CN111041520A - Coating electrode for catalytic hydrogen evolution and preparation method thereof - Google Patents
Coating electrode for catalytic hydrogen evolution and preparation method thereof Download PDFInfo
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- CN111041520A CN111041520A CN201911299175.6A CN201911299175A CN111041520A CN 111041520 A CN111041520 A CN 111041520A CN 201911299175 A CN201911299175 A CN 201911299175A CN 111041520 A CN111041520 A CN 111041520A
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- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0635—Carbides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
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- 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
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- 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
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention relates to a coated electrode for catalytic hydrogen evolution, which comprises a Ti substrate and a (W, Fe) C-P coating arranged on the surface of the Ti substrate. According to the coating electrode, the (W, Fe) C-P coating with catalytic activity is directly prepared on the Ti substrate electrode, and compared with a traditional coating electrode prepared by adopting a binder, the coating electrode has better bonding force and better stability, and the service life of the electrode is prolonged; the (W, Fe) C alloy with low price has higher hydrogen evolution catalytic activity, and the P element is introduced into the (W, Fe) C alloy to further improve the catalytic activity of the (W, Fe) C alloy for catalyzing hydrogen evolution, improve the working efficiency of catalyzing hydrogen evolution and reduce the cost for preparing the coating electrode for catalyzing hydrogen evolution.
Description
Technical Field
The invention relates to a coating electrode for catalytic hydrogen evolution and a preparation method thereof.
Background
The energy is an important basis for human survival and is a driving force for promoting national economy and social development. With the increasing demand for energy and the increasing problem of environmental pollution, the search for clean and sustainable energy has become an urgent issue for human beings. Hydrogen (H)2) The hydrogen is not naturally present and needs to be prepared by a certain method. The hydrogen production by water electrolysis has the advantages of low cost, high efficiency, environmental friendliness, good safety and the like, is an ideal path for converting electric energy into chemical energy, and is popular among people. The solid-state catalyst with the best electrocatalytic hydrogen evolution activity is noble metal platinum (Pt), but the high cost and low reserves severely limit the industrial application of noble metal materials. In addition, most of electrodes for catalyzing hydrogen evolution reaction adopt a binder to coat powdery catalytic materials on a substrate electrode, and the binder is easy to fall off in the electrolysis process due to the poor adhesive force of the binder, so that the working stability of the electrode is reduced. At the same time, the binder causes an increase in the resistance of the electrode, a decrease in the active sites exposed to the solution, and a decrease in the diffusion rate of the reactive ions, thereby greatly decreasing the hydrogen evolution efficiency of the electrode. Therefore, a catalytic material with low cost and high stability is urgently needed to realize large-scale production and wide application of hydrogen production by water electrolysis.
Disclosure of Invention
The invention aims to provide a coating electrode which is used for catalyzing hydrogen evolution, has good catalytic activity and high stability and is low in price.
In order to achieve the purpose, the invention provides the following technical scheme: a coated electrode for catalytic hydrogen evolution comprises a Ti substrate and a (W, Fe) C-P coating layer arranged on the surface of the Ti substrate.
Further, the (W, Fe) C-P coating includes a (W, Fe) C coating and a P element embedded within the (W, Fe) C coating.
Further, the thickness of the (W, Fe) C coating is 3um-6 um.
The invention also provides a preparation method for preparing the coating electrode for catalytic hydrogen evolution, which comprises the following steps:
s1, providing a Ti substrate, and roughening the surface of the Ti substrate;
s2, depositing a (W, Fe) C coating on the surface of the Ti substrate;
s3, performing phosphating treatment on the (W, Fe) C coating to obtain the (W, Fe) C-P coating.
Further, the roughening is to put the Ti substrate into picric acid to be heated for 30min to etch the surface thereof.
Further, the (W, Fe) C coating is formed by deposition preparation of a magnetron sputtering technology.
Further, the magnetron sputtering technology uses a W target and an Fe target, and the reaction gas is C2H2。
Further, before depositing the (W, Fe) C coating, the preparation method of the coating electrode further comprises the pretreatment of cleaning and drying the Ti substrate, the W target and the Fe target.
Further, after the pretreatment of cleaning and drying the Ti substrate, the preparation method of the coating electrode also comprises the steps of cleaning the Ti substrate by ion bombardment and activating atoms on the Ti substrate.
Further, the phosphorus source used in the phosphating treatment is sodium phosphite.
