CN110791770B - Preparation and application of photo-assisted thermoelectric coupling oxygen precipitation electrode - Google Patents
Preparation and application of photo-assisted thermoelectric coupling oxygen precipitation electrode Download PDFInfo
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000001301 oxygen Substances 0.000 title claims abstract description 74
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 74
- 238000001556 precipitation Methods 0.000 title claims abstract description 34
- 230000008878 coupling Effects 0.000 title claims abstract description 32
- 238000010168 coupling process Methods 0.000 title claims abstract description 32
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000000694 effects Effects 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000011521 glass Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 229910001868 water Inorganic materials 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000003197 catalytic effect Effects 0.000 claims abstract description 9
- 230000009467 reduction Effects 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 5
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 4
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 37
- 229910052710 silicon Inorganic materials 0.000 claims description 37
- 239000010703 silicon Substances 0.000 claims description 37
- 238000012360 testing method Methods 0.000 claims description 30
- 229910002640 NiOOH Inorganic materials 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 22
- 238000004070 electrodeposition Methods 0.000 claims description 19
- 239000002105 nanoparticle Substances 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000005286 illumination Methods 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 12
- 239000003792 electrolyte Substances 0.000 claims description 12
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 12
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 12
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
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- 238000005406 washing Methods 0.000 claims description 9
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
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- 238000000151 deposition Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
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- 239000007864 aqueous solution Substances 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
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- XEMZLVDIUVCKGL-UHFFFAOYSA-N hydrogen peroxide;sulfuric acid Chemical compound OO.OS(O)(=O)=O XEMZLVDIUVCKGL-UHFFFAOYSA-N 0.000 claims description 2
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- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims 2
- 230000005619 thermoelectricity Effects 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 2
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- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
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- 238000005265 energy consumption Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
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- 229910052759 nickel Inorganic materials 0.000 description 1
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- 229910000510 noble metal Inorganic materials 0.000 description 1
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- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
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- 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
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- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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Abstract
The invention relates to a light-assisted thermoelectric coupling oxygen precipitation electrode, wherein conductive glass or a photoanode is used as a substrate layer, a substance with a surface plasma resonance effect is a photo-thermal layer, and a metal basic oxide is used as a catalytic layer. The light irradiates the photothermal layer to generate heat, the heat drives the high-valence metal basic oxide to oxidize water and generate oxygen, the basic oxide is reduced into hydroxide, and the hydroxide is oxidized into the basic oxide by using lower positive pressure, so that the thermoelectricity coupling of the oxygen generation reaction is realized. The light-assisted thermoelectric coupling oxygen precipitation electrode designed by the invention complementarily uses electric energy, heat energy and light energy, and realizes cascade utilization of various energy sources. The photo-assisted thermoelectric coupling oxygen precipitation electrode designed by the invention can be used as a proton donor to be applied to systems of water electrolysis, electrocatalytic carbon dioxide reduction and electrocatalytic nitrogen reduction, and the preparation method is simple, convenient to use and easy for industrial production.
Description
The technical field is as follows:
the invention relates to a light-assisted thermoelectric coupling oxygen precipitation electrode; the invention also relates to the structure, the material, the preparation method and the application of the oxygen evolution electrode.
Background art:
as the global environment is increasingly deteriorated and the shortage of fossil energy is gradually increased, people are deeply aware that the development of energy cascade utilization and the development of renewable energy are imminent. Therefore, the rational utilization of low-grade energy such as industrial waste heat, low-ebb electricity and intermittent renewable energy (light, wind, tide and the like) is receiving wide attention of researchers. Wherein, H is2O、CO2、N2The conversion of inert molecules into energetic molecules is an effective way, and in these reaction systems, the proton donor is a key part.
Oxygen Evolution Reaction (OER) is a general proton donor Reaction[1]. However, the oxygen evolution reaction kinetics is slow and requires a high overpotential; the catalyst with excellent performance is Ir-based and Ru-based noble metal and oxides thereof, and has low reserve and high price; the above factors result in high application cost of oxygen precipitation reaction, and limit its wide application[2,3]。
Reference documents:
[1]Xu Z.,Yan S.C.,Zou Z.G.,et al.Interface Manipulation to Improve Plasmon-Coupled Photoelectrochemical Water Splitting onα-Fe2O3Photoanodes[J],ChemSusChem,2018,11:237-244.
