CN117144403A - Preparation method of photosynthetically resistant cuprous oxide-based composite photoelectrode - Google Patents
Preparation method of photosynthetically resistant cuprous oxide-based composite photoelectrode Download PDFInfo
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- CN117144403A CN117144403A CN202310806236.3A CN202310806236A CN117144403A CN 117144403 A CN117144403 A CN 117144403A CN 202310806236 A CN202310806236 A CN 202310806236A CN 117144403 A CN117144403 A CN 117144403A
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- cuprous oxide
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- 239000002131 composite material Substances 0.000 title claims abstract description 29
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 26
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005260 corrosion Methods 0.000 claims abstract description 14
- 230000008021 deposition Effects 0.000 claims abstract description 8
- 230000005684 electric field Effects 0.000 claims abstract description 3
- 239000002086 nanomaterial Substances 0.000 claims abstract description 3
- 239000010949 copper Substances 0.000 claims description 37
- 239000003792 electrolyte Substances 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000011521 glass Substances 0.000 claims description 15
- 238000000151 deposition Methods 0.000 claims description 12
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000011065 in-situ storage Methods 0.000 claims description 5
- 239000004310 lactic acid Substances 0.000 claims description 5
- 235000014655 lactic acid Nutrition 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 238000000486 photoelectrochemical deposition Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 238000004070 electrodeposition Methods 0.000 claims description 2
- 238000009832 plasma treatment Methods 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000008351 acetate buffer Substances 0.000 claims 3
- 230000007797 corrosion Effects 0.000 claims 2
- 239000000126 substance Substances 0.000 claims 1
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 230000006872 improvement Effects 0.000 abstract description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- 229910052697 platinum Inorganic materials 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000001569 carbon dioxide Substances 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229940075397 calomel Drugs 0.000 description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 238000001259 photo etching Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000006701 autoxidation reaction Methods 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- DCRNVZUOGPNBNM-UHFFFAOYSA-K [Au+3].[O-][Cl](=O)=O.[O-][Cl](=O)=O.[O-][Cl](=O)=O Chemical compound [Au+3].[O-][Cl](=O)=O.[O-][Cl](=O)=O.[O-][Cl](=O)=O DCRNVZUOGPNBNM-UHFFFAOYSA-K 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- 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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Abstract
The invention discloses a preparation method of a photosynthetically resistant cuprous oxide-based composite photoelectrode, which comprises a cuprous oxide-based composite photoelectrode, wherein the general formula of the cuprous oxide-based composite photoelectrode is as follows: A/Cu 2 O@B A is an interfacial charge transport carrierB is a bulk charge transport carrier; a is attached to Cu 2 O@B, B is a nanomaterial with excellent charge transport properties, and B can be embedded into Cu by a deposition electric field 2 In the O-phase, the invention provides the cuprous oxide-based composite photoelectrode which is used for photoelectrocatalysis and is resistant to photo-corrosion by double improvement of charge transmission of the phase and the interface.
Description
Technical Field
The invention relates to the technical field of semiconductor photoelectricity, in particular to a preparation method of a photo-corrosion-resistant cuprous oxide-based composite photoelectrode.
Background
Fossil fuels play an important role in the development of modern society. However, the large consumption of coal, oil and gas causes serious climate and environmental problems, including global warming and atmospheric pollution. Solar energy is a clean energy source rich in resources, and can be obtained through water (H 2 O) decomposition and carbon dioxide (CO) 2 ) Reduction to form a catalyst comprising hydrogen (H) 2 ) And carbon-based fuels, can alleviate climate and environmental crisis to some extent. Thus, the production and utilization of solar fuel has received extensive attention and continued research by global students.
