CN117144403A - Preparation method of photosynthetically resistant cuprous oxide-based composite photoelectrode - Google Patents

Preparation method of photosynthetically resistant cuprous oxide-based composite photoelectrode Download PDF

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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
based composite
electrolyte
composite photoelectrode
preparing
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李铮
许辰宇
高超
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Shaoxing Research Institute Of Zhejiang University
Zhejiang University ZJU
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Shaoxing Research Institute Of Zhejiang University
Zhejiang University ZJU
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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

Preparation method of photosynthetically resistant cuprous oxide-based composite photoelectrode
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.
CN202310806236.3A 2023-07-04 2023-07-04 Preparation method of photosynthetically resistant cuprous oxide-based composite photoelectrode Pending CN117144403A (en)

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