[2]Yao Y.F.,Yan S.C.,Zou Z.G.,et al.Unlocking the potential of graphene for water oxidation using an orbital hybridization strategy[J],Energy&Environment Science,2018,11:407-416.
[3]Dotan H.,Rothschild A.,Grader G.S.,et al.Decoupled hydrogen and oxygen evolution by a two-step electrochemical–chemical cycle for efficient overall water splitting[J],Nature Energy,2019,4:786-795.
the invention content is as follows:
the first purpose of the invention is to design and develop a light-assisted thermoelectric oxygen precipitation electrode and illustrate the working mechanism; the second object of the present invention is to provide a method for producing the above-mentioned photo-assisted thermoelectric coupling oxygen evolution electrode; the third object of the present invention is to provide the use of the above-mentioned photo-assisted thermoelectric coupling oxygen evolution electrode.
The invention has the technical scheme that the photo-assisted thermoelectric coupling oxygen precipitation electrode comprises a substrate layer, a photo-thermal layer and a catalytic layer; the substrate layer is ITO, FTO transparent conductive glass or TiO2、Si/SiOx、Fe2O3An isophotonic anode, which needs to be pretreated before use; the photothermal layer is metal nanoparticles with a plasma resonance effect, such as Au or Au alloy, and nanostructure Ag or Ag alloy, and is prepared by a dropping coating method or an electrodeposition method, wherein the particle size of the particles is 50-400 nm; the catalyst layer is metal basic oxide, the metal is one or more of Fe, Co, Ni and Mn, and the catalyst layer is prepared by an electrodeposition method.
The substrate layer is preferably FTO conductive glass and n-type Si/SiOxA photo-anode; the thickness of the FTO conductive glass is 1-3 mm, and the resistance is 5-15 omega cm-2(ii) a n-type Si/SiOxThe photo-anode has a thickness of 300-500 μm and a resistivity of 1-10 Ω cm-2。
The photothermal layer is preferably Au nanoparticles, and the particle size of the Au nanoparticles is 50-400 nm, and more preferably 100-300 nm.
The catalytic layer is preferably basic nickel oxide NiOOH.
The preparation method of the photo-assisted thermoelectric coupling oxygen precipitation electrode comprises the following steps:
the method comprises the following steps: and (4) preprocessing a base layer.
FTO conductive glass: and ultrasonically cleaning the FTO conductive glass for 20 minutes by using acetone, ethanol and deionized water respectively to remove surface impurities, and placing the FTO conductive glass in the ethanol for later use.
n-type Si/SiOxPhoto-anode: (1) placing the cut n-type single polished silicon wafer in acetone, ethanol and deionized water in sequence for ultrasonic cleaning, taking out, washing with the deionized water, drying with high-purity nitrogen, and then soaking the silicon wafer in a concentrated sulfuric acid-hydrogen peroxide mixed solution for ultrasonic cleaning by adopting an RCA SC-1 cleaning mode to remove metal elements existing on the surface; (2) taking out the silicon wafer cleaned in the step (1), washing with deionized water, and then putting the silicon wafer into dilute hydrofluoric acid to dissolve a silicon oxide layer naturally formed on the surface; (3) taking out the silicon wafer in the step (2), soaking the silicon wafer into a mixed solution of water, concentrated hydrochloric acid and hydrogen peroxide in an RCA SC-2 cleaning mode, treating at 70-90 ℃, and generating a compact silicon oxide layer on the surface of the silicon wafer in situ; (4) and (4) taking out the silicon wafer in the step (3), washing with deionized water, drying with high-purity nitrogen, and placing in ethanol for later use.
Step two: and preparing the Au nanoparticle photothermal layer. Two methods are used for preparing the photothermal layer:
and (3) a dropping method: 50-200 mL of HAuCl4Boiling the solution, adding 0.5-5 mL of sodium citrate aqueous solution, and keeping for 5-20 min to obtain Au nano-particle suspension; naturally cooling, and pressing at 100-500 μ L cm-2The suspension liquid is coated on the substrate pretreated in the step one, the substrate is dried at the temperature of 60-80 ℃, heat treatment is carried out for 15-30 min at the temperature of 200-400 ℃, and the preparation of the Au nanoparticle photo-thermal layer is finished to obtain the electrode containing the photo-thermal layer;
an electrodeposition method: placing the substrate pretreated in the first step in HAuCl4And carrying out electrodeposition on the solution under the voltage of 0-1.0V vs. Ag/AgCl, wherein the amount of deposited electric charge is 5-20 mC, and obtaining the electrode containing the photo-thermal layer after the preparation of the Au nano-particle photo-thermal layer is finished.
