CN107617435A - A kind of SrTiO3Titanium oxide nanotubes heterojunction photocatalyst of load and its preparation method and application - Google Patents
A kind of SrTiO3Titanium oxide nanotubes heterojunction photocatalyst of load and its preparation method and application Download PDFInfo
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- CN107617435A CN107617435A CN201711050897.9A CN201711050897A CN107617435A CN 107617435 A CN107617435 A CN 107617435A CN 201711050897 A CN201711050897 A CN 201711050897A CN 107617435 A CN107617435 A CN 107617435A
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Abstract
The invention provides a kind of SrTiO3Titanium oxide nanotubes heterojunction photocatalyst of load and its preparation method and application, the wherein photochemical catalyst are prepared with the following method:1) electrolyte, is added in plastic containers, applies 15 25V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches 5 15h, being warming up to 350 800 DEG C and 1 3h of calcining with 38 DEG C/min programming rate obtains titania nanotube array;2), the titanium oxide nanotubes prepared are put into the water heating kettle containing finite concentration precursor liquid, are put into baking oven with 100 300 DEG C of the 15h of thermotonus 5;3) and then with 0.1M hydrochloric acid clean, 3 5h are calcined under the conditions of 300 800 DEG C and obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Description
Technical field
The invention belongs to catalyst technical field, and in particular to a kind of SrTiO3The titanium oxide nanotubes hetero-junctions light of load
Catalyst and its preparation method and application.
Background technology
With the growth of demographic and economic, environment and energy problem turn into the two big factors for restricting human development.Semiconductor
Photochemical catalyst is in reduction CO2Aspect has unique advantage, can be by CO2Energy fuel is converted into, while alleviates environment and energy danger
Machine.With conventional process photo catalytic reduction CO2Compare, photoelectrocatalysis reduction CO2Light induced electron and hole, table can quickly be separated
Reveal preferable catalytic efficiency.
Existing SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load is also to be synthesized with easy hydrothermal method,
The material prepared mainly has following deficiency:1. existing Hydrothermal Synthesiss SrTiO3The titanium oxide nanotubes hetero-junctions light of load is urged
Change mainly exists in powder form, and it prepares cumbersome, and utilization rate is low, it is difficult to repeatedly uses.2. existing SrTiO3It is negative
The titanium oxide nanotubes heterojunction photocatalyst of load mainly reduces CO in photocatalytic system2, catalytic efficiency is low, catalytic activity
It is poor.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of SrTiO3The titanium oxide nanotubes hetero-junctions light of load
Catalyst.
Its technical problem to be solved can be implemented by the following technical programs.
A kind of SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load, its feature are that the photochemical catalyst is using such as
It is prepared by lower section method:
1) electrolyte, is added in plastic containers, using titanium sheet as anode, platinized platinum applies 15-25V electricity as negative electrode
Pressure, 5-15h is etched, 350-800 DEG C is warming up to 3-8 DEG C/min programming rate and calcines 1-3h and obtain titanium oxide nanotubes battle array
Row;
2), the titanium oxide nanotubes prepared are put into the water heating kettle containing finite concentration precursor liquid, be put into baking oven with
100-300 DEG C of thermotonus 5-15h;
3) and then with 0.1M hydrochloric acid clean, 3-5h is calcined under the conditions of 300-800 DEG C and obtains SrTiO3The titanium oxide of load
Nano tube hetero-junction photochemical catalyst.
As the further improvement of the technical program, plastic containers are beaker, and described electrolyte is 30ml0.2MH3PO4
And 30ml0.4MNH4F mixed solution.
As one of the preferred embodiments of the present invention, the precursor liquid is 0.04M Sr (OH)2Solution.
One of another preferred embodiment as the present invention, the voltage applied in step 1) is 20V.
Also serve as the further improvement of the technical program, the preparation condition of titania nanotube array is with 5 in step 1)
DEG C/min programming rate is warming up to 450 DEG C of calcining 2h.
