CN110054215A - Morphology controllable SrTiO3The preparation and its application of flower ball-shaped serial nano material - Google Patents
Morphology controllable SrTiO3The preparation and its application of flower ball-shaped serial nano material Download PDFInfo
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- CN110054215A CN110054215A CN201910214470.0A CN201910214470A CN110054215A CN 110054215 A CN110054215 A CN 110054215A CN 201910214470 A CN201910214470 A CN 201910214470A CN 110054215 A CN110054215 A CN 110054215A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002086 nanomaterial Substances 0.000 title description 4
- 229910002367 SrTiO Inorganic materials 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 10
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- APQHKWPGGHMYKJ-UHFFFAOYSA-N Tributyltin oxide Chemical compound CCCC[Sn](CCCC)(CCCC)O[Sn](CCCC)(CCCC)CCCC APQHKWPGGHMYKJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 238000009415 formwork Methods 0.000 claims 1
- 230000002045 lasting effect Effects 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 238000005287 template synthesis Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 14
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 238000004886 process control Methods 0.000 abstract 1
- 238000005556 structure-activity relationship Methods 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 7
- 239000004098 Tetracycline Substances 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- 229960002180 tetracycline Drugs 0.000 description 6
- 229930101283 tetracycline Natural products 0.000 description 6
- 235000019364 tetracycline Nutrition 0.000 description 6
- 150000003522 tetracyclines Chemical class 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 238000001338 self-assembly Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000000243 photosynthetic effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000009418 renovation Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
-
- B01J35/39—
-
- B01J35/40—
-
- B01J35/51—
-
- B01J35/61—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The present invention relates to a kind of formation flower ball-shaped SrTiO3The preparation method of photochemical catalyst, step are related to no template without using in the case where organic template, synthesize to green high-efficient the flower-shaped SrTiO of morphology controllable3Catalysis material.The beneficial effects of the present invention are:, by simple hydro-thermal method, the modulation reaction time has obtained a series of SrTiO of different surface morphologies in the case where not adding any surfactant and template3Catalysis material has studied its structure-activity relationship by light-catalyzed reaction while realizing self assembling process control.
Description
Technical field
The invention belongs to nano material preparation and applied technical fields, are related to the flower ball-shaped series SrTiO of morphology controllable3Light
The controllable preparation and application of catalyst.
Background technique
In in the past few decades, people increasingly increase the worry of global environmental pollution and fossil energy shortage, this draws
The numerous studies explored to advanced methods such as environmental improvement and energy conversions are sent out.Light-catalysed first was reported in 1972
TiO2Electrode water splitting processes, numerous attentions have been focused into photocatalysis technology to environmental renovation and energy conversion etc..
By years of researches, photocatalysis has been considered as an economic and environmental-friendly technology, which can be adapted for dirt
Dye purification, Driven by Solar Energy water decomposition and CO 2It reduces and organic photosynthetic acts on.
In the photochemical catalyst reported, strontium titanates (SrTiO3) be used as typical perovskite structural material due to its structure
Flexibility, good stability, hypotoxicity and effective photocatalytic activity and be widely studied.However, SrTiO3Broadband
Gap (about 3.2eV) limits its application in the photocatalytic pollutant degradation or water decomposition of visible optical drive.Therefore, many
The emphasis of research report is to improve its visible light capture ability, including energy band engineering, and form control is multiple with narrow gap semiconductor
It closes, surface treatment etc..
In general, the photocatalytic activity of photochemical catalyst is heavily dependent on their form, microstructure and composition.Most
Closely, the broad interest of scientific circles is caused by three-dimensional (3D) layered structure that nanostructures assemble, because they are with many excellent
Point: (1) large specific surface area, usually reaction provides a large amount of reaction sites;(2) highly developed porous structure, usually as anti-
Answer the approach of diffusion and the transport of object and product;(3) resistant to aggregation ability is received since the stability of material on a microscopic scale is higher than
Metrical scale;(4) since size layered is greater than its component, there is good separability, to realize good
Recyclability;(5) benefit of building blocks is kept;(6) by the multiple reflections of the light in middle layer layered and scattering come
Enhance light capture ability.Up to the present, it has been proposed that many strategies synthesize various layered structures, such as template, electrostatic
Spinning technique, self-assembly method and topochemistry conversion.In above-mentioned strategy, self assembly is the most simple side for constructing layered architecture
Method.
In view of factors above, the SrTiO that easy hot solvent method has synthesized flower ball-shaped is utilized in we3, and pass through letter
The forming process regulated and controled to observe bouquet in single reaction time, and to the SrTiO under its different conditions3Performance has been carried out to grind
Study carefully.
