CN110773162A - Preparation method and application of carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal - Google Patents
Preparation method and application of carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal Download PDFInfo
- Publication number
- CN110773162A CN110773162A CN201911065092.0A CN201911065092A CN110773162A CN 110773162 A CN110773162 A CN 110773162A CN 201911065092 A CN201911065092 A CN 201911065092A CN 110773162 A CN110773162 A CN 110773162A
- Authority
- CN
- China
- Prior art keywords
- molybdenum oxide
- carbon
- coated
- noble metal
- oxide compound
- 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.)
- Pending
Links
- 229910000476 molybdenum oxide Inorganic materials 0.000 title claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 32
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 18
- -1 molybdenum oxide compound Chemical class 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000011343 solid material Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000002135 nanosheet Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229960003638 dopamine Drugs 0.000 claims abstract description 8
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims abstract description 8
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000000967 suction filtration Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 11
- 239000007769 metal material Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000010411 electrocatalyst Substances 0.000 claims description 5
- 239000007983 Tris buffer Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229960000281 trometamol Drugs 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000004502 linear sweep voltammetry Methods 0.000 description 5
- 238000013461 design Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000005078 molybdenum compound Substances 0.000 description 1
- 150000002752 molybdenum compounds Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000010963 scalable process Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000001075 voltammogram 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/652—Chromium, molybdenum or tungsten
- B01J23/6525—Molybdenum
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention provides a preparation method and application of a carbon-coated two-dimensional layered molybdenum oxide compound supported noble metal, which comprises the following steps: weighing a certain amount of molybdenum oxide and calcining in air; adding the obtained nanosheets into a mixed solution of water and ethanol, ultrasonically dispersing uniformly, adding tris (hydroxymethyl) aminomethane and dopamine, reacting at room temperature, and then performing suction filtration, washing and drying; dispersing the dried material in an aqueous solution, uniformly dispersing by using ultrasonic waves, adding a certain amount of ruthenium chloride solution, stirring while heating to a certain temperature, and evaporating water to dryness to obtain a solid material; the solid material obtained is then mixed with a certain amount of melamine and treated under inert protection. The preparation method is simple, convenient to operate, low in cost, beneficial to industrial production and has a certain use value.
Description
Technical Field
The invention relates to the field of materials, in particular to a preparation method and application of a carbon-coated two-dimensional layered molybdenum oxide compound supported noble metal.
Background
Hydrogen has attracted considerable attention in recent years by researchers as a potential green and sustainable alternative to traditional fossil energy sources. Electrochemical water splitting without other byproducts is considered an efficient and sustainable technology for the generation of hydrogen. Disappointingly, the rate of hydrogen generation and the consumption of electrical energy are severely hampered by the large overpotential of the electrode reactions. At present, Pt-based noble metals are the best choice for lowering the overpotential, but the high cost and low durability cannot meet the requirement of large-scale application for hydrogen production. Therefore, the development of efficient and robust catalysts for HER is a significant challenge.
Among various non-noble metal catalysts, carbon-coated two-dimensional layered molybdenum oxide compounds supporting noble metals are receiving much attention due to their excellent catalytic activity, low cost and excellent durability. Thus, the design of 2D molybdenum-based compounds with high conductivity and rich active sites remains a challenge. In addition to two-dimensional morphology, the formation of porous structures is an effective way to optimize the catalytic performance of HER catalysts. Such a structural design will facilitate the diffusion of the electrolyte and the release of the generated hydrogen. Particularly, the controllable assembly of the heteroatom loaded on the carbon atom and the molybdenum compound is also an important way for improving the conductivity and reducing the size of the metal nano particle, so that the electron transfer in the catalytic process can be accelerated, and abundant active sites can be provided.
Disclosure of Invention
The invention provides a preparation method and application of a carbon-coated two-dimensional layered molybdenum oxide compound supported noble metal, and aims to solve the problems.
The technical scheme of the invention is realized as follows:
a preparation method of carbon-coated two-dimensional layered molybdenum oxide compound supported noble metal comprises the following steps: weighing a certain amount of molybdenum oxide and calcining in air; adding the obtained nanosheets into a mixed solution of water and ethanol, ultrasonically dispersing uniformly, adding tris (hydroxymethyl) aminomethane and dopamine, reacting at room temperature, and then performing suction filtration, washing and drying; dispersing the dried material in an aqueous solution, uniformly dispersing by using ultrasonic waves, adding a certain amount of ruthenium chloride solution, stirring while heating to a certain temperature, and evaporating water to dryness to obtain a solid material; the solid material obtained is then mixed with a certain amount of melamine and treated under inert protection.