The preferred embodiments of the present invention equally are used as, in an oven with 150 DEG C of thermotonus 10h.
In addition, sintering temperature last in step 3) is 600 DEG C.
Another technical problem to be solved by this invention is to provide a kind of SrTiO3The titanium oxide nanotubes of load are heterogeneous
The preparation method of photochemical catalyst is tied, it comprises the following steps:
1) electrolyte, is added in plastic containers, using titanium sheet as anode, platinized platinum applies 15-25V electricity as negative electrode
Pressure, 5-15h is etched, 350-800 DEG C is warming up to 3-8 DEG C/min programming rate and calcines 1-3h and obtain titanium oxide nanotubes battle array
Row;
2), the titanium oxide nanotubes prepared are put into the water heating kettle containing finite concentration precursor liquid, be put into baking oven with
100-300 DEG C of thermotonus 5-15h;
3) and then with 0.1M hydrochloric acid clean, 3-5h is calcined under the conditions of 300-800 DEG C.
Another technical problem to be solved by this invention is to provide a kind of titanium oxide nanotubes of foregoing SrTiO3 loads
Heterojunction photocatalyst reduces CO in the photoelectrocatalysis that light anode drives2Application process.
Technical scheme of the present invention compared with prior art, has advantages below and prominent effect:Above-mentioned technical proposal
Used in chemical reagent be common agents, it is cheap and easy to get, method technique is simple, can with it is large batch of production and can
Repeatedly utilize.Meanwhile the photochemical catalyst is used for the photoelectrocatalysis reduction CO of light anode driving2Preferably catalysis is shown to live
Property.
The present invention be using titanium sheet as electrode slice made of substrate, and as light anode be applied to photoelectrocatalysis reduction two
In the system of carbonoxide.First, titanium oxide be in the form of nanotube present, the pattern can preferably improve catalytic efficiency from
And improve catalytic activity.Secondly compared to the SrTiO reported in existing literature3The titanium dioxide powder system of load, party's legal system
The electrode slice preparation process obtained is easier, there is the repeatable utilization of good chemical stability and non-secondary pollution.Last SrTiO3
The titanium oxide nanotubes heterojunction photocatalyst of load mostly be applied to the full decomposition water of photocatalysis in, the technical program prove its
Also preferably activity and catalytic efficiency are shown in carbon dioxide reduction.
Technical scheme of the present invention compared with prior art, has advantages below and prominent effect:Above-mentioned technical proposal
Used in chemical reagent be common agents, it is cheap and easy to get, method technique is simple, and can be with large batch of production.Together
When, the photochemical catalyst is used for photoelectrocatalysis reduction CO2When have very high activity.
Brief description of the drawings
Fig. 1 is obtained best sample SrTiO3The X of the titanium oxide nanotubes heterojunction photocatalyst sample of load is penetrated
Ray diffraction diagram is composed;
Fig. 2 is obtained best sample SrTiO3The titanium oxide nanotubes heterojunction photocatalyst sample section of load
High resolution scanning electron microscope;
Fig. 3 is obtained best sample SrTiO3The titanium oxide nanotubes heterojunction photocatalyst sample plane of load
High resolution scanning electron microscope;Fig. 4 is obtained best sample SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load
Scheme outside the solid violet of sample;
Fig. 5 is obtained best sample SrTiO3The not spy of the titanium oxide nanotubes heterojunction photocatalyst sample of load
Schottky curve;
Fig. 6 is pure titanium oxide nanotubes photochemical catalyst sample, pure SrTiO3Photochemical catalyst sample and obtained
Best sample SrTiO3The titanium oxide nanotubes heterojunction photocatalyst sample of load is at different temperatures by CO2Reduce formic acid
Active testing figure;
Fig. 7 is sample SrTiO3The photoelectricity of the titanium oxide nanotubes heterojunction photocatalyst sample light anode driving of load is urged
Change reduction CO2The application apparatus figure of active testing.
