CN114703505A - 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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- CN114703505A CN114703505A CN202210350739.XA CN202210350739A CN114703505A CN 114703505 A CN114703505 A CN 114703505A CN 202210350739 A CN202210350739 A CN 202210350739A CN 114703505 A CN114703505 A CN 114703505A
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 123
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 70
- 239000002184 metal Substances 0.000 title claims abstract description 70
- 125000004429 atom Chemical group 0.000 title claims abstract description 41
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 125000004432 carbon atom Chemical group C* 0.000 title claims description 9
- 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 30
- 150000001721 carbon Chemical group 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 20
- 238000000034 method Methods 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
- 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 26
- 239000012876 carrier material Substances 0.000 claims description 12
- 230000035939 shock Effects 0.000 claims description 11
- 239000012528 membrane Substances 0.000 claims description 7
- 239000002134 carbon nanofiber Substances 0.000 claims description 6
- 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
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 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
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 5
- 239000001257 hydrogen Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 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
- 239000003575 carbonaceous material Substances 0.000 description 9
- 150000003624 transition metals Chemical group 0.000 description 9
- 238000005520 cutting process Methods 0.000 description 7
- 238000002635 electroconvulsive therapy Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 5
- 229910052723 transition metal Inorganic materials 0.000 description 5
- 239000003153 chemical reaction reagent Substances 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
- 238000012545 processing Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000000694 effects Effects 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
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000002133 porous carbon nanofiber Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001308 synthesis method Methods 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
Abstract
The invention discloses a preparation method of a metal atom electrocatalyst with stable carbon atom coordination, belonging to the field of new chemical material catalysis2Carrying out high-temperature treatment in the atmosphere to obtain a porous carbon carrier, then preparing a metal salt precursor, dropwise adding 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 using joule heat to obtain a metal atom electrocatalyst with stable carbon atom coordination; the carbon coordination atoms of the electrocatalyst prepared by the invention can effectively adjust the electronic structure of the metal active center, and the self-supporting macroscopic structure is beneficial to reducing the interface contact resistance in the electrocatalysis process, and has good application prospect in the fields of electrocatalysis 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 transition metal atoms loaded on the carbon-based material has the maximum atom utilization efficiency, and the interaction between the metal atoms and the carrier can adjust the electrocatalytic activity, so that the catalyst is a promising electrocatalyst for a plurality of energy-related reactions. However, the surface of metal atoms has high surface free energy, which is very easy to cause atom agglomeration and instability. At present, nitrogen-coordinated metal atom electrocatalysts have been more studied than carbon coordination. Carbon atoms are less electronegative than nitrogen atoms, and coordination of a metal atom to carbon can redistribute the charge at the center of the metal atom. The pure carbon atom coordination can effectively adjust the electronic structure of the metal active center, and the self-supporting macroscopic structure is favorable for reducing the interface contact resistance in the electrocatalysis process. Some conventional synthesis methods have the problems of high energy consumption, harsh conditions, complex procedures, uncontrollable capacity, low loading capacity and the like, and the development of the transition metal site electrocatalyst is seriously hindered. Therefore, it is currently a major challenge to simply and efficiently prepare electrocatalysts of carbon-coordinated transition metal atoms at normal temperature and pressure.
Disclosure of Invention
The invention provides a preparation method of a metal atom electrocatalyst with stable carbon atom coordination, aiming at the problems of the preparation method and coordination control of the existing transition metal atom electrocatalyst.
The preparation method of the metal atom electrocatalyst with stable carbon atom coordination adopts the self-supporting carbon-based carrier material without nitrogen element in CO2Carrying out high-temperature treatment in the atmosphere to obtain a porous carbon carrier, then preparing a metal salt precursor, dropwise adding 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 using joule heat to obtain a metal atom electrocatalyst with stable carbon atom coordination; the electrocatalytic hydrogen evolution under high current density has excellent catalytic activity.
The nitrogen-free self-supporting carbon-based carrier material is carbon cloth, carbon paper or a PVA-based carbon nanofiber membrane.
The metal salt is one or more of cobalt nitrate, nickel chloride and cobalt acetylacetonate, and the loading capacity of the metal salt is 1-20% of the mass of the porous carbon carrier.
The high-temperature treatment temperature of the nitrogen-free self-supporting carbon-based carrier material is 200-1000 ℃, and the treatment time is 15-600 min.
The current is applied by a programmable direct current power supply, the current parameter is 0.5A-5.5A, the number of thermal shocks is 1-20, and the oscillation time is 0.5-20 s each time.
The invention also aims to provide the metal atom electrocatalyst with stable carbon atom coordination, which is prepared by the method.
The invention has the following beneficial effects:
compared with the existing preparation method of the transition metal atom electrocatalyst and nitrogen atom coordination regulation, the preparation method has the advantages of short time consumption, easy regulation and simple operation; the carbon atom is used as a central atom, can have strong interaction with the metal atom, not only can simply and efficiently prepare the metal atom electrocatalyst, but also can stably show excellent electrocatalytic activity through coordination of the carbon atom.