Optionally, the calcination condition of the molybdenum oxide is to heat up to 600-700 ℃ at a heating rate of 1-2 ℃/min in the air and keep the temperature for 10-12 h.
Optionally, mixing the obtained nanosheets with water and ethanol at a ratio of 1:1:1, adding Tris and dopamine at a ratio of 1:2.45 and 1:2.
optionally, the drying condition is that the drying oven is placed for 2 to 3 hours at the temperature of between 60 and 80 ℃.
Alternatively, the concentration of the ruthenium chloride solution is from 8mg/ml to 12 mg/ml.
Optionally, the drying condition is that after stirring for 20min-30min, the temperature is gradually increased to 75-85 ℃, and the temperature is kept unchanged until the solution is dried by distillation.
Alternatively, the mixing ratio of the solid material to melamine is 1: 7.5.
Optionally, the inert gas protection treatment condition is that the temperature is respectively raised to 300/500/700/900 ℃ at the temperature raising rate of 5 ℃/min-10 ℃/min in a tube furnace filled with argon, and the temperature is kept for 1.5h-2.5 h.
The carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal material is prepared based on the preparation method.
The application of the carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal material in preparing the electrocatalyst is also within the protection scope of the invention.
The invention has the beneficial effects that: a series of catalysts of carbon-coated two-dimensional layered molybdenum oxide compound supported noble metal materials are synthesized by a hydrothermal-pyrolysis method, the chemical composition of the catalysts is easy to adjust, and the problems of few active sites, low diffusion speed of electrolyte, agglomeration and the like of the traditional catalysts are solved. In particular, melamine is used as a carbon and nitrogen source to form an N-doped carbon matrix, further enhancing conductivity and mitigating agglomeration. The electrocatalyst obtained by the method has excellent electrocatalysis performances such as smaller overpotential and lower Tafel slope; more importantly, this simple and scalable process provides a route for future design and preparation of other molybdenum metal-based electrocatalysts; the preparation method is simple, convenient to operate, low in cost, beneficial to industrial production and has a certain use value.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an SEM image of an in-air calcined molybdenum oxide prepared according to an example of the present invention.
FIG. 2 shows that the noble metal supported by the carbon-coated two-dimensional layered molybdenum oxide compound prepared in the embodiment of the present invention is at 0.5mol/LH
2SO
4Linear Sweep Voltammetry (LSV) profile of the catalytic hydrogen evolution reaction in solution.
Fig. 3 is a Tafel slope diagram of the carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal prepared in the embodiment of the present invention.
FIG. 4 shows that the noble metal supported by the carbon-coated two-dimensional layered molybdenum oxide compound prepared in the embodiment of the present invention is at 0.5mol/LH
2SO
4Linear Sweep Voltammetry (LSV) plots before and after 10000 cycles of circulation in solution.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
As shown in fig. 1 to 4, the application discloses a preparation method of a carbon-coated two-dimensional layered molybdenum oxide compound supported noble metal, which comprises the following steps: weighing a certain amount of molybdenum oxide and calcining in air; adding the obtained nanosheets into a mixed solution of water and ethanol, ultrasonically dispersing uniformly, adding tris (hydroxymethyl) aminomethane and dopamine, reacting at room temperature, and then performing suction filtration, washing and drying; dispersing the dried material in an aqueous solution, uniformly dispersing by using ultrasonic waves, adding a certain amount of ruthenium chloride solution, stirring while heating to a certain temperature, and evaporating water to dryness to obtain a solid material; the solid material obtained is then mixed with a certain amount of melamine and treated under inert protection.
Optionally, the calcination condition of the molybdenum oxide is to heat up to 600-700 ℃ at a heating rate of 1-2 ℃/min in the air and keep the temperature for 10-12 h.
Optionally, mixing the obtained nanosheets with water and ethanol at a ratio of 1:1:1, adding Tris and dopamine at a ratio of 1:2.45 and 1:2.
alternatively, the reaction conditions at room temperature are preferably kept at 25 ℃ on a stirrer and the reaction is stirred for 24 hours.
Optionally, the suction filtration conditions are vacuum filtration.
Optionally, the drying condition is that the drying oven is placed for 2 to 3 hours at the temperature of between 60 and 80 ℃.
Alternatively, the concentration of the ruthenium chloride solution is from 8mg/ml to 12 mg/ml.
