CN112853418A - Catalyst for battery anode reaction and preparation method and application thereof - Google Patents
Catalyst for battery anode reaction and preparation method and application thereof Download PDFInfo
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- CN112853418A CN112853418A CN202011631861.1A CN202011631861A CN112853418A CN 112853418 A CN112853418 A CN 112853418A CN 202011631861 A CN202011631861 A CN 202011631861A CN 112853418 A CN112853418 A CN 112853418A
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/06—Combination of fuel cells with means for production of reactants or for treatment of residues
- H01M8/0606—Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants
- H01M8/0656—Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants by electrochemical means
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Abstract
The invention belongs to the field of electrochemistry, and particularly relates to a catalyst for battery anode reaction, a preparation method and application thereof. The method comprises the following steps: step (1): selecting a conductive material with a porous structure as a substrate; step (2): preparing an electroplating solution; and (3): electrochemical deposition is carried out by adopting a constant current step wave pulse electroplating mode, and the Ni/Ni-P catalyst with the nano metal glass structure is prepared on the substrate. The invention combines nano metal glass with nickel and phosphorus elements with good catalytic performance, utilizes pulse electrodeposition technology and combines porous structure characteristics to prepare Ni/Ni-P novel nano metal glass catalyst, and improves the reaction rate of the catalyst on the anode of a battery; the invention can be widely applied to the fields of energy, chemical industry, environmental protection and the like.
Description
Technical Field
The invention belongs to the field of electrochemistry, and particularly relates to a catalyst for battery anode reaction, a preparation method and application thereof.
Background
Clean energy sources (renewable energy sources such as wind energy, solar energy, hydrogen energy and the like) play an important role in the historical progress and sustainable development of human society. The effective clean energy technology can not only promote the high-efficient utilization of energy, but also solve the existing environmental problems. At present, hydrogen fuel (mainly containing H2) can replace traditional fossil fuel due to its advantages of high energy density, environmental protection and the like, and is praised as sustainable clean energy. Currently, hydrogen production by catalytic water electrolysis seems to be a promising environmental protection method, however, it is well known that the efficiency of water electrolysis is limited by the slow Oxygen Evolution Reaction (OER) of the anode, and the water electrolysis requires a high overpotential (1.23V), which greatly limits the efficiency of hydrogen production energy and severely restricts the commercialization of hydrogen energy.
In addition to the use of OER catalysts, another solution is to incorporate "sacrificial agents" in the electrolyte, which have more easily oxidizable molecules. Thus, the oxidation reaction of the "sacrificial agent" can replace the slow OER to perform an active cell anode reaction. These include common organic compounds such as methanol, ethanol, ammonia, and urea. In the case of the sacrificial agent urea, the widely metabolic waste-derived material of urea generally gives people a "dirty" and "stale" impressive impression compared to "clean" and "advanced" hydrogen fuels. When in contact with atmospheric and groundwater, urea decomposes into ammonia and nitrates, which can cause serious health and environmental problems. However, in recent years, the use of urea as an alternative fuel in fuel cells has been significantly increased due to its high availability, stability and non-flammability. To solve these problems associated with urea, a method for generating clean energy simultaneously is to perform Urea Oxidation (UOR) using urea as a sacrificial agent for the anodic reaction. This reaction equation is as follows:
CO(NH2)2+H2O→N2+3H2+CO2
thermodynamically, urea oxidative decomposition requires a low potential of 0.37V for the reaction, compared to the theoretical voltage of water electrolysis of 1.23V, which means that an inexpensive method for producing hydrogen is provided by the urea oxidation reaction rather than by water electrolysis. Compared with other candidate sacrificial agents, the urea has rich properties and reasonable industrial production cost.
