CN115121261A - NaNbO for photoelectrocatalysis 3 /Co(OH) 2 Preparation method of/Ag composite film material - Google Patents
NaNbO for photoelectrocatalysis 3 /Co(OH) 2 Preparation method of/Ag composite film material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000151 deposition Methods 0.000 claims abstract description 14
- 230000008021 deposition Effects 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000004528 spin coating Methods 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- 239000002105 nanoparticle Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 7
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 5
- 239000003792 electrolyte Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- 229910052724 xenon Inorganic materials 0.000 claims description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000000486 photoelectrochemical deposition Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 230000033116 oxidation-reduction process Effects 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000031700 light absorption Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 abstract 4
- 238000004070 electrodeposition Methods 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- 101710134784 Agnoprotein Proteins 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000010335 hydrothermal treatment Methods 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000006557 surface reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000010893 electron trap Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/898—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with vanadium, tantalum, niobium or polonium
-
- B01J35/23—
-
- B01J35/33—
-
- B01J35/39—
Abstract
The invention discloses NaNbO for photoelectrocatalysis 3 /Co(OH) 2 The preparation method of the/Ag composite film material comprises the steps of firstly preparing NaNbO by a hydrothermal method 3 Preparing NaNbO powder by using spin coating method 3 A film; then the electrochemical deposition method is used to deposit Co (OH) 2 Deposition to NaNbO 3 To finally obtain the NaNbO 3 /Co(OH) 2 A thin film composite. Finally, Ag nano particles are deposited to NaNbO by using a redox method 3 /Co(OH) 2 Finally obtaining NaNbO 3 /Co(OH) 2 The Ag/film composite material. The prepared composite film material improves NaNbO 3 The visible light absorption promotes the improvement of the photoelectric catalytic performance; the preparation method is simple and easy to operate, and the overall cost is low.
Description
Technical Field
The invention belongs to the technical field of preparation of a photoelectrocatalysis film material, and particularly relates to NaNbO for photoelectrocatalysis 3 /Co(OH) 2 A preparation method of/Ag composite film material.
Background
With the rapid development of modern industry, pollution and energy shortage have become global problems. Hydrogen energy has great development potential as a secondary energy source. With advances in technology, researchers have developed many efficient methods of producing hydrogen, such as: biological hydrogen production, water electrolysis hydrogen production, photocatalytic hydrogen production and the like. The photoelectrochemistry decomposition water hydrogen production is considered as the most promising hydrogen production method due to the characteristics of economy, environmental protection, high efficiency and the like, and has attracted the research interest all over the world. NaNbO 3 As a typical perovskite semiconductor material, researchers have attracted much attention because of its advantages such as excellent nonlinear optical and ionic conductivity properties. And, as an n-type semiconductor, NaNbO 3 Having [ NbO 6 ] - The unique crystal structure of the co-angle octahedral unit is also beneficial to improving charge transfer in the crystal. However, NaNbO 3 The slow surface reaction kinetics result in a low separation efficiency of the photogenerated electron-hole pairs and the wide band gap limits its photoresponse in the ultraviolet region, since only about 4% to 5% of the solar spectrum falls in the ultraviolet range. Thus, efficient use of visible light remains a significant challenge.
With the advent of transition metal hydroxides as electrocatalysts, researchers have focused on their use to drive oxygen evolution reactions due to their chemical stability under oxidizing conditions and low price. The unique hole extraction function and the special surface dimension of the transition metal hydroxide can accelerate the surface reaction kinetics of a semiconductor and enhance the separation of photo-generated electron-hole pairs, so that people have increasing research interest on the transition metal hydroxide. However, the low stability of transition metal hydroxides limits their use. Loading appropriate noble metal nanoparticles as electron traps facilitates significant improvement in PEC performance. Silver is unique in many different noble metals, it does not corrode during photoreaction, and it also functions to reduce active sites and effectively trap photogenerated electrons from the semiconductor surface. Therefore, it is prepared from Co (OH) 2 Loaded on NaNbO together with Ag 3 Film surface to improve NaNbO 3 The photoelectrocatalysis performance of the base film composite material.
Disclosure of Invention
To solve the problem of NaNbO 3 The invention aims to provide a preparation method of a photoelectrocatalysis composite film material, which can improve the NaNbO 3 The photocatalytic performance of (a).
