CN114703505B - Preparation method of metal atom electrocatalyst with stable carbon atom coordination - Google Patents
Preparation method of metal atom electrocatalyst with stable carbon atom coordination Download PDFInfo
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- CN114703505B CN114703505B CN202210350739.XA CN202210350739A CN114703505B CN 114703505 B CN114703505 B CN 114703505B CN 202210350739 A CN202210350739 A CN 202210350739A CN 114703505 B CN114703505 B CN 114703505B
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 116
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 66
- 239000002184 metal Substances 0.000 title claims abstract description 66
- 125000004429 atom Chemical group 0.000 title claims abstract description 35
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 34
- 125000004432 carbon atom Chemical group C* 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 100
- 150000003839 salts Chemical class 0.000 claims abstract description 31
- 239000002243 precursor Substances 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000001721 carbon Chemical group 0.000 claims abstract description 15
- 239000012876 carrier material Substances 0.000 claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052802 copper Inorganic materials 0.000 claims abstract description 10
- 239000010949 copper Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 4
- 238000004873 anchoring Methods 0.000 claims abstract description 3
- 239000004744 fabric Substances 0.000 claims description 25
- 239000012528 membrane Substances 0.000 claims description 8
- 239000002134 carbon nanofiber Substances 0.000 claims description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 7
- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 239000003575 carbonaceous material Substances 0.000 description 9
- 150000003624 transition metals Chemical group 0.000 description 8
- 238000002635 electroconvulsive therapy Methods 0.000 description 7
- 230000035939 shock Effects 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 238000005520 cutting process Methods 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000002133 porous carbon nanofiber Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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
Abstract
The invention discloses a preparation method of a metal atom electrocatalyst with stable coordination of carbon atoms, which belongs to the field of new chemical material catalysis, and comprises the steps of placing a self-supporting carbon-based carrier material without nitrogen elements in CO 2 Performing high-temperature treatment in an atmosphere to obtain a porous carbon carrier, preparing a metal salt precursor, dripping the metal salt precursor onto the porous carbon carrier, drying, connecting the dried porous carbon carrier to a conductive copper sheet, applying current to the dried porous carbon carrier in an inert atmosphere, and dispersing and anchoring metal atoms on a carbon substrate by utilizing Joule heat to obtain a metal atom electrocatalyst with stable carbon atom coordination; the prepared electrocatalyst has the advantages that the carbon coordination atoms can effectively adjust the electronic structure of the metal active center, and the self-supporting macrostructure is favorable for reducing the interface contact resistance in the electrocatalytic process, so that the electrocatalyst has good application prospect in the fields of electrocatalytic hydrogen evolution under high current density and the like.
Description
Technical Field
The invention relates to a preparation method of a metal atom electrocatalyst with stable carbon atom coordination, belonging to the field of new chemical material catalysis.
Background
The catalyst with carbon-based material loaded with transition metal atoms has the maximum atom utilization efficiency, and the interaction between metal atoms and a carrier can adjust the electrocatalytic activity, so that the catalyst is a promising electrocatalyst for reactions related to a plurality of energies. However, the surface of metal atoms has higher surface free energy, which is extremely easy to cause the phenomena of atom aggregation and instability. Currently, metal atom electrocatalysts coordinated with nitrogen have been studied more than carbon coordination. The electronegativity of carbon atoms is lower than that of nitrogen atoms, and coordination of metal atoms to carbon can redistribute the charge in the center of the metal atoms. The electronic structure of the metal active center can be effectively regulated by pure carbon atom coordination, and the self-supporting macroscopic structure is beneficial to reducing interface contact resistance in the electrocatalytic process. The conventional synthesis methods have the problems of high energy consumption, severe conditions, complicated procedures, uncontrollable capacity, low loading capacity and the like, and seriously hamper the development of electrocatalysts of transition metal sites. Thus, simple and efficient preparation of electrocatalysts of carbon-coordinated transition metal atoms at ambient temperature and pressure is a current challenge.