The invention has the beneficial effects that: compared with the traditional coating type electrode prepared by adopting an adhesive, the coating electrode has better bonding force and better stability, and prolongs the service life of the electrode; the (W, Fe) C alloy with low price has higher hydrogen evolution catalytic activity, and the P element is introduced into the (W, Fe) C alloy to further improve the catalytic activity of the (W, Fe) C alloy for catalyzing hydrogen evolution, improve the working efficiency of catalyzing hydrogen evolution and reduce the cost for preparing the coating electrode for catalyzing hydrogen evolution.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
Fig. 1 is a schematic structural diagram of a coated electrode for catalytic hydrogen evolution according to an embodiment of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the mechanism or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Referring to fig. 1, a coated electrode for catalytic hydrogen evolution according to an embodiment of the present invention includes a Ti substrate 1 and a (W, Fe) C-P coating 2 disposed on a surface of the Ti substrate 1. The (W, Fe) C — P coating layer 2 includes a (W, Fe) C coating layer (not shown) and a P element (not shown) embedded in the (W, Fe) C coating layer. The thickness of the (W, Fe) C coating is 3um-6 um. The metals W and Fe belong to medium overpotential metals in the hydrogen evolution reaction process, when the W and Fe are combined with the C, the d-bands of the two metals shrink, the energy center of the d-band is close to the Fermi level, and the formed (W, Fe) C alloy shows higher hydrogen evolution catalytic activity. When P and C are codoped with W and Fe, a synergistic effect of promoting hydrogen evolution reaction is formed. Therefore, the P element is introduced into the (W, Fe) C to further improve the catalytic activity of the electrolyzed water.
The invention also provides a preparation method for preparing the coating electrode for catalytic hydrogen evolution, which comprises the following steps:
step 1, providing a Ti substrate 1, and roughening the surface of the Ti substrate 1. Specifically, the Ti substrate 1 is placed into picric acid solution to be heated for 30min, and the surface of the Ti substrate 1 is etched.
And 2, carrying out ultrasonic cleaning and drying on the Ti substrate 1 with the roughened surface and the W target and the Fe target used for magnetron sputtering, and then putting the Ti substrate and the W target and the Fe target into a vacuum cavity of a magnetron sputtering instrument.
And 3, cleaning the Ti substrate 1 by ion bombardment and activating atoms on the Ti substrate 1. Specifically, the vacuum is pumped and heated until the vacuum degree reaches 1.0 × 10-3Introducing argon (Ar) with the purity of 99.999 percent above Pa, controlling the pressure at 1Pa-2Pa, starting an arc ion source to carry out ion bombardment on the Ti substrate 1, controlling the current at 40A-80A, controlling the bias voltage at 100V-1000V, controlling the duty ratio at 30-50 percent, and controlling the ion bombardment time at 20min-40 min.
And 4, depositing a (W, Fe) C coating on the surface of the Ti substrate 1. Specifically, the (W, Fe) C coating is prepared by deposition by a magnetron sputtering technology and is vacuumized to 1.0x10-3Vacuum degree above Pa, introducing C2H2As reaction gas, the pressure is controlled at 0.1Pa-0.2Pa, the substrate bias is controlled at 60V-100V, the flow rate of Ar is 30ccm, the W target and the Fe target are turned on, C2H2Reacting with sputtering deposition W and Fe to deposit a (W, Fe) C layer, wherein the thickness of the (W, Fe) C layer is controlled to be 3-6 um.
And 5, carrying out phosphating treatment on the (W, Fe) C coating to obtain the (W, Fe) C-P coating 2. Specifically, a phosphorus source used in phosphating is sodium phosphite, a Ti substrate 1 with a (W, Fe) C coating on the surface obtained by magnetron sputtering is placed into a tubular furnace, 0.5g-1g of hypophosphorous acid is placed upstream, Ar is introduced, the flow rate of Ar is 150ccm-300ccm, the phosphating reaction temperature is 250 ℃ -350 ℃, the phosphating time is 2h, and after the reaction is finished, the reaction is cooled to room temperature along with the furnace and then taken out.
The prepared coating electrode shows good catalytic activity in 1.0mol/L KOH solution and has the thickness of 10mAcm-2The overpotential under the current density of (1) is 90mV-140mV, and the Tafel slope is 70mVdec-1-100mV dec-1。
In conclusion, the (W, Fe) C-P coating with catalytic activity is directly prepared on the Ti substrate electrode by the coating electrode for catalytic hydrogen evolution, and compared with the traditional coating electrode prepared by adopting the adhesive, the coating electrode has better bonding force and better stability, and the service life of the electrode is prolonged; the (W, Fe) C alloy with low price has higher hydrogen evolution catalytic activity, and the P element is introduced into the (W, Fe) C alloy to further improve the catalytic activity of the (W, Fe) C alloy for catalyzing hydrogen evolution, improve the working efficiency of catalyzing hydrogen evolution and reduce the cost for preparing the coating electrode for catalyzing hydrogen evolution.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A coated electrode for catalytic hydrogen evolution, characterized in that it comprises a Ti substrate and a (W, Fe) C-P coating provided on the surface of the Ti substrate.