Optionally, the drying condition is that after stirring for 20min-30min, the temperature is gradually increased to 75-85 ℃, and the temperature is kept unchanged until the solution is dried by distillation. Preferably, occasional sonication is used during the evaporation to ensure uniform dispersion of the solution.
Alternatively, the mixing ratio of the solid material to melamine is 1: 7.5. Preferably, the mixing is carried out under conditions of grinding uniformity.
Optionally, the inert gas protection treatment condition is that the temperature is respectively raised to 300/500/700/900 ℃ at the temperature raising rate of 5 ℃/min-10 ℃/min in a tube furnace filled with argon, and the temperature is kept for 1.5h-2.5 h.
The carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal material is prepared based on the preparation method.
The application of the carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal material in preparing the electrocatalyst is also within the protection scope of the invention.
With the above examples, the preferred specific preparation steps are as follows:
weighing 100mg of molybdenum oxide, heating to 600 ℃ in air at a heating rate of 1 ℃/min, and preserving heat for 10 h; then weighing 50mg of the obtained nanosheets, adding the nanosheets into 50ml of mixed solution of water and ethanol respectively, adding 121mg of tris (hydroxymethyl) aminomethane and 100mg of dopamine after ultrasonic dispersion is uniform, stirring at room temperature, keeping the temperature at 25 ℃ for reaction for 24 hours, carrying out vacuum filtration, washing, and drying in a 60 ℃ oven; weighing 30mg of the dried material, dispersing the weighed material in 10ml of aqueous solution, uniformly dispersing by ultrasonic, adding 0.5ml (variable) of ruthenium chloride solution (10mg/ml), stirring for 30min, heating to 75 ℃, keeping the temperature unchanged, and stirring until water is evaporated to dryness to obtain a solid material; and finally, grinding and mixing the obtained solid material 20mg and 150mg of melamine, putting the mixture into a quartz boat and a tubular furnace, heating to 500 ℃ at the heating rate of 5 ℃/min under the argon atmosphere, keeping the temperature for 2 hours, and naturally cooling to room temperature to obtain the carbon-coated two-dimensional layered molybdenum oxide compound-loaded noble metal material.
The SEM image of the above-obtained molybdenum oxide calcined in air is shown in fig. 1, and it can be seen that the molybdenum oxide calcined in air has a two-dimensional sheet structure.
The noble metal supported by the obtained carbon-coated two-dimensional layered molybdenum oxide compound is 0.5mol/L H
2SO
4The Linear Sweep Voltammetry (LSV) graph of the catalytic hydrogen evolution reaction in the solution is shown in figure 2, and the graph can show that the material has lower initial potential and overpotential, which indicates that the material has good catalytic performance.
The Tafel slope diagram of the carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal is shown in FIG. 3, and a smaller Tafel slope can be seen from the Tafel slope diagram, which shows that the material has a better catalytic kinetic speed.
The noble metal supported by the obtained carbon-coated two-dimensional layered molybdenum oxide compound is 0.5mol/L H
2SO
4Linear Sweep Voltammogram (LSV) before and after 10000 cycles of circulation in solution, as shown in fig. 4. It can be seen that the material is at 0.5mol/LH
2SO
4LSV graphs before and after 10000 CV cycles in the solution are almost the same, which shows that the material has better stability.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of carbon-coated two-dimensional layered molybdenum oxide compound supported noble metal is characterized by comprising the following steps: weighing a certain amount of molybdenum oxide and calcining in air; adding the obtained nanosheets into a mixed solution of water and ethanol, ultrasonically dispersing uniformly, adding tris (hydroxymethyl) aminomethane and dopamine, reacting at room temperature, and then performing suction filtration, washing and drying; dispersing the dried material in an aqueous solution, uniformly dispersing by using ultrasonic waves, adding a certain amount of ruthenium chloride solution, stirring while heating to a certain temperature, and evaporating water to dryness to obtain a solid material; the solid material obtained is then mixed with a certain amount of melamine and treated under inert protection.
2. The method for preparing the noble metal supported by the carbon-coated two-dimensional layered molybdenum oxide compound as claimed in claim 1, wherein the molybdenum oxide is calcined under the conditions of heating to 600-700 ℃ at a heating rate of 1-2 ℃/min in air and keeping the temperature for 10-12 h.
3. The method for preparing the noble metal supported by the carbon-coated two-dimensional layered molybdenum oxide compound according to claim 1, wherein the obtained nanosheets are mixed with water and ethanol at a ratio of 1:1:1 to 1, and the added tris and dopamine are mixed with the nanosheets at a ratio of 1:2.45 to 1:2.
