CN105529404B - A kind of organic solar batteries with two-dimensional nano bowl array light trapping structure and preparation method thereof - Google Patents
A kind of organic solar batteries with two-dimensional nano bowl array light trapping structure and preparation method thereof Download PDFInfo
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- CN105529404B CN105529404B CN201510955864.3A CN201510955864A CN105529404B CN 105529404 B CN105529404 B CN 105529404B CN 201510955864 A CN201510955864 A CN 201510955864A CN 105529404 B CN105529404 B CN 105529404B
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
- H10K30/151—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising titanium oxide, e.g. TiO2
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/80—Constructional details
- H10K30/87—Light-trapping means
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/18—Deposition of organic active material using non-liquid printing techniques, e.g. thermal transfer printing from a donor sheet
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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
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
The invention belongs to polymer solar battery technical field, and in particular to a kind of two-dimentional bowl array light trapping structure organic solar batteries based on nano hot stamping technology and preparation method thereof, this method specifically includes:TiO is prepared using PS beads template and sol-gal process2Two-dimensional nano bowl array masterplate, light trapping structure masterplate is used as by the use of two-dimensional nano bowl array, equally distributed two-dimensional nano bowl array is directly imprinted out on active layer by nano marking press, this method innovation quickly prepares impression formboard using PS bead combination colloidal sol coagulations, not only shorten the time, and it is cost-effective.Meanwhile two-dimensional nano periodic structure is produced using nanometer embossing, light absorbs can be effectively increased, improve the utilization rate to sunshine.Therefore, the present invention not only innovates impression formboard preparation method, meanwhile, the efficiency of organic solar batteries is effectively improved, the development for following nano impression and organic solar batteries has very big reference.
Description
Technical field
The invention belongs to organic solar batteries technical field, and in particular to a kind of two dimension based on nano hot stamping technology
Organic solar batteries of nano bowl array light trapping structure and preparation method thereof.
Background technology
The ordered micro-cellular structure of two and three dimensions photovoltaic, photocatalysis, optical detection, sensor and it is super-hydrophobic etc. all
With very big application value, the light trapping structure of the orderly micropore of two and three dimensions also has extensively in terms of organic solar batteries
General application, and when preparing two dimension or three-dimensional ordered micro-cellular structure, different templates material is often used, it is relatively more normal at present
Mould material is mostly silica or silicon template.But because earth silicon material is not easy to etch, and the fragility of material
Also increase the difficulty of image transfer.Its masterplate preparation technology is complicated and is difficult to the needs for meeting large-scale production, and this is very big
Limit application of the light trapping structure in organic solar batteries.Impression formboard based on silica and silicon materials is using
When to pass through cutting, photoetching, burn into such as removes photoresist, cleaned at the set-up procedure, and the preparatory period is longer, and process is cumbersome.In order to solve these
Problem, it would be desirable to quickly prepare light trapping structure masterplate with new technique and method and be applied to organic solar electricity
Pond.
The content of the invention
It is an object of the invention to provide a kind of based on the transoid organic solar batteries of nano hot stamping technology and its preparation
Method.This method prepares two-dimensional nano bowl array masterplate using PS beads, and it prepares TiO in the masterplate using sol-gal process2
Two-dimensional nano bowl array directly imprints out equally distributed two by nano marking press as light trapping structure template on active layer
Nano bowl array is tieed up, so that simpler convenience is operated, and two-dimensional nano bowl array can strengthen suction of the device for light
Receive, improve the performance of device.
The two-dimentional bowl array light trapping structure organic solar batteries based on nano hot stamping technology in the present invention prepare master
To include two parts:1, PS bead template and sol-gal process prepare TiO2Two-dimensional nano bowl array is as light trapping structure mould
Version:2, prepared by light trapping structure transoid organic solar batteries.
Organic solar batteries prepared by the present invention, from bottom to up, ITO Conducting Glass, TiO successively2Electronics passes
Defeated layer, PCDTBT:PCBM active layers, MoO3Hole transmission layer, Ag anodes composition, i.e., structure is glass/ITO/TiO2/PCDTBT:
PCBM/MoO3/ Ag, it is characterised in that:With MoO3The PCDTBT that hole transmission layer is in contact:PCBM activity layer surface has for height
The two-dimensional nano bowl array light trapping structure of sequence, a diameter of 350~450nm of nano bowl, is highly 170~230nm;TiO2Electronics
The thickness of transport layer is 30~50nm, PCDTBT:The thickness of PCBM active layers is 200~300nm, MoO3The thickness of hole transmission layer
The thickness spent for 3~5nm, Ag anodes is 80~120nm.