2. The coated electrode for catalytic hydrogen evolution of claim 1, wherein the (W, Fe) C-P coating comprises a (W, Fe) C coating and a P element embedded within the (W, Fe) C coating.
3. The coated electrode for catalytic hydrogen evolution according to claim 2, characterized in that the (W, Fe) C coating has a thickness of 3um to 6 um.
4. A method for preparing a coated electrode for catalytic hydrogen evolution according to any of claims 1 to 3, characterized in that it is as follows:
s1, providing a Ti substrate, and roughening the surface of the Ti substrate;
s2, depositing a (W, Fe) C coating on the surface of the Ti substrate;
s3, performing phosphating treatment on the (W, Fe) C coating to obtain the (W, Fe) C-P coating.
5. The method of preparing a coated electrode for catalytic hydrogen evolution according to claim 4, wherein the roughening is to etch the surface of the Ti substrate by heating it in picric acid for 30 min.
6. The process for the preparation of a coated electrode for the catalytic hydrogen evolution according to claim 4, characterized in that said (W, Fe) C coating is deposited by magnetron sputtering technique.
7. The process for the preparation of a coated electrode for the catalytic hydrogen evolution according to claim 6, characterized in that said magnetron sputtering technique uses a W target and a Fe target, the reaction gas being C2H2。
8. The method of preparing a coated electrode for catalytic hydrogen evolution according to claim 7, wherein the method of preparing the coated electrode further comprises a pre-treatment of washing and baking the Ti substrate, the W target and the Fe target before depositing the (W, Fe) C coating.
9. The method of preparing a coated electrode for catalytic hydrogen evolution according to claim 8, wherein after pre-treating a Ti substrate for cleaning and drying, the method of preparing the coated electrode further comprises cleaning the Ti substrate by ion bombardment and activating atoms on the Ti substrate.
10. The method of claim 4, wherein the phosphorous source used in the phosphating is sodium phosphite.
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| CN201911299175.6A CN111041520A (en) | 2019-12-17 | 2019-12-17 | Coating electrode for catalytic hydrogen evolution and preparation method thereof |
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| CN201911299175.6A CN111041520A (en) | 2019-12-17 | 2019-12-17 | Coating electrode for catalytic hydrogen evolution and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2356964C1 (en) * | 2007-08-16 | 2009-05-27 | Вадим Георгиевич Глебовский | Manufacturing method of sputtering targets from cast disilicide of refractory metal and facility for its implementation |
| CN104630822A (en) * | 2015-01-14 | 2015-05-20 | 太原理工大学 | Foam transition-metal solid (gas) phosphated self-support hydrogen evolution electrode and preparation method thereof |
| JP2016050327A (en) * | 2014-08-29 | 2016-04-11 | 株式会社豊田中央研究所 | Semiconductor electrode, light energy conversion device and method for producing semiconductor electrode |
| CN109136981A (en) * | 2018-08-30 | 2019-01-04 | 合肥工业大学 | A kind of FeCo base metal glass film elctro-catalyst and the preparation method and application thereof |
| CN110237847A (en) * | 2019-07-22 | 2019-09-17 | 清华大学 | Elctro-catalyst, electrode and its preparation method and application |
-
2019
- 2019-12-17 CN CN201911299175.6A patent/CN111041520A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2356964C1 (en) * | 2007-08-16 | 2009-05-27 | Вадим Георгиевич Глебовский | Manufacturing method of sputtering targets from cast disilicide of refractory metal and facility for its implementation |
| JP2016050327A (en) * | 2014-08-29 | 2016-04-11 | 株式会社豊田中央研究所 | Semiconductor electrode, light energy conversion device and method for producing semiconductor electrode |
| CN104630822A (en) * | 2015-01-14 | 2015-05-20 | 太原理工大学 | Foam transition-metal solid (gas) phosphated self-support hydrogen evolution electrode and preparation method thereof |
| CN109136981A (en) * | 2018-08-30 | 2019-01-04 | 合肥工业大学 | A kind of FeCo base metal glass film elctro-catalyst and the preparation method and application thereof |
| CN110237847A (en) * | 2019-07-22 | 2019-09-17 | 清华大学 | Elctro-catalyst, electrode and its preparation method and application |
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Application publication date: 20200421 |