In order to achieve the aim, the invention provides photoelectrocatalysis NaNbO 3 /Co(OH) 2 The preparation method of the/Ag composite film material comprises the following steps in sequence:
(1) dissolving niobium pentoxide in sodium hydroxide solution, heating and stirring in water bath at a certain temperatureStirring for a certain time at a certain temperature to obtain a precursor solution, transferring the precursor solution into a reaction kettle, carrying out hydrothermal reaction for a certain time at a certain temperature, washing, filtering and drying a reacted sample to obtain the NaNbO 3 And (3) powder. Then, a film was prepared by spin coating.
(2) The prepared NaNbO 3 Film deposition of Co (OH) by photoelectrochemical deposition 2 The NaNbO prepared in the step (1) is added 3 The film is used as a working electrode, Ag/AgCl is used as a reference electrode, a Pt sheet is used as a counter electrode, and the electrolyte is Co (OH) 2 Growing the solution to prepare NaNbO under certain deposition conditions 3 /Co(OH) 2 A photoelectrocatalysis composite film material.
(3) The prepared NaNbO 3 /Co(OH) 2 Depositing Ag nano particles on the composite film by a redox method, and carrying out the preparation of the NaNbO prepared in the step (2) 3 /Co(OH) 2 The composite film is used as a substrate to prepare NaNbO under the condition of certain Ag growth solution concentration 3 /Co(OH) 2 The Ag photoelectrocatalysis composite film material.
In the step (1), the concentration of the sodium hydroxide is 4M, the using amount of the niobium pentoxide is 0.025mmol, the water bath heating temperature and the stirring time are 45 ℃ and 0.5h respectively, and the hydrothermal temperature and the hydrothermal time are 160-180 ℃ and 8-10 h respectively.
In step (2), the Co (OH) 2 The growth solution is Co (NO) 3 ) 2 Solution, Co (NO) 3 ) 2 The concentration of the solution was: 50 to 60 mM. The deposition condition is that the light source is 100mW cm -2 The applied voltage of the xenon lamp is-1 to-0.8V, and the deposition time is 200 to 400 s.
In the step (3), the concentration of the Ag growth solution is 10-15 mM, and the soaking time is 5-15 min.
The invention provides NaNbO for photoelectrocatalysis 3 /Co(OH) 2 The preparation method of the/Ag composite film material has the following beneficial effects:
(1) the invention can effectively widen the light absorption range and promote the separation of the photo-generated electron-hole pairs.
(2) The preparation method is simple and easy to operate, and the overall cost is low.
(3) The NaNbO prepared by the invention 3 /Co(OH) 2 the/Ag composite film material has excellent photoelectric catalytic performance.
Drawings
FIG. 1 shows NaNbO obtained in example 3 /Co(OH) 2 Linear scanning voltammogram of the/Ag composite film material.
Detailed Description
The following examples are presented to enable those skilled in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
NaNbO for photoelectrocatalysis 3 /Co(OH) 2 The preparation method of the/Ag composite film material comprises the following steps:
(1) 8g of sodium hydroxide are dissolved in 50mL of water with constant stirring, 6.64g of niobium pentoxide are then added and stirring is carried out at constant temperature of 45 ℃ for 0.5 h. And cooling the prepared precursor solution to room temperature, transferring the precursor solution into a 100mL reaction kettle, and carrying out hydrothermal treatment at 160 ℃ for 8 h. After washing, filtering and drying, NaNbO is obtained 3 And (3) powder. Finally, NaNbO is prepared by a spin coating method 3 A film substrate.
(2) 0.87g of Co (NO) 3 ) 2 ·6H 2 Dissolving O into 50mL of deionized water, and stirring by magnetic force to fully dissolve the O to obtain Co (OH) 2 The growth solution is ready for use. NaNbO 3 The film is used as a working electrode, Ag/AgCl is used as a reference electrode, a Pt sheet is used as a counter electrode, and the electrolyte is Co (OH) 2 Growth solution at 100mW cm -2 Under the irradiation of xenon lamp, depositing for 300s by applying a voltage of-1V, finally taking out, washing for many times by deionized water, and drying at 65 ℃ to obtain NaNbO 3 /Co(OH) 2 A film material.
(3) 0.025g of AgNO was weighed 3 Adding the solution into 10mL of deionized water, and fully dissolving the solution by magnetic stirring to obtain an Ag growth solution for later use. NaNbO is reacted with 3 /Co(OH) 2 Immersing the film into an Ag growth solution for 5min, then washing the film for multiple times by deionized water, and drying the film at 65 ℃ to obtain NaNbO 3 /Co(OH) 2 the/Ag composite film material.
