CN109126834B - FeSe-based amorphous thin film catalyst and preparation method and application thereof - Google Patents
FeSe-based amorphous thin film catalyst and preparation method and application thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- 239000010409 thin film Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001301 oxygen Substances 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 10
- 229910045601 alloy Inorganic materials 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 239000013077 target material Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 26
- 239000010408 film Substances 0.000 description 23
- 230000003197 catalytic effect Effects 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910002546 FeCo Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001370 Se alloy Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000009412 basement excavation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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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
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- 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 discloses a FeSe-based amorphous thin film catalyst and a preparation method and application thereof, wherein the structural formula of the FeSe-based amorphous thin film catalyst according to the atomic percent of each element is as follows: fexCoySezWherein x is more than or equal to 20 and less than or equal to 50, y is more than or equal to 20 and less than or equal to 50, z is more than or equal to 5 and less than or equal to 35, x + y + z is 100, and y is more than or equal to x + z. The FeSe-based amorphous thin film catalyst is prepared by a magnetron sputtering coating method, has good oxygen evolution performance and can be used as an oxygen evolution catalyst.
Description
Technical Field
The invention belongs to the field of amorphous alloy, and particularly relates to a FeSe-based amorphous thin film catalyst and a preparation method and application thereof.
Background
The water electrolysis hydrogen and oxygen production technology is considered as a promising clean energy technology due to rich resources and low carbon emission. The oxygen evolution reaction is an important half reaction of the electrocatalytic hydrolysis reaction and is a hot point of research of people at present. In the early stage of the research of oxygen evolution reaction electrocatalysts, people pay attention to noble metal materials such as Ir, Ru and the like. Precious metal materials have limited their widespread commercial use due to high cost and scarcity. In order to avoid high cost, the research on the electrocatalysis of the oxygen evolution reaction of the transition alloy and the boride, carbide, oxide, sulfide, phosphide and selenide thereof is widely regarded.
Compared with crystalline alloys, amorphous alloys have been considered as potential catalysts because of their excellent stability and high catalytic activity due to their special structure (long-range disorder, porous structure without crystal defects such as dislocation, uniform composition, etc.). The film as a two-dimensional material has larger specific surface area, smaller raw material requirement and good development potential compared with strip and block materials. At present, most of Fe-Co-Se alloy catalysts are of mosaic structures of FeCo and Se nanospheres deposited electrochemically, but the components cannot be well controlled, and an iron-based film has high instability in a catalytic medium, so that the excavation of an amorphous film with a more compact structure and high catalytic activity has great application prospects.
Disclosure of Invention
In order to avoid the defects of the prior art, the invention discloses a FeSe-based amorphous thin film catalyst and a preparation method and application thereof, aiming at obtaining the catalyst with good oxygen evolution catalytic performance by reasonably designing alloy components and groping preparation conditions.
In order to realize the purpose of the invention, the following technical scheme is adopted:
the invention discloses a FeSe-based amorphous thin film catalyst, which has the structural formula according to the atomic percent of each element: fexCoySezWherein x is more than or equal to 20 and less than or equal to 50, y is more than or equal to 20 and less than or equal to 50, z is more than or equal to 5 and less than or equal to 35, x + y + z is 100, and y is more than or equal to x + z. Preferably, the structural formula of the FeSe-based amorphous thin film catalyst according to the atomic percent of each element is as follows: fe40Co40Se20The investigation and the test on different components prove that the Fe40Co40Se20The amorphous thin film catalyst has optimal oxygen evolution catalytic performance.
The preparation method of the FeSe-based amorphous thin film catalyst comprises the following steps: according to the atomic percentage of each element, Fe powder, Co powder and Se powder are used as raw materials to prepare an alloy target material; then preparing the FeSe-based amorphous thin film catalyst by a vacuum magnetron sputtering method.
Preferably, the vacuum magnetron sputtering conditions are as follows: background vacuum degree higher than 3.0 × 10-4Pa, working pressure of 0.60Pa, power of 100W, and substrate temperature of 25-120 ℃.
Preferably, the purity of each raw material is more than or equal to 99.9 wt.%.
