CN113880060A - Method for synchronously doping monoatomic ions in ferric thiophosphate crystal through electrochemical auxiliary stripping - Google Patents
Method for synchronously doping monoatomic ions in ferric thiophosphate crystal through electrochemical auxiliary stripping Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 28
- 150000002500 ions Chemical class 0.000 title claims description 9
- RYYWUUFWQRZTIU-UHFFFAOYSA-K thiophosphate Chemical compound [O-]P([O-])([O-])=S RYYWUUFWQRZTIU-UHFFFAOYSA-K 0.000 title claims description 8
- 229910005318 FePS3 Inorganic materials 0.000 claims abstract description 20
- LHKPMCGMFJZPRM-UHFFFAOYSA-K iron(3+) thiophosphate Chemical compound P(=S)([O-])([O-])[O-].[Fe+3] LHKPMCGMFJZPRM-UHFFFAOYSA-K 0.000 claims abstract description 12
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 11
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical class CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 7
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 32
- 239000003792 electrolyte Substances 0.000 claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 6
- SHFJWMWCIHQNCP-UHFFFAOYSA-M hydron;tetrabutylazanium;sulfate Chemical compound OS([O-])(=O)=O.CCCC[N+](CCCC)(CCCC)CCCC SHFJWMWCIHQNCP-UHFFFAOYSA-M 0.000 claims description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 239000011574 phosphorus Substances 0.000 claims description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 4
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 239000002064 nanoplatelet Substances 0.000 claims description 2
- -1 tetrabutyl ammonium tetrafluoroborate Chemical compound 0.000 claims description 2
- MCZDHTKJGDCTAE-UHFFFAOYSA-M tetrabutylazanium;acetate Chemical compound CC([O-])=O.CCCC[N+](CCCC)(CCCC)CCCC MCZDHTKJGDCTAE-UHFFFAOYSA-M 0.000 claims description 2
- 230000005518 electrochemistry Effects 0.000 claims 1
- 238000004299 exfoliation Methods 0.000 claims 1
- 239000002135 nanosheet Substances 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000012467 final product Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000001360 synchronised effect Effects 0.000 abstract description 3
- 239000012065 filter cake Substances 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000138 intercalating agent Substances 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Images
Classifications
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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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/14—Sulfur, selenium, or tellurium compounds of phosphorus
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
The invention discloses a method for stripping synchronous doped monoatomic atoms of iron thiophosphate crystals by electrochemical assistance, which takes propylene carbonate as a solvent, tetrabutylammonium salt as an intercalating agent and metal chloride as a doped metal source, and adopts the electrochemical assistance method to strip macroscopic sheet FePS synthesized by a chemical vapor transport method3Single crystal is treated by ultrasonic to obtain the single atom doped FePS3Nanosheets; filtering, washing and separating to obtain a filter cake, and drying to obtain a final product. The beneficial effect of this application is: simple process, rapid reaction, high quality of the obtained doped nano-sheet, complete crystal form and larger size.
Description
Technical Field
The invention relates to the technical field of preparation of novel two-dimensional materials, in particular to a method for synchronously doping monoatomic ions in a ferric thiophosphate crystal through electrochemical auxiliary stripping.
Background
Novel two-dimensional material FePS3Due to their excellent magnetic, electronic and optical properties, there has been a great deal of interest in applications in catalysis, energy storage and optoelectronic devices. Although the two-dimensional material has higher specific surface area, the material can be exposedMore active sites and surface atoms are exposed, and the surface controllability is good; however, the surface modification method of the two-dimensional material at present usually needs to be realized by relatively multi-step reactions, and the high-performance FePS can not be prepared quickly and efficiently3The deficiency of the functional material. Thus, FePS was developed3The novel synthesis method of stripping and surface modification coupling is beneficial to fast and efficiently preparing high-performance FePS3Functional materials to meet the existing industrial requirements.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for realizing FePS by using a one-step method3The method for synchronously doping the monoatomic ions in the ferric thiophosphate crystal through electrochemical auxiliary stripping of coupled high-quality stripping of the crystal and surface monoatomic modification.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for stripping synchronously doped monoatomic iron thiophosphate crystals by electrochemical assistance comprises the following steps:
(1) preparation of macroscopic sheet FePS3A crystal;
(2) dispersing tetrabutylammonium salt and metal chloride in a solvent to obtain an electrolyte;
(3) FePS obtained in the step (1)3Immersing the crystal serving as a working electrode and a platinum wire serving as a counter electrode into the electrolyte obtained in the step (2), and applying constant direct-current voltage to strip;
(4) collecting the solid sample obtained in the step (3), carrying out ultrasonic dispersion in N, N-dimethylformamide, cleaning, and drying to obtain the final product of the single-atom-doped FePS3Nanosheets.
