CN115779931A - Heterojunction photocatalytic material based on cubic cuprous oxide and preparation method thereof - Google Patents
Heterojunction photocatalytic material based on cubic cuprous oxide and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 23
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 21
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 16
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000004073 vulcanization Methods 0.000 claims abstract description 6
- 239000010949 copper Substances 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 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 3
- 229960000999 sodium citrate dihydrate Drugs 0.000 claims description 3
- 238000005486 sulfidation Methods 0.000 claims description 3
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 239000000969 carrier Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000010276 construction Methods 0.000 abstract 1
- 230000031700 light absorption Effects 0.000 abstract 1
- 230000005012 migration Effects 0.000 abstract 1
- 238000013508 migration Methods 0.000 abstract 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 4
- 229960005070 ascorbic acid Drugs 0.000 description 3
- 235000010323 ascorbic acid Nutrition 0.000 description 3
- 239000011668 ascorbic acid Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000013032 photocatalytic reaction Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- -1 sensors Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 102100030310 5,6-dihydroxyindole-2-carboxylic acid oxidase Human genes 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 101000773083 Homo sapiens 5,6-dihydroxyindole-2-carboxylic acid oxidase Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229960004106 citric acid Drugs 0.000 description 1
- 238000011278 co-treatment Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a heterojunction photocatalytic material based on cubic cuprous oxide and a preparation method thereof 2 O cubic particles, using NaS.9H in climate under normal temperature condition 2 O solution to Cu 2 And carrying out surface micro-vulcanization on the O cube to construct a heterojunction structure. Based on reasonable construction of a heterostructure, the advantages of multiple components can be integrated, separation and migration of photon-generated carriers are promoted, and the light absorption range is expanded. Cu prepared by the invention 2 The O/CuS heterojunction photocatalytic material has good photoelectrochemical performance, simple process and mild condition.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a cubic cuprous oxide-based heterojunction photocatalytic material and a preparation method thereof.
Background
With the development of economic society, global warming and energy crisis become two problems to be solved urgently in the world. In order to reduce the use of fossil energy, reduce the discharge of pollutants and improve the sewage treatment efficiency, the photocatalytic reaction gradually receives wide attention from scientific research workers at home and abroad. The photocatalytic reaction utilizes photocatalyst (usually semiconductor material) to implement the hydrogen production by photoinduced decomposition of water or degradation of organic pollutant, and has the advantages of no secondary pollution, low energy consumption and the like in the aspects of green energy preparation and sewage treatment. In order to realize efficient and stable photocatalytic reaction, the development of a catalyst with excellent photoelectric properties and a stable structure is a key point of research. Because the band gap of the existing typical photocatalyst, such as titanium dioxide (TiO 2), is too wide, and only can absorb and utilize the energy of an ultraviolet band (the wavelength is less than 387 nm) in sunlight, the development of a photocatalytic material with a narrow band gap and high charge separation efficiency is the key for improving the photocatalytic efficiency in the future.
Disclosure of Invention
Aiming at the technical problem, the invention uses cuprous oxide (Cu) 2 O) is an important P-type semiconductor material as a research object of photocatalytic materials, and has a forbidden band width of about 2.17eV, can be excited by visible light, can efficiently and rapidly generate carriers under the irradiation of sunlight, and has excellent photoelectric response performance. Simultaneously, the cuprous oxide has the advantages of no toxicity, good environmental acceptability, low price, high activity and the like, and the Cu 2 O is one of the most potential visible light photocatalysts at present, and has wide application in the aspects of solar cells, carbon monoxide oxidation, photocatalysts, sensors, chemical templates and the like.
The invention uses cupric salt CuSO 4 Adding appropriate reducing agent such as ascorbic acid, glucose, hydrazine hydrate, citric acid, etc., and surfactant (such as CATB) into raw materials, heating in water bath, and stirring to obtain monodisperse Cu with appropriate size 2 O nano/micro particles. With the prepared Cu 2 Carrying out surface micro-vulcanization on the O particle material as the basis to construct Cu 2 And the O/CuS heterojunction regulates and controls the structure and the components of the surface nano-micro structure and the heterojunction by adjusting the temperature and the time of the vulcanization reaction and the concentration of a sulfur source.
