CN112958093A - Cobalt ferrite photocatalyst with oxygen-containing defect and preparation method and application thereof - Google Patents
Cobalt ferrite photocatalyst with oxygen-containing defect and preparation method and application thereof Download PDFInfo
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- CN112958093A CN112958093A CN202110160476.1A CN202110160476A CN112958093A CN 112958093 A CN112958093 A CN 112958093A CN 202110160476 A CN202110160476 A CN 202110160476A CN 112958093 A CN112958093 A CN 112958093A
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- photocatalyst
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- cobalt ferrite
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000001301 oxygen Substances 0.000 title claims abstract description 54
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 54
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 50
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 44
- 239000010941 cobalt Substances 0.000 title claims abstract description 44
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 44
- 230000007547 defect Effects 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 150000001868 cobalt Chemical class 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 150000002505 iron Chemical class 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 24
- 230000002950 deficient Effects 0.000 claims description 19
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical group O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims description 7
- 230000000593 degrading effect Effects 0.000 claims description 7
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical group O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 7
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000006731 degradation reaction Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 claims description 4
- 239000002738 chelating agent Substances 0.000 claims description 4
- 239000003344 environmental pollutant Substances 0.000 claims description 4
- 231100000719 pollutant Toxicity 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 230000032683 aging Effects 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 2
- MEYVLGVRTYSQHI-UHFFFAOYSA-L cobalt(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Co+2].[O-]S([O-])(=O)=O MEYVLGVRTYSQHI-UHFFFAOYSA-L 0.000 claims description 2
- 239000000356 contaminant Substances 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910003321 CoFe Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- -1 and usually Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Classifications
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
- B01D2259/802—Visible light
Abstract
The invention belongs to the technical field of photocatalytic materials, and particularly discloses a photocatalyst with oxygen defects of cobalt ferrite, and a preparation method and application thereof. Adding iron salt and cobalt salt into deionized water, magnetically stirring, dropwise adding ethylene glycol, and drying to obtain a precursor; grinding the precursor, calcining in an inert gas environment or an air environment, and naturally cooling to obtain the cobalt ferrite photocatalyst with oxygen defects. The oxygen defect of the cobalt ferrite material prepared by the method can activate lattice oxygen to participate in catalytic reaction, and can adsorb and degrade organic pollutants, so that the photocatalytic activity is improved.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a cobalt ferrite photocatalyst with oxygen-containing defects, and a preparation method and application thereof.
Background
In recent years, the problem of environmental pollution has become one of the major problems of global concern, with gaseous pollution always being considered as one of the most serious environmental problems threatening human survival. Among the numerous environmental purification methods, various environmental catalysis techniques such as photocatalysis and electrocatalysis have attracted attention. The photocatalysis technology is an environment-friendly technology, realizes the degradation of gaseous pollutants by utilizing sunlight, and has the characteristics of no secondary pollution, recycling, regeneration and the like.
Cobalt ferrite (CoFe)2O4) The magnetic material has a spinel crystal structure, is a soft magnetic material with excellent performance, has the outstanding advantages of extremely high resistivity and good magnetic spectrum characteristics, and is extremely suitable for application under high frequency and ultrahigh frequency. The characteristics determine the recyclability of the material, and in the aspect of catalysis, the prepared cobalt ferrite nano particles have the remarkable characteristic of fine and uniform particle size. And the semiconductor is a narrow-band gap semiconductor and can absorb most visible light in sunlight. Relevant theoretical calculations and experiments also confirm that oxygen vacancies can increase the surface reactive sites of the material. Therefore, the introduction of oxygen vacancy has important influence on the physicochemical properties of the material, including the electronic structure, the geometrical structure, the light absorption property and the surface adsorption property of the system. Oxygen defects may also enhance catalytic activity. The introduction of oxygen vacancies can also affect the light absorption characteristics and surface adsorption characteristics of the material, and usually, metal atoms of metal oxides have the characteristic of coordination saturation and cannot activate oxygen molecules through chemical adsorption. The construction of the oxygen vacancy defect overcomes the defect and promotes the efficient transfer of the photo-generated electrons from the oxide catalyst to oxygen molecules.
Disclosure of Invention
The invention aims to provide a cobalt ferrite photocatalyst with oxygen-containing defects and a preparation method thereof, and the method is simple, convenient, low in cost, mild in conditions and beneficial to large-scale production.
In order to achieve the purpose, the invention adopts the technical scheme that: the preparation method of the cobalt ferrite photocatalyst with oxygen defects comprises the following steps:
1) adding iron salt and cobalt salt into deionized water, magnetically stirring for 1-2h, aging for 24h, dropwise adding a chelating agent, and drying to obtain a precursor;
2) grinding the precursor, calcining in an inert gas environment or an air environment, and naturally cooling to obtain the cobalt ferrite photocatalyst with oxygen defects.
Preferably, in the above-mentioned cobalt ferrite oxygen-deficient photocatalyst, in step 1), the cobalt salt is cobalt nitrate hexahydrate, cobalt sulfate heptahydrate or cobalt chloride hexahydrate.