Photoelectrocatalysis (PEC) can be effectively used for H 2 O decomposition and CO 2 The reduction has wide development prospect. Many studies have focused on the preparation of highly efficient and stable photocathodes for promoting Hydrogen Evolution Reactions (HERs) and CO 2 Reduction Reaction (CRR). Cuprous oxide (Cu) 2 O) is a photocathode material with development potential, but the autoxidation and the autoreduction of cuprous oxide cause serious photo-corrosion, which prevents the continuous and stable progress of the photocatalysis. Taking HER as an example, the main reactions on the photoelectrocatalytic electrode are as follows:
Cu 2 O + 2H + + 2e - → 2Cu + H 2 o (self-reduction) (1)
Cu 2 O + 2OH - + 2h + → 2CuO + H 2 O (autoxidation) (2)
2H + + 2e - → H 2 (normal photocathode reaction) (3)
4OH - + 4h + → O 2 + 2H 2 O (Normal photo anode reaction) (4)
Wherein, the reaction (1) and the reaction (2) are respectively self-reduction photo-corrosion and self-oxidation photo-corrosion of cuprous oxide, and the reaction (3) and the reaction (4) are normal photo-cathode reaction and photo-anode reaction.
It is known that the above reaction and the photo-etching mechanism are combined, and the accumulation of electrons and holes is a main cause of the photo-etching of the electrode in the photoelectrocatalysis system, so that the improvement of the charge transport on the electrode is an effective strategy for avoiding or slowing down the photo-etching in future research. How to design a stable and efficient composite photoelectrode to effectively improve charge transmission is an important point and difficulty in photoelectrocatalysis research. In view of the above problems, a solution is proposed below.
Disclosure of Invention
The invention aims to provide a preparation method of a photo-corrosion-resistant cuprous oxide-based composite photoelectrode, which has the advantage of providing a photo-corrosion-resistant cuprous oxide-based composite photoelectrode for photoelectrocatalysis.
The technical aim of the invention is realized by the following technical scheme:
by double improvement of charge transmission of bulk phase and interface, the cuprous oxide-based composite photoelectrode with photo-corrosion resistance for photoelectrocatalysis is provided, and the general formula of the cuprous oxide-based composite photoelectrode is as follows: A/Cu 2 O@B wherein a is an interfacial charge transport carrier; b is a bulk charge transport carrier. Characterized in that A is attached to Cu 2 The noble metals on the surface of O@B comprise gold, silver, platinum and the like; b is a nanomaterial with excellent charge transport property, including reduced graphene oxide, carbon nanotube, carbon quantum dot, etc., and can be embedded into Cu by a deposition electric field 2 And O phase.
The method for preparing the photoelectrocatalysis light-corrosion-resistant cuprous oxide-based composite photoelectrode comprises the following steps:
s1: under ultrasonic treatment, cleaning conductive glass with multiple solvents for more than 10 minutes respectively, and after the conductive glass is completely dried, performing oxygen plasma treatment for more than 5 minutes;
s2: preparing a buffer copper acetate solution as an electrolyte one containing Cu 2 (CH 3 COO) 4 、NaH 2 PO 4 And lactic acid;
s3: stirring the first electrolyte, dropwise adding a NaOH solution, and regulating the pH to 10-12;
s4: dispersing the powder B in deionized water, and adding the powder B into the electrolyte I to reach the concentration of 0.05-0.50 mg/ml;
s5: deposition of Cu on conductive glass by electrochemical deposition 2 O@B layers;
s6: the obtained Cu 2 Placing a O@B sample in an oven for drying for more than 2 hours;
s7: preparing 0.01-0.10M of A salt solution as electrolyte II;
s8: photoelectrochemical deposition of Cu 2 Depositing an A layer on the O@B sample in situ to obtain A/Cu 2 O@B photoelectrodes.
The beneficial effects of the invention are as follows:
1. the cuprous oxide-based composite photoelectrode has good charge transmission property, can greatly avoid and relieve photo-corrosion, and has good working stability;
2. the preparation method is simple and easy to operate, the types of preparation raw materials are few, the required equipment cost is low, and the cuprous oxide-based composite photoelectrode prepared by the method has higher photoreaction activity than a single cuprous oxide-based photoelectrode.
Detailed Description
The following description is only of the preferred embodiments of the present invention, and the scope of the present invention should not be limited to the examples, but should be construed as falling within the scope of the present invention.