Summary of the invention
The technical problem to be solved by the present invention is to develop a kind of environment-friendly and green efficiently to synthesize SrTiO3The conjunction of catalysis material
At method, and explore its controllable preparation process and photocatalytic applications prospect.
Based on the above issues, the present invention mainly realizes under the conditions of Template-free method, and green high-efficient prepares SrTiO3Light is urged
The research work of agent, especially for self assembling process research in terms of be made that and valuably explore, material preparation aspect, tool
Body includes following committed step:
After mixing, 20 mL strontium nitrate aqueous solutions are added, most in the ethylene glycol of 25 mL and 3.40 mL butyl titanates (TBOT)
The NaOH of 15 mL is added afterwards, reaction system continuous slow is stirred and is uniformly dissolved with reaching.Then, solution is moved on into 100 mL
Polytetrafluoroethyllining lining hydrothermal reaction kettle in, preheat to be warming up at 200 DEG C after 0.5 h at 100 DEG C and carry out reaction t hours,
Reaction time t is variable;
Further, the concentration of strontium nitrate solution is 0.5 M in the step, and the concentration of NaOH is 5 M;
Further, after NaOH solution being added in the step, continuing mixing time is 1 h;
Further, hydro-thermal time t is respectively 12 h, 24 h, 36 h, 48 h in the step.
Further, it is unreacted miscellaneous that the series catalyst agent material passes through ethyl alcohol, deionized water replaces washing removal
Matter notices that water-washing process is avoided using ultrasonic treatment, to keep flower-like structure as far as possible.Flower-shaped SrTiO is obtained after drying3Light is urged
Agent.
The catalytic performance of series flower shape catalyst material mainly passes through photocatalytic degradation tetracycline and is characterized, according to
Following step carries out:
It weighs 20 mg catalyst and is put into light and urge in pipe, 50 mL, 30 mg/L tetracycline is added, uses 500 W mercury lamps as light
Source carries out photocatalytic degradation reaction.Dark reaction time is 60 min, and every 10 min takes time sample after illumination, is centrifuged, is then surveyed
Its absorbance.
The beneficial effects of the present invention are: (1) the preparation synthesis process is completely avoided using surfactant, self assembly
Journey is completed by itself crystal self assembling process, is had the characteristics that environmentally protective;(2) preparation condition method is relatively simple, passes through
Reaction time modulation is easy to control and produces in batches;(3) light prepared by is urged in micron level, and being easily recycled property repeats to make
With;(4) catalyst has specific surface abundant, and catalytic efficiency is higher, is subject to as a kind of ideal catalyst carrier into one
Walk research and utilization.
Detailed description of the invention
The following further describes the present invention with reference to the drawings.
Fig. 1 is the SrTiO after 12 h of hydro-thermal that the embodiment of the present invention 1 is prepared3Nano particle;
Fig. 2 is the SrTiO after 24 h that the embodiment of the present invention 1 is prepared3Petal;
Fig. 3 is the SrTiO after 36 h that the embodiment of the present invention 1 is prepared3Flower cage;
Fig. 4,5 are SrTiO after 48 h that the embodiment of the present invention 1 is prepared3Bouquet;
Fig. 6 is the SrTiO under the different hydro-thermal times that the embodiment of the present invention 1 is prepared3 XRD diagram;
Fig. 7 is the SrTiO for the different the hydro-thermal reaction times that the embodiment of the present invention 1 is prepared3Photocatalyst for degrading tetracycline
Concentration is with light application time variation diagram.
Specific embodiment
Presently in connection with specific embodiment, the invention will be further described, following embodiment be intended to illustrate invention rather than
Limitation of the invention further.
After mixing, 20 mL nitre are added in the ethylene glycol of embodiment 1:25 mL and 3.40 mL butyl titanates (TBOT)
Sour strontium aqueous solution, is eventually adding the NaOH of 15 mL, and reaction system is continued stirring to reach uniform.Later, solution is moved on to
In the hydrothermal reaction kettle of 100 mL, certain time is kept at 200 DEG C.
As shown in the surface sweeping electron microscope of Fig. 1,2,3,4,5, the SrTiO of present embodiment preparation3Photochemical catalyst is in different water
Final product micron order flower ball-shaped SrTiO is finally obtained to the formation of flower cage from nano particle to petal under conditions of the hot time3,
There is no the addition of additional template and organic solvent in entire reaction process, passes through simple and environmentally-friendly hydrothermal method, regulation
The SrTiO under several typical product patterns (especially different sizes and surface topography) can be obtained in reaction time3Photocatalysis
Agent material.
