CN110787820A - Heteroatom nitrogen surface modification MoS2Preparation and application of nano material - Google Patents
Heteroatom nitrogen surface modification MoS2Preparation and application of nano material Download PDFInfo
- Publication number
- CN110787820A CN110787820A CN201910837039.1A CN201910837039A CN110787820A CN 110787820 A CN110787820 A CN 110787820A CN 201910837039 A CN201910837039 A CN 201910837039A CN 110787820 A CN110787820 A CN 110787820A
- Authority
- CN
- China
- Prior art keywords
- water
- mos
- reaction kettle
- carbon cloth
- thiourea
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 125000005842 heteroatom Chemical group 0.000 title claims abstract description 14
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 14
- 238000012986 modification Methods 0.000 title claims description 4
- 230000004048 modification Effects 0.000 title claims description 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 32
- 239000004744 fabric Substances 0.000 claims abstract description 31
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 26
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 26
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 24
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 22
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 22
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 22
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 22
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 17
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 239000002135 nanosheet Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 6
- 239000010411 electrocatalyst Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 229910052723 transition metal Inorganic materials 0.000 claims description 3
- -1 transition metal salt Chemical class 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 13
- 239000001301 oxygen Substances 0.000 abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 abstract description 13
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000007605 air drying Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
-
- 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
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
-
- 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
- H01M4/90—Selection of catalytic material
- H01M4/9091—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Electrochemistry (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
Heteroatom nitrogen surface modified MoS2The preparation and application of nanometer material, and belongs to the field of electrocatalytic material synthesizing technology. The prepared catalyst has excellent electrocatalytic oxygen evolution performance. The preparation process comprises the following steps: (1) carbon cloth (3 x 3cm) is respectively treated with ultrasonic treatment in acetone, ethanol and water for 10 minutes; (2) mixing ammonium molybdate and thiourea in water in proportion, reacting the mixture with clean carbon cloth in a reaction kettle at a high temperature, cooling to room temperature, washing the carbon cloth with ethanol and water in sequence, and drying; (3) MoS obtained in the step (2)2The nanosheet and ammonia water are placed in the reaction kettle to be highReacting at a certain temperature for a certain time to obtain heteroatom nitrogen modified MoS2And (3) nano materials. The catalyst obtained by the invention has excellent electro-catalytic performance, and the preparation process is simple, low in cost and suitable for large-scale production.
Description
Technical Field
The technical field of electrocatalytic material synthesis, in particular to heteroatom nitrogen surface modified MoS2Preparation and application of nanometer material.
Background
As an alternative to traditional fossil fuels, hydrogen energy is available due to its high energy density, zero pollutant emissions and abundant reservesAnd is receiving wide attention. Electrolysis of water provides an ideal production method for renewable pure hydrogen without the formation of by-products. The electrolyzed water consists of two half-reactions, namely cathodic hydrogen evolution and anodic oxygen evolution. The anodic oxygen evolution reaction is a four-electron-proton coupling reaction, and higher energy (higher overpotential) is needed, so that the oxygen evolution overpotential is far higher than the theoretical decomposition voltage (1.23V) of water. In order to reduce overpotential and promote reaction kinetics during electrolysis of water, a highly efficient electrocatalyst is essential. Noble metal materials such as platinum, iridium, ruthenium and the like, which are the most effective electrolytic water reaction catalysts so far, have high price and limited reserves, and seriously affect the wide application. Therefore, high activity, inexpensive and abundant non-noble metal electrocatalysts are of paramount importance for the wide application of electrocatalytic water splitting. The present research shows that the transition metal sulfide has excellent electrocatalytic performance, wherein MoS of a layered structure2Is a high-efficiency nano material for hydrogen evolution reaction. However, for the other half-reaction oxygen evolution reaction of the water splitting reaction, MoS2There is no catalytic effect. Therefore, for MoS2Modification to reduce the overpotential during oxygen evolution is critical for the water decomposition reaction.
Disclosure of Invention
In order to solve the problems that a noble metal catalyst is expensive in price, small in reserve and difficult to widely apply, and a non-noble metal catalyst is high in overpotential and wastes energy, the invention provides heteroatom nitrogen surface modified MoS2The preparation and the application of the nano material solve the problem of the prior MoS2The catalyst preparation method is complex and has low oxygen evolution activity.