Noble metal-based catalysts are often used as a benchmark for battery anode reaction catalysts. However, expensive and scarce drawbacks have largely limited their development in current scientific research and future technology commercialization. Under such circumstances, the design and demand for non-noble metal transition metal based catalysts is imminent, and numerous experiments have demonstrated that such catalysts can perform as well as, or even exceed, noble metal catalysts. Of these, nickel is the most reported non-noble metal element because it effectively catalyzes the cell anode reaction at a lower overpotential.
The metallic glass has excellent catalytic performance due to the structural characteristics of long-range disorder and the thermodynamic characteristics of a metastable state. However, in recent years, a metallic glass having a novel amorphous structural feature is known to the world, that is, Nano-glass (NG). As shown in fig. 4, NG is composed of nano-sized amorphous clusters and interfaces between connected clusters (referred to as glass/glass interfaces). In the structural model of NG, the glass/glass interface is a few nanometers wide, locally reducing the density relative to adjacent clustered particles, which makes NG have significant structural non-uniformities on the nanometer scale. Meanwhile, the density of active sites of the catalyst can be effectively increased by increasing the interface, so that the catalytic activity is improved.
Disclosure of Invention
Aiming at the defects of the existing non-noble metal in the catalysis technology of the battery anode reaction, the invention provides a preparation method of a high-efficiency novel catalyst for the battery anode reaction by combining an economical and simple pulse plating process and the outstanding catalysis performance of amorphous materials.
The technical solution for realizing the purpose of the invention is as follows: a method for preparing a catalyst for an anode reaction of a battery, comprising the steps of:
step (1): selecting a conductive material with a porous structure as a substrate;
step (2): preparing an electroplating solution;
and (3): electrochemical deposition is carried out by adopting a constant current step wave pulse electroplating mode, and the Ni/Ni-P catalyst with the nano metal glass structure is prepared on the substrate.
Further, the substrate in the step (1) is foamed nickel or porous carbon paper.
Further, the step (2) of preparing the electroplating solution specifically comprises the following steps: taking nickel sulfate hexahydrate, nickel chloride hexahydrate, boric acid and phosphorous acid according to the weight ratio of 200 g/L: 25 g/L: 24 g/L: deionized water is added into the solution in a ratio of 4.5-6g/L to prepare 500mL of electroplating solution, and then the solution is placed in a water bath kettle at 50 ℃ and stirred by magnetic force until the solution is transparent and uniform.
Further, the step (1) further comprises a pre-treatment, specifically: respectively putting the substrate, the platinum sheet electrode, the platinum electrode clamp and the electrolytic cell into absolute ethyl alcohol for ultrasonic cleaning for 10-30 minutes, then putting the substrate, the platinum sheet electrode, the platinum electrode clamp and the electrolytic cell into deionized water for ultrasonic cleaning for 10-30 minutes, removing oil stains and dust on the surface, and drying the cleaned objects for later use; and (4) washing the saturated calomel electrode by using deionized water, and wiping the saturated calomel electrode dry for later use.
Further, the pulse plating in the step (3) is specifically as follows: slowly introducing the uniformly stirred electroplating solution into an electrolytic cell, firmly clamping a square substrate by a platinum electrode clamp, inserting the square substrate, a platinum sheet electrode and a saturated calomel electrode into the electrolytic cell together, connecting an electrochemical workstation with the electrolytic cell through a three-electrode wire, taking the platinum sheet electrode as an auxiliary electrode and the saturated calomel electrode as reference electrodes, taking a conductive substrate as a working electrode, and then switching on a power supply to select a constant current step wave pulse electroplating mode (namely inputting constant current according to current density and area of a sample and inputting time required by the current to pass) to carry out electrochemical deposition.
Further, the deposition temperature of the pulse plating is 30-50 ℃, and the current density of the pulse is 20-50mA/cm2And the deposition time is determined according to the thickness of the finished product.
A catalyst for anode reaction of battery is prepared by the method.
The application of the catalyst is used for battery anode reaction.
Further, the current density of the anode used for the battery is 10mA/cm2The reaction voltage was 1.36V in the urea oxidation reaction.