Example 1
S1: under ultrasonic treatment, cleaning FTO glass for 15 minutes by using hydrogen peroxide solution, acetone, ethanol and deionized water respectively, and treating for 5 minutes by oxygen plasma after the FTO glass is completely dried;
s2: preparation of buffered copper acetate solution containing 0.1M Cu as electrolyte I 2 (CH 3 COO) 4 、0.2M NaH 2 PO 4 And 1.0M lactic acid;
s3: stirring the electrolyte, dropwise adding a 1.0M NaOH solution, and adjusting the pH to 10;
(4) Dispersing Carbon Nanotubes (CNTs) in deionized water and adding the dispersion to the electrolyte I to reach the concentration of 0.50mg/ml;
(5) A two electrode system was used with a platinum sheet as the counter electrode. At a constant current density of-0.1 mA/cm 2 Is operated in constant current mode to deposit Cu on FTO glass 2 An O@CNT layer;
(6) The obtained Cu 2 Placing the O@CNT sample in an oven for drying for 3 hours;
(7) Preparing a 0.01M gold chlorate solution as electrolyte II;
(8) Under a three-electrode system, a platinum electrode is used as a counter electrode, a calomel electrode is used as a reference electrode, a deposition potential of 0V vs. RHE is set, and a mercury lamp light source is turned on to irradiate Cu 2 O@CNT sample prepared by photoelectrochemical deposition method on Cu 2 In-situ depositing an Au layer for 1 hour on the O@CNT sample to obtain Au/Cu 2 O@CNT composite photoelectrode.
Example 2
S1: under ultrasonic treatment, cleaning FTO glass for 15 minutes by using hydrogen peroxide solution, acetone, ethanol and deionized water respectively, and treating for 5 minutes by oxygen plasma after the FTO glass is completely dried;
s2: preparation of buffered copper acetate solution containing 0.1M Cu as electrolyte I 2 (CH 3 COO) 4 、0.2M NaH 2 PO 4 And 1.0M lactic acid;
s3: stirring the first electrolyte, dropwise adding a 1.0M NaOH solution, and adjusting the pH to 11;
s4: adding graphene oxide powder (GO) into deionized water for dispersion, and adding into the electrolyte I to reach the concentration of 0.10mg/ml;
s5: a two electrode system was used with a platinum sheet as the counter electrode. At a constant current density of-0.5 mA/cm 2 Is operated in constant current mode, GO is reduced to reduced graphene oxide (rGO) and deposited on FTO glass to obtain Cu 2 An O@rGO layer;
s6: the obtained Cu 2 Placing the O@rGO sample in an oven for drying for 3 hours;
s7: preparing a 0.05M chloroplatinic acid solution as electrolyte II;
s8: in the case of a three-electrode system,the platinum electrode is used as a counter electrode, the calomel electrode is used as a reference electrode, the deposition potential is set to be 0V vs. RHE, and a mercury lamp light source is turned on to irradiate Cu 2 O@rGO sample prepared by photoelectrochemical deposition method on Cu 2 In-situ depositing a Pt layer for 1 hour on the O@rGO sample to obtain Pt/Cu 2 O@rGO composite photoelectrode.
Example 3
S1: under ultrasonic treatment, cleaning FTO glass for 15 minutes by using hydrogen peroxide solution, acetone, ethanol and deionized water respectively, and treating for 5 minutes by oxygen plasma after the FTO glass is completely dried;
s2: preparation of buffered copper acetate solution containing 0.1M Cu as electrolyte I 2 (CH 3 COO) 4 、0.2M NaH 2 PO 4 And 1.0M lactic acid;
s3: stirring the first electrolyte, dropwise adding a 1.0M NaOH solution, and regulating the pH to 12;
s4: adding carbon quantum dots (CQP) into deionized water for dispersion, and adding into the electrolyte I to reach the concentration of 0.05mg/ml;
s5: a two electrode system was used with a platinum sheet as the counter electrode. At a constant current density of-1.0 mA/cm 2 Is deposited on FTO glass to obtain Cu 2 An O@CQP layer;
s6: the obtained Cu 2 Placing the O@CQP sample in an oven for drying for 3 hours;
s7: preparing 0.10M silver nitrate solution as electrolyte II;
s8: under a three-electrode system, a platinum electrode is used as a counter electrode, a calomel electrode is used as a reference electrode, a deposition potential of 0V vs. RHE is set, and a mercury lamp light source is turned on to irradiate Cu 2 O@CQP sample prepared by photoelectrochemical deposition method on Cu 2 Depositing an Ag layer on the O@CQP sample in situ for 1 hour to obtain Ag/Cu 2 O@CQP composite photoelectrode.