Embodiment
Below in conjunction with the accompanying drawings and the technical characterstic of the present invention is expanded on further in specific embodiment.
The defects of it is an object of the invention to for present in prior art and meet market needs, there is provided a kind of SrTiO3
The titanium oxide nanotubes heterojunction photocatalyst preparation method of load, it is low and can be with that it prepares simple and easy, the high cost of yield
Produce in enormous quantities.
The concrete technical scheme of the present invention is as follows:
A kind of SrTiO3The preparation method of the titanium oxide nanotubes heterojunction photocatalyst of load, comprises the following steps:
Presoma is added in water heating kettle, titanium oxide nanotubes are put into kettle, 300-800 is warming up to 3-8 DEG C/min programming rate
DEG C calcining 3-5h, is then rinsed with 0.1M hydrochloric acid, obtains a kind of SrTiO3The titanium oxide nanotubes heterojunction photocatalysis of load
Agent.
The SrTiO provided3The titanium oxide nanotubes heterojunction photocatalyst of load, using Sr (OH)2Solution is forerunner
Body, and the use of titania nanotube array is substrate, synthesized under different calcining heats, gained catalyst has efficient photoelectricity treater
Catalysis reduction CO2Performance.
Its efficient CO being related to2The preparation method of photoelectric is reduced, specially with a certain amount of presoma and oxidation
Titanium nano-tube array is put into water heating kettle reaction and synthesis is calcined in Muffle furnace, gained catalyst with ultraviolet light with
Photoelectrocatalysis CO2It is restored to the performance of formic acid.
Therefore we utilize perovskite SrTiO3Relatively negative conduction band positions (- 1.2eV) modification titania nanotube array, structure
Into hetero-junctions there is good reduction CO2Ability, CO is reduced in photoelectrocatalysis2On have very big application prospect, can apply to
In solar cell.
Product prepared by the present invention carries out structural characterization by the following means:Using in Rigaku RigakuD/Max-RB
The X-ray diffraction measured on type X-ray diffractometer carries out the structural analysis of sample;Scanned using Japanese JEOLJSM-6380LV types
The stereoscan photograph that Electronic Speculum obtains, using domestic CHI660E mornings China's electrochemical workstation.
It is making further detailed, clear and complete description of how realizing to the present invention with reference to specific embodiment, institute
Row embodiment is only further described to the present invention, not thereby limiting the invention:
Embodiment 1:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
3h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.04M Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then use
0.1M hydrochloric acid cleans, and 600 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Embodiment 2:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
5h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.04M Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then use
0.1M hydrochloric acid cleans, and 600 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Embodiment 3:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
7h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.04M Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then use
0.1M hydrochloric acid cleans, and 600 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Embodiment 4:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
9h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.04M Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then use
0.1M hydrochloric acid cleans, and 600 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Embodiment 5:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
11h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.04M Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then use
0.1M hydrochloric acid cleans, and 600 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Embodiment 6:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
7h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.02M Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then use
0.1M hydrochloric acid cleans, and 600 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Embodiment 7:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
7h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.03M Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then use
0.1M hydrochloric acid cleans, and 600 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Embodiment 8:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
7h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.05M Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then use
0.1M hydrochloric acid cleans, and 600 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Embodiment 9:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
7h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.06M S Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then
Cleaned with 0.1M hydrochloric acid, 600 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Embodiment 10:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
7h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.04M Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then use
0.1M hydrochloric acid cleans, and 450 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Embodiment 11:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
7h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.04M Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then use
0.1M hydrochloric acid cleans, and 600 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
Embodiment 12:
Electrolyte is added in plastic beaker, applies 20V voltage as negative electrode using titanium sheet as anode, platinized platinum, etches
7h, is warming up to 450 DEG C and is calcined 2h and obtain titania nanotube array with 5 DEG C/min programming rate.Then will prepare
Titanium oxide is put into containing 0.04M Sr (OH)2In the water heating kettle of solution, baking oven is put into 150 DEG C of thermotonus 10h.Then use
0.1M hydrochloric acid cleans, and 750 DEG C of roasting 2h obtain SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load.