The preparation method comprises the following steps:
(1) 239mg of anhydrous copper sulfate and 147mg of sodium citrate dihydrate are added into 80mL of deionized water;
(2) Under the heating condition of a water bath at 60 ℃, dropwise adding 20mL of NaOH aqueous solution (1.25M) and 50mL of ascorbic acid aqueous solution (0.03M) into the solution obtained in the step (1), and magnetically stirring at a constant speed of 120 revolutions per minute for 10min;
(3) Standing and aging the solution obtained in the step (2) for 1h at the temperature of 60 ℃;
(4) And (4) centrifuging the solution obtained in the step (3), collecting the solution, and drying the solution at the temperature of 60 ℃. The rotating speed of the centrifugation is 8000r/min, and the time of the centrifugation is 3min.
(5) Taking 50mg of the product obtained in the step (4) and NaS.9H 2 O aqueous solution (0.8 mM) was mixed and left standing for 1 hour.
And (5) adopting a method of surface micro-vulcanization at normal temperature.
Cu prepared by the invention 2 The O/CuS has excellent photoelectric properties.
Compared with the prior art, the invention has the following advantages:
1. CuSO is utilized for the purpose of utilizing visible light in solar energy with high efficiency and low cost 4 Heating and stirring in water bath to generate Cu 2 O, and further sulfurizing to form Cu 2 An O/CuS heterojunction.
2. And Cu 2 Cu obtained by surface micro-sulfurization of O cubic particles 2 The O/CuS has better photoresponse characteristics, i.e. exhibits a larger contact potential difference with/without illumination, see fig. 3-4 for comparison.
Drawings
FIG. 1 shows example Cu 2 Scanning electron microscope pictures of O cubic particles.
FIG. 2 shows example Cu 2 Scanning electron microscope pictures of O/CuS cubic particles.
FIG. 3 shows example Cu 2 The O-cube particles were exposed to potential difference contrast pictures on the surface with/without light.
FIG. 4 shows example Cu 2 The O/CuS cubic particles were exposed to potential difference contrast pictures on the surface with/without light.
FIG. 5 shows example Cu 2 O/CuS cube particles example formulations were prepared and corresponding photographs of the solutions after 1h of standing.
FIG. 6 shows the photocatalytic CO treatment of the catalytic material prepared under the micro-sulfidation condition on the surfaces 1-5 in Table 1 2 The gas phase product properties obtained in the experiment are compared with a histogram.
Detailed Description
The specific technical scheme of the invention is described by combining the embodiment.
Cu based on cubic cuprous oxide of this embodiment 2 O and Cu 2 O/CuS heterojunction photocatalytic material, the Cu 2 O and Cu 2 O/CuS heterojunction photocatalytic material in Cu 2 Sulfidation of Cu on O 2 An O/CuS heterojunction; the Cu 2 O and Cu 2 The size of the O/CuS heterojunction photocatalytic material is 700 nm-1000 nm.
The embodiment also provides a method for preparing the cubic cuprous oxide Cu2O and Cu2O/CuS heterojunction photocatalytic material, which comprises the following steps:
(1) 239mg of anhydrous copper sulfate and 147mg of sodium citrate dihydrate are added into 80mL of deionized water;
(2) Under the heating condition of a water bath at 60 ℃, dropwise adding 20mL of NaOH aqueous solution (1.25M) and 50mL of ascorbic acid aqueous solution (0.03M) into the solution obtained in the step (1), and magnetically stirring at a constant speed of 120 revolutions per minute for 10min;
(3) Standing and aging the solution obtained in the step (2) for 1h at the temperature of 60 ℃;
(4) And (4) centrifuging the solution obtained in the step (3), collecting the solution, and drying the solution at the temperature of 60 ℃.