Example 2
NaNbO for photoelectrocatalysis 3 /Co(OH) 2 The preparation method of the/Ag composite film material comprises the following steps:
(1) 8g of sodium hydroxide are dissolved in 50mL of water with constant stirring, 6.64g of niobium pentoxide are then added and stirring is carried out at a constant temperature of 45 ℃ for 0.5 h. And cooling the prepared precursor solution to room temperature, transferring the precursor solution into a 100mL reaction kettle, and carrying out hydrothermal treatment at 160 ℃ for 10 hours. After washing, filtering and drying, NaNbO is obtained 3 And (3) powder. Finally, NaNbO is prepared by a spin coating method 3 A film substrate.
(2) 0.72g of Co (NO) 3 ) 2 ·6H 2 Dissolving O into 50mL of deionized water, and stirring by magnetic force to fully dissolve the O to obtain Co (OH) 2 The growth solution is ready for use. NaNbO 3 The film is used as a working electrode, Ag/AgCl is used as a reference electrode, a Pt sheet is used as a counter electrode, and the electrolyte is Co (OH) 2 Growth solution at 100mW cm -2 Under the irradiation of xenon lamp, depositing for 200s by applying a voltage of-0.9V, finally taking out, washing for many times by deionized water, and drying at 65 ℃ to obtain NaNbO 3 /Co(OH) 2 A film material.
(3) 0.025g of AgNO was weighed 3 Adding the solution into 10mL of deionized water, and fully dissolving the solution by magnetic stirring to obtain an Ag growth solution for later use. Mixing NaNbO 3 /Co(OH) 2 Immersing the film into an Ag growth solution for 10min, then washing the film for multiple times by deionized water, and drying the film at 65 ℃ to obtain NaNbO 3 /Co(OH) 2 the/Ag composite film material.
Example 3
NaNbO for photoelectrocatalysis 3 /Co(OH) 2 The preparation method of the/Ag composite film material comprises the following steps:
(1) 8g of sodium hydroxide are dissolved in 50mL of water with constant stirring, 6.64g of niobium pentoxide are then added and stirring is carried out at a constant temperature of 45 ℃ for 0.5 h. And cooling the prepared precursor solution to room temperature, transferring the precursor solution into a 100mL reaction kettle, and carrying out hydrothermal treatment at 180 ℃ for 8 h. After washing, filtering and drying, NaNbO is obtained 3 And (3) powder. Most preferablyThen, NaNbO is prepared by a spin coating method 3 A film substrate.
(2) 0.87g of Co (NO) 3 ) 2 ·6H 2 Dissolving O into 50mL of deionized water, and stirring by magnetic force to fully dissolve the O to obtain Co (OH) 2 The growth solution is ready for use. NaNbO 3 The film is used as a working electrode, Ag/AgCl is used as a reference electrode, a Pt sheet is used as a counter electrode, and the electrolyte is Co (OH) 2 Growth solution at 100mW cm -2 Under the irradiation of a xenon lamp, depositing for 400s by applying a voltage of-0.8V, finally taking out, washing for many times by deionized water, and drying at 65 ℃ to obtain NaNbO 3 /Co(OH) 2 A film material.
(3) Weighing 0.017g of AgNO 3 Adding the solution into 10mL of deionized water, and fully dissolving the solution by magnetic stirring to obtain an Ag growth solution for later use. NaNbO is reacted with 3 /Co(OH) 2 Immersing the film into an Ag growth solution for 15min, then washing the film for multiple times by deionized water, and drying the film at 65 ℃ to obtain NaNbO 3 /Co(OH) 2 The Ag/Ag composite film material.
Claims (4)
1. NaNbO for photoelectrocatalysis 3 /Co(OH) 2 The preparation method of the/Ag composite film material is characterized by comprising the following steps: the preparation method comprises the following steps which are carried out in sequence:
(1) dissolving niobium pentoxide in a sodium hydroxide solution, stirring for a certain time at a certain temperature by adopting a water bath heating and stirring mode to obtain a precursor solution, transferring the precursor solution into a reaction kettle, carrying out hydrothermal reaction for a certain time at a certain temperature, washing, filtering and drying a reacted sample to obtain NaNbO 3 And (3) powder. Then, a film was formed by spin coating.
(2) The prepared NaNbO 3 Film deposition of Co (OH) by photoelectrochemical deposition 2 The NaNbO prepared in the step (1) is added 3 The film is used as a working electrode, Ag/AgCl is used as a reference electrode, a Pt sheet is used as a counter electrode, and the electrolyte is Co (OH) 2 Growing the solution to prepare NaNbO under certain deposition conditions 3 /Co(OH) 2 A photoelectrocatalysis composite film material.