Step three: with Ni (NO)3)2The concentration of the prepared metal ions is 0.05-0.25 mol L-1An aqueous solution of (a). And (4) placing the electrode containing the photo-thermal layer prepared in the step two in the metal ion solution, and performing electrodeposition under the voltage of-1.5 to-0.5V vs. Ag/AgCl, wherein the deposition charge quantity is 10-40 mC.And (5) completing the preparation of the NiOOH catalyst layer to obtain the light-assisted thermoelectric coupling oxygen precipitation electrode.
Preferably, in the dispensing method of step two, HAuCl4The mass fraction of the solution is 0.005-0.05 wt.%.
Preferably, in the dropping coating method of the second step, the mass fraction of the sodium citrate solution is 0.5-5 wt.%.
Preferably, in the electrodeposition process of the second step, HAuCl4The concentration of the solution is 0.001-0.01 mol L-1。
Preferably, in the electrodeposition process of the second step, HAuCl4The temperature of the solution is 20-50 ℃.
Preferably, the temperature of the metal ion solution for electrodeposition in the third step is 20-50 ℃.
The light-assisted thermoelectric coupling oxygen precipitation electrode is prepared from an alkaline electrolyte, the temperature of the electrolyte is 40-90 ℃, and the illumination intensity is 0-1000 mW cm-2. The novel light-assisted thermoelectric coupling oxygen precipitation electrode can be applied to reaction systems of water electrolysis, electrocatalysis carbon dioxide reduction and electrocatalysis nitrogen reduction.
The light-assisted thermoelectric coupling oxygen precipitation electrode has the advantages that the basic physical and chemical properties of materials selected by each part are key factors for determining the performance of the electrode.
The working mechanism of the photo-assisted thermoelectric coupling oxygen precipitation electrode is as follows: firstly, after the electrode is illuminated, light excites Au nano particles to generate a plasma resonance effect, so that the local temperature of the electrode is increased, a thermally-driven reaction (i) is carried out, the metal Ni of the catalytic electrode is reduced from III valence to II valence, and O is released2(ii) a In the second step, a lower positive voltage (voltage lower than the oxygen evolution voltage) drives the reaction (II) to occur, so that the catalytic electrode metal Ni is oxidized from II valence to III valence.
Ni(OH)2+OH-→NiOOH+H2O+e- (ii)
Compared with the prior art, the invention has the following advantages and beneficial effects: (1) the novel oxygen precipitation electrode designed by the invention complementarily uses electric energy, heat energy and light energy, provides an efficient utilization way for industrial waste heat and off-peak electricity, and couples the light energy, thereby realizing the cascade utilization of various energy sources. (2) The invention couples electrochemical reaction and thermochemical reaction, reduces the voltage required by oxygen precipitation reaction, and greatly reduces the electric energy consumption. (3) The novel photo-assisted thermoelectric coupling oxygen precipitation electrode designed by the invention has a simple preparation method, and the existing industrial equipment can meet the operation of all operation steps, so that the novel photo-assisted thermoelectric coupling oxygen precipitation electrode has a certain industrialization prospect.
Drawings
FIG. 1 shows that in example 1, voltages of 0V, 0.2V, 0.4V and 0.6V (respectively shown in FIG. 1a, FIG. 1b, FIG. 1c and FIG. 1d) are applied to the surface of an n-type silicon photoanode relative to an Ag/AgCl reference electrode, and Au nanoparticle-loaded SiO with a diameter of 50-300 nm is preparedx/Si electrode (Au/SiO)x/Si) SEM picture. The amount of deposited charge was 5 mC.
FIG. 2 is a Au/SiO solid phase shown in comparative example 1-1xThe oxygen precipitation activity test result chart of the/Si pole piece under different illumination conditions.
