CN113308711B - Preparation method and application of F-doped CBO nanorod array photocathode material - Google Patents

Preparation method and application of F-doped CBO nanorod array photocathode material Download PDF

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CN113308711B
CN113308711B CN202110579182.2A CN202110579182A CN113308711B CN 113308711 B CN113308711 B CN 113308711B CN 202110579182 A CN202110579182 A CN 202110579182A CN 113308711 B CN113308711 B CN 113308711B
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cbo
nanorod array
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array photocathode
photocathode
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CN113308711A (en
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马德琨
李自新
武翔
郭长莲
徐全龙
齐陈泽
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University of Shaoxing
Wenzhou University
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • 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
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    • C25B1/28—Per-compounds
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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
    • C25B1/50—Processes
    • C25B1/55—Photoelectrolysis
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
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    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/133—Renewable energy sources, e.g. sunlight

Abstract

The invention discloses a preparation method of an F-doped CBO nanorod array photocathode material, which comprises the steps of synthesizing a CBO seed layer; synthesizing a CBO nanorod array photocathode by using the CBO seed layer; and (4) synthesizing an F-doped CBO nanorod array photocathode, soaking the CBO nanorod array photocathode obtained in the step S2 in NaF solution for 2h, taking out and drying, and annealing at 300 ℃ for 1h to obtain the F-doped CBO nanorod array photocathode material. The invention has the beneficial effects that: the required raw materials are green and nontoxic, have rich sources, and the preparation method has good repeatability and can be synthesized on a large scale; the material prepared by the invention can be used for photoelectrocatalysis reduction of O 2 Production of H 2 O 2 The method has the advantages of high reaction efficiency, simple operation, good stability of the prepared material, and good practical value and application prospect.

Description

Preparation method and application of F-doped CBO nanorod array photocathode material
Technical Field
The invention belongs to the field of inorganic nano materials, and particularly relates to a preparation method of an F-doped CBO nanorod array photocathode material.
Background
Energy is a driving force for serving and providing modern human society, and with the intensive consumption of fossil fuels and the increasing deterioration of environmental destruction, people have an increasing demand for alternative clean energy. Solar energy is considered a clean, economical, renewable natural resource. PEC systems, which can address the needs of future human life by using semiconductor photoelectrodes to absorb solar energy and perform chemical reactions by which chemical fuels are produced, are one of the most attractive strategies.
Currently, a great deal of effort is focused on producing hydrogen (from water split) and carbonaceous fuels, such as methanol (from carbon dioxide reduction) by converting solar energy. In addition, H2O 2 production by PEC systems is also being increasingly scheduled. H2O 2 is not only a promising clean fuel, but also a value-added chemical, widely used in organic synthesis, pulp bleaching, wastewater treatment and medical disinfection. The importance of H2O 2 is reflected in a yield approaching 600 million tons in 2016. However, the green chemicals with wide application are mainly produced by the anthraquinone process with high energy consumption at present, and the production process is complex. The production of H2O 2 using solar energy is an ideal green sustainable technology where only water, oxygen and sunlight are necessary. Therefore, the conversion of solar energy into sustainable resources using PEC ORR technology is of great importance. Currently, due to the lack of suitable photocathodes, particularly inorganic semiconductor photocathodes, the related research is still in the beginning.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a F-doped CBO nanorod array photocathode material, which can be used for PEC ORR to reduce oxygen to produce H2O 2 due to a series of advantages of low price, low toxicity, proper band gap (1.5-1.8eV), higher theoretical current density (19.7-29.0mA/cm < 2 >) and positive initial potential of the CBO photocathode. However, to date, few semiconductor materials have been reported for the photoelectrocatalytic synthesis of H2O 2 by PEC ORR.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an F-doped CBO nanorod array photocathode material comprises the following steps:
s1 synthesizing a CBO seed layer;
s2, synthesizing the CBO nanorod array photocathode by using the CBO seed layer;
s3, synthesizing an F-doped CBO nanorod array photocathode, soaking the CBO nanorod array photocathode obtained in the step S2 in NaF solution for 2 hours, taking out and drying the obtained product, and annealing the obtained product at 300 ℃ for 1 hour to obtain the F-doped CBO nanorod array photocathode material.