The method mainly comprises the following steps:
(1) sequentially carrying out ultrasonic treatment on carbon cloth (3 x 3cm) in acetone, ethanol and water for 10 minutes for later use;
(2) mixing ammonium molybdate and thiourea in water according to a ratio, wherein the molar ratio of the ammonium molybdate to the thiourea is 1:5, and stirring until the ammonium molybdate and the thiourea are completely dissolved to obtain a uniform solution;
(3) transferring the uniformly stirred solution into a reaction kettle with a stainless steel substrate, putting an ultrasonic carbon cloth into the reaction kettle, and putting the reaction kettle into the reaction kettleKeeping the temperature of 180 ℃ in a forced air drying oven for 12 hours; cooling to room temperature, taking out the carbon cloth, washing with ethanol and water in sequence, and drying to obtain MoS2A nano-platelet catalyst.
(4) The obtained MoS2Adding ammonia water with different volumes into a reaction kettle with a stainless steel substrate, and adding MoS2Above the ammonia, there is no contact with the ammonia. Putting the reaction kettle in a blast drying oven for high-temperature reaction, cooling to room temperature, taking out the carbon cloth, sequentially washing with ethanol and water, and drying to obtain the heteroatom nitrogen surface modified MoS2And (3) nano materials.
The molar ratio of the transition metal salt to the thiourea in the step (2) is 1: 5.
The volume of the ammonia water in the step (3) is 5mL, 10mL and 15 mL.
The high-temperature reaction temperature in the step (3) is 90 ℃, 150 ℃ and 180 ℃.
The high-temperature reaction time in the step (3) is 8 hours, 12 hours and 18 hours.
According to the method of the invention, a heteroatom nitrogen surface modified MoS is provided2The preparation method of the nano material applied to the electrocatalyst.
The electrocatalyst is used for catalyzing the oxygen evolution reaction of the fuel cell or the electrolytic cell.
In general, compared to the prior art, the above technical solution contemplated by the present invention prepares hetero-atomic surface modified MoS by a simple hydrothermal method2The nano material catalyst improves the oxygen evolution catalytic performance, has mild reaction conditions, easy control, simple reaction process and low raw material price, and is suitable for large-scale production.
Drawings
FIG. 1a is a Scanning Electron Microscope (SEM) schematic of example 1 of the invention, showing the MoS formed2Has a sheet-like structure.
FIG. 1b is a Scanning Electron Microscope (SEM) schematic diagram of example 2 of the invention, which shows that ammonia water treatment has a great influence on the morphology.
FIG. 2a is a schematic contact angle diagram of example 1 of the present invention, showing the MoS formed2The hydrophilicity is poor.
Fig. 2b is a schematic diagram of the contact angle of example 2 of the present invention, which shows that the material treated with ammonia has excellent hydrophilicity.
FIG. 3 is a graph showing the oxygen evolution performance of examples 1 and 2 of the present invention, and shows that the prepared material has excellent electrocatalytic oxygen evolution performance.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
The first step is as follows: sequentially carrying out ultrasonic treatment on carbon cloth (3 x 3cm) in acetone, ethanol and water for 10 minutes for later use;
the second step is that: mixing ammonium molybdate and thiourea in water according to a ratio, wherein the molar ratio of the ammonium molybdate to the thiourea is 1:5, and stirring until the ammonium molybdate and the thiourea are completely dissolved to obtain a uniform solution, wherein the volume of the water is 35 mL;
the third step: transferring the uniformly stirred solution to a reaction kettle with a stainless steel substrate, putting the reaction kettle into carbon cloth subjected to ultrasonic treatment, and putting the reaction kettle in an air-blowing drying oven to keep the temperature of 180 ℃ for 12 hours; cooling to room temperature, taking out the carbon cloth, washing with ethanol and water in sequence, and drying to obtain MoS2A nano-platelet catalyst.
Example 2
The first step is as follows: sequentially carrying out ultrasonic treatment on carbon cloth (3 x 3cm) in acetone, ethanol and water for 10 minutes for later use;
the second step is that: mixing ammonium molybdate and thiourea in water according to a ratio, wherein the molar ratio of the ammonium molybdate to the thiourea is 1:5, and stirring until the ammonium molybdate and the thiourea are completely dissolved to obtain a uniform solution, wherein the volume of the water is 35 mL;
the third step: transferring the uniformly stirred solution to a reaction kettle with a stainless steel substrate, putting the reaction kettle into carbon cloth subjected to ultrasonic treatment, and putting the reaction kettle in an air-blowing drying oven to keep the temperature of 180 ℃ for 12 hours; cooling to room temperature, taking out the carbon cloth, washing with ethanol and water in sequence, and drying to obtain MoS2A nanosheet catalyst.