Disclosure of Invention
Aiming at the problems of the existing preparation method and coordination regulation of the transition metal atom electrocatalyst, the invention provides the preparation method of the metal atom electrocatalyst with stable coordination of carbon atoms, which not only can simply and efficiently prepare the metal atom electrocatalyst, but also can show excellent electrocatalytic activity through the coordination stability of the carbon atoms.
The preparation method of the metal atom electrocatalyst with stable coordination of carbon atoms of the invention leads the self-supporting carbon-based carrier material without nitrogen element to be in CO 2 Performing high-temperature treatment in an atmosphere to obtain a porous carbon carrier, preparing a metal salt precursor, dripping the metal salt precursor onto the porous carbon carrier, drying, connecting the dried porous carbon carrier to a conductive copper sheet, applying current to the dried porous carbon carrier in an inert atmosphere, and dispersing and anchoring metal atoms on a carbon substrate by utilizing Joule heat to obtain a metal atom electrocatalyst with stable carbon atom coordination; electrocatalytic hydrogen evolution has excellent catalytic activity under high current density.
The self-supporting carbon-based carrier material without nitrogen element is carbon cloth, carbon paper or PVA-based carbon nanofiber membrane.
The metal salt is one or more of cobalt nitrate, nickel chloride and cobalt acetylacetonate, and the load of the metal salt is 1% -20% of the mass of the porous carbon carrier.
The temperature of the high-temperature treatment of the self-supporting carbon-based carrier material without nitrogen element is 200-1000 ℃, and the treatment time is 15-600 min.
The applied current is a programmable direct current power supply, the current parameter is 0.5A-5.5A, the times of thermal oscillation are 1-20 times, and the time of each oscillation is 0.5 s-20 s.
It is another object of the present invention to provide a metal atom electrocatalyst with stable coordination of carbon atoms produced by the above method.
The beneficial effects of the invention are as follows:
compared with the existing preparation method of the transition metal atom electrocatalyst and the nitrogen atom coordination regulation, the preparation method has the advantages of short time consumption, easy regulation and control and simple operation; the carbon atom is taken as a central atom, and can have stronger interaction with the metal atom, so that the metal atom electrocatalyst can be simply and efficiently prepared, and the excellent electrocatalyst activity can be stably shown through coordination of the carbon atom.
Drawings
FIG. 1 is a photograph of carbon cloth used in the preparation of example 1.
Fig. 2 is an SEM image of the carbon cloth prepared in example 1.
FIG. 3 is a spherical aberration electron microscope image of an electrocatalyst with transition metal cobalt atom sites supported on carbon cloth prepared in example 1;
FIG. 4 is a BET characterization of the raw carbon cloth and the carbon cloth of the supported transition metal atom sites prepared in example 1;
FIG. 5 is an electrocatalytic hydrogen LSV curve of the original carbon cloth and supported transition metal atom site carbon cloth prepared in example 1.
Detailed Description
The present invention will be described in further detail by way of examples, but the scope of the present invention is not limited to the above description; the methods in the examples are all conventional methods unless specified otherwise, and the reagents are all conventional commercial reagents or reagents prepared by conventional methods unless specified otherwise;
example 1
Selecting carbon cloth as a self-supporting carbon-based carrier material, cutting the carbon cloth, and then placing the cut carbon cloth in a tubular furnace CO 2 Treating at 900deg.C for 180min to obtain porous carbon carrier, and weighing Co (NO) 3 ) 2 ·6H 2 O preparing a metal salt precursor solution, wherein the loading amount of the metal salt is 3% of the mass of the porous carbon carrier, then dripping the metal salt precursor solution onto the porous carbon carrier, drying at 60 ℃, respectively connecting two ends of the porous carbon carrier onto a conductive copper sheet, applying current to carbon cloth for a plurality of times by using a programmable direct current power supply in an Ar environment, setting the current to be 5A, carrying out 10 times of heat shock treatment on the carbon-based material by using generated Joule heat, and finally obtaining the metal Co atom electrocatalyst with a self-supporting structure and stable carbon atom coordination, wherein the time of each shock is 5 s.