It should be noted that the synthesized CBO seed layer in step S1 includes:
s1.1, dissolving CuSO 4-5H 2O in deionized water, and stirring to completely dissolve the CuSO 4-5H 2O;
s1.2, adding sodium bismuth ethylene diamine tetraacetate (C10H 12 BiN 2 NaO 8) into the mixed solution finally obtained in the step S1.1, and continuously stirring to completely dissolve the sodium bismuth ethylenediamine tetraacetate;
s1.3, dripping the solution obtained in the step S1.2 on FTO glass, putting the sample into an oven at 80 ℃ for drying for 1h, and then annealing in a tube furnace at 550 ℃ for 2h to obtain the FTO containing the CBO seed layer.
It should be noted that the synthesized CBO nanorod array photocathode of step S2 includes:
s2.1, adding Bi (NO 3) 3-5H 2O into deionized water, and stirring to dissolve;
s2.2, adding Cu (NO) 3-3H 2O into the mixed solution finally obtained in the step S2.1, and continuously stirring to completely dissolve the Cu (NO) 3-3H 2O;
s2.3, adding a NaOH solution into the mixed solution finally obtained in the step S2.2, and continuously stirring for 2 hours;
s2.4, adding sodium dodecyl benzene sulfonate into the solution obtained in the step S2.3, and stirring for 2 hours;
s2.5, placing FTO containing a CBO seed layer into a high-pressure reaction kettle, pouring the FTO into the mixed solution finally obtained in the step S2.4, sealing the high-pressure reaction kettle, placing the sealed high-pressure reaction kettle into a drying box, reacting at a constant temperature of 180 ℃ for 24 hours, naturally cooling to room temperature after the reaction is finished, washing the obtained product with deionized water and ethanol for 3 times respectively, drying the product in a vacuum drying box at 60 ℃, and finally annealing at 550 ℃ for 1 hour to obtain the CBO nanorod array photocathode.
Preferably, in step S1.1 of the present invention, 0.05mmol of CuSO 4-5H 2O is dissolved in 10mL of deionized water; in step S1.2, 0.1mmol of sodium bismuth ethylenediaminetetraacetate is dissolved in the solution finally obtained in step S1.1.
Preferably, in step S2.1 of the present invention, 0.605g of Bi (NO 3) 3-5H 2O is dissolved in 20mL of deionized water; in step S2.2, adding 0.45g of Cu (NO) 3-3H 2O into the mixed solution finally obtained in step S2.1, and stirring for dissolving; in step S2.3, 1mL of a solution containing 0.34g of NaOH is added dropwise to the mixed solution finally obtained in step S2.2; in step S2.4, 1g of sodium dodecylbenzenesulfonate is added to the mixed solution finally obtained in step S2.3 and stirred for 2 hours.
Preferably, the NaF solution described in step S3 of the present invention is prepared by dissolving 10mg NaF in 10mL of deionized water.
The invention also provides application of the prepared F-CBO nanorod array photocathode material in a photoelectric catalyst.
The invention has the beneficial effects that:
1. the method has the advantages of rich sources of required raw materials, green route, good method repeatability and large-scale synthesis;
2. the material prepared by the invention can be used for producing H2O 2 by photoelectrocatalysis reduction of O2. The reaction is efficient, the operation is simple, and the prepared material has good stability, high selectivity and good practical value and application prospect.