The fourth step: 10mL of ammonia water is put into a reaction kettle, and MoS is put into the reaction kettle2The nano-sheet is arranged above the ammonia water and is not connected with the ammonia waterAnd (3) keeping the reaction kettle in a forced air drying oven at 150 ℃ for 12 hours, cooling to room temperature, taking out the carbon cloth, sequentially washing with ethanol and water, and drying to obtain the heteroatom nitrogen surface modified MoS2A nanomaterial catalyst.
Example 3
The first step is as follows: sequentially carrying out ultrasonic treatment on carbon cloth (3 x 3cm) in acetone, ethanol and water for 10 minutes for later use;
the second step is that: mixing ammonium molybdate and thiourea in water according to a ratio, wherein the molar ratio of the ammonium molybdate to the thiourea is 1:5, and stirring until the ammonium molybdate and the thiourea are completely dissolved to obtain a uniform solution, wherein the volume of the water is 35 mL;
the third step: transferring the uniformly stirred solution to a reaction kettle with a stainless steel substrate, putting the reaction kettle into carbon cloth subjected to ultrasonic treatment, and putting the reaction kettle in an air-blowing drying oven to keep the temperature of 180 ℃ for 12 hours; cooling to room temperature, taking out the carbon cloth, washing with ethanol and water in sequence, and drying to obtain MoS2A nanosheet catalyst.
The fourth step: 5mL of ammonia water is placed in a reaction kettle, and MoS is added2Placing the nanosheet above ammonia water without contacting with the ammonia water, placing the reaction kettle in a forced air drying oven at 150 ℃ for 8 hours, cooling to room temperature, taking out the carbon cloth, sequentially washing with ethanol and water, and drying to obtain the heteroatom nitrogen surface modified MoS2A nanomaterial catalyst.
Example 4
The first step is as follows: sequentially carrying out ultrasonic treatment on carbon cloth (3 x 3cm) in acetone, ethanol and water for 10 minutes for later use;
the second step is that: mixing ammonium molybdate and thiourea in water according to a ratio, wherein the molar ratio of the ammonium molybdate to the thiourea is 1:5, and stirring until the ammonium molybdate and the thiourea are completely dissolved to obtain a uniform solution, wherein the volume of the water is 35 mL;
the third step: transferring the uniformly stirred solution to a reaction kettle with a stainless steel substrate, putting the reaction kettle into carbon cloth subjected to ultrasonic treatment, and putting the reaction kettle in an air-blowing drying oven to keep the temperature of 180 ℃ for 12 hours; cooling to room temperature, taking out the carbon cloth, washing with ethanol and water in sequence, and drying to obtain MoS2A nanosheet catalyst.
The fourth step: 10mL of ammonia water is placed in a reactionReaction in a kettle, adding MoS2Placing the nanosheet above ammonia water without contacting with the ammonia water, placing the reaction kettle in a forced air drying oven, keeping the temperature at 180 ℃ for 18 hours, cooling to room temperature, taking out the carbon cloth, sequentially washing with ethanol and water, and drying to obtain the heteroatom nitrogen surface modified MoS2A nanomaterial catalyst.
Example 5
The first step is as follows: sequentially carrying out ultrasonic treatment on carbon cloth (3 x 3cm) in acetone, ethanol and water for 10 minutes for later use;
the second step is that: mixing ammonium molybdate and thiourea in water according to a ratio, wherein the molar ratio of the ammonium molybdate to the thiourea is 1:5, and stirring until the ammonium molybdate and the thiourea are completely dissolved to obtain a uniform solution, wherein the volume of the water is 35 mL;
the third step: transferring the uniformly stirred solution to a reaction kettle with a stainless steel substrate, putting the reaction kettle into carbon cloth subjected to ultrasonic treatment, and putting the reaction kettle in an air-blowing drying oven to keep the temperature of 180 ℃ for 12 hours; cooling to room temperature, taking out the carbon cloth, washing with ethanol and water in sequence, and drying to obtain MoS2A nanosheet catalyst.
The fourth step: 15mL of ammonia water is put into a reaction kettle, and MoS is put into the reaction kettle2Placing the nanosheet above ammonia water without contacting with the ammonia water, placing the reaction kettle in a forced air drying oven, keeping the temperature at 90 ℃ for 12 hours, cooling to room temperature, taking out the carbon cloth, sequentially washing with ethanol and water, and drying to obtain the heteroatom nitrogen surface modified MoS2A nanomaterial catalyst.
Example 6
The product prepared in the example was tested for oxygen evolution performance, the prepared carbon cloth was fixed on an electrode holder as a working electrode, and then the oxygen evolution performance was tested on an electrochemical workstation using a three-electrode method (reversible hydrogen as a reference electrode, carbon rod as an auxiliary electrode).