FIG. 3 is a NiOOH @ Au/SiO solid solution as described in comparative examples 1-2xthe/Si light-assisted thermoelectricity is coupled with an oxygen precipitation electrode, and an oxygen precipitation activity test result graph is obtained under different illumination conditions.
FIG. 4 is a Au/SiO solid phase diagram of comparative examples 1-3x/Si pole piece and NiOOH @ Au/SiOxa/Si light-assisted thermoelectric coupling oxygen evolution electrode catalytic activity test result graph.
FIG. 5 is an SEM image of the FTO conductive glass electrode (FIG. 5a, FTO), the photothermal layer-containing electrode (FIG. 5b, Au/FTO), the light-assisted thermoelectric coupling oxygen evolution electrode (FIG. 5c, NiOOH @ Au/FTO) corresponding to example 2 and the matte thermal layer-free electrode (FIG. 5d, NiOOH/FTO) corresponding to comparative example 2.
FIG. 6 is a graph showing the results of the oxygen evolution activity test of the photothermal layer-containing electrode (Au/FTO) of comparative example 2-1 at 20 ℃ under different illuminations.
FIG. 7 is a graph showing the results of the oxygen evolution activity test of the matte thermal layer electrode (NiOOH/FTO) of comparative example 2-2 at 20 ℃ under different illuminations.
FIG. 8 is a graph showing the results of the oxygen evolution activity test of the photo-assisted thermoelectric coupled oxygen evolution electrode (NiOOH @ Au/FTO) described in comparative examples 2-3, under different illuminations at 20 ℃.
FIG. 9 is a graph showing the results of the oxygen evolution activity test of the photothermal layer-containing electrode (Au/FTO) of comparative examples 2-4 at different electrolyte temperatures in the absence of light.
FIG. 10 is a graph of the results of testing the oxygen evolution activity of the matte thermal layer electrode (NiOOH/FTO) of comparative examples 2-5 at different electrolyte temperatures without illumination.
FIG. 11 is a graph showing the results of testing the oxygen evolution activity of the photo-assisted thermoelectric coupled oxygen evolution electrodes (NiOOH @ Au/FTO) described in comparative examples 2-6, in the absence of light, at different electrolyte temperatures.
FIG. 12 is a graph showing the results of testing the effect of light irradiation on the oxygen evolution activity of the electrode plate at 60 ℃ in the light-assisted thermoelectric coupling of the oxygen evolution electrodes (NiOOH @ Au/FTO) described in comparative examples 2-7.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention are described in further detail, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without inventive step, are within the scope of the present invention.
The oxygen evolution activity test conditions used in the present invention were: at 1.0mol L-1KOH is used as electrolyte for oxygen precipitation, a test is carried out by adopting a three-electrode system, a platinum sheet is used as a counter electrode, the purity is higher than 99.99 percent, saturated Ag/AgCl is used as a reference electrode, and a test instrument is a Shanghai Chenghua CHI 730e electrochemical workstation.
Example 1
(1) Cutting n-type single polished silicon wafer (1 × 1 cm)2) Sequentially placing the silicon wafer in acetone, ethanol and deionized water for ultrasonic cleaning for 10 minutes, taking out the silicon wafer, washing the silicon wafer with the deionized water, drying the silicon wafer with high-purity nitrogen, and then soaking the silicon wafer in concentrated sulfuric acid by adopting an RCA SC-1 cleaning mode: and (3) ultrasonically treating the mixed solution of hydrogen peroxide (the volume ratio is 3:1) for 15min to remove metal elements existing on the surface.
(2) And (2) taking out the silicon wafer cleaned in the step (1), washing with deionized water, and then putting into 10% hydrofluoric acid by volume ratio to dissolve the silicon oxide layer naturally formed on the surface.
(3) Taking out the silicon wafer in the step (2), and soaking the silicon wafer into water by adopting an RCA SC-2 cleaning mode: concentrated hydrochloric acid: treating the silicon wafer in a mixed solution of hydrogen peroxide (volume ratio 5:1:1) at 75 ℃ for 1h to generate a compact silicon oxide layer on the surface of the silicon wafer in situ to obtain a silicon photo-anode (SiO)x/Si)。
(4) The silicon photo-anode (SiO) in the step (3)xand/Si), washing with deionized water, drying with high-purity nitrogen, and placing in ethanol for later use.