4. the method for preparing the noble metal supported by the carbon-coated two-dimensional layered molybdenum oxide compound as claimed in claim 1, wherein the drying is performed in an oven at 60-80 ℃ for 2-3 h.
5. The method for preparing a noble metal supported by a carbon-coated two-dimensional layered molybdenum oxide compound according to claim 1, wherein the concentration of the ruthenium chloride solution is 8mg/ml to 12 mg/ml.
6. The method for preparing the carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal according to claim 1, wherein the evaporation is performed under the condition that after stirring for 20min to 30min, the temperature is gradually increased to 75 ℃ to 85 ℃, and the temperature is kept unchanged until the solution is evaporated to dryness.
7. The method for preparing a noble metal supported by a carbon-coated two-dimensional layered molybdenum oxide compound according to claim 6, wherein the mixing ratio of the solid material to the melamine is 1: 7.5.
8. The method for preparing the carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal according to claim 1, wherein the inert gas is used for protection under the conditions that the temperature is respectively raised to 300/500/700/900 ℃ at the temperature raising rate of 5 ℃/min-10 ℃/min in a tube furnace filled with argon and is kept for 1.5h-2.5 h.
9. The preparation method according to any one of claims 1 to 8, wherein the carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal material is prepared.
10. Use of the carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal material according to claim 9 in the preparation of an electrocatalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911065092.0A CN110773162A (en) | 2019-11-04 | 2019-11-04 | Preparation method and application of carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911065092.0A CN110773162A (en) | 2019-11-04 | 2019-11-04 | Preparation method and application of carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110773162A true CN110773162A (en) | 2020-02-11 |
Family
ID=69388791
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911065092.0A Pending CN110773162A (en) | 2019-11-04 | 2019-11-04 | Preparation method and application of carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110773162A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387385A (en) * | 2021-08-16 | 2021-09-14 | 河南师范大学 | Preparation method and application of two-dimensional amorphous molybdenum-based oxide composite material with oxygen-rich vacancy defects |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829588A (en) * | 2010-05-27 | 2010-09-15 | 复旦大学 | Synthetic method of load type molybdenum carbide catalyst |
| CN104733716A (en) * | 2014-12-04 | 2015-06-24 | 辽宁石油化工大学 | Molybdenum oxide/nitrogen-doped carbon composite electrode material and preparation method thereof |
| CN104752074A (en) * | 2015-04-21 | 2015-07-01 | 扬州大学 | Molybdenum oxide/carbon sphere composite material preparation method |
| CN106129407A (en) * | 2016-08-29 | 2016-11-16 | 上海大学 | MoS2the synthetic method of@graphene composite nano material |
| CN107335433A (en) * | 2017-08-08 | 2017-11-10 | 郑州大学 | A kind of preparation method for aoxidizing molybdenum base efficient electric catalytic hydrogen evolution catalyst |
| CN107337473A (en) * | 2017-07-25 | 2017-11-10 | 济南大学 | The growth in situ MoO on earthenware3The method and gas sensor of nanometer sheet |
| CN108404950A (en) * | 2017-02-09 | 2018-08-17 | 邢台旭阳科技有限公司 | A method of handling industrial wastewater for the catalyst of catalytic ozonation, preparation method and using it |
| CN108682873A (en) * | 2018-05-28 | 2018-10-19 | 南京晓庄学院 | A kind of Ru-MoO3-x/ rGO composite material and preparation methods and application |
| CN110252335A (en) * | 2019-05-31 | 2019-09-20 | 苏州大学 | A kind of carbon-coating nickel ruthenium nano material and its preparation method and application |
-
2019
- 2019-11-04 CN CN201911065092.0A patent/CN110773162A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829588A (en) * | 2010-05-27 | 2010-09-15 | 复旦大学 | Synthetic method of load type molybdenum carbide catalyst |
| CN104733716A (en) * | 2014-12-04 | 2015-06-24 | 辽宁石油化工大学 | Molybdenum oxide/nitrogen-doped carbon composite electrode material and preparation method thereof |
| CN104752074A (en) * | 2015-04-21 | 2015-07-01 | 扬州大学 | Molybdenum oxide/carbon sphere composite material preparation method |
| CN106129407A (en) * | 2016-08-29 | 2016-11-16 | 上海大学 | MoS2the synthetic method of@graphene composite nano material |
| CN108404950A (en) * | 2017-02-09 | 2018-08-17 | 邢台旭阳科技有限公司 | A method of handling industrial wastewater for the catalyst of catalytic ozonation, preparation method and using it |