Flower-shaped SrTiO prepared by embodiment 13The crystal phase structure of photochemical catalyst by 2500 PC of Rigaku D/max from
Turn x-ray diffractometer analysis, wherein X-ray is Cu target K α (λ=1.54056), 40 kV of voltage, 100 mA of electric current, and step-length is
0.02 °, 5 ° ~ 80 ° of scanning range.X ray diffracting spectrum as shown in fig. 6, with the hydro-thermal time increase, serial SrTiO3Material
Diffraction maximum gradually increase.Therefore, the modulation in reaction time can not only have an impact for the exterior appearance of product, to product
Also different effect degrees is produced on crystal crystallization degree, this may be because crystal not only has occurred in water-heat process
Growth and assembling process, also have occurred inorganic crystal material gradually to single crystallization change process.
This patent is for prepared serial flower ball-shaped SrTiO3Material has done preliminary Photocatalytic Degradation Property research.Tool
Body is as follows: the flower-shaped SrTiO that will be prepared in embodiment 13Photochemical catalyst is for tetracycline of degrading, and wherein tetracycline is dense
Degree is 20 mg/L, takes 20 mg of catalyst, first 60 min of dark reaction that solution is made to reach adsorption-desorption balance, then carry out ultraviolet light and urge
Change reaction, using 500 W mercury lamps as light source, extracts 3 mL reaction solutions in centrifuge tube every 10 min dropper, be put into height
After being centrifuged 3 min in fast centrifuge, supernatant is taken, with its photocatalytic degradation effect of ultraviolet specrophotometer measurement & characterization.Fig. 7 is
SrTiO3The degradation rate curve graph of the degradation tetracycline under uv light irradiation of material.7 it can be known by figure, the self assembly of bouquet
The exterior appearance of direct modulation product is capable of in the reaction time control of process, and then can be realized for flower-shaped SrTiO3Material
The preliminary screening of photocatalysis performance.
Claims (5)
1. a kind of morphology controllable flower ball-shaped SrTiO3Catalyst without template synthesis method: the ethylene glycol of 25 mL and 3.40 mL
TBOT after mixing, be added 20 mL strontium nitrate aqueous solutions, be eventually adding the NaOH of 15 mL, by reaction system continue stirring with
Reach uniformly, solution is moved on in the hydrothermal reaction kettle of 100 mL, modulation reaction time t at 200 DEG C.
2. SrTiO according to claim 13Photochemical catalyst preparation method, feature first is that: nitric acid in the step
The concentration of strontium solution is 0.5 M, and the concentration of NaOH is 5 M.
3. SrTiO according to claim 13Photochemical catalyst preparation method, feature first is that: whole synthesis processes do not make
With any organic formwork agent or pattern controlling agent.
4. SrTiO according to claim 13Photochemical catalyst preparation method, feature first is that: be added in the step
Lasting mixing time after NaOH is 1 h.
5. SrTiO according to claim 13Photochemical catalyst preparation method, feature first is that: hydro-thermal in the step
Time t is respectively 12 h, 24 h, 36 h, 48 h.
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CN201910214470.0A CN110054215A (en) | 2019-03-20 | 2019-03-20 | Morphology controllable SrTiO3The preparation and its application of flower ball-shaped serial nano material |
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CN201910214470.0A CN110054215A (en) | 2019-03-20 | 2019-03-20 | Morphology controllable SrTiO3The preparation and its application of flower ball-shaped serial nano material |
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Cited By (3)
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CN111495352A (en) * | 2020-04-27 | 2020-08-07 | 昆明理工大学 | Method for efficiently carrying out photocatalytic oxidation on elemental mercury through metal doping modification of strontium titanate |
CN112058289A (en) * | 2020-06-23 | 2020-12-11 | 四川大学 | Strontium titanate/strontium carbonate heterojunction photocatalyst and preparation method and application thereof |
CN113797910A (en) * | 2020-06-16 | 2021-12-17 | 中国科学院化学研究所 | Defect-containing nano microspheric perovskite catalyst and preparation method and application thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111495352A (en) * | 2020-04-27 | 2020-08-07 | 昆明理工大学 | Method for efficiently carrying out photocatalytic oxidation on elemental mercury through metal doping modification of strontium titanate |
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CN113797910A (en) * | 2020-06-16 | 2021-12-17 | 中国科学院化学研究所 | Defect-containing nano microspheric perovskite catalyst and preparation method and application thereof |
CN113797910B (en) * | 2020-06-16 | 2023-06-16 | 中国科学院化学研究所 | Defect-containing nano microspherical perovskite catalyst and preparation method and application thereof |
CN112058289A (en) * | 2020-06-23 | 2020-12-11 | 四川大学 | Strontium titanate/strontium carbonate heterojunction photocatalyst and preparation method and application thereof |
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