The conventional amorphous alloy is generally prepared by rapidly cooling a melt at a high temperature to avoid crystallization to obtain an amorphous sample, and by adopting the method, if the cooling rate is reduced, the crystalline sample is obtained. The invention prepares the FeSe-based amorphous thin film catalyst by the vacuum magnetron sputtering coating technology, avoids the problems and has the following advantages: the consistency of the formed film is good, and even under the condition of cathode sputtering with the length of several meters, the consistency of the film layer can be still ensured; the temperature rise of the substrate is low; the energy of sputtered particles is about tens of electron volts, the formed film is compact, and the film/base combination is good; the magnetron sputtering adjusting parameters can tune the film performance; the coating is particularly suitable for large-area coating, and the large-area film layer is deposited uniformly; the film grows layer by layer, and surface atoms have very high relaxation and diffusion capacities due to large vibration amplitude of the surface atoms; thin films are relatively thin and amorphous films are formed with a greater compositional range than bulk amorphous films.
The FeSe-based amorphous thin film catalyst has good oxygen evolution catalytic performance and can be used as an oxygen evolution catalyst.
The invention has the beneficial effects that:
1. the invention discloses a FeSe-based amorphous thin film catalyst which has good oxygen evolution catalytic performance through reasonable component design, and provides more catalyst choices for enterprises and research institutions in the aspect of water electrolysis.
2. The FeSe-based amorphous film catalyst is prepared by a vacuum magnetron sputtering method, and the film has uniform component distribution and stable amorphous structure.
Drawings
FIG. 1 shows Fe obtained in example 140Co40Se20XRD pattern of amorphous thin film;
FIG. 2 shows Fe obtained in example 140Co40Se20DSC curve of amorphous thin film;
FIG. 3 shows Fe obtained in example 140Co40Se20Electrochemical catalytic oxygen evolution curve of amorphous thin film.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof will be described in detail with reference to the following examples. The following is merely exemplary and illustrative of the inventive concept and various modifications, additions and substitutions of similar embodiments may be made to the described embodiments by those skilled in the art without departing from the inventive concept or exceeding the scope of the claims defined thereby.
Example 1
This example Fe40Co40Se20The amorphous film catalyst has a structural formula according to the atomic percent of each element: fe40Co40Se20The preparation method comprises the following steps:
step 1, according to Fe40Co40Se20The alloy composition general formula needs the atomic ratio, and Fe powder, Co powder and Se powder are used as raw materials (the purity of each raw material is more than or equal to 99.9 wt.%) to prepare the alloy target material (ordered by new materials in Beijing).
And 2, cleaning the alloy target obtained in the step 1 by using absolute ethyl alcohol, drying, and placing on a target head in a chamber of a vacuum magnetron sputtering coating machine.
In order to meet the requirements of different tests on the substrate, three substrates of carbon paper, glass sheets and silver foils are taken, cleaned by acetone and absolute ethyl alcohol and then adhered to a substrate of a vacuum magnetron sputtering coating machine.
Step 3, sealing the chamber, vacuumizing to the vacuum degree of 3.0 multiplied by 10-4Below Pa, argon is then injected to maintain the working pressure of the chamber at 0.60 Pa.
And 4, opening a temperature control table, raising the temperature of the base plate to 120 ℃, rotating at the speed of 40r/min, and turning on a direct current power supply to adjust the power to 100W for pre-sputtering.
And 5, removing the baffle plate after the arc light on the surface of the target material is stable, and starting sputtering.
And 6, closing the baffle to close the power supply and stop sputtering when the film thickness definition shows 1.5 mu m. And (4) flushing argon to more than 200Pa, cooling the sample along with the furnace, and taking out the sample.
Characterization of glass flake-based Fe by X-ray diffraction (equipment model: X' Pert Pro MPD X-ray diffractometer, Panacaceae (Panalytical), the Netherlands)40Co40Se20The structure of the amorphous film sample, the results are shown in FIG. 1. It can be seen from fig. 1 that the XRD profile of the film, except for the diffuse steamed bun peaks, has no sharp diffraction peaks,
characterization of the Fe on silver foil by differential scanning calorimetry (equipment type: STA449F3, Germany Steed)40Co40Se20The thermodynamic parameter of the amorphous film sample is that the heating rate is 20K/min. The DSC curve is shown in figure 2, and has a distinct exothermic crystallization peak, which indicates that the alloy film is completely amorphous.
Fe based on carbon paper40Co40Se20The amorphous film sample was used as an oxygen evolution electrode using an electrochemical workstation (type of equipment used: [ H ]]Electrochemical workstation, [ H ]]Shanghai chen instruments ltd) measured the oxygen evolution performance of the samples in a 1mol/L KOH solution, and the results are shown in fig. 3. It can be seen that Fe is present in KOH solution40Co40Se20The amorphous film has good oxygen evolution performance, and when the current reaches 10mA/cm2The overpotential required is 300 mV. Table 1 is Fe40Co40Se20Comparing EDX components before and after electrochemical catalytic oxygen evolution test of the amorphous film, and showing that the components before and after the measurement of the sample are unchanged.