As shown in drawings, Fig. 1 is obtained best sample SrTiO3The titanium oxide nanotubes heterojunction photocatalysis of load
The X ray diffracting spectrum of agent sample, as seen from the figure SrTiO3Synthesis.
Fig. 2 is obtained best sample SrTiO3The titanium oxide nanotubes heterojunction photocatalyst sample section of load
High resolution scanning electron microscope, as seen from the figure SrTiO3It is well-proportioned to be distributed in TiO2On nanotube.
Fig. 3 is obtained best sample SrTiO3The titanium oxide nanotubes heterojunction photocatalyst sample plane of load
High resolution scanning electron microscope, as seen from the figure SrTiO3Block distribution is presented in TiO2On nanotube.
Fig. 4 is obtained best sample SrTiO3The solid of the titanium oxide nanotubes heterojunction photocatalyst sample of load
Ultraviolet figure, the energy gap of the material is 3.4eV as seen from the figure.
Fig. 5 is obtained best sample SrTiO3The not spy of the titanium oxide nanotubes heterojunction photocatalyst sample of load
Schottky curve, the conduction band positions of the material are -1.2eV as seen from the figure.
Fig. 6 is obtained best sample SrTiO3The titanium oxide nanotubes heterojunction photocatalyst sample CO of load2Reduction
The active testing figure of formic acid at different temperatures, as seen from the figure when sintering temperature is 600 DEG C, activity is optimal.
Fig. 7 is sample SrTiO3The application apparatus of the titanium oxide nanotubes heterojunction photocatalyst sample activity test of load
Figure, the sample is reacted as light anode, copper foam as negative electrode as seen from the figure.
The invention provides a kind of easy hydrothermal synthesis method to be prepared for SrTiO3It is supported on TiO2It is heterogeneous on nanotube
Knot.During preparation, first using titanium sheet as substrate, Nano tube array of titanium dioxide is etched by the method for anodic oxidation and roasted
Burn.The TiO that will be prepared2Nanotube is put into the water heating kettle containing presoma, and reaction a few hours are finally in Muffle furnace high temperature
Roasting forms the SrTiO using titanium sheet as substrate3/TiO2Hetero-junctions.The catalyst of gained under the action of uv light, utilizes light
Electrocatalysis device, using material as light anode material to CO2Reduced to obtain product formic acid.The present invention uses the synthesis of hydro-thermal
Method, the photochemical catalyst of ultraviolet light response is obtained in Muffle kiln roasting, in photoelectrocatalysis CO2Middle display preferably activity.This
Class method for preparing catalyst is simple, and the large batch of production of energy, and pollution, extensive use will not be produced to environment in preparation process
In fields such as solar cell, antibacterial and photocatalysis pollutant processes.
Described above is presently preferred embodiments of the present invention, but the present invention should not be limited to disclosed in the embodiment
Content.So every do not depart from the equivalent or modification completed under principles of this disclosure, the model that the present invention protects is both fallen within
Enclose.
Claims (9)
- A kind of 1. SrTiO3The titanium oxide nanotubes heterojunction photocatalyst of load, it is characterised in that the photochemical catalyst is using as follows It is prepared by method:1) electrolyte, is added in plastic containers, applies 15-25V voltage as negative electrode using titanium sheet as anode, platinized platinum, carves 5-15h is lost, 350-800 DEG C is warming up to 3-8 DEG C/min programming rate and calcines 1-3h and obtain titania nanotube array;2), the titanium oxide nanotubes prepared are put into the water heating kettle containing finite concentration precursor liquid, are put into baking oven with 100- 300 DEG C of thermotonus 5-15h;3) and then with 0.1M hydrochloric acid clean, 3-5h is calcined under the conditions of 300-800 DEG C and obtains SrTiO3The TiOx nano of load Pipe heterojunction photocatalyst.