The invention is used for photoelectric catalytic reduction H which is designed by oneself 2 O and CO 2 The composite photoelectrode prepared by the example is tested on a platform. Under a three-electrode system, a platinum electrode is used as a counter electrode, a calomel electrode is used as a reference electrode, and the composite photoelectrode is placed in 0.1M KHCO 3 Setting the deposition potential at 0V vs. RHE in the electrolyte, and using the power of 100mW/cm 2 The xenon lamp light source of the above example was irradiated for 24 hours, and the photocurrent was recorded with an electrochemical workstation, and the composite photoelectrodes prepared in the above example all had a 24 hour photocurrent decay of less than 20%.
The technical problems, technical solutions and advantageous effects solved by the present invention have been further described in detail in the above-described embodiments, and it should be understood that the above-described embodiments are only illustrative of the present invention and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the scope of protection of the present invention.
Claims (5)
1. The preparation method of the cuprous oxide-based composite photoelectrode resistant to photo-corrosion comprises a cuprous oxide-based composite photoelectrode, and is characterized in that the cuprous oxide-based composite photoelectrode has the following general formula: A/Cu 2 O@B wherein A is an interfacial charge transport carrier and B is a bulk charge transport carrier; the A is attached to Cu 2 O@B, B is a nanomaterial with excellent charge transport properties and is capable of being embedded into Cu by a deposited electric field 2 And O phase.
2. The method for preparing the cuprous oxide-based composite photoelectrode with light resistance according to claim 1, wherein the method for preparing the cuprous oxide-based composite photoelectrode comprises the following steps,
s1: under ultrasonic treatment, cleaning conductive glass with multiple solvents for more than 10 minutes respectively, and after the conductive glass is completely dried, performing oxygen plasma treatment for more than 5 minutes;
s2: preparing a copper acetate buffer solution as an electrolyte;
s3: stirring the first electrolyte, dropwise adding a NaOH solution into the first electrolyte, and adjusting the pH value of the first electrolyte;
s4: dispersing the B powder in deionized water, and adding the B powder into the electrolyte I until the concentration of the B substance in the electrolyte I is 0.05-0.50 mg/ml;
s5: deposition of Cu on conductive glass by electrochemical deposition 2 O@B layers;
s6: the obtained Cu 2 Placing a O@B sample in an oven for drying for more than 2 hours;
s7: preparing 0.01-0.10M of A salt solution as electrolyte II;
s8: photoelectrochemical deposition of Cu 2 Depositing an A layer on the O@B sample in situ to obtain A/Cu 2 O@B photoelectrodes.
3. The method for preparing a photosynthetically active corrosion-resistant cuprous oxide-based composite photoelectrode according to claim 2, wherein in step S2, the prepared copper acetate buffer solution contains Cu 2 (CH 3 COO) 4 、NaH 2 PO 4 And lactic acid.
4. The method for preparing a photosynthetically active corrosion-resistant cuprous oxide-based composite photoelectrode according to claim 2, wherein in step S3, the pH of the copper acetate buffer solution is adjusted to 10 to 12.
5. The method for preparing a photo-corrosion resistant cuprous oxide-based composite photoelectrode according to claim 2, wherein in step S4, the concentration of B in the electrolyte is 0.05-0.50 mg/ml.
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