Compared with the prior art, the invention has the remarkable advantages that:
1. the invention prepares a novel catalyst by a pulse electrodeposition method, which is an economic and convenient electroplating preparation method and can be widely applied to production and scientific research.
2. The invention utilizes the catalysis of the anode reaction of the battery to generate clean energy (hydrogen energy), and well accords with the concept of the development of modern green energy. In the invention, taking urea oxidation reaction as an example, the overpotential of hydrogen energy generation is lower, the productivity efficiency is higher, and the harmful substance urea is oxidized and decomposed to generate clean energy hydrogen energy, so that green development of waste utilization, new energy regeneration and capacity efficiency improvement is realized.
3. The elements used in the invention are non-noble metal Ni and P elements, and the Ni element and the P element are mutually promoted under the synergistic action and have good catalytic effect. The prepared nano metal glass realizes the application of the nano metal glass which is a new material in the catalytic performance of the anodic oxidation reaction of the battery for the first time, and has stronger catalytic performance.
4. The invention takes the conductive material with a porous structure (such as foamed nickel, porous carbon paper and the like) as a substrate to prepare the novel catalyst, and utilizes the abundant specific surface area of the porous structure and the excellent catalytic performance of Ni element to bidirectionally promote the catalytic performance.
Drawings
FIG. 1 is a schematic diagram of the preparation of a novel high-efficiency catalyst Ni/Ni-P for anode reaction of a battery.
FIG. 2 is the LSV plot of the prepared novel catalyst Ni/Ni-P in UOR (comparative sample is foamed nickel).
FIG. 3 is an X-ray diffraction pattern of the prepared novel catalyst Ni/Ni-P.
FIG. 4 is a high-resolution transmission electron microscope (HE-TEM) image of the prepared novel catalyst Ni/Ni-P.
FIG. 5 is the scanning electron microscope and X-ray energy spectrum of the prepared novel catalyst Ni/Ni-P.
Detailed Description
The present invention is described in further detail below with reference to the attached drawing figures.
A schematic diagram of the design and preparation method of a novel high-efficiency catalyst for battery anode reaction is shown in figure 1, porous foam nickel is used as a substrate material, urea oxidation reaction is used as a performance detection case, and detailed preparation and test steps are as follows:
pre-treatment: respectively putting the porous foamed nickel, the platinum sheet electrode, the platinum electrode clamp and the electrolytic cell into absolute ethyl alcohol for ultrasonic cleaning for 10 minutes, then putting the porous foamed nickel, the platinum sheet electrode, the platinum electrode clamp and the electrolytic cell into deionized water for ultrasonic cleaning for 10 minutes to remove oil stains and dust on the surface, and drying the cleaned objects for later use; washing the saturated calomel electrode with deionized water, and wiping to dry for later use;
preparing an electroplating solution: taking nickel sulfate hexahydrate (6H)2O·NiSO4) Nickel chloride hexahydrate (6H)2O·NiCl2) Boric acid (H)2BO3) And phosphorous acid (H)2PO3) According to the ratio of 200 g/L: 25 g/L: 24 g/L: deionized water is added into the solution in a ratio of 4.82g/L to prepare 500mL of electroplating solution, and then the solution is placed in a water bath kettle at 50 ℃ for magnetic stirring until the solution is transparent and uniform;
pulse plating: slowly introducing the uniformly stirred electroplating solution into an electrolytic cell, taking a 2cm multiplied by 2cm square porous material foamed nickel substrate, firmly clamping the substrate by a platinum electrode clamp, inserting the substrate, a platinum sheet electrode and a saturated calomel electrode into the electrolytic cell, connecting an electrochemical workstation and the electrolytic cell through three-electrode wires (the platinum sheet electrode is an auxiliary electrode, the saturated calomel electrode is a reference electrode and the foamed nickel is a working electrode), then switching on a power supply to carry out electrochemical deposition by adopting a constant current step wave pulse electroplating mode, wherein the deposition time is 1 hour, the deposition temperature is 50 ℃, and the pulse current density is 37.5mA/cm2. The prepared catalyst sample is washed by deionized water and is in air conditionAnd naturally drying.