The embodiment successfully prepares the electrocatalyst with stable coordination of carbon atoms and metal cobalt atoms, as shown in fig. 1, the carbon cloth has good conductivity and larger specific surface area, the electron transmission rate is improved, the SEM image of the carbon cloth is shown in fig. 2, and the carbon cloth is a three-dimensional network structure formed by interweaving carbon cloth fibers. After 10 times of periodic high-temperature heat shock, it is obvious that single metal Co atoms are dispersedly loaded on the carbon substrate, as shown in FIG. 3. The carbon cloth loaded with the transition metal atoms prepared in this example has a high specific surface area, as shown in fig. 4. The electrocatalyst prepared in this example was applied to electrocatalytic hydrogen evolution reaction, and the result is shown in fig. 5, in which the metal atom electrocatalyst with stable carbon coordination shows excellent hydrogen evolution performance at high current density.
Example 2
Selecting carbon paper as a self-supporting carbon-based carrier material, cutting the carbon paper, and then placing the cut carbon paper in a tube furnace CO 2 Treating at 200deg.C for 600min to obtain porous carbon carrier, and weighing NiCl 2 ·6H 2 O preparing a metal salt precursor solution, wherein the loading amount of the metal salt is 10% of the mass of the porous carbon carrier, then dripping the metal salt precursor solution onto the porous carbon carrier, drying at 60 ℃, respectively connecting two ends of the porous carbon carrier onto a conductive copper sheet, applying current to carbon paper for a plurality of times by using a programmable direct current power supply in an Ar environment, setting the current to be 5.5A, carrying out 20 times of heat shock treatment on the carbon-based material by using generated Joule heat, and obtaining the metal Ni atom electrocatalyst with a self-supporting structure and stable carbon atom coordination after 8s of each shock time.
Example 3
PVA-based carbon nanofiber membrane (Dong Keqi. Electrostatic spinning method can be used for preparing PVA-based whole porous carbon nanofiber membrane and electrochemical performance research [ D ]]Prepared by the method in the university of east China) is a self-supporting carbon-based carrier material, and a PVA-based carbon nanofiber membrane is cut and then placed in a tube furnace CO 2 Treating at 1000deg.C for 15min to obtain porous carbon carrier, weighing cobalt acetylacetonate to prepare metal salt precursor solution, loading metal salt with 5% of porous carbon carrier mass, dripping metal salt precursor solution onto porous carbon carrier, drying at 60deg.C, connecting two ends of porous carbon carrier to conductive copper sheets, and placing under Ar environmentAnd applying current to the carbon paper for a plurality of times by using a programmable direct current power supply, setting the current to be 3A, and performing 15 times of thermal shock treatment on the carbon-based material by using generated Joule heat, wherein the shock time is 15s each time, so as to finally obtain the metal Ni atom electrocatalyst with a self-supporting structure and stable carbon atom coordination.
Example 4
Selecting carbon paper as a self-supporting carbon-based carrier material, cutting the carbon paper, and then placing the cut carbon paper in a tube furnace CO 2 And (3) processing at 700 ℃ for 100min in an atmosphere to obtain a porous carbon carrier, weighing cobalt acetylacetonate to prepare a metal salt precursor solution, wherein the metal salt loading amount is 1% of the mass of the porous carbon carrier, then dripping the metal salt precursor solution onto the porous carbon carrier, drying at 60 ℃, respectively connecting two ends of the porous carbon carrier onto a conductive copper sheet, repeatedly applying current to the porous carbon carrier by using a programmable direct current power supply in an Ar environment, setting the current to be 0.5A, carrying out 5 times of thermal shock treatment on the carbon-based material by using generated Joule heat, and obtaining the metal Co atom electrocatalyst with a self-supporting structure and stable carbon atom coordination every time is 12 s.