Claims (5)
1. Heteroatom nitrogen surface modification MoS2The preparation and application of the nano material comprise the following steps:
(1) sequentially carrying out ultrasonic treatment on carbon cloth (3 x 3cm) in acetone, ethanol and water for 10 minutes for later use;
(2) mixing ammonium molybdate and thiourea in water according to a ratio, wherein the molar ratio of the ammonium molybdate to the thiourea is 1:5, and stirring until the ammonium molybdate and the thiourea are completely dissolved to obtain a uniform solution;
(3) transferring the uniformly stirred solution to a reaction kettle with a stainless steel substrate, putting the reaction kettle into carbon cloth subjected to ultrasonic treatment, and putting the reaction kettle in an air-blowing drying oven to keep the temperature of 180 ℃ for 12 hours; cooling to room temperature, taking out the carbon cloth, washing with ethanol and water in sequence, and drying to obtain MoS2Nanosheets;
(4) the obtained MoS2Adding nanosheets and ammonia water with different volumes into a reaction kettle with a stainless steel substrate, and adding MoS2The nanosheet is above the ammonia and is not in contact with the ammonia. Putting the reaction kettle in a blast drying oven for high-temperature reaction, cooling to room temperature, taking out the carbon cloth, sequentially washing with ethanol and water, and drying to obtain the heteroatom nitrogen surface modified MoS2And (3) nano materials.
2. The method according to claim 1, wherein the molar ratio of the transition metal salt to thiourea is 1: 5.
3. The method according to claim 1, wherein the ammonia water used in step (4) has a volume of 5mL, 10mL, or 15 mL.
4. The application of the material as claimed in claim 1 to electrocatalyst, characterized in that the high temperature reaction temperature in step (4) is 90 ℃, 150 ℃, 180 ℃.
5. The application of the material as claimed in claim 1 to an electrocatalyst, wherein the high temperature reaction time in step (4) is 8 hours, 12 hours, 18 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910837039.1A CN110787820B (en) | 2019-09-05 | 2019-09-05 | Heteroatom nitrogen surface modification MoS2Preparation and application of nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910837039.1A CN110787820B (en) | 2019-09-05 | 2019-09-05 | Heteroatom nitrogen surface modification MoS2Preparation and application of nano material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110787820A true CN110787820A (en) | 2020-02-14 |
| CN110787820B CN110787820B (en) | 2021-06-29 |
Family
ID=69427198
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910837039.1A Active CN110787820B (en) | 2019-09-05 | 2019-09-05 | Heteroatom nitrogen surface modification MoS2Preparation and application of nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110787820B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111185201A (en) * | 2020-02-25 | 2020-05-22 | 辽宁大学 | Rhenium-doped molybdenum sulfide nanosheet/carbon cloth composite material, preparation method thereof and application thereof in hydrogen production by electrocatalysis of water |
| CN113793763A (en) * | 2021-09-17 | 2021-12-14 | 安徽工业技术创新研究院六安院 | MOS for all-solid-state flexible supercapacitor2Preparation method of-RCC composite electrode |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104028293A (en) * | 2014-06-24 | 2014-09-10 | 常州大学 | Method for preparing low-temperature nitrogen-doped graphene supported nano Pd hydrogenation catalyst |
| KR101623736B1 (en) * | 2015-05-29 | 2016-05-24 | 이화여자대학교 산학협력단 | Molybdenum disulphide nanosheet and preparing method of the same |
| CN107442138A (en) * | 2017-06-15 | 2017-12-08 | 江苏大学 | A kind of preparation method of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction material of molybdenum disulfide/carbon cloth |
| CN108425128A (en) * | 2018-03-12 | 2018-08-21 | 华南理工大学 | A kind of porous amino functional graphene catalysis material and preparation and application |
| CN110075872A (en) * | 2019-04-28 | 2019-08-02 | 湖南大学 | Utilize electrochemical activation molybdenum disulfide/carbon composite electrocatalytic hydrogen evolution method |
| CN110155998A (en) * | 2019-05-13 | 2019-08-23 | 东南大学 | A kind of ribbon nitrogen-doped graphene and its preparation method and application |
-
2019
- 2019-09-05 CN CN201910837039.1A patent/CN110787820B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104028293A (en) * | 2014-06-24 | 2014-09-10 | 常州大学 | Method for preparing low-temperature nitrogen-doped graphene supported nano Pd hydrogenation catalyst |
| KR101623736B1 (en) * | 2015-05-29 | 2016-05-24 | 이화여자대학교 산학협력단 | Molybdenum disulphide nanosheet and preparing method of the same |