Macroscopic sheet FePS in step (1)3Mixing phosphorus, iron and sulfur powder according to a stoichiometric molar ratio of 1:1:3, vacuum-sealing the mixture in a quartz container, placing the quartz container in a double-temperature-zone tube furnace, and reacting at constant temperature to obtain macroscopic sheet FePS3And (4) crystals.
The temperature of the hot end of the double-temperature-zone tubular furnace used in the step (1) is 700-800 ℃, the temperature difference between the two ends is 40-80 ℃, and the constant temperature time is 7-12 days.
FePS synthesized in step (1)3Crystal transverse rulerThe inch is 5-10 mm.
The tetrabutylammonium salt in the step (2) is one or a combination of more than two of tetrabutylammonium hydrogen sulfate, tetrabutylammonium bromide, tetrabutylammonium tetrafluoroborate and tetrabutylammonium acetate.
And (3) the metal chloride in the step (2) is one of nickel dichloride or cobalt dichloride.
The solvent in the step (2) can be propylene carbonate, N-dimethylformamide or N-methylpyrrolidone and the like, and the propylene carbonate with the best effect is preferred.
The molar concentration of tetrabutylammonium in the electrolyte in the step (2) is 0.02-0.5M, and the molar concentration of metal chloride is 1-10 mM.
Ultrasonically dispersing tetrabutylammonium salt and metal chloride in the step (2) in a solvent, wherein the power of ultrasonic dispersion is 100-160W, and the time is 15-25 min; preferably, the power of the ultrasonic dispersion in the step (2) is 120W.
And (3) the direct current voltage is-2 to-8V.
The stripping time in the step (3) is 2-20min, and the complete stripping can be finished.
And (4) cleaning by sequentially using N, N-dimethylformamide and isopropanol, and then drying. Wherein the power of ultrasonic dispersion is 100-160W, and the time is 15-25 min.
The obtained single-atom doped FePS3The average thickness of the nano-sheets is about 5.5nm, the average transverse size is about 1 mu m, and the doping atoms are monodisperse and have no particle agglomeration.
Compared with the prior art, the beneficial effects of this application are: simple process, rapid reaction, high quality of the obtained doped nano-sheet, complete crystal form and larger size.
Drawings
FIG. 1 shows FePS prepared in example 13An optical photograph of the crystal;
FIG. 2 shows Co-doped FePS prepared in example 13TEM images of the nanoplates;
FIG. 3 shows Co-doped FePS prepared in example 13AFM images of the nanoplatelets.
Detailed Description
The following description of the present invention will be made with reference to the following embodiments and accompanying drawings for electrochemically assisted stripping of iron thiophosphate (FePS)3) The method for synchronously doping single atoms in the crystal is further detailed.
A method for stripping synchronously doped monoatomic iron thiophosphate crystals by electrochemical assistance comprises the following preferred steps:
(1) mixing phosphorus powder, iron powder and sulfur powder according to a stoichiometric molar ratio of 1:1:3, vacuum-sealing the mixture in a quartz container, placing the quartz container in a double-temperature-zone tubular furnace, wherein the temperature of the hot end of the double-temperature-zone tubular furnace is 730-780 ℃, the temperature difference between the two ends is 50-70 ℃, the constant temperature time is 8-10 days, and carrying out constant temperature reaction to obtain macroscopic flake FePS3Crystalline, synthetic FePS3The transverse dimension of the crystal is 5-10 mm.
(2) Ultrasonically dispersing tetrabutylammonium salt and metal chloride in propylene carbonate to obtain electrolyte; wherein the molar concentration of tetrabutylammonium in the electrolyte is 0.1-0.3M, and the molar concentration of metal chloride is 3-7 mM; the power of ultrasonic dispersion is 120W, and the time is 15-25 min.
(3) FePS obtained in the step (1)3Taking the crystal as a working electrode, taking a platinum wire as a counter electrode, immersing the crystal into the electrolyte obtained in the step 2), applying constant direct current voltage for stripping, wherein the direct current voltage is-4 to-8V; the stripping time is 5-18 min.