Drawings
FIG. 1 is a scanning electron microscope image of a CBO nanorod array;
FIG. 2 is a scanning electron microscope image of the F-CBO nanorod array;
FIG. 3 is a high resolution transmission electron microscope image of the F-CBO nanorod prepared in the present invention;
FIG. 4 is a schematic diagram of the powder X-ray diffraction patterns of the CBO and F-CBO nanorod array materials prepared by the method;
FIG. 5 is a Raman spectrum of the CBO and F-CBO nanorod array material prepared according to the present invention;
FIG. 6 is a solid diffuse reflectance spectrum of the CBO and F-CBO nanorod array material prepared according to the present invention;
FIG. 7 is a band gap diagram of the CBO and F-CBO nanorod array material prepared according to the present invention;
FIG. 8 is an impedance spectrum of the CBO and F-CBO nanorod array material prepared according to the present invention;
FIG. 9 shows the difference in charge current density between the CBO and F-CBO nanorod array materials prepared according to the present invention at different scanning rates;
FIG. 10 is a current density-potential diagram of a nano-rod array photoelectrode of CBO and F-CBO under the condition that O2 is introduced and O2 is not introduced into a 0.1M KOH solution;
FIG. 11 is a current density-time diagram of a photoelectrode of a CBO and F-CBO nanorod array under the conditions of O2 introduction and O2 non-introduction in a 0.1M KOH solution;
FIG. 12 is a graph of the change of the concentration of H2O 2 produced by photoelectrode of CBO and F-CBO nanorod arrays with time;
FIG. 13 is a graph of electron transfer number n of photoelectrode of CBO and F-CBO nanorod arrays as a function of potential;
FIG. 14 is a graph of the change of photoelectrode HO 2-% of CBO and F-CBO nanorod arrays as a function of potential.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, and it should be noted that the following examples are provided to illustrate the detailed embodiments and specific operations based on the technical solutions of the present invention, but the scope of the present invention is not limited to the examples.
Example 1
A preparation method of an F-doped CBO nanorod array photocathode material is characterized by comprising the following steps:
s1 synthesizing a CBO seed layer:
s1.1, firstly, dissolving 0.05mmol of CuSO 4-5H 2O in 10mL of deionized water, and stirring to completely dissolve the solution;
s1.2, adding 0.1mmol of sodium bismuth ethylene diamine tetraacetate into the mixed solution finally obtained in the step S1.1, and continuously stirring to completely dissolve the sodium bismuth ethylene diamine tetraacetate;
s1.3, dropwise coating the solution obtained in the S1.2 on FTO glass, drying the sample in an oven at 80 ℃ for 1h, and then annealing in a tube furnace at 550 ℃ for 2 h;
s2 synthesis of the CBO nanorod array photocathode:
s2.1, adding 0.65g of Bi (NO 3) 3-5H 2O into deionized water, and stirring for dissolving;
s2.2, adding 0.45g of Cu (NO) 3-3H 2O into the mixed solution finally obtained in the step S2.1, and continuously stirring to completely dissolve the Cu (NO) 3-3H 2O;
s2.3, adding 1mL of deionized water solution containing 0.34g of NaOH into the mixed solution finally obtained in the step S2.2, and continuously stirring for 2 h;
s2.4, adding 1g of sodium dodecyl benzene sulfonate into the solution obtained in the step S2.3, and stirring for two hours;
s2.5, placing the FTO containing the CBO seed layer obtained in the step S1.3 into a high-pressure reaction kettle, pouring the FTO into the mixed solution finally obtained in the step S2.4, sealing the high-pressure reaction kettle, placing the high-pressure reaction kettle into a drying box, reacting at a constant temperature of 180 ℃ for 24 hours, naturally cooling to room temperature after the reaction is finished, washing the obtained product with deionized water and ethanol for 3 times respectively, drying at 60 ℃ in a vacuum drying box, and finally annealing at 550 ℃ for 1 hour to obtain the CBO nanorod array photocathode.
S3 Synthesis of F-doped CBO nanorod array photocathode:
s3.1, the CBO nanorod array photocathode obtained in the step S2.5 is placed into 10mL of deionized water solution containing 10mg of NaF to be soaked for 2 hours, taken out and dried, and annealed at 300 ℃ for 1 hour to obtain the F-doped CBO nanorod array material.
The F-CBO photoelectric cathode is F-ion doped CuBi 2O 4, and the shape of the F-CBO photoelectric cathode is a nanorod array.