(5) Before electrochemical deposition, a silicon photoanode (SiO) is requiredx/Si) for packaging. Indium particles are used as ohmic back contacts to be attached to the surface of the silicon wafer, copper wires are connected with the indium particles, and insulating silica gel is used for packaging the whole back and the side edges to prevent electrolyte from permeating.
(6) The gold nanoparticles are deposited on an electrochemical workstation in an electrochemical way, and the electroplating solution is 0.01mol L-1HAuCl4Solution (high purity nitrogen gas was bubbled before use to drain dissolved oxygen). In the electrochemical deposition process, 0V, 0.2V, 0.4V and 0.6V vs. Ag/AgCl potentials are selected respectively, and the deposition charge amount is 5 mC. SEM images of different potential deposition samples are shown in FIG. 1.
(7) Photothermal layer-containing electrode (Au/SiO) deposited with 0.4V in step (6)x/Si) is placed in 0.1mol L-1Ni (NO) of3)2In the solution, the voltage of-1.0V vs. Ag/AgCl is selected in the electrochemical deposition process, and the deposition charge amount is 40 mC. The preparation of the NiOOH catalyst layer is completed to obtain the light-assisted thermoelectric coupling oxygen precipitation electrode (NiOOH @ Au/SiO)x/Si)。
Comparative examples 1 to 1
The Au/SiO prepared by 0.4V electrodeposition in step (6) of example 1 was selectedxThe method comprises the steps of testing the oxygen precipitation activity of the pole piece under different illumination conditions, wherein the test result is shown in figure 2. The different lighting conditions were: matt (Dark), 600mW cm-2Light intensity of 1000mW cm-2The intensity of the light.
Comparative examples 1 to 2
NiOOH @ Au/SiO prepared in step (7) of example 1 was takenxthe/Si light-assisted thermoelectric coupling oxygen precipitation electrode is used for testing the oxygen precipitation activity of the electrode under different illumination conditions, and the test result is shown in figure 3. The different lighting conditions were: matt (Dark), 600mW cm-2Light intensity of 1000mW cm-2The intensity of the light.
Comparative examples 1 to 3
At 600mW cm-2Comparison of Au/SiO in light intensityx/Si pole piece and NiOOH @ Au/SiOxThe catalytic activity of the/Si light-assisted thermoelectric coupling oxygen evolution electrode and the test results are shown in FIG. 4.
Example 2
(1) And ultrasonically cleaning the FTO conductive glass for 20min by using acetone, ethanol and deionized water in sequence to remove surface impurities, and placing the FTO conductive glass in the ethanol for later use. An SEM image of the treated FTO transparent conductive glass is shown in fig. 5.
(2) And (2) drying the FTO conductive glass in the step (1) by using high-purity nitrogen, boiling 100mL of chloroauric acid solution, adding 2mL of 1.0 wt.% sodium citrate aqueous solution, and keeping for 10min to obtain Au nano-particle suspension. After natural cooling, pressing the mixture according to 300 mu L cm-2The suspension was applied to the FTO substrate in 50. mu.L drops for a total of six drops. And then drying the substrate in an electrothermal blowing drying oven at 80 ℃, and continuously carrying out heat treatment at 350 ℃ for 30min to obtain the Au nanoparticle photo-thermal layer. An SEM image of an electrode containing a photothermal layer (Au/FTO) is shown in FIG. 5.
(3) Placing the electrode containing the photothermal layer prepared in the step (2) in 0.1mol L-1Ni (NO) of3)2In the solution, the voltage of-1.0V vs. Ag/AgCl is selected in the electrochemical deposition process, and the deposition charge quantity is 30 mC. And (3) completing preparation of the NiOOH catalyst layer to obtain a light-assisted thermoelectric coupling oxygen precipitation electrode (NiOOH @ Au/FTO). The SEM image of this electrode is shown in fig. 5.
Comparative example 2-1
The photothermal layer-containing electrode (Au/FTO) prepared in step (2) of example 2 was used to test the oxygen evolution activity under different light irradiation at 20 ℃, and the test results are shown in fig. 6. The different lighting conditions were: matt (Dark), 600mW cm-2Light intensity of 1000mW cm-2The intensity of the light.