Drawings
Fig. 1 is a picture of a 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 an electron micrograph of an electrocatalyst with transition metal cobalt atomic sites supported on carbon cloth prepared in example 1;
FIG. 4 is a BET characterization of the raw carbon cloth and the carbon cloth with supported transition metal atomic sites prepared in example 1;
fig. 5 is an LSV plot of electrocatalytic hydrogen evolution for the original carbon cloth prepared in example 1 and the carbon cloth with supported transition metal atomic sites.
Detailed Description
The present invention is further illustrated by the following examples, without limiting the scope of the invention thereto; in the examples, unless otherwise specified, all methods are conventional methods, and all reagents, unless otherwise specified, are conventional commercially available reagents or reagents prepared by conventional methods;
example 1
Selecting carbon cloth as self-supporting carbon-based carrier material, cutting the carbon cloth, and placing the cut carbon cloth in a tube furnace for CO2Treating at 900 deg.C for 180min to obtain porous carbon carrier, and weighing Co (NO)3)2·6H2O preparing a metal salt precursor solution, wherein the loading capacity of the metal salt is 3 percent of the mass of the porous carbon carrier, and then, preparing the metal salt precursor solutionDripping the driving liquid on a porous carbon carrier, drying at 60 ℃, then respectively connecting two ends of the porous carbon carrier to a conductive copper sheet, applying current to the carbon cloth for multiple times by using a programmable direct current power supply in an Ar environment, setting the current to be 5A, performing 10 times of thermal shock treatment on the carbon-based material by using generated Joule heat, wherein the shock time is 5s each time, and finally obtaining the metal Co atom electrocatalyst with a self-supporting structure and stable carbon atom coordination.
In this example, an electrocatalyst with metal cobalt atoms whose carbon atom coordination is stable is successfully prepared, as shown in fig. 1, the electron transport rate of the carbon cloth is improved because the carbon cloth has good conductivity and a large specific surface area, and as shown in fig. 2, the SEM image of the carbon cloth shows that the carbon cloth is a three-dimensional network structure formed by interweaving carbon cloth fibers. After 10 periodic high temperature heat shocks, it is obvious that a single metal Co atom is dispersedly loaded on the carbon substrate, as shown in FIG. 3. The transition metal atom-supporting carbon cloth prepared in this example had a high specific surface area, as shown in fig. 4. When the electrocatalyst prepared in the embodiment is applied to the electrocatalytic hydrogen evolution reaction, the result is shown in fig. 5, and the metal atom electrocatalyst with stable carbon coordination shows excellent hydrogen evolution performance under 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 for CO2Treating at 200 deg.C for 600min to obtain porous carbon carrier, and weighing NiCl2·6H2Preparing metal salt precursor liquid by O, wherein the loading capacity of metal salt is 10% of the mass of the porous carbon carrier, then dropwise adding the metal salt precursor liquid onto the porous carbon carrier, respectively connecting two ends of the porous carbon carrier to conductive copper sheets after drying at 60 ℃, applying current to the carbon paper for multiple times by using a programmable direct current source in an Ar environment, setting the current to be 5.5A, performing 20 times of thermal shock treatment on the carbon-based material by using generated Joule heat, wherein the shock time is 8s each time, and finally obtaining the metal Ni atom electrocatalyst with a self-supporting structure and stable carbon atom coordination.
Example 3
The PVA-based carbon nanofiber membrane (as referred to as "Donke" electrostatic spinning method for control)PVA-based whole-body porous carbon nanofiber membrane and electrochemical performance research thereof [ D]Made by the method in eastern China university) as a self-supporting carbon-based carrier material, cutting the PVA-based carbon nanofiber membrane, and then CO in a tubular furnace2Processing at 1000 ℃ for 15min in the atmosphere to obtain a porous carbon carrier, weighing cobalt acetylacetonate to prepare a metal salt precursor solution, wherein the load capacity of metal salt is 5% of the mass of the porous carbon carrier, then dropwise adding the metal salt precursor solution onto the porous carbon carrier, drying at 60 ℃, then respectively connecting two ends of the porous carbon carrier to conductive copper sheets, applying current to carbon paper for multiple times by using a programmable direct current power supply in an Ar environment, setting the current to be 3A, performing 15 times of thermal shock treatment on a carbon-based material by using generated Joule heat, wherein the shock time is 15s each time, and finally obtaining 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 for CO2Processing at 700 ℃ for 100min in the atmosphere to obtain a porous carbon carrier, weighing cobalt acetylacetonate to prepare a metal salt precursor solution, wherein the load capacity of metal salt is 1% of the mass of the porous carbon carrier, then dropwise adding the metal salt precursor solution onto the porous carbon carrier, respectively connecting two ends of the porous carbon carrier to conductive copper sheets after drying at 60 ℃, applying current to the porous carbon carrier for multiple times by using a programmable direct current source in an Ar environment, setting the current to be 0.5A, performing 5 times of thermal shock treatment on a carbon-based material by using generated Joule heat, wherein the shock time is 12s each time, and finally obtaining the carbon atom coordination stable metal Co atom electrocatalyst with a self-supporting structure.