Preferably, in the above-mentioned cobalt ferrite oxygen-deficient photocatalyst, in step 1), the iron salt is ferric nitrate nonahydrate or ferric chloride.
Preferably, in the above-mentioned cobalt ferrite oxygen-deficient photocatalyst, in step 1), the molar ratio of cobalt salt to iron salt is 1: 1-2.
Preferably, in the above-mentioned cobalt ferrite oxygen-deficient photocatalyst, in step 1), the chelating agent is ethylene glycol.
Preferably, in the step 2), the calcination temperature is 400-600 ℃, and the calcination time is 2-6 h.
Preferably, in the above-mentioned cobalt ferrite photocatalyst containing oxygen defects, in step 2), the inert gas is nitrogen gas or argon gas.
The invention provides an application of a cobalt ferrite oxygen-containing defect photocatalyst in low-temperature catalytic degradation of gaseous pollutants.
Preferably, the gaseous contaminant is isopropanol.
Preferably, the method is as follows: adding a photocatalyst with oxygen defects of cobalt ferrite into a sealed reaction container, adding isopropanol, and carrying out catalytic degradation under a xenon lamp.
The invention has the beneficial effects that: the invention utilizes iron salt and cobalt salt to prepare the cobalt ferrite catalyst, and constructs a large number of oxygen defect structures, and the oxygen defects can activate lattice oxygen and adsorb organic pollutants, thereby improving the photocatalytic activity. The preparation method provided by the invention has the advantages of cheap raw materials, simple operation, no pollution to the environment, realization of green chemistry and effective degradation of gas pollutants, and greatly reduces the cost.
Drawings
FIG. 1 is an XRD pattern of oxygen-deficient cobalt ferrite photocatalysts prepared in examples 1-5 of the present invention.
FIG. 2 is a graph showing the activity of the photocatalyst for the oxygen defect of cobalt ferrite prepared in examples 1 to 5 of the present invention in degrading isopropanol gas.
Detailed Description
EXAMPLE 1 cobalt ferrite oxygen deficient photocatalyst
The preparation method comprises the following steps
1) 1.455g of cobalt nitrate hexahydrate and 4.04g of ferric nitrate nonahydrate are added into 100ml of deionized water, the mixture is aged for 24h after being magnetically stirred for 1h, then 10ml of ethylene glycol is dropwise added under stirring, and the mixture is dried for 4h at 120 ℃ to obtain a precursor.
2) Grinding the precursor, calcining at 600 ℃ for 4h in an air environment at the heating rate of 5 ℃/min, and then naturally cooling to obtain the photocatalyst with the oxygen-containing defect of the cobalt ferrite, which is marked as A.
EXAMPLE 2 cobalt ferrite oxygen deficient photocatalyst
The preparation method comprises the following steps
1) 1.455g of cobalt nitrate hexahydrate and 4.04g of ferric nitrate nonahydrate are added into 100ml of deionized water, the mixture is aged for 24h after being magnetically stirred for 1h, then 10ml of ethylene glycol is dropwise added under stirring, and the mixture is dried for 4h at 120 ℃ to obtain a precursor.
2) Grinding the precursor, calcining at 400 ℃ for 4h in an air environment at the heating rate of 5 ℃/min, and then naturally cooling to obtain the photocatalyst with the oxygen-containing defect of the cobalt ferrite, which is marked as B.
EXAMPLE 3 cobalt ferrite oxygen deficient photocatalyst
The preparation method comprises the following steps
1) 1.455g of cobalt nitrate hexahydrate and 4.04g of ferric nitrate nonahydrate are added into 100ml of deionized water, the mixture is aged for 24h after being magnetically stirred for 1h, then 10ml of ethylene glycol is dropwise added under stirring, and the mixture is dried for 4h at 120 ℃ to obtain a precursor.
2) Grinding the precursor, calcining at 500 ℃ for 4h in an air environment at the heating rate of 5 ℃/min, and then naturally cooling to obtain the photocatalyst with the oxygen-containing defect of the cobalt ferrite, which is marked as C.
EXAMPLE 4 cobalt ferrite oxygen deficient photocatalyst
The preparation method comprises the following steps
1) 1.455g of cobalt nitrate hexahydrate and 2.02g of ferric nitrate nonahydrate are added into 100ml of deionized water, the mixture is aged for 24h after being magnetically stirred for 1h, then 10ml of ethylene glycol is dropwise added under stirring, and the mixture is dried for 4h at 120 ℃ to obtain a precursor.
2) Grinding the precursor, calcining at 600 ℃ for 4h in an air environment at the heating rate of 5 ℃/min, and then naturally cooling to obtain the photocatalyst with the oxygen-containing defect of the cobalt ferrite, which is marked as D.
EXAMPLE 5 cobalt ferrite oxygen deficient photocatalyst
1) 1.455g of cobalt nitrate hexahydrate and 3.03g of ferric nitrate nonahydrate are added into 100ml of deionized water, the mixture is aged for 24h after being magnetically stirred for 1h, then 10ml of ethylene glycol is dropwise added under stirring, and the mixture is dried for 4h at 120 ℃ to obtain a precursor.