Two-dimensional nano bowl array light trapping structure masterplate is prepared using PS beads template and sol-gal process, is pressed using nanometer
For print technology by pattern transfer to active layer, it is simple that PS bead template methods prepare light trapping structure masterplate technique, and by special
Directly equally distributed two-dimensional nano bowl array light trapping structure is made in active layer surface in nano marking press.When sunshine irradiation
When, due to the presence of interface light trapping structure, coupling of the device for light can be greatly improved, so as to strengthen device for
The absorption of sunshine.Photogenerated current so can be greatly improved, so as to improve the performance of device.
The preparation of two-dimentional bowl array light trapping structure organic solar batteries of the present invention based on nano hot stamping technology
Method, its step are as follows:
First, TiO2The preparation of two-dimensional nano bowl array masterplate
1)TiO2The preparation of colloidal sol
5~20mL C is added into 30~60mL absolute ethyl alcohol16H36O4Ti, stir 50~90 minutes;Addition 5~
20mL glacial acetic acid and 10~30mL absolute ethyl alcohols, stir 20~40 minutes;Add 5~20mL acetylacetone,2,4-pentanediones and 10~30mL is anhydrous
Ethanol, stir 20~40 minutes;5~20mL deionized waters and 10~30mL absolute ethyl alcohols are added, stirs 15~30h;Standing 2~
4 days, obtain TiO2Colloidal sol;
2) processing of substrate
Glass substrate is cleaned by ultrasonic 10~30 minutes with acetone, ethanol, deionized water successively, nitrogen drying;
3) preparation of PS beads template
The monodisperse layer of a diameter of 300~500nm polystyrene PS beads is by being done in the self assembly of water/Air Interface
What method was formed.First, prepare mass fraction 5wt%~10wt% PS beads water and ethanol (volume ratio of water and ethanol is
1:1) single dispersing liquid;Secondly, add deionized water in culture dish, and to deionized water surface be slowly added to PS beads water and
Ethanol single dispersing liquid, PS beads scatter in the water surface, continuously add dispersion liquid until PS beads are paved with the whole water surface;Then, Xiang Shui
Face instills 2wt%~5wt% C12H25NaO4The S aqueous solution adjusts the surface tension of the water surface, makes the arrangement of PS beads close, and then control
The system regulation PS bead sizes of space;Subsequently, the glass substrate after cleaning treatment is inserted in water at a slant and slowly lifted, made
Close PS beads monodisperse layer is arranged to be transferred in glass substrate;Finally, the glass substrate of PS bead monodisperse layers will be loaded with
Dried in Muffle furnace under the conditions of 90 DEG C~150 DEG C 15~30 minutes and remove solvent, so as to be obtained closely in glass substrate surface
Arrangement, the orderly small ball arrays of two-dimentional PS;
4)TiO2The preparation of two-dimensional nano bowl array
First, the glass substrate covered with the small ball arrays of PS step 3) obtained is vertically slowly immersed in step 1) and obtained
TiO23~5 minutes in sol solution, make TiO2Colloidal sol fills up the gap of PS bead templates;Then, will be from TiO2Sol solution
The glass substrate of middle taking-up is annealed 1.5~2.5 hours in Muffle furnace under the conditions of 350~500 DEG C, naturally cool to after room temperature
The TiO of high-sequential is obtained in glass substrate2Two-dimensional nano bowl array;Nano bowl array structure 350~450nm of diameter, height
About 170~230nm;
2nd, prepared by organic solar batteries.
1) ITO electro-conductive glass is put into beaker, is cleaned by ultrasonic 20~30 with acetone, absolute ethyl alcohol, deionized water respectively
Minute, dried up after cleaning with nitrogen;
2) by TiO2Colloidal sol is spin-coated on ITO surfaces, and spin speed is 3000~5000rpm;Then TiO will be carried2Colloidal sol
ITO electro-conductive glass Muffle furnace is annealed 2~3h under the conditions of 350~500 DEG C;After natural cooling cools to room temperature, you can in ITO
Upper obtained TiO2Film, the thickness of film is 30~50nm;
3) under room temperature condition, by donor material PCDTBT and acceptor material PCBM (mass ratioes 1:4) it is dissolved in organic solvent two
In chlorobenzene (Beijing lark prestige company), 5~10mg/mL solution is configured to, is then stirred under 100~400rpm mixing speed
Mix 24~48h, you can be configured to PCDTBT:PCBM mixed solution;
4) in TiO2Spin coating PCDTBT on film:PCBM mixed solutions, rotating speed are 1000~2500rpm;Then, by sample
It is put into the glove box full of argon gas, is annealed 30~50 minutes with 70~100 DEG C in thermal station, so as in TiO2It is made on film
PCDTBT:PCBM active layers, thickness are 200~300nm;
5) sample of the active layer of spin coating is placed in nano hot stamping machine, using the TiO prepared2Two-dimensional nano bowl battle array
Row are used as masterplate, then set pressed temperature as 50~70 DEG C, 60~80 DEG C of pressurize temperature, 10~20 minutes dwell times, let out
30~60 DEG C of temperature is pressed, so as in PCDTBT:The light trapping structure of two-dimensional nano bowl array is made in the surface of PCBM active layers;
6) again pressure be 1 × 10-4~1 × 10-5Under the conditions of Pa, in the work with two-dimensional nano bowl array light trapping structure
MoO is deposited on property layer3(Chemical Reagent Co., Ltd., Sinopharm Group) hole transmission layer, thickness are 3~5nm, and the speed of growth is
7) finally pressure be 1 × 10-5~1 × 10-3In MoO under the conditions of Pa3Ag (Chinese medicines groups are deposited on hole transmission layer
Chemical reagent Co., Ltd) electrode, thickness is 80~120nm, and the speed of growth isAnd then institute of the present invention is prepared
The two-dimensional nano bowl array light trapping structure organic solar batteries stated.