Comparative examples 2 to 2
The FTO treated in the step (1) of example 2 was taken and charged in an amount of 0.1mol L-1Ni (NO) of3)2In the solution, the voltage of-1.0V vs. Ag/AgCl is selected in the electrochemical deposition process, and the deposition amount is 30 mC. The NiOOH catalytic layer was completed and a matte thermal layer electrode (NiOOH/FTO) was obtained, the SEM image of which is shown in fig. 5. The oxygen evolution activity of the electrodes under different illumination conditions at 20 ℃ was tested, and the test results are shown in FIG. 7. The different lighting conditions were: matt (Dark), 600mW cm-2Light intensity of 1000mW cm-2The intensity of the light.
Comparative examples 2 to 3
The light-assisted thermoelectric coupling oxygen evolution electrode (NiOOH @ Au/FTO) prepared in the step (3) of example 2 was used to test the oxygen evolution activity under different illumination conditions at 20 ℃, and the test results are shown in FIG. 8. The different lighting conditions were: matt (Dark), 600mW cm-2Light intensity of 1000mW cm-2The intensity of the light.
Comparative examples 2 to 4
The photothermal layer-containing electrode (Au/FTO) prepared in step (2) of example 2 was used to test the oxygen evolution activity at different electrolyte temperatures in the absence of light, and the test results are shown in fig. 9.
Comparative examples 2 to 5
The matte thermal layer electrode (NiOOH/FTO) prepared in comparative example 2-2 was taken and tested for oxygen evolution activity at different electrolyte temperatures in the absence of light, and the test results are shown in fig. 10.
Comparative examples 2 to 6
The light-assisted thermoelectric coupling oxygen evolution electrode (NiOOH @ Au/FTO) prepared in the step (3) of example 2 was used to test the oxygen evolution activity at different electrolyte temperatures in the absence of light, and the test results are shown in FIG. 11.
Comparative examples 2 to 7
The light-assisted thermoelectric coupling oxygen evolution electrode (NiOOH @ Au/FTO) prepared in the step (3) of the example 2 is taken, the influence of illumination on the oxygen evolution activity of the pole piece is tested at 60 ℃, and the test result is shown in FIG. 12.
With reference to fig. 1-12, the following conclusions can be drawn: the gold nanoparticles electrodeposited on the surface of the n-type silicon photo-anode are distributed in an island shape, and the coverage of the silicon photo-anode by the gold nanoparticles is increased along with the increase of the applied potential relative to the Ag/AgCl reference electrode. For the FTO electrode, gold particles prepared by a dripping method are used as a photothermal layer, and a NiOOH water oxidation catalyst layer is further electrodeposited on the base of the photothermal layer, so that the oxygen precipitation activity can be obviously improved. As shown in fig. 9 to 12, the light-assisted thermoelectric coupling oxygen evolution electrode can obtain higher oxygen evolution activity than the applied temperature by utilizing the coupling action between the heat generated by the plasmon resonance effect of Au and the NiOOH water oxidation layer.