2) Grinding the precursor, calcining at 600 ℃ for 4h in an air environment at the heating rate of 5 ℃/min, and then naturally cooling to obtain the photocatalyst with oxygen-containing defects of cobalt ferrite, which is marked as E.
FIG. 1 is an XRD test chart of the photocatalyst containing oxygen defects of cobalt ferrite prepared in examples 1 to 5. As can be seen from FIG. 1, the successful synthesis of CoFe was demonstrated by comparing it with a standard card2O4A material.
Example 6 application
The oxygen-deficient photocatalyst of cobalt ferrite prepared in examples 1 to 5 was placed at 4cm in length2In the glass groove, the glass groove loaded with the photocatalyst is respectively placed into 224ml reactors containing atmospheric pressure air, 5ul of isopropanol liquid is finally injected into the reactors, the reactors are heated by illumination of a 300W xenon lamp, timing is started after 10min, and a needle is drawn out of the samples every 20 min for testing. The acetone produced was subjected to gas chromatography using a FID detector (GC1690, Jiedo technologies, Ltd.). After the reaction was completed, the reactor was cooled to room temperature, and the catalyst was collected for further characterization.
FIG. 2 is a comparison graph of activities of cobalt ferrite oxygen-deficient photocatalysts prepared in examples 1 to 5 for degrading isopropanol gas, and it can be seen that all the prepared photocatalysts can effectively degrade isopropanol, and it is obvious that photocatalyst D prepared in example 4 has the highest photocatalytic activity, which is about 2.12 times of the rate of degrading isopropanol by photocatalyst A prepared in example 1, photocatalyst B prepared in example 2 is about 1.92 times of the rate of degrading isopropanol by photocatalyst A prepared in example 1, photocatalyst C prepared in example 3 is about 2.02 times of the rate of degrading isopropanol by photocatalyst A prepared in example 1, and photocatalyst E prepared in example 5 is about 1.93 times of the rate of degrading isopropanol by photocatalyst A prepared in example 1, because there are a large number of oxygen defects, which can not only activate lattice oxygen to participate in catalytic reaction, but also can adsorb and degrade organic pollutants, thereby improving the photocatalytic activity.
Claims (10)
1. The cobalt ferrite photocatalyst with oxygen defects is characterized by comprising the following steps:
1) adding iron salt and cobalt salt into deionized water, magnetically stirring for 1-2h, aging for 24h, dropwise adding a chelating agent, and drying to obtain a precursor;
2) grinding the precursor, calcining in an inert gas environment or an air environment, and naturally cooling to obtain the cobalt ferrite photocatalyst with oxygen defects.
2. The cobalt ferrite oxygen deficient photocatalyst of claim 1 wherein in step 1) said cobalt salt is cobalt nitrate hexahydrate, cobalt sulfate heptahydrate or cobalt chloride hexahydrate.
3. The cobalt ferrite oxygen deficient photocatalyst of claim 1 wherein in step 1) the iron salt is ferric nitrate nonahydrate or ferric chloride.
4. The cobalt ferrite oxygen-deficient photocatalyst according to claim 1, wherein in step 1), the molar ratio of cobalt salt to iron salt is 1: 1-2.
5. The cobalt ferrite oxygen deficient photocatalyst of claim 1 wherein in step 1) said chelating agent is ethylene glycol.
6. The cobalt ferrite oxygen-deficient photocatalyst as set forth in claim 1, wherein in the step 2), the calcination is carried out at a temperature of 400-600 ℃ for a period of 2-6 h.
7. The cobalt ferrite oxygen deficient photocatalyst of claim 1 wherein in step 2) the inert gas is nitrogen gas or argon gas.
8. Use of the cobalt ferrite oxygen deficient photocatalyst according to any one of claims 1 to 7 for the low temperature catalytic degradation of gaseous pollutants.
9. The use of claim 8, wherein the gaseous contaminant is isopropanol.
10. Use according to claim 9, characterized in that the method is as follows: adding the cobalt ferrite oxygen-containing defect photocatalyst of any one of claims 1 to 7 into a sealed reaction vessel, adding isopropanol, and catalyzing and degrading under a xenon lamp.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114558561A (en) * | 2022-03-15 | 2022-05-31 | 辽宁大学 | Preparation method and application of zinc titanate oxygen-containing defect photocatalyst |
| CN116618051A (en) * | 2023-06-06 | 2023-08-22 | 中国计量大学 | Oxygen-defect-containing cobalt ferrite nanorod and preparation method and application thereof |
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2021
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114558561A (en) * | 2022-03-15 | 2022-05-31 | 辽宁大学 | Preparation method and application of zinc titanate oxygen-containing defect photocatalyst |
| CN114558561B (en) * | 2022-03-15 | 2023-12-08 | 辽宁大学 | Preparation method and application of zinc titanate oxygen-containing defect photocatalyst |
| CN116618051A (en) * | 2023-06-06 | 2023-08-22 | 中国计量大学 | Oxygen-defect-containing cobalt ferrite nanorod and preparation method and application thereof |
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