| CN107337473A (en) * | 2017-07-25 | 2017-11-10 | 济南大学 | The growth in situ MoO on earthenware3The method and gas sensor of nanometer sheet |
| CN107335433A (en) * | 2017-08-08 | 2017-11-10 | 郑州大学 | A kind of preparation method for aoxidizing molybdenum base efficient electric catalytic hydrogen evolution catalyst |
| CN108682873A (en) * | 2018-05-28 | 2018-10-19 | 南京晓庄学院 | A kind of Ru-MoO3-x/ rGO composite material and preparation methods and application |
| CN110252335A (en) * | 2019-05-31 | 2019-09-20 | 苏州大学 | A kind of carbon-coating nickel ruthenium nano material and its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| ZHE LV ET AL.: "Well-dispersed molybdenum nitrides on a nitrogen-doped carbon matrix for highly efficient hydrogen evolution in alkaline media", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| 程永: "高性能纳米析氢催化剂的制备和应用研究", 《中国优秀硕士论文电子期刊网》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387385A (en) * | 2021-08-16 | 2021-09-14 | 河南师范大学 | Preparation method and application of two-dimensional amorphous molybdenum-based oxide composite material with oxygen-rich vacancy defects |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110350211B (en) | Preparation method of ZIF-8 derived N, S-codoped non-metallic carbon-based nano oxygen reduction electrocatalyst | |
| CN110739463B (en) | Preparation method and application of bimetal organic framework composite material | |
| CN105344369B (en) | The nitrogen co-doped charcoal base oxygen reduction catalyst of cobalt and its preparation and application with three-dimensional graded porous structure | |
| CN110075902B (en) | Defective covalent triazine framework material derivative material catalyst and preparation method and application thereof | |
| CN106602092B (en) | Preparation method and application of single-walled carbon nanotube hollow sphere oxygen reduction catalyst | |
| CN107399729A (en) | A kind of bimetallic MOFs nitrogenous graphitized carbon material | |
| CN112652780B (en) | Fe/Fe 3 Preparation method of C nano-particle loaded porous nitrogen-doped carbon-based oxygen reduction catalyst | |
| CN103372428A (en) | Preparation method of nitrogen-doped graphene loaded platinum nano-particle catalyst | |
| CN111659423A (en) | Preparation method and application method of cobalt-tellurium diatomic site catalyst | |
| CN111450851B (en) | Preparation method of sulfur-doped cobalt-based nano oxygen evolution electrocatalyst | |
| CN113054210A (en) | Oxygen reduced iron-iron nitride @ monoatomic iron and nitrogen co-doped amorphous carbon-carbon black composite catalyst and preparation and application thereof | |
| CN112357902A (en) | Mesoporous carbon material with high specific surface area, and preparation method and application thereof | |
| CN115896848A (en) | Nitrogen/sulfur co-doped porous carbon loaded zinc monoatomic/metallic copper series catalyst and preparation method and application thereof | |
| CN110649276A (en) | Based on N2Plasma-etched three-dimensional porous nitrogen-doped carbon nanotube electrocatalyst and preparation method thereof | |
| CN113285079A (en) | Double-heteroatom-doped CoFe/SNC composite material and preparation and application thereof | |
| CN111450842B (en) | Preparation method of micro-flower structure black lead-copper ore phase metal oxide electrocatalyst, electrocatalyst and application thereof | |
| CN110773162A (en) | Preparation method and application of carbon-coated two-dimensional layered molybdenum oxide compound-supported noble metal | |
| CN108963283B (en) | High-dispersion load type core-shell structure Pd @ Ni/WC direct alcohol fuel cell catalyst and preparation method thereof | |
| CN108963275B (en) | Non-metal self-supporting air electrode and preparation method thereof | |
| CN114653371B (en) | Preparation method of atomic-level dispersed metal catalyst supported by high-defect boron nitride | |
| CN110055556A (en) | Hydrogen evolution reaction catalyst and preparation method and application thereof | |
| CN111514911B (en) | Carbon-doped WP nanosheet electrocatalyst with mesoporous structure and preparation method thereof | |
| CN110550619B (en) | Nano carbon material, preparation method thereof and application thereof in fuel cell | |
| CN113764684A (en) | Preparation method of fuel cell cathode catalyst material | |
| CN112331863A (en) | Non-noble metal oxygen reduction electrocatalyst W/N/C 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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200211 |
|
| RJ01 | Rejection of invention patent application after publication |