- 2. SrTiO according to claim 13The titanium oxide nanotubes heterojunction photocatalyst of load, it is characterised in that institute It is beaker to state plastic containers, and described electrolyte is 30ml0.2MH3PO4And 30ml0.4MNH4F mixed solution.
- 3. SrTiO according to claim 13The titanium oxide nanotubes heterojunction photocatalyst of load, it is characterised in that institute State the Sr (OH) that precursor liquid is 0.04M2Solution.
- 4. SrTiO according to claim 13The titanium oxide nanotubes heterojunction photocatalyst of load, it is characterised in that step It is rapid 1) applied in voltage be 20V.
- 5. SrTiO according to claim 13The titanium oxide nanotubes heterojunction photocatalyst of load, it is characterised in that step It is rapid 1) in titania nanotube array preparation condition be with 5 DEG C/min programming rate be warming up to 450 DEG C calcining 2h.
- 6. SrTiO according to claim 13The titanium oxide nanotubes heterojunction photocatalyst of load, it is characterised in that With 150 DEG C of thermotonus 10h in baking oven.
- 7. SrTiO according to claim 13The titanium oxide nanotubes heterojunction photocatalyst of load, it is characterised in that step It is rapid 3) in last sintering temperature be 600 DEG C.
- A kind of 8. SrTiO3The preparation method of the titanium oxide nanotubes heterojunction photocatalyst of load, it is characterised in that including as follows Step:1) electrolyte, is added in plastic containers, applies 15-25V voltage as negative electrode using titanium sheet as anode, platinized platinum, carves 5-15h is lost, 350-800 DEG C is warming up to 3-8 DEG C/min programming rate and calcines 1-3h and obtain titania nanotube array;2), the titanium oxide nanotubes prepared are put into the water heating kettle containing finite concentration precursor liquid, are put into baking oven with 100- 300 DEG C of thermotonus 5-15h;3) and then with 0.1M hydrochloric acid clean, 3-5h is calcined under the conditions of 300-800 DEG C.
- 9. SrTiO described in any claim in claim 1 to 73The titanium oxide nanotubes heterojunction photocatalyst of load is in light The photoelectrocatalysis reduction CO of anode drive2Application.
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CN109569593A (en) * | 2018-11-29 | 2019-04-05 | 全球能源互联网研究院有限公司 | A kind of analysis oxygen elctro-catalyst of strontium doping metal oxide containing precious metals and preparation method thereof |
CN115779895A (en) * | 2022-11-08 | 2023-03-14 | 清华大学 | Perovskite type catalyst and preparation method and application thereof |
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Cited By (6)
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CN108479811A (en) * | 2018-03-27 | 2018-09-04 | 辽宁大学 | A kind of Z-type sound catalyst and its preparation method and application of degradation antibiotic waste water |
CN108479811B (en) * | 2018-03-27 | 2021-01-08 | 辽宁大学 | Z-shaped acoustic catalyst for degrading antibiotic wastewater and preparation method and application thereof |
CN109569593A (en) * | 2018-11-29 | 2019-04-05 | 全球能源互联网研究院有限公司 | A kind of analysis oxygen elctro-catalyst of strontium doping metal oxide containing precious metals and preparation method thereof |
CN109569593B (en) * | 2018-11-29 | 2021-05-28 | 全球能源互联网研究院有限公司 | Oxygen evolution electrocatalyst of strontium-doped noble metal oxide and preparation method thereof |
CN115779895A (en) * | 2022-11-08 | 2023-03-14 | 清华大学 | Perovskite type catalyst and preparation method and application thereof |
CN115779895B (en) * | 2022-11-08 | 2024-04-30 | 清华大学 | Perovskite catalyst and preparation method and application thereof |
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