(5) Taking 50mg of the product obtained in the step (4) and NaS.9H 2 Mixing the O aqueous solution and standing for 1h. As shown in fig. 5. NaS.9H in FIG. 5 2 The concentration of the O aqueous solution is 0.2-1.2mM, and the following table 1 is specifically adopted:
TABLE 1
With Cu as shown in FIG. 1 2 Compared with O cubic particles, cu shown in figure 2 obtained by surface micro-sulfurization 2 The O/CuS has better light response characteristics, namely in the presence/absence of lightShowing a larger contact potential difference in the following, see fig. 3 in comparison with fig. 4.
Catalytic material prepared under the condition of micro-vulcanization of surfaces No. 1-5 in Table 1 is used for photocatalysis of CO 2 The gas phase product performance profiles obtained in the experiments are shown in figure 6.
Claims (6)
1. The preparation method of the heterojunction photocatalytic material based on the cubic cuprous oxide is characterized in that a water bath heating and stirring method is adopted to synthesize Cu 2 Cubic O particles using NaS.9H 2 O solution to Cu 2 And carrying out surface micro-vulcanization on the O cube to construct a heterojunction structure.
2. The method for preparing a cubic cuprous oxide based heterojunction photocatalytic material according to claim 1, comprising the steps of:
(1) 239mg of anhydrous copper sulfate and 147mg of sodium citrate dihydrate are added into 80mL of deionized water;
(2) Under the heating condition of water bath at 60 ℃, dropwise adding 20mL of 1.25M NaOH aqueous solution and 50mL of 0.03M reducing agent aqueous solution into the solution obtained in the step (1), and magnetically stirring;
(3) Standing and aging the solution obtained in the step (2) for 1h at the temperature of 60 ℃;
(4) And (4) centrifuging the solution obtained in the step (3), collecting the solution, and drying the solution at the temperature of 60 ℃.
(5) Taking 50mg of the product obtained in the step (4) and NaS.9H 2 Mixing the O aqueous solution and standing for 1h.
3. The preparation method of the cubic cuprous oxide based heterojunction photocatalytic material according to claim 2, wherein in step (2), the uniform magnetic stirring is performed at a rotation speed of 120 rpm for 10min.
4. The preparation method of the cubic cuprous oxide based heterojunction photocatalytic material according to claim 2, wherein the rotation speed of the centrifugation in the step (4) is 8000r/min, and the time of the centrifugation is 3min.
5. The preparation method of the cubic cuprous oxide based heterojunction photocatalytic material according to claim 2, wherein the surface micro-sulfidation method at normal temperature is adopted in the step (5).
6. A heterojunction photocatalytic material based on cubic cuprous oxide, obtained by the preparation method according to any one 2 of claims 1 to 5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116651467A (en) * | 2023-06-02 | 2023-08-29 | 常州大学 | Hollow Cu 2-x S@ cadmium manganese sulfide composite photocatalyst and preparation method and application thereof |
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| CN109395745A (en) * | 2018-12-03 | 2019-03-01 | 安徽工程大学 | A kind of adjustable high energy structure copper sulfide-cuprous oxide compound of Lacking oxygen and its preparation method and application |
| CN111960481A (en) * | 2020-09-04 | 2020-11-20 | 重庆文理学院 | A kind of Ni (OH)2Preparation method of @ CuS composite material |
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- 2022-12-07 CN CN202211580390.5A patent/CN115779931A/en active Pending
Patent Citations (5)
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| CN102357659A (en) * | 2011-07-27 | 2012-02-22 | 西安交通大学 | Preparation method of Cu-Cu2O heterogenous junction |
| CN106830049A (en) * | 2017-03-14 | 2017-06-13 | 吉林大学 | A kind of Cu of nanometer sheet composition9 S5The preparation method of hollow 26 face body |
| CN107089683A (en) * | 2017-04-25 | 2017-08-25 | 中国计量大学 | A kind of preparation method of molybdenum disulfide/copper sulfide/cuprous nano composite |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116651467A (en) * | 2023-06-02 | 2023-08-29 | 常州大学 | Hollow Cu 2-x S@ cadmium manganese sulfide composite photocatalyst and preparation method and application thereof |
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