(3) Will make intoThe obtained NaNbO 3 /Co(OH) 2 Depositing Ag nano particles on the composite film by an oxidation-reduction method, and carrying out the preparation of the NaNbO prepared in the step (2) 3 /Co(OH) 2 The composite film is used as a substrate to prepare NaNbO under the condition of certain Ag growth solution concentration 3 /Co(OH) 2 The Ag photoelectrocatalysis composite film material.
2. NaNbO for photoelectrocatalysis according to claim 1 3 /Co(OH) 2 The preparation method of the/Ag composite film material is characterized by comprising the following steps: in the step (1), the concentration of the sodium hydroxide is 4M, the dosage of the niobium pentoxide is 0.025mmol, the water bath heating temperature and the stirring time are 45 ℃ and 0.5h respectively, and the hydrothermal temperature and the hydrothermal time are 160-180 ℃ and 8-10 h respectively.
3. NaNbO for photoelectrocatalysis according to claim 1 3 /Co(OH) 2 The preparation method of the/Ag composite film material is characterized by comprising the following steps: in step (2), the Co (OH) 2 The growth solution is Co (NO) 3 ) 2 Solution, Co (NO) 3 ) 2 The concentration of the solution was: 50 to 60 mM. The deposition condition is that the light source is 100mW cm -2 The applied voltage of the xenon lamp is-1 to-0.8V, and the deposition time is 200 to 400 s.
4. NaNbO for photoelectrocatalysis according to claim 1 3 /Co(OH) 2 The preparation method of the/Ag composite film material is characterized by comprising the following steps: in the step (3), the concentration of the Ag growth solution is 10-15 mM, and the soaking time is 5-15 min.
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|---|---|---|---|---|
| CN103127932A (en) * | 2013-03-13 | 2013-06-05 | 江南大学 | Preparation method of nanometer niobium-series photocatalyst |
| CN103706363A (en) * | 2013-12-18 | 2014-04-09 | 江苏大学 | Method for preparing composite photocatalyst with silver loaded on surface of nano sodium tantalate |
| CN105110289A (en) * | 2014-12-03 | 2015-12-02 | 江苏大学 | Method for preparing Ag-loaded potassium tantalite catalyst for decomposing water for hydrogen production |
| US20160129427A1 (en) * | 2013-06-17 | 2016-05-12 | Hindustan Petroleum Corporation Ltd. | Catalyst Composition for Photocatalytic Reduction of Carbon Dioxide |
| CN106906488A (en) * | 2017-01-18 | 2017-06-30 | 常州大学 | A kind of method for preparing cobalt hydroxide modified titanic oxide light anode |
| CN107983347A (en) * | 2017-12-14 | 2018-05-04 | 聊城大学 | A kind of NaNbO3/Ag2The preparation method of O sonophotocatalysis materials |
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- 2022-06-28 CN CN202210738276.4A patent/CN115121261A/en active Pending
Patent Citations (6)
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| CN103127932A (en) * | 2013-03-13 | 2013-06-05 | 江南大学 | Preparation method of nanometer niobium-series photocatalyst |
| US20160129427A1 (en) * | 2013-06-17 | 2016-05-12 | Hindustan Petroleum Corporation Ltd. | Catalyst Composition for Photocatalytic Reduction of Carbon Dioxide |
| CN103706363A (en) * | 2013-12-18 | 2014-04-09 | 江苏大学 | Method for preparing composite photocatalyst with silver loaded on surface of nano sodium tantalate |
| CN105110289A (en) * | 2014-12-03 | 2015-12-02 | 江苏大学 | Method for preparing Ag-loaded potassium tantalite catalyst for decomposing water for hydrogen production |
| CN106906488A (en) * | 2017-01-18 | 2017-06-30 | 常州大学 | A kind of method for preparing cobalt hydroxide modified titanic oxide light anode |
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Non-Patent Citations (2)
| Title |
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| KAZUHIKO MAEDA: ""Modification of Wide-Band-Gap Oxide Semiconductors with Cobalt Hydroxide Nanoclusters for Visible-Light Water Oxidation"", 《ANGEW. CHEM. INT. ED.》, 25 May 2016 (2016-05-25), pages 8309 - 8313 * |
| ***等: ""Ag2O/NaNbO3纳米复合材料的制备及其光催化性质"", 《宜春学院学报》, vol. 42, no. 3, 31 March 2020 (2020-03-31), pages 27 - 30 * |
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