Example 2
This example prepared Fe in the same manner as in example 140Co40Se20Amorphous thin film catalyst, differing only in that the temperature in step 4 was 25 ℃.
The sample obtained in the embodiment is completely amorphous and has good oxygen evolution performance, and when the current reaches 10mA/cm in KOH solution2The overpotential required is 330mV, and the chemical composition is unchanged.
Example 3
This example prepared Fe in the same manner as in example 140Co40Se20Amorphous thin film catalyst, differing only in that the temperature in step 4 was 200 ℃.
The sample obtained in the embodiment is a mixture of crystal and amorphous, the oxygen evolution performance is good, and when the current reaches 10mA/cm in KOH solution2The overpotential required was 297mV, but the chemical composition changed before and after the measurement, i.e., the state of the catalyst was unstable.
Example 4
This example prepared Fe in the same manner as in example 140Co40Se20Amorphous thin film catalyst, differing only in that the temperature in step 4 was 300 ℃.
The sample obtained in the embodiment is in a crystal state and has poor oxygen evolution performance by characterization, and when the current reaches 10mA/cm in a KOH solution2The overpotential required for this time was 333mV and the composition changed before and after the measurement, i.e., the catalyst was unstable.
TABLE 1
| Examples | 1 | 2 | 3 | 4 |
| Temperature of | 25℃ | 120℃ | 200℃ | 300℃ |
| Ingredients before testing | Fe39.2Co39.26Se21.54 | Fe38.59Co40.73Se20.68 | Fe41.53Co41.47Se17 | Fe37.94Co38.26Se23.80 |
| After testing the composition | Fe40.23Co40.30Se19.47 | Fe40.42Co40.79Se18.79 | Fe45.05Co47Se7.95 | Fe45.67Co51.78Se2.55 |
The present invention is not limited to the above exemplary embodiments, and any modifications, equivalent replacements, and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A FeSe-based amorphous thin film catalyst is characterized in that: the structural formula of the FeSe-based amorphous thin film catalyst in atomic percent of each element is as follows: fe40Co40Se20。
2. A method for preparing a FeSe-based amorphous thin film catalyst according to claim 1, characterized in that: according to the atomic percentage of each element, Fe powder, Co powder and Se powder are used as raw materials to prepare an alloy target material; then preparing a FeSe-based amorphous thin film catalyst by a vacuum magnetron sputtering method;
the conditions of the vacuum magnetron sputtering are as follows: background vacuum degree higher than 3.0X 10-4Pa, working pressure of 0.60Pa, power of 100W, and substrate temperature of 25-120 ℃.
3. The method of claim 2, wherein: the purity of each raw material is more than or equal to 99.9 wt.%.
4. The use of the FeSe-based amorphous thin film catalyst as claimed in claim 1, wherein: used as an oxygen evolution catalyst.
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Citations (5)
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|---|---|---|---|---|
| CN102925869A (en) * | 2012-10-26 | 2013-02-13 | 西安交通大学 | Method for preparing amorphous/nanometer crystal multilayer-structure film |
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| CN103805920A (en) * | 2014-01-23 | 2014-05-21 | 浙江大学 | Metallic glass film for plastic deformation processing and preparation method of micro-component of metallic glass film |
| CN105002467A (en) * | 2015-08-18 | 2015-10-28 | 合肥工业大学 | Cu-Ti amorphous alloy film and preparation method thereof |
| CN107217219A (en) * | 2017-06-08 | 2017-09-29 | 合肥工业大学 | It is a kind of for Fe Co P C systems amorphous elctro-catalyst of efficient evolving hydrogen reaction and preparation method thereof |
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|---|---|---|---|---|
| CN102925869A (en) * | 2012-10-26 | 2013-02-13 | 西安交通大学 | Method for preparing amorphous/nanometer crystal multilayer-structure film |
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| CN103805920A (en) * | 2014-01-23 | 2014-05-21 | 浙江大学 | Metallic glass film for plastic deformation processing and preparation method of micro-component of metallic glass film |
| CN105002467A (en) * | 2015-08-18 | 2015-10-28 | 合肥工业大学 | Cu-Ti amorphous alloy film and preparation method thereof |
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Non-Patent Citations (1)
| Title |
|---|
| Phase Exploration and Identification of Multinary Transition-Metal Selenides as High-Efficiency Oxygen Evolution Electrocatalysts through Combinatorial Electrodeposition;Xi Cao，等;《ACS Catal.》;20180725;第8卷;第8273-8289页 * |
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