The oxygen precipitation electrode prepared in the embodiment can be used as a proton donor to be applied to reaction systems of water electrolysis, electrocatalysis carbon dioxide reduction and electrocatalysis nitrogen reduction.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (4)
1. The preparation method of the light-assisted thermoelectric coupling oxygen evolution electrode is characterized by comprising the following steps: the oxygen precipitation electrode consists of a substrate layer, a photothermal layer and a catalytic layer; the substrate layer is made of FTO conductive glass and n-type Si/SiO x A photo-anode; the thickness of the FTO conductive glass is 1-3 mm, and the resistance is 5-15 omega cm−2(ii) a n-type Si/SiO x The photo-anode has a thickness of 300-500 μm and a resistivity of 1-10 Ω cm−2；
The photothermal layer is Au nanoparticles, and the particle size of the nanoparticles is 100-300 nm;
the catalyst layer is basic nickel oxide NiOOH;
the preparation method comprises the following steps:
the method comprises the following steps: pre-treating a substrate layer;
FTO conductive glass: ultrasonically and sequentially cleaning the FTO conductive glass for 20 minutes by using an acetone or ethanol solvent and deionized water respectively to remove surface impurities, and placing the FTO conductive glass in ethanol for later use;
n-type Si/SiO x Photo-anode: (1) placing the cut n-type single polished silicon wafer in an acetone or ethanol solvent and deionized water in sequence for ultrasonic cleaning, taking out the silicon wafer, washing the silicon wafer with the deionized water, drying the silicon wafer with high-purity nitrogen, and then immersing the silicon wafer in a concentrated sulfuric acid-hydrogen peroxide mixed solution for ultrasonic cleaning to remove metal elements existing on the surface by adopting an RCA SC-1 or SC-1 cleaning mode; (2) taking out the silicon wafer cleaned in the step (1), washing with deionized water, and then putting the silicon wafer into dilute hydrofluoric acid to dissolve a silicon oxide layer naturally formed on the surface; (3) taking out the silicon wafer in the step (2), and soaking the silicon wafer into a mixed solution of water, concentrated hydrochloric acid and hydrogen peroxide in a 70-90% manner by adopting an RCA SC-2 cleaning modeoC, processing, namely generating a compact silicon oxide layer on the surface of the silicon wafer in situ; (4) taking out the silicon wafer in the step (3), washing with deionized water, drying with high-purity nitrogen, and placing in ethanol for later use;
step two: the substance with the surface plasma resonance effect is prepared by adopting a dripping coating method or an electrodeposition method;
step three: the metal basic oxide is prepared by an electrodeposition method; i.e. preparation of NiOOH catalyst layer with Ni (NO)3)2The concentration of the prepared metal ions is 0.05-0.25 mol L−1An aqueous solution of (a); placing an electrode containing the photo-thermal layer in the metal ion solution, and performing electrodeposition under the voltage of-1.5 to-0.5V vs. Ag/AgCl, wherein the deposition charge quantity is 10 to 40 mC; and (5) completing the preparation of the NiOOH catalyst layer to obtain the light-assisted thermoelectric coupling oxygen precipitation electrode.
2. The method for producing an oxygen evolving electrode according to claim 1, wherein:
step two: preparing an Au nanoparticle photothermal layer;
the preparation of the smooth thermal layer is carried out by adopting one of two methods:
and (3) a dropping method: 50-200 mL of HAuCl4Boiling the solution, adding 0.5-5 mL of sodium citrate aqueous solution, and keeping for 5-20 min to obtain Au nano-particle suspension; naturally cooling, and pressing at 100-500 μ L cm−2The suspended liquid is coated on the FTO substrate pretreated in the step one by the density of 60-80%oC, drying at 200-400 DEGoUnder the condition C, carrying out heat treatment for 15-30 min, and finishing the preparation of the Au nanoparticle photo-thermal layer to obtain a photo-thermal layer-containing electrode; in the dispensing method, HAuCl4The mass fraction of the solution is 0.005-0.05 wt%; the mass fraction of the sodium citrate solution is 0.5-5 wt%;
an electrodeposition method: placing the FTO substrate pretreated in the step one in HAuCl4Performing electrodeposition with a solution at a voltage of 0-1.0V/s and Ag/AgCl, wherein the amount of deposited electric charge is 5-20 mC, and the preparation of the Au nanoparticle photo-thermal layer is finished4The concentration of the solution is 0.001-0.01 mol L−1，HAuCl4The temperature of the solution is 20-50 DEG CoC; and obtaining the electrode containing the photo-thermal layer.
3. Use of an oxygen evolving electrode according to any of claims 1-2, wherein: the light-assisted thermoelectric coupling oxygen precipitation electrode can be used as a proton generation electrode and applied to a reaction system which needs to consume protons for water electrolysis, electrocatalytic carbon dioxide reduction and electrocatalytic nitrogen reduction; comprises using alkaline electrolyte with a temperature of 40-90 deg.CoC, the illumination intensity is 0-1000 mW cm−2。
4. Use of an oxygen evolving electrode according to any of claims 1-2, wherein: the oxygen evolution activity test conditions used were: at 1.0mol L−1KOH is used as electrolyte for oxygen precipitation, a three-electrode system is tested, a platinum sheet is used as a counter electrode, the purity is higher than 99.99 percent, and saturated Ag/AgCl is used as a reference electrode.
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