Carrying out structural characterization and UOR performance detection on the novel catalyst Ni/Ni-P, wherein the specific test steps and results are as follows:
to demonstrate the efficient performance of the novel catalyst, linear voltammetric sweep (LSV) testing and structural characterization in UOR was now performed:
the LSV test procedure in UOR is as follows:
solution proportioning: firstly, deionized water is used as a solvent to prepare a KOH solution with the substance amount concentration of 1mol/L, and then 1mol/L KOH is used as a solvent to prepare a urea solution with the substance amount concentration of 0.33mol/L for later use.
LSV test: pouring the prepared urea solution into a four-necked flask with about 250mL, connecting the three electrodes with an electrochemical workstation (in the same manner as the preparation method), and introducing high-purity oxygen (O) before LSV test2) The solution was saturated with oxygen for 30 minutes. The LSV curve was then tested by the electrochemical workstation for a test interval of 0.2V-0.8V and a scan rate of 5mV/s to obtain the current-voltage curve for the LSV test in UOR, as shown in FIG. 2. Found that the current density j is 10mA/cm2The potential is 1.36V (vs RHE), which indicates that the novel catalyst has stronger catalytic performance in the currently discovered UOR catalyst.
The prepared novel catalyst is analyzed on a sample by X-ray diffraction (XRD) (figure 3), and only one obvious and wide diffraction peak is found, thereby showing that the novel catalyst is an amorphous material; the Ni-P metal prepared by the pulse electrodeposition method at the current density was characterized as nano metallic glass by a high-resolution transmission electron microscope (HE-TEM) (FIG. 4); the scanning electron microscope picture of the prepared novel catalyst Ni/Ni-P is shown in FIG. 5, and the distribution of Ni and P elements in the prepared novel catalyst is found to be uniform by using X-ray energy spectrum analysis (EDS), and the distribution is shown in FIG. 5.
Therefore, the method for preparing the high-efficiency novel catalyst for the battery anode is an effective way for simply, efficiently and economically obtaining the catalyst with high catalytic performance.
Claims (9)
1. A method for preparing a catalyst for an anode reaction of a battery, comprising the steps of:
step (1): selecting a conductive material with a porous structure as a substrate;
step (2): preparing an electroplating solution;
and (3): electrochemical deposition is carried out by adopting a constant current step wave pulse electroplating mode, and the Ni/Ni-P catalyst with the nano metal glass structure is prepared on the substrate.
2. The method of claim 1, wherein the substrate in step (1) is foamed nickel or porous carbon paper.
3. The method according to claim 2, wherein the step (2) of preparing the electroplating solution comprises: taking nickel sulfate hexahydrate, nickel chloride hexahydrate, boric acid and phosphorous acid according to the weight ratio of 200 g/L: 25 g/L: 24 g/L: deionized water is added into the solution in a ratio of 4.5-6g/L to prepare 500mL of electroplating solution, and then the solution is placed in a water bath kettle at 50 ℃ and stirred by magnetic force until the solution is transparent and uniform.
4. The method according to claim 3, wherein step (1) further comprises a pre-treatment, in particular: respectively putting the substrate, the platinum sheet electrode, the platinum electrode clamp and the electrolytic cell into absolute ethyl alcohol for ultrasonic cleaning for 10-30 minutes, then putting the substrate, the platinum sheet electrode, the platinum electrode clamp and the electrolytic cell into deionized water for ultrasonic cleaning for 10-30 minutes, removing oil stains and dust on the surface, and drying the cleaned objects for later use; and (4) washing the saturated calomel electrode by using deionized water, and wiping the saturated calomel electrode dry for later use.