(4) Collecting the solid sample obtained in the step (3), ultrasonically dispersing the solid sample in N, N-dimethylformamide, sequentially cleaning the solid sample with the N, N-dimethylformamide and isopropanol, and freeze-drying the solid sample at the temperature of between 50 ℃ below zero and 80 ℃ below zero to obtain a final product, namely the single-atom-doped FePS3Nanosheets, wherein the power of ultrasonic dispersion is 120W, and the time is 15-25 min.
The single-atom doped FePS prepared by the method of the invention3The average thickness of the nano-sheet is about 5.5nm, the average transverse size is about 1 mu m, doping atoms are monodisperse, no particle agglomeration exists, the reaction is quicker, the nano-sheet stripping and doping can be synchronously completed within 15min, the crystal form is complete, and the size is larger.
Example 1
A method for electrochemically assisting stripping of a ferric thiophosphate crystal to synchronously dope a monoatomic atom comprises the following steps:
(1) taking 2g of mixed powder of phosphorus, iron and sulfur with the stoichiometric molar ratio of 1:1:3, sealing the powder in a quartz tube in vacuum, placing the quartz tube in a double-temperature-zone tube furnace, wherein the temperature of the hot end of the double-temperature-zone tube furnace is 800 ℃, the temperature difference of the two ends is 80 ℃, the constant temperature time is 8 days, and carrying out constant temperature reaction to obtain macroscopic sheet FePS3Crystalline, synthetic FePS3The transverse dimension of the crystal is 5-10 mm.
(2) 0.1M tetrabutylammonium bromide and 5mM cobalt dichloride were ultrasonically dispersed in 1L of propylene carbonate to obtain an electrolytic solution.
(3) The FePS is prepared3The crystal as a working electrode and a platinum wire as a counter electrode were immersed in the above electrolyte, and peeled off by applying a DC voltage of-5V.
(4) Collecting the stripped solid sample, ultrasonically dispersing in N, N-dimethylformamide, sequentially cleaning with N, N-dimethylformamide and isopropanol, and drying to obtain final product, namely the FePS doped with cobalt monoatomic3Nanosheets.
The macroscopic flake FePS obtained in step (1) of the above example3The crystal is shown in figure 1, and the macroscopic sheet crystal with a complete structure is easy to carry out subsequent stripping and synchronous doping. The obtained FePS doped with cobalt monoatomic3The nano-sheet has a complete sheet structure as shown in FIG. 2, and the transverse dimension of the nano-sheet acts at 1 micron; as shown in FIG. 3, Co-doped FePS3The average thickness of the nano-sheets is 5.5 nm.
Example 2
A method for electrochemically assisting stripping of a ferric thiophosphate crystal to synchronously dope a monoatomic atom comprises the following steps:
(1) taking 2g of mixed powder of phosphorus, iron and sulfur with the stoichiometric molar ratio of 1:1:3, sealing the powder in a quartz tube in vacuum, placing the quartz tube in a double-temperature-zone tube furnace, wherein the temperature of the hot end of the double-temperature-zone tube furnace is 750 ℃, the temperature difference of the two ends of the double-temperature-zone tube furnace is 50 ℃, the constant temperature time is 7 days, and carrying out constant temperature reaction to obtain macroscopic sheet FePS3Crystalline, synthetic FePS3The transverse dimension of the crystal is 5-10 mm.
(2) 0.2M tetrabutylammonium hydrogen sulfate and 5mM nickel dichloride were ultrasonically dispersed in 1L of propylene carbonate to obtain an electrolytic solution.
(3) The FePS is prepared3The crystal as a working electrode and a platinum wire as a counter electrode were immersed in the above electrolyte, and peeled off by applying a DC voltage of-8V.
(4) Collecting the stripped solid sample, ultrasonically dispersing in N, N-dimethylformamide, sequentially cleaning with N, N-dimethylformamide and isopropanol, and drying to obtain final product, namely the FePS doped with nickel monoatomic salt3Nanosheets.
The macroscopic flake FePS obtained in step (1) of the above example3The crystal also has a macroscopic sheet crystal with a complete structure as shown in FIG. 1, and is easy to carry out subsequent stripping and synchronous doping. The obtained FePS doped with nickel monoatomic3The nano sheet has a complete sheet structure, and the transverse size of the nano sheet is 1 micron; nickel doped FePS3The average thickness of the nano-sheets is 5.5 nm.
The above embodiments are only some of the embodiments of the present invention, and the embodiments are not intended to limit the scope of the present invention, and all equivalent changes made by using the contents of the present invention are covered by the scope of the present invention claimed in the claims.