Brief description of the drawings
Fig. 1:Impression formboard of the present invention prepares schematic diagram;
Fig. 2:The structural representation of organic solar batteries of the present invention;
Fig. 3:Transoid organic solar batteries prepared by the present invention and traditional transoid organic solar batteries photocurrent curve
Contrast.
As shown in figure 1, step 1 is growth PS beads, for step 2 to control to adjust the PS bead sizes of space, step 3 is TiO2
Formed, step 4 is to form two-dimensional nanostructure after annealing.Each several part is entitled:PS beads 11, TiO2Sol layer 12, glass lined
Bottom 13.
As shown in Fig. 2 the structural representation of organic solar batteries of the present invention, 1 is ITO Conducting Glass, and 2 are
TiO2Electron transfer layer, 3 be active layer, and 4 be MoO3Hole transmission layer, 5 be Ag electrodes.
As shown in figure 3, in 100mw/cm2Xenon light shining under measured V-I characteristic curves, a is comparative device, and b is changes
Device after making.Fig. 3 results illustrate the transoid organic solar batteries of the invention prepared and traditional transoid organic solar batteries
The contrast of photocurrent curve, its battery short circuit electric current, fill factor, curve factor, energy conversion efficiency significantly improve.
Embodiment
Embodiment 1
First, TiO2The preparation of two-dimensional nano bowl array masterplate.
1)TiO2The preparation steps of colloidal sol
10mL C is added into 40mL absolute ethyl alcohol16H36O4Ti stirs 60 minutes;Add 10mL glacial acetic acid and
20mL absolute ethyl alcohols, stir 30 minutes;10mL acetylacetone,2,4-pentanediones and 20mL absolute ethyl alcohols are added, is stirred 30 minutes;10mL is added to go
Ionized water and 20mL absolute ethyl alcohols, stir 24h;3 days are stood, ultimately forms TiO2Colloidal sol.
2) processing of substrate
Glass substrate is cleaned by ultrasonic 20 minutes with acetone, ethanol, deionized water successively, nitrogen drying.
3) preparation of PS beads template
The monodisperse layer of a diameter of 420nm polystyrene PS beads is by the self assembly method shape in water/Air Interface
Into.First, preparing the monodispersed water/ethanol of PS beads that mass fraction is 5w%, (volume ratio of water and ethanol is 1:1) mix
Close solution;Secondly, deionized water is loaded in culture dish, and PS beads are slowly injected to deionized water surface with microsyringe
Monodisperse liquor, the small clubs of PS scatter in the water surface, continue injection until bead be paved with the whole water surface;Then, instilled to the water surface
2wt% C12H25NaO4The S aqueous solution adjusts the surface tension of the water surface, control PS bead arrangements;Subsequently, glass substrate is tilted
In insertion water and slowly lift, PS beads is transferred in glass substrate;Finally, the glass of PS bead monodisperse layers will be loaded with
Substrate is dried 25 minutes under the conditions of 100 DEG C in Muffle furnace and removes solvent, so as to obtain close-packed arrays in glass substrate surface, have
The small ball arrays of two-dimentional PS of sequence.
4)TiO2The preparation of two-dimensional nano bowl array
First, the glass substrate film normal that will be covered with the small ball arrays of PS is slowly immersed in TiO2Time in sol solution
5 minutes, after substrate is totally immersed into, it is slowly lifted, makes TiO2Colloidal sol fills up the gap of PS bead templates;Then, will be from
TiO2The glass substrate film taken out in sol solution is annealed 2 hours in Muffle furnace under the conditions of 450 DEG C, naturally cools to room