Example 5
Selecting carbon cloth as self-supporting carbon-based material, cutting the carbon cloth, and then placing the cut carbon cloth in a tubular furnace CO 2 Treating at 500 deg.C for 400min to obtain porous carbon carrier, and weighing NiCl 2 ·6H 2 O preparing a metal salt precursor solution, wherein the loading amount of the metal salt is 15% of the mass of the porous carbon carrier, then dripping the metal salt precursor solution onto the porous carbon carrier, drying at 60 ℃, respectively connecting two ends of the porous carbon carrier onto a conductive copper sheet, applying current to the porous carbon carrier for a plurality of times by using a programmable direct current power supply in an Ar environment, setting the current to be 5.5A, carrying out 1 time of heat shock treatment on the carbon-based material by using generated Joule heat, wherein the shock time is 20s each time, and finally obtaining the metal Ni atom electrocatalyst with a self-supporting structure and stable carbon atom coordination.
Example 6
Selecting a PVA-based carbon nanofiber membrane as a self-supporting carbon-based carrier material, cutting the PVA-based carbon nanofiber membrane, and then placing the cut PVA-based carbon nanofiber membrane in a tubular furnace CO 2 Treating at 800 deg.C for 480min in atmosphere to obtain porous materialAnd (3) weighing the cobalt acetylacetonate to prepare a metal salt precursor solution, wherein the loading amount of the metal salt is 15% of the mass of the porous carbon carrier, then dripping the metal salt precursor solution onto the porous carbon carrier, drying at 60 ℃, respectively connecting two ends of the porous carbon carrier onto a conductive copper sheet, applying current to the porous carbon carrier for a plurality of times by using a programmable direct current power supply in an Ar environment, setting the current to be 4A, carrying out 10 times of heat shock treatment on the carbon-based material by using generated Joule heat, and obtaining the metal Co atom electrocatalyst with a self-supporting structure and stable carbon atom coordination after 20s of each shock time.
Example 7
Selecting carbon cloth as a self-supporting carbon-based carrier material, cutting the carbon cloth, and then placing the cut carbon cloth in a tubular furnace CO 2 And (3) treating at 400 ℃ in the atmosphere for 400min to obtain a porous carbon carrier, weighing cobalt acetylacetonate to prepare a metal salt precursor solution, wherein the metal salt loading amount is 20% of the mass of the porous carbon carrier, then dripping the metal salt precursor solution onto the porous carbon carrier, drying at 60 ℃, respectively connecting two ends of the porous carbon carrier onto a conductive copper sheet, applying current to the carbon cloth for a plurality of times by using a programmable direct current power supply in an Ar environment, setting the current to be 2.5A, carrying out 15 times of thermal shock treatment on the carbon-based material by using generated Joule heat, and obtaining the metal Co atomic electro-catalyst with a self-supporting structure and stable carbon atom coordination after each shock time is 8 s.
Claims (2)
1. Use of a metal atom electrocatalyst with stable coordination of carbon atoms in electrocatalytic hydrogen evolution;
the metal atom electrocatalyst with stable coordination of carbon atoms is prepared by mixing self-supporting carbon-based carrier material without nitrogen element in CO 2 Performing high-temperature treatment in an atmosphere to obtain a porous carbon carrier, preparing a metal salt precursor, dripping the metal salt precursor onto the porous carbon carrier, drying, connecting the dried porous carbon carrier to a conductive copper sheet, applying current to the dried porous carbon carrier in an inert atmosphere, and dispersing and anchoring metal atoms on a carbon substrate by utilizing Joule heat to obtain a metal atom electrocatalyst with stable carbon atom coordination;
the temperature of the high-temperature treatment of the self-supporting carbon-based carrier material without nitrogen element is 800-1000 ℃, and the treatment time is 180-400 min;
the current is applied by a programmable direct current power supply, the current parameter is 0.5A-5.5A, the times of thermal oscillation are 10-20 times, and the time of each oscillation is 5 s-20 s;
the metal salt is one or more of cobalt nitrate, nickel chloride and cobalt acetylacetonate; the load of the metal salt is 3% -5% of the mass of the porous carbon carrier.
2. The use according to claim 1, characterized in that: the self-supporting carbon-based carrier material without nitrogen element is carbon cloth, carbon paper or PVA-based carbon nanofiber membrane.
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Inventor after: Zhu Yuanzhi Inventor after: Peng Cheng Inventor before: Peng Cheng Inventor before: Zhu Yuanzhi |
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