Further, the scanning electron image of the CBO nanorod array photocathode obtained in step S2.5 is shown in fig. 1.
Further, the scanning electron mirror image of the F-CBO nanorod array photocathode obtained in the step S3.1 is shown in FIG. 2.
FIG. 3 is a high-resolution transmission electron image of the F-CBO nanorod array photocathode material prepared by the present example.
FIG. 4 shows the X-ray diffraction patterns of the photocathode materials of CBO and F-CBO nanorod arrays prepared in this example.
FIG. 5 is the Raman spectra of the CBO and F-CBO nanorod array photocathode materials prepared in this example.
The X-ray diffraction pattern and Raman spectrum showed that the sample prepared was CBO.
As can be seen from the diffuse reflection of UV light shown in FIG. 6, all samples show strong absorption in the range of 200-1000 nm.
FIG. 7 is a band gap diagram calculated from the ultraviolet diffuse reflection data of the photocathode material of the CBO and F-CBO nanorod arrays prepared in the example.
FIG. 8 is an impedance spectrum of a photocathode of the CBO and F-CBO nanorod array prepared in this example, and research results show that, in light and darkness, the F-CBO nanorod array electrode shows a smaller semicircular diameter than the CBO nanorod array electrode, and mass transfer resistance of the CBO is effectively reduced after doping of F-ions, thereby showing excellent photoelectrocatalysis performance.
Example 2
FIG. 9 is the difference between the charge current densities at different scanning rates of the photocathodes of the CBO and F-CBO nanorod arrays prepared in example 1, which shows that the photocathode of the F-CBO nanorod array has a photocatalytic active area larger than that of CBO.
Example 3
The difference in activity of photocathodes for photocatalytically reducing oxygen of the CBO and F-CBO nanorod arrays prepared in example 1 was tested by the following experiment.
Electrochemical measurements were performed in a standard three-electrode system at room temperature using a platinum wire as the counter electrode and saturated SCE as the reference electrode. The electrolyte was a 0.1M KOH solution. Measured on CHI760D electrochemical workstation, and chopper chopped light, the light source was a solar simulator (AM 1.5G), and the intensity was adjusted to 100mW/cm 2. The photoelectrode was immersed in the solution in an area of 1cm 2, and the working electrode was irradiated from the front. Testing the photocurrent density: with LSV, a voltage sweep range of 0.2-1.4Vvs. RHE was set, a sweep rate of 10mV/s, and a sensitivity set at 10-4, as shown in FIG. 10, indicating that after F-doping, the current density increased slightly and the oxygen reduction reaction was superior to the water decomposition reaction. Photoelectrochemical stability test (IT): rhe was set at a voltage of 0.65vvs.rhe and sensitivity was set at 10-4, as shown in fig. 11, indicating increased stability after F-doping. For comparison, all SCE electrode potentials were converted to RHE using the nernst equation e (RHE) ═ e (SCE) +0.242+0.059 × pH.
Example 4
The difference in H2O 2 production by photocathode photocatalytic reduction of oxygen by the CBO and F-CBO nanorod arrays prepared in example 1 was tested by the following experiment.
In the photoelectrochemical reaction process, continuously blowing oxygen bubbles into a working electrode chamber until the reaction is finished, testing in an ice bath (283K), continuously stirring in the testing process, sampling once every 15min, and immediately putting the sampled sample into a refrigerator for refrigeration to prevent the decomposition of the generated H2O 2. As shown in FIG. 12, the yield of H2O 2 was 0.3mmol/L H2O 2 concentration at 45min before doping, and the concentration of H2O 2 after doping was 0.85mmol/L, which is 2.8 times that before doping, indicating that F-ion doping is helpful for H2O 2 generation.
Example 5
The selectivity of H2O 2 generation for the CBO and F-CBO nanorod array photocathodes of example 1 was investigated by conventional rotating disk electrode (RRDE) technology. RRDE activity results of the photoelectrode are shown in FIGS. 13-14, and the results show that the F-CBO nanorod array photocathode material has higher H2O 2 generation selectivity.