Claims (10)
1. A method for stripping synchronously doped monoatomic iron thiophosphate crystals by electrochemical assistance is characterized by comprising the following steps:
(1) preparation of macroscopic sheet FePS3A crystal;
(2) dispersing tetrabutylammonium salt and metal chloride in a solvent to obtain an electrolyte;
(3) FePS obtained in the step (1)3Immersing the crystal serving as a working electrode and a platinum wire serving as a counter electrode into the electrolyte obtained in the step (2), and applying constant direct-current voltage to strip;
(4) collecting the solid sample after the step (3), carrying out ultrasonic dispersion in N, N-dimethylformamide, washing, and then drying.
2. According to the claimsSolving 1 the method for synchronously doping monatomics in the process of stripping the ferric thiophosphate crystal under the assistance of electrochemistry, which is characterized in that in the step (1), macroscopic sheet FePS is adopted3Mixing phosphorus, iron and sulfur powder according to a stoichiometric molar ratio of 1:1:3, vacuum-sealing the mixture in a quartz container, placing the quartz container in a double-temperature-zone tube furnace, and reacting at constant temperature to obtain macroscopic sheet FePS3And (4) crystals.
3. The method for synchronously doping the monoatomic ions in the crystal of the iron thiophosphate by electrochemical-assisted stripping according to claim 2, wherein the temperature of the hot end of the double-temperature-zone tubular furnace used in the step (1) is 700-800 ℃, the temperature difference between the two ends is 40-80 ℃, and the constant temperature time is 7-12 days; synthetic FePS3The transverse dimension of the crystal is 5-10 mm.
4. The method for synchronously doping monoatomic atoms in the ferric thiophosphate crystals through electrochemical assistance in stripping according to claim 1, wherein the tetrabutyl ammonium salt in the step (2) is one or a combination of more than two of tetrabutyl ammonium hydrogen sulfate, tetrabutyl ammonium bromide, tetrabutyl ammonium tetrafluoroborate and tetrabutyl ammonium acetate; the metal chloride is one of nickel dichloride or cobalt dichloride.
5. The method for synchronously doping monoatomic atoms in an electrochemically-assisted stripping iron thiophosphate crystal according to claim 4, wherein the molar concentration of tetrabutylammonium and the molar concentration of metal chloride in the electrolyte in the step (2) are respectively 0.02-0.5M and 1-10 mM.
6. The method for synchronously doping the monoatomic atoms in the iron thiophosphate crystal through electrochemical auxiliary stripping according to claim 5, wherein the solvent in the step (2) is propylene carbonate, N-dimethylformamide or N-methylpyrrolidone.
7. The method for synchronously doping monoatomic atoms in the iron thiophosphate crystal through electrochemical-assisted stripping according to claim 6, wherein the tetrabutylammonium salt and the metal chloride in the step (2) are ultrasonically dispersed in the solvent, wherein the ultrasonic dispersion power is 100-160W, and the time is 15-25 min.
8. The method for stripping the monoatomic ions synchronously doped with the iron thiophosphate crystals through the electrochemical assistance in the claim 1 is characterized in that the direct-current voltage in the step (3) is-2 to-8V, and the stripping time is 2 to 20 min.
9. The method for synchronously doping the monoatomic ions in the iron thiophosphate crystals through electrochemical auxiliary stripping according to claim 1, wherein the cleaning in the step (4) is sequentially performed by using N, N-dimethylformamide and isopropanol, and then drying; wherein the power of ultrasonic dispersion is 100-160W, and the time is 15-25 min.
10. The method for synchronously doping the monoatomic ions in the crystal of iron thiophosphate by electrochemical-assisted exfoliation according to claim 1, wherein the monoatomic ions are doped with FePS3The average thickness of the nanoplatelets was 5.5nm and the average lateral dimension was 1 μm.
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| CN111517294A (en) * | 2020-06-26 | 2020-08-11 | 昆明理工大学 | Preparation method of metal-doped nano black phosphorus |
| CN112853396A (en) * | 2020-12-30 | 2021-05-28 | 浙江大学衢州研究院 | Two-dimensional ultrathin metal organic framework nanosheet electrocatalyst, and preparation method and application thereof |
| CN113151857A (en) * | 2021-03-29 | 2021-07-23 | 浙江大学衢州研究院 | Two-dimensional ultrathin nickel-doped molybdenum disulfide nanosheet and preparation method and application thereof |
| CN113351230A (en) * | 2021-06-21 | 2021-09-07 | 华侨大学 | Isolated cobalt atom doped single-layer or few-layer MoS2Process for preparing catalyst |
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