Example 5
Selecting carbon cloth as self-supporting carbon-based material, cutting the carbon cloth, and placing the cut carbon cloth in a tube furnace for CO2Treating at 500 deg.C for 400min to obtain porous carbon carrier, and weighing NiCl2·6H2O preparing metal salt precursor liquid, wherein the load capacity of the metal salt is 15% of the mass of the porous carbon carrier, then dripping the metal salt precursor liquid on the porous carbon carrier, respectively connecting the two ends of the porous carbon carrier to conductive copper sheets after drying at 60 ℃, and in an Ar environment, utilizing a programmable direct current power supply to supply the porous carbon with a programmable direct current power supplyAnd (3) applying current to the carrier for multiple times, setting the current to be 5.5A, and carrying out 1-time thermal shock treatment on the carbon-based material by using the generated Joule heat, wherein the shock time is 20s each time, so as to finally obtain 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 carrying out CO (carbon monoxide) treatment in a tubular furnace2Processing at 800 ℃ for 480min in the atmosphere to obtain a porous carbon carrier, weighing cobalt acetylacetonate to prepare a metal salt precursor solution, wherein the load capacity of metal salt is 15% of the mass of the porous carbon carrier, then dropwise adding the metal salt precursor solution onto the porous carbon carrier, respectively connecting two ends of the porous carbon carrier to a conductive copper sheet after drying at 60 ℃, applying current to the porous carbon carrier for multiple times by using a programmable direct current power supply in an Ar environment, setting the current to be 4A, performing 10 times of thermal shock treatment on a carbon-based material by using generated joule heat, wherein the shock time is 20s each time, and finally obtaining the carbon atom coordination stable metal Co atom electrocatalyst with a self-supporting structure.
Example 7
Selecting carbon cloth as self-supporting carbon-based carrier material, cutting the carbon cloth, and placing the cut carbon cloth in a tube furnace for CO2Treating at the high temperature of 400 ℃ in the atmosphere for 400min to obtain a porous carbon carrier, weighing cobalt acetylacetonate to prepare a metal salt precursor solution, wherein the load capacity of metal salt is 20% of the mass of the porous carbon carrier, then dropwise adding the metal salt precursor solution onto the porous carbon carrier, drying at 60 ℃, then respectively connecting the two ends of the porous carbon carrier to conductive copper sheets, applying current to the carbon cloth for multiple times by using a programmable direct current source in an Ar environment, setting the current to be 2.5A, performing 15 times of thermal shock treatment on the carbon-based material by using generated Joule heat, wherein the shock time is 8s each time, and finally obtaining the carbon atom coordination stable metal Co atom electrocatalyst with a self-supporting structure.
Claims (7)
1. A preparation method of a metal atom electrocatalyst with stable carbon atom coordination is characterized by comprising the following steps: the nitrogen-free self-supporting carbon-based carrier material is placed in CO2High-temperature treatment under atmosphere to obtain porous carbonAnd (2) preparing a metal salt precursor, dropwise adding the precursor to a 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 using joule heat to obtain the metal atom electrocatalyst with stable carbon atom coordination.
2. The method for preparing a metal atom electrocatalyst with stable coordination of carbon atoms according to claim 1, wherein: the self-supporting carbon-based carrier material without nitrogen element is carbon cloth, carbon paper or PVA-based carbon nanofiber membrane.
3. The method for preparing a metal atom electrocatalyst with stable coordination of carbon atoms according to claim 1, wherein: the metal salt is one or more of cobalt nitrate, nickel chloride and cobalt acetylacetonate.
4. The method for preparing a metal atom electrocatalyst with stable coordination of carbon atoms according to claim 1, wherein: the high-temperature treatment temperature of the nitrogen-free self-supporting carbon-based carrier material is 200-1000 ℃, and the treatment time is 15-600 min.
5. The method for preparing a metal atom electrocatalyst with stable coordination of carbon atoms according to claim 1, characterized in that: the loading amount of the metal salt is 1% -20% of the mass of the porous carbon carrier.
6. The method for preparing a metal atom electrocatalyst with stable coordination of carbon atoms according to claim 1, wherein: the current is applied by a programmable direct current power supply, the current parameter is 0.5A-5.5A, the frequency of thermal shock is 1-20 times, and the time of each shock is 0.5 s-20 s.
7. The metal atom electrocatalyst with stable coordination of carbon atoms prepared by the method for preparing a metal atom electrocatalyst with stable coordination of carbon atoms according to any one of claims 1 to 6.
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