placing the polymer sample in a porcelain boat, placing in the center of a tube furnace, placing a dry pot containing 5g of sodium hypophosphite at the position with the distance of 20cm from the sample at the front end of the gas flow, vacuumizing and introducing Ar gas to clean the furnace body for three times, wherein the Ar gas rate is kept at 5 sccm. The carbonization is kept for 1h at the temperature of 800 ℃ at the temperature of 10 ℃ per minute to 800 ℃. And naturally cooling the tube furnace. 100mg of the sample obtained by the heat treatment, HF (40% 10ml) and 50ml of deionized water were mixed, homogenized by sonication, and the reaction was maintained for 6 hours with stirring. And filtering and drying to obtain the N/P co-doped carbon material with the framework structure.
It should be understood that the above description is illustrative of the preferred embodiment of the present invention and is not to be construed as limiting the scope of the invention, which is defined by the appended claims.
Claims (5)
1. A preparation method of a heteroatom doped carbon material with a framework structure is characterized by comprising the following steps:
(1) adding silica spheres with the size of 2 nm-200 nm into deionized water, and performing ultrasonic dispersion for a period of time to form silica sphere dispersion liquid;
(2) under the condition of keeping magnetic stirring at 200-2000 rpm, directly adding dopamine into the silicon dioxide sphere dispersion liquid, and after complete dissolution, adding a tris-HCl solution for polymerization reaction;
(3) filtering the black suspension liquid after the polymerization reaction, washing the black suspension liquid for 3-5 times by using deionized water, and drying filter residues in a drying box to obtain a dried sample for staying overnight;
(4) placing the dried sample in a porcelain boat, placing in the middle of a tube furnace, placing a compound containing non-metal heteroatom in inert gas Ar or N at the upstream of the gas flow of the tube furnace2Keeping heating under protection for doping;
(5) and (3) adding the sample obtained in the step (4) into a mixed solution of deionized water and hydrofluoric acid, ultrasonically stirring for 5 hours to remove silicon, filtering, washing with deionized water for 3-5 times, and drying filter residues in a drying oven overnight to obtain the heteroatom doped carbon material with the frame structure.
2. The method according to claim 1, wherein the polymerization is carried out for 1 to 72 hours while controlling the pH value to 7 to 14.
3. The method according to claim 1, wherein the amounts of the silica spheres, dopamine, tris-HC and deionized water are as follows: 1-20 g, 0.1-10 g, 2-80 g: 1000 ml.
4. The method for producing a heteroatom-doped carbon material having a framework structure according to claim 1, wherein the heteroatom-doped carbon material is produced in an inert gas Ar or N2Doping under protection, wherein the flow rate of the inert gas is 5-100 sccm, the heating temperature of the tubular furnace is 300-1000 ℃, the heating temperature rise rate of the tubular furnace is 1-20 ℃ per min, and the doping time is 3-8 hours.
5. The method according to claim 1, wherein the non-metal heteroatom-containing compound is selected from the group consisting of sodium hypophosphite, dicyanodiamine, melamine, thiourea, triphenylphosphine, phytic acid, diboron trioxide, ammonium chloride, ammonium fluoride and sulfur.
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Application publication date: 20210115 |