5. The method according to claim 4, wherein the pulse plating in step (3) is specifically: slowly introducing the uniformly stirred electroplating solution into an electrolytic cell, firmly clamping a square substrate by a platinum electrode clamp, inserting the square substrate, a platinum sheet electrode and a saturated calomel electrode into the electrolytic cell, connecting an electrochemical workstation with the electrolytic cell through a three-electrode wire, taking the platinum sheet electrode as an auxiliary electrode and the saturated calomel electrode as reference electrodes, taking a conductive substrate as a working electrode, and then turning on a power supply to select a constant current step wave pulse electroplating mode to carry out electrochemical deposition.
6. The method of claim 5, wherein the deposition temperature of the pulse plating is 30-50 ℃ and the current density of the pulse is 20-50mA/cm2And the deposition time is determined according to the thickness of the finished product.
7. A catalyst for use in an anode reaction of a battery, prepared by the method of any one of claims 1 to 6.
8. Use of the catalyst of claim 7 in a battery anode reaction.
9. Use according to claim 8, characterised in that the current density is 10mA/cm for the battery anode2The reaction voltage was 1.36V in the urea oxidation reaction.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150159242A1 (en) * | 2013-12-09 | 2015-06-11 | Glassimetal Technology, Inc. | Bulk nickel-based glasses bearing chromium, niobium, phosphorus and silicon |
| CN112080759A (en) * | 2020-08-27 | 2020-12-15 | 浙江工业大学 | Preparation method of bismuth-doped bimetallic sulfide electrode for electrocatalytic oxidation of urea |
| CN112090436A (en) * | 2020-09-14 | 2020-12-18 | 江浩 | Nickel-based catalyst, preparation method and application |
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- 2020-12-31 CN CN202011631861.1A patent/CN112853418A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150159242A1 (en) * | 2013-12-09 | 2015-06-11 | Glassimetal Technology, Inc. | Bulk nickel-based glasses bearing chromium, niobium, phosphorus and silicon |
| CN112080759A (en) * | 2020-08-27 | 2020-12-15 | 浙江工业大学 | Preparation method of bismuth-doped bimetallic sulfide electrode for electrocatalytic oxidation of urea |
| CN112090436A (en) * | 2020-09-14 | 2020-12-18 | 江浩 | Nickel-based catalyst, preparation method and application |
Non-Patent Citations (5)
| Title |
|---|
| CHUNYU GUO ET AL: "Ni-P nanoglass prepared by multi-phase pulsed electrodeposition", 《MATERIALS RESEARCH LETTERS》, vol. 5, no. 5, 12 December 2016 (2016-12-12), pages 293 - 299 * |
| DAWEN YANG ET AL: "Nanostructured Ni2P-C as an efficient catalyst for urea electro-oxidation", 《CHEMELECTROCHEM》, vol. 5, 28 December 2017 (2017-12-28), pages 659 - 664 * |
| GANG WANG ET AL: "Porous Ni2P nanoflower supported on nickel foam as an efficient three-dimensional electrode for urea electro-oxidation in alkaline medium", 《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》, vol. 43, 21 April 2018 (2018-04-21), pages 9316 - 9325 * |
| W.Y. CHEN ET AL: "Compositionally modulated microstructure in nano-layered Ni-P metallic glass composite coating prepared by electrodeposition", 《SURFACE & COATINGS TECHNOLOGY》, vol. 389, 12 March 2020 (2020-03-12), pages 125636, XP086137147, DOI: 10.1016/j.surfcoat.2020.125636 * |
| ZHAOTAO CUI ET AL: "Ultrastable Ni-P amorphous alloy formed via high temperature electrodeposition", 《JOURNAL OF NON-CRYSTALLINE SOLIDS》, vol. 551, 30 September 2020 (2020-09-30), pages 120398, XP086318501, DOI: 10.1016/j.jnoncrysol.2020.120398 * |
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