| CN107442138A (en) * | 2017-06-15 | 2017-12-08 | 江苏大学 | A kind of preparation method of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction material of molybdenum disulfide/carbon cloth |
| CN108425128A (en) * | 2018-03-12 | 2018-08-21 | 华南理工大学 | A kind of porous amino functional graphene catalysis material and preparation and application |
| CN110075872A (en) * | 2019-04-28 | 2019-08-02 | 湖南大学 | Utilize electrochemical activation molybdenum disulfide/carbon composite electrocatalytic hydrogen evolution method |
| CN110155998A (en) * | 2019-05-13 | 2019-08-23 | 东南大学 | A kind of ribbon nitrogen-doped graphene and its preparation method and application |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111185201A (en) * | 2020-02-25 | 2020-05-22 | 辽宁大学 | Rhenium-doped molybdenum sulfide nanosheet/carbon cloth composite material, preparation method thereof and application thereof in hydrogen production by electrocatalysis of water |
| CN111185201B (en) * | 2020-02-25 | 2022-07-19 | 辽宁大学 | Rhenium-doped molybdenum sulfide nanosheet/carbon cloth composite material, preparation method thereof and application thereof in hydrogen production by electrocatalysis of water |
| CN113793763A (en) * | 2021-09-17 | 2021-12-14 | 安徽工业技术创新研究院六安院 | MOS for all-solid-state flexible supercapacitor2Preparation method of-RCC composite electrode |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110787820B (en) | 2021-06-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107020075B (en) | Simple substance bismuth catalyst for electrochemical reduction of carbon dioxide and preparation and application thereof | |
| CN109321933B (en) | Preparation method and application of MOF/carbon dot nanocomposite catalyst | |
| CN109628951B (en) | Nickel sulfide hydrogen evolution electrocatalyst and preparation method and application thereof | |
| CN113652707B (en) | Nickel telluride hydrogen evolution catalyst and preparation method and application thereof | |
| CN113136597B (en) | Copper-tin composite material and preparation method and application thereof | |
| CN113967480A (en) | Preparation method and application of phosphorus-doped molybdenum disulfide/porous carbon composite material | |
| CN110787820B (en) | Heteroatom nitrogen surface modification MoS2Preparation and application of nano material | |
| CN111644195A (en) | Preparation method of catalyst for electrocatalytic degradation of hydrazine environmental pollutants and hydrogen production | |
| CN110629248A (en) | Fe-doped Ni (OH)2Preparation method of/Ni-BDC electrocatalyst | |
| CN112023944A (en) | Preparation method for in-situ synthesis of rhenium and rhenium disulfide heterostructure composite material | |
| CN116876019A (en) | High-efficiency dual-function electrocatalyst for producing hydrogen by electrolyzing ammonia and preparation method thereof | |
| CN111589459A (en) | Bifunctional catalyst for efficiently electrolyzing water, and preparation method and application thereof | |
| CN114481209A (en) | Preparation method of Ru-modified iron-based self-supporting hydrogen evolution electrode | |
| CN114892206A (en) | Multi-metal nitride heterojunction nanorod array composite electrocatalyst and preparation method and application thereof | |
| CN113584504A (en) | Ru/RuO2/MoO2Composite material and preparation method and application thereof | |
| CN114045521A (en) | Preparation method of nano-scale electrocatalyst | |
| CN113322478A (en) | Two-dimensional bimetal organic framework synthesized by electrochemical method and application thereof in electrocatalytic oxygen evolution | |
| Liu et al. | Self‐supported bimetallic array superstructures for high‐performance coupling electrosynthesis of formate and adipate | |
| CN114232017B (en) | Silver selenide nano catalyst and preparation method and application thereof | |
| CN115029709B (en) | Cobalt-nickel metal sulfide bifunctional electrocatalyst and preparation method and application thereof | |
| CN114134537B (en) | Sulfur-doped molybdenum compound self-supporting electrode, preparation method and method for catalytically decomposing water | |
| CN115057479B (en) | CoAl (cobalt aluminum alloy) 2 O 4 Preparation method of electrocatalytic material and application of ENRR thereof | |
| CN115449830A (en) | Preparation of ultrathin Mo-Ni sulfide and application of ultrathin Mo-Ni sulfide in electrocatalytic oxidation furfuraldehyde coupling hydrogen production | |
| CN116145184A (en) | Preparation method and application of graphene-based composite binary metal sulfide electrocatalyst | |
| CN117265585A (en) | Cobalt ruthenium oxide catalytic electrode for nitrate radical reduction and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |