CN114411199A - Flower-shaped MoSe2-CuPd nano composite material and synthetic method and application thereof - Google Patents
Flower-shaped MoSe2-CuPd nano composite material and synthetic method and application thereof Download PDFInfo
- Publication number
- CN114411199A CN114411199A CN202111592025.1A CN202111592025A CN114411199A CN 114411199 A CN114411199 A CN 114411199A CN 202111592025 A CN202111592025 A CN 202111592025A CN 114411199 A CN114411199 A CN 114411199A
- Authority
- CN
- China
- Prior art keywords
- cupd
- flower
- mose
- shaped
- nano
- 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
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000010189 synthetic method Methods 0.000 title description 2
- 229910016001 MoSe Inorganic materials 0.000 claims abstract description 19
- 239000002135 nanosheet Substances 0.000 claims abstract description 17
- 239000002086 nanomaterial Substances 0.000 claims abstract description 6
- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- ZKXWKVVCCTZOLD-UHFFFAOYSA-N copper;4-hydroxypent-3-en-2-one Chemical compound [Cu].CC(O)=CC(C)=O.CC(O)=CC(C)=O ZKXWKVVCCTZOLD-UHFFFAOYSA-N 0.000 claims description 10
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 claims description 10
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- HYAVEDMFTNAZQE-UHFFFAOYSA-N (benzyldiselanyl)methylbenzene Chemical compound C=1C=CC=CC=1C[Se][Se]CC1=CC=CC=C1 HYAVEDMFTNAZQE-UHFFFAOYSA-N 0.000 claims description 8
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 239000011733 molybdenum Substances 0.000 claims description 8
- 150000001412 amines Chemical class 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 2
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 2
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 claims description 2
- 230000009471 action Effects 0.000 claims description 2
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 11
- 239000002131 composite material Substances 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 238000001308 synthesis method Methods 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000012295 chemical reaction liquid Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 229910021397 glassy carbon Inorganic materials 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 229920000557 Nafion® Polymers 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
- C25B11/097—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds comprising two or more noble metals or noble metal alloys
-
- 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
- C25B1/04—Hydrogen or oxygen by electrolysis of water
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses flower-shaped MoSe2-CuPd nano composite material and synthesis method and application thereof, belonging to the technical field of nano material preparation, and characterized in that: the MoSe is2The CuPd nano composite material is powder, the crystalline phase is a hexagonal phase structure, the morphology is a flower-shaped structure constructed by nano sheets, the size is 80-100 nm, and metal nano particles with the size of 2-10 nm are uniformly distributed on the surfaces of the nano sheets; MoSe prepared by the invention2the-CuPd nano composite material has a flower-like structure and is formed by stacking a large number of nano sheets to form flower-like MoSe2the-CuPd composite material has pore structures with various sizes, so that the specific surface area of the material is improved, and the nano particles have the characteristic of high activity and can effectively improve the catalytic performance.
Description
Technical Field
The invention belongs to the technical field of preparation of nano materials, and particularly provides flower-shaped MoSe2-CuPd nano composite material and its synthesis method and application.
Background
With the rapid progress and development of human society and the massive use of traditional fossil fuels, on one hand, serious pollution is caused to the environment, and on the other hand, the shortage of non-renewable energy sources gradually threatens and restricts the development of society, so that the exploration of new energy sources is a problem which needs to be solved by scientists urgently. Hydrogen energy is considered to be one of the most suitable alternative energy sources to fossil energy, and electrochemical decomposition of water is a simple method for producing high-purity hydrogen by converting electric energy into chemical energy. The most active and stable hydrogen evolution reaction catalysts reported to date are noble metals and their compounds, typically including Pt, Pt-based alloys/compounds, but the expensive price, low abundance and poor durability limit the industrial application of these noble metal catalysts. Therefore, it is an important task to develop a non-noble metal catalyst that is abundant in resources, efficient, and economically efficient.
In recent years, MoSe2Receiving more and more attention due to their unique physical and chemical properties, many researchers have been working on developing various moses2Base materials as hydrogen evolution catalysts, but due to MoSe2The conductivity of the catalyst is low, the catalytic active sites are relatively insufficient, and the electrochemical activity is still limited to a certain extent. Therefore, it is necessary to provide MoSe2The structure of (a) is modified to improve its electrochemical performance. Such as by adding to MoSe2Heterogeneous metal or non-metal elements are introduced to change the electronic structure of the catalyst and increase the number of active sites, thereby improving the catalytic activity (RSC adv.,2017,7, 25867-. Such as MoSe2In combination with one or more other compounds having unique properties to form a composite material, thereby enhancing the catalytic effect thereof (J.Mater. chem.A., 2017,5, 1558-1566).
The present invention has been made based on this.
Disclosure of Invention
The first aspect of the invention aims at providing flower-shaped MoSe2-a CuPd nanocomposite characterized in that: the MoSe2the-CuPd nano composite material is powder, the crystalline phase is a hexagonal phase structure, the morphology is a flower-shaped structure constructed by nano sheets, the size of the flower-shaped structure constructed by the nano sheets is 80-100 nm, and a large number of metal nano particles with the size of 2-10 nm are uniformly distributed in the nano sheetsAnd (5) rice sheet surface.
Flower-like MoSe of the invention2the-CuPd nano composite material is a nano flower-shaped structure formed by mutually interweaving a plurality of nano sheets according to a certain rule. This particular structure preserves MoSe2The characteristic of high activity of CuPd nano-sheets, and the flower-like structure formed by the mutual interweaving of the nano-sheets enables MoSe2The CuPd has pore structures with various sizes, so that the specific surface area of the catalyst is effectively improved, and the catalytic performance of the composite is improved due to the loading of metal particles. Therefore, the flower-shaped MoSe constructed by the nano-sheets with special structures2the-CuPd nano composite material shows excellent application potential in the field of catalysis.
The second aspect of the invention is to provide the flower-shaped MoSe2-a method for the synthesis of a CuPd nanocomposite, characterized in that it comprises the following steps:
(1) weighing a certain amount of molybdenum acetylacetonate and dibenzyl diselenide, and adding the weighed materials into organic amine;
(2) under the action of stirring in an inert atmosphere, mixing the solution at 100-150 ℃ for 30-50 min to make the solution brown yellow;
(3) heating the solution in the step (2) to 240-300 ℃ at a heating rate of 10 ℃/min, and reacting for 20-40 min;
(4) weighing a certain amount of copper acetylacetonate and palladium acetylacetonate, dispersing the copper acetylacetonate and the palladium acetylacetonate in 0.5-1 mL of organic amine, and placing the mixture into a 70 ℃ oven after uniform ultrasonic dispersion;
(5) when the temperature of the solution in the step (3) is reduced to 140-180 ℃, injecting the solution (4) into the solution, and continuously reacting for 20-40 min at 140-180 ℃;
(6) after the reaction in the step (5) is finished, naturally cooling to room temperature, centrifuging, washing for at least 5 times by using normal hexane and toluene in sequence, and finally dispersing in toluene to obtain flower-shaped MoSe2-a CuPd nanomaterial.
Further settings are as follows:
in the step (1):
the mass ratio of the molybdenum acetylacetonate and the dibenzyl diselenide is 1: 1-2, preferably 1: 1;
in the step (2):
the inert atmosphere is selected from any one of argon, helium and nitrogen.
The inert atmosphere is preferably argon, the reaction temperature is preferably 140 ℃, and the reaction time is preferably 40 min;
in the step (3):
the reaction temperature is preferably 240 ℃, and the reaction time is preferably 20 min;
in the step (4):
the mass ratio of copper acetylacetonate to palladium acetylacetonate is 1: 1;
the organic amine is selected from oleylamine, dodecylamine, tetradecylamine, hexadecylamine, octadecylamine, etc.
In the step (5):
the reaction temperature is preferably 140 ℃ and the reaction time is preferably 30 min.
The flower-shaped MoSe is prepared by2The synthesis method of the-CuPd nano composite material has the following beneficial effects:
(1) and a surfactant is not used in the reaction process, annealing treatment is not needed, and the production cost of the material is reduced.
(2) The synthesis method is simple and easy to operate, the product has good repeatability, and the raw materials are cheap and easy to obtain.
The third aspect of the invention aims at providing flower-shaped MoSe2Application of the-CuPd nano composite material in electrocatalytic hydrogen evolution.
MoSe prepared by the invention2the-CuPd nano composite material has a flower-like structure and is formed by stacking a large number of nano sheets to form flower-like MoSe2the-CuPd composite material has pore structures with various sizes, so that the specific surface area of the material is improved, and the nano particles have the characteristic of high activity and can effectively improve the catalytic performance.
The invention is further described with reference to the following figures and detailed description.
Drawings
FIG. 1 is a Transmission Electron Microscope (TEM) photograph of the product of example 1 of the present invention;
FIG. 2 is an X-ray diffraction pattern (XRD) of the product of example 1 of the present invention;
FIG. 3 is an X-ray Energy Dispersive Spectroscopy (EDS) of the product of example 1 of the present invention;
FIG. 4 is an X-ray photoelectron spectroscopy (XPS) analysis of the product of example 1 of the present invention;
FIG. 5 is a Transmission Electron Microscope (TEM) photograph of the product of example 2 of the present invention;
FIG. 6 is a comparison of the effects of the electrocatalytic hydrogen evolution reaction of example 1 and example 2 of the present invention;
FIG. 7 shows example 1 of the present invention and comparative example (MoSe)2) Is applied to the comparison of the effect of the electrocatalytic hydrogen evolution reaction.
Detailed Description
Example 1:
0.0326g of molybdenum acetylacetonate and 0.034g of dibenzyl diselenide are weighed into 6mL of oleylamine, stirred for 40min at 140 ℃ under Ar gas, and then directly heated to 240 ℃ at the heating rate of 10 ℃/min to react for 20 min. 0.026g of copper acetylacetonate and 0.03g of palladium acetylacetonate were weighed and dispersed in 0.5mL of oleylamine, and after uniform ultrasonic dispersion, the mixture was put into an oven at 70 ℃. And when the temperature of the reaction liquid is reduced to 140 ℃, pouring oleylamine solution containing copper acetylacetonate and palladium acetylacetonate into the reaction liquid, and continuously reacting for 30min at the temperature of 140 ℃. After the reaction is finished, naturally cooling to room temperature, centrifuging, washing for at least 5 times by using normal hexane and toluene in sequence, and finally dispersing in the toluene to obtain the nano flower-shaped MoSe2-a CuPd composite material.
The structure of the product is confirmed:
the TEM result (figure 1) visually shows that the product is a flower-shaped structure constructed by the nano-sheets, the size is about 100nm, and a large number of metal nano-particles with the size of about 10nm are uniformly distributed on the surfaces of the nano-sheets without agglomeration. XRD results (FIG. 2) and MoSe2Standard card (JCPDS No.17-0887) was matched, indicating that the product was hexagonal phase MoSe2Structure, no diffraction peaks corresponding to Cu and Pd were observed in the XRD chart because of the small contents of Cu and Pd, but the EDS chart (fig. 3) and XPS chart (fig. 4) of the product confirmed the presence of Cu and Pd in the product.
Example 2:
weigh 0.0326g ofAdding molybdenum acetylacetonate and 0.034g of dibenzyl diselenide into 6mL of oleylamine, stirring for 30min at 150 ℃ under Ar gas, and directly heating to 300 ℃ at the heating rate of 10 ℃/min to react for 20 min. 0.026g of copper acetylacetonate and 0.03g of palladium acetylacetonate were weighed and dispersed in 0.5mL of oleylamine, and after uniform ultrasonic dispersion, the mixture was put into an oven at 70 ℃. And when the temperature of the reaction liquid is reduced to 150 ℃, pouring oleylamine solution containing copper acetylacetonate and palladium acetylacetonate into the reaction liquid, and continuously reacting for 30min at the temperature of 150 ℃. After the reaction is finished, naturally cooling to room temperature, centrifuging, washing for at least 5 times by using normal hexane and toluene in sequence, and finally dispersing in the toluene to obtain the nano flaky MoSe2-a CuPd composite material.
The structure of the product is confirmed:
the TEM result (FIG. 5) visually shows that the product is a flower-like structure constructed by the nanosheets, the size of the flower-like structure is about 80nm, and a large number of metal nanoparticles with the size of about 2nm are uniformly distributed on the surfaces of the nanosheets without agglomeration.
Comparative example:
0.0326g of molybdenum acetylacetonate and 0.034g of dibenzyl diselenide are weighed into 6mL of oleylamine, stirred for 40min at 140 ℃ under Ar gas, and then directly heated to 240 ℃ at the heating rate of 10 ℃/min to react for 20 min. After the reaction is finished, naturally cooling to room temperature, centrifuging, washing for at least 5 times by using normal hexane and toluene in sequence, and finally dispersing in the toluene to obtain the nano flower-shaped MoSe2。
Application example 1:
the nanoflower MoSe prepared in the examples 1 and 2 of the present invention2the-CuPd composite materials are respectively used for electrocatalytic hydrogen evolution reaction, and the catalytic effect of the-CuPd composite materials is statistically analyzed.
Taking 4mg of MoSe2The CuPd sample and 20. mu.l of nafion solution were dispersed in 1ml of an ethanol aqueous solution in a volume ratio of 1:3, and then the ethanol solution containing the sample was subjected to ultrasonic treatment for 1 hour to obtain a uniform dispersion. Dropping 5 μ l of the above dispersion liquid into a glassy carbon electrode (phi 3mm), and naturally drying to obtain MoSe2-a CuPd modified glassy carbon electrode. The modified electrode, the platinum electrode and the saturated calomel electrode are respectively used as a working electrode and a counter electrodeElectrode and reference electrode, constituting a three-electrode system, at 0.5mol/L H2SO4The electrolyte was scanned linearly to obtain their electrochemical polarization curves, as shown in fig. 6, and the electrocatalytic hydrogen evolution effect was analyzed and is summarized in table 1. As can be seen from fig. 6 and table 1, the electrocatalytic hydrogen evolution effects of example 1 and example 2 are comparable.
Application example 2:
inventive example 1 (MoSe)2CuPd) and comparative example (MoSe)2) Are respectively used for electrocatalytic hydrogen evolution reaction.
Taking 4mg of MoSe2-CuPd or MoSe2The sample and 20. mu.l of nafion solution were dispersed in 1ml of an ethanol aqueous solution in a volume ratio of 1:3, and then the ethanol solution containing the sample was subjected to ultrasonic treatment for 1 hour to obtain a uniform dispersion. Dropping 5 μ l of the above dispersion liquid into a glassy carbon electrode (phi 3mm), and naturally drying to obtain MoSe2-CuPd or MoSe2And modifying the glassy carbon electrode. The modified electrode, the platinum electrode and the saturated calomel electrode are respectively used as a working electrode, a counter electrode and a reference electrode to form a three-electrode system, and the concentration is 0.5mol/L H2SO4The linear scan was performed in the electrolyte to obtain their electrochemical polarization curves, as shown in fig. 7, and the electrocatalytic hydrogen evolution effect was analyzed and counted in table 1.
As can be seen from FIG. 7 and Table 1, MoSe2-CuPd to MoSe2The initial hydrogen evolution potential is low, and the current density is 10mA/cm2Low overpotential required, indicating MoSe2-CuPd to MoSe2Has better electrocatalytic hydrogen evolution effect.
TABLE 1 comparison of catalytic Performance of composites prepared according to the invention with existing products
To summarize:
(1) as can be seen from the above examples, the present invention provides a flower-shaped MoSe2The liquid phase synthesis method of the-CuPd nano material has the advantages of common raw materials, mild conditions, simple operation and high yieldHigh in efficiency and can be widely popularized.
(2) Flower-shaped MoSe prepared by the invention2-CuPd nanomaterial, the product having a flower-like structure and being formed by stacking a large number of nanosheets so as to form flower-like MoSe2the-CuPd composite material has pore structures with various sizes, so that the specific surface area of the material is improved, and the nano particles have the characteristic of high activity and can effectively improve the catalytic performance.
Claims (10)
1. Flower-shaped MoSe2-a CuPd nanocomposite characterized in that: MoSe2the-CuPd nano composite material is powder, the crystalline phase is a hexagonal phase structure, the morphology is a flower-shaped structure constructed by nano sheets, the size is 80-100 nm, and metal nano particles with the size of 2-10 nm are uniformly distributed on the surfaces of the nano sheets.
2. Flower-like MoSe according to claim 12-a method for the synthesis of a CuPd nanocomposite, characterized in that it comprises the following steps:
(1) weighing a certain amount of molybdenum acetylacetonate and dibenzyl diselenide, and adding the weighed materials into organic amine;
(2) under the action of stirring in an inert atmosphere, mixing the solution at 100-150 ℃ for 30-50 min to make the solution brown yellow;
(3) heating the solution in the step (2) to 240-300 ℃ at a heating rate of 10 ℃/min, and reacting for 20-40 min;
(4) weighing a certain amount of copper acetylacetonate and palladium acetylacetonate, dispersing the copper acetylacetonate and the palladium acetylacetonate in 0.5-1 mL of organic amine, and placing the mixture into a 70 ℃ oven after uniform ultrasonic dispersion;
(5) when the temperature of the solution in the step (3) is reduced to 140-180 ℃, injecting the solution (4) into the solution, and continuously reacting for 20-40 min at 140-180 ℃;
(6) after the reaction in the step (5) is finished, naturally cooling to room temperature, centrifuging, washing for at least 5 times by using normal hexane and toluene in sequence, and finally dispersing in toluene to obtain flower-shaped MoSe2-a CuPd nanomaterial.
3. According to claim2 the flower-shaped MoSe2-a process for the synthesis of a CuPd nanocomposite, characterized in that in step (1): the ratio of the amount of the molybdenum acetylacetonate to the amount of the dibenzyl diselenide is 1:1 to 2.
4. The flower-shaped MoSe according to claim 32-a process for the synthesis of a CuPd nanocomposite, characterized in that in step (1): the mass ratio of the molybdenum acetylacetonate to the dibenzyl diselenide is 1: 1.
5. The flower-shaped MoSe according to claim 22-a process for the synthesis of a CuPd nanocomposite, characterized in that in step (2): the inert atmosphere is selected from any one of argon, helium and nitrogen.
6. The flower-shaped MoSe according to claim 22-a process for the synthesis of a CuPd nanocomposite, characterized in that in step (2): the inert atmosphere is preferably argon, the reaction temperature is 140 ℃, and the reaction time is 40 min.
7. The flower-shaped MoSe according to claim 22-a process for the synthesis of a CuPd nanocomposite, characterized in that in step (3): the reaction temperature was 240 ℃ and the reaction time was 20 min.
8. The flower-shaped MoSe according to claim 22-a process for the synthesis of a CuPd nanocomposite, characterized in that in step (4): the mass ratio of copper acetylacetonate to palladium acetylacetonate is 1: 1; the organic amine is selected from one of oleylamine, dodecylamine, tetradecylamine, hexadecylamine and octadecylamine.
9. The flower-shaped MoSe according to claim 22-a process for the synthesis of a CuPd nanocomposite, characterized in that in step (5): the reaction temperature was 140 ℃ and the reaction time was 30 min.
10. Flower-like MoSe according to claim 12Application of the-CuPd nanocomposite material in electrocatalytic hydrogen evolution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111592025.1A CN114411199A (en) | 2021-12-23 | 2021-12-23 | Flower-shaped MoSe2-CuPd nano composite material and synthetic method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111592025.1A CN114411199A (en) | 2021-12-23 | 2021-12-23 | Flower-shaped MoSe2-CuPd nano composite material and synthetic method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114411199A true CN114411199A (en) | 2022-04-29 |
Family
ID=81266741
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111592025.1A Pending CN114411199A (en) | 2021-12-23 | 2021-12-23 | Flower-shaped MoSe2-CuPd nano composite material and synthetic method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114411199A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105463566A (en) * | 2015-11-25 | 2016-04-06 | 中国科学技术大学 | Liquid phase method for epitaxial growth of MoSe2-XnSem heterogeneous nano structures |
| CN106669763A (en) * | 2016-12-30 | 2017-05-17 | 华南理工大学 | Nitrogen-doped carbon-coated nanoflower-shaped MoSe2 composite material and preparation and application |
| CN108593743A (en) * | 2018-05-09 | 2018-09-28 | 山东理工大学 | A kind of preparation method and application of the interlayer type immunosensor of the compound two selenizings molybdenum label of platinum palladium |
| CN110586162A (en) * | 2019-09-24 | 2019-12-20 | 华东师范大学 | Layered titanium nitride nano composite material doped with molybdenum diselenide, preparation method and application |
-
2021
- 2021-12-23 CN CN202111592025.1A patent/CN114411199A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105463566A (en) * | 2015-11-25 | 2016-04-06 | 中国科学技术大学 | Liquid phase method for epitaxial growth of MoSe2-XnSem heterogeneous nano structures |
| CN106669763A (en) * | 2016-12-30 | 2017-05-17 | 华南理工大学 | Nitrogen-doped carbon-coated nanoflower-shaped MoSe2 composite material and preparation and application |
| CN108593743A (en) * | 2018-05-09 | 2018-09-28 | 山东理工大学 | A kind of preparation method and application of the interlayer type immunosensor of the compound two selenizings molybdenum label of platinum palladium |
| CN110586162A (en) * | 2019-09-24 | 2019-12-20 | 华东师范大学 | Layered titanium nitride nano composite material doped with molybdenum diselenide, preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| WEN XU等: "One pot colloidal synthesis of MoSe2–Pt nanofowers and their enhanced electrocatalytic hydrogen evolution performance", 《RESEARCH ON CHEMICAL INTERMEDIATES》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Shen et al. | Bifunctional Cu3P decorated g-C3N4 nanosheets as a highly active and robust visible-light photocatalyst for H2 production | |
| Hu et al. | Urea Electrooxidation: Current Development and Understanding of Ni‐Based Catalysts | |
| Xiong et al. | CuSn alloy nanoparticles on nitrogen‐doped graphene for electrocatalytic CO2 reduction | |
| CN107321368B (en) | Au atom modified CoSe2Nanobelt and preparation method and application thereof | |
| CN110127655B (en) | Method for preparing biomass carbon-loaded cobalt phosphide electrode material by one-step calcination method | |
| CN110756188B (en) | Preparation method of three-dimensional carbon network supported FeCo bifunctional oxygen catalyst | |
| Li et al. | Ultrathin ZnIn2S4 nanosheets-supported metallic Ni3FeN for photocatalytic coupled selective alcohol oxidation and H2 evolution | |
| Wei et al. | Composition-dependent activity of ZnxCd1-xSe solid solution coupled with Ni2P nanosheets for visible-light-driven photocatalytic H2 generation | |
| CN111359613B (en) | Cobalt nanoparticle composite material with dual-functional graphene oxide loaded core-shell structure | |
| CN113042085B (en) | Preparation method and application of nitrogen-phosphorus double-doped graphene-supported nickel-cobalt-palladium nano catalyst | |
| CN113522263B (en) | Preparation method and application of phosphorus-doped graphene-loaded nickel-platinum nano-catalyst | |
| CN108855173A (en) | A kind of photoelectrocatalysis decompose aquatic products hydrogen method and its used in plasma catalyst and preparation method | |
| Xue et al. | Efficient Electrocatalytic Nitrogen Reduction to Ammonia on Ultrafine Sn Nanoparticles | |
| Zhang et al. | Recent advances in multilevel nickel-nitrogen-carbon catalysts for CO2electroreduction to CO | |
| Zhang et al. | Synthesis of Co2FeAl alloys as highly efficient electrocatalysts for alkaline hydrogen evolution reaction | |
| CN114700096A (en) | Mo @ Mo2Synthesis method of C nano composite material | |
| Salarizadeh et al. | Comparison of methanol oxidation reaction process for NiCo2O4/X (X= rGO, MWCNTs, HCNs) nanocatalyst | |
| CN108745403B (en) | Preparation method and application of boron nitride loaded Ni-MoOx nano catalyst | |
| Chutia et al. | Durable and Stable Bifunctional Co3O4-Based Nanocatalyst for Oxygen Reduction/Evolution Reactions | |
| Chen et al. | Mechanosynthesized electroactive materials for sustainable energy and environmental applications: A critical review | |
| CN113174608A (en) | Preparation method of double-doped porous cobalt phosphide nanosheet electrocatalytic material | |
| Zhang et al. | Plasmon-driven photothermal conversion with two-dimensional ultra-thin PdFe nanosheets for ethylene glycol electrooxidation | |
| CN108393500B (en) | Mo-Ni alloy nanoparticle composite material and preparation method and application thereof | |
| CN114411199A (en) | Flower-shaped MoSe2-CuPd nano composite material and synthetic method and application thereof | |
| Long et al. | Ultrafine and Well-Dispersed Nickel Nanoparticles with Hierarchical Structure for Catalytically Breaking a Boron–Hydrogen Bond |
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: 20220429 |
|
| RJ01 | Rejection of invention patent application after publication |