Various corresponding changes and modifications can be made by those skilled in the art based on the above technical solutions and concepts, and all such changes and modifications should be included in the protection scope of the present invention.

Claims (6)

1. A preparation method of an F-doped CBO nanorod array photocathode material is characterized by comprising the following steps:
s1 synthesizing a CBO seed layer;
s2, synthesizing a CBO nanorod array photocathode by using the CBO seed layer;
s3, synthesizing an F-doped CBO nanorod array photocathode, soaking the CBO nanorod array photocathode obtained in the step S2 in NaF solution for 2 hours, taking out and drying the soaked CBO nanorod array photocathode, and annealing the soaked CBO nanorod array photocathode at 300 ℃ for 1 hour to obtain an F-doped CBO nanorod array photocathode material; wherein, the CBO is CuBi 2 O 4 。
2. The method for preparing the F-doped CBO nanorod array photocathode material according to claim 1, wherein the synthesized CBO seed layer of the step S1 includes:
s1.1 adding CuSO 4 ·5H 2 Dissolving O in deionized water, and stirring to completely dissolve O;
s1.2, adding the sodium bismuth ethylene diamine tetraacetate into the mixed solution finally obtained in the step S1.1, and continuously stirring to completely dissolve the sodium bismuth ethylene diamine tetraacetate;
s1.3, dripping the solution obtained in the step S1.2 on FTO glass, putting the sample into an oven at 80 ℃ for drying for 1h, and then annealing in a tube furnace at 550 ℃ for 2h to obtain the FTO containing the CBO seed layer.
3. The method of claim 1, wherein the synthesized CBO nanorod array photocathode of step S2 comprises:
s2.1 reaction of Bi (NO) 3 ) 3 ·5H 2 Adding O into deionized water, and stirring for dissolving;
s2.2 adding Cu (NO) into the mixed solution finally obtained in the step S2.1 3 ·3H 2 O, continuously stirring to completely dissolve the materials;
s2.3, adding a NaOH solution into the mixed solution finally obtained in the step S2.2, and continuously stirring for 2 hours;
s2.4, adding sodium dodecyl benzene sulfonate into the solution obtained in the step S2.3, and stirring for 2 hours;
s2.5, placing FTO containing a CBO seed layer into a high-pressure reaction kettle, pouring the FTO into the mixed solution finally obtained in the step S2.4, sealing the high-pressure reaction kettle, placing the sealed high-pressure reaction kettle into a drying box, reacting at a constant temperature of 180 ℃ for 24 hours, naturally cooling to room temperature after the reaction is finished, washing the obtained product with deionized water and ethanol for 3 times respectively, drying the product in a vacuum drying box at 60 ℃, and finally annealing at 550 ℃ for 1 hour to obtain the CBO nanorod array photocathode.
4. The method for preparing the F-doped CBO nanorod array photocathode material according to claim 2, wherein in step S1.1, 0.05mmol of CuSO is added 4 ·5H 2 Dissolving O in 10mL of deionized water; in step S1.2, 0.1mmol of sodium bismuth ethylenediaminetetraacetate is dissolved in the solution finally obtained in step S1.1.
5. The method for preparing F-doped CBO nanorod array photocathode material according to claim 3, wherein in step S2.1, 0.605gBi (NO) is added 3 ) 3 ·5H 2 Dissolving O in 20mL of deionized water; in step S2.2, 0.45g of Cu (NO) is added to the mixed solution finally obtained in step S2.1 3 ·3H 2 O, stirring and dissolving; in step S2.3, 1mL of a solution containing 0.34g of NaOH is added dropwise to the mixed solution finally obtained in step S2.2; in step S2.4, 1g of sodium dodecylbenzenesulfonate is added to the mixed solution finally obtained in step S2.3 and stirred for 2 hours.
6. The method for preparing the F-doped CBO nanorod array photocathode material according to claim 1, wherein the NaF solution in the step S3 is prepared by dissolving 10mg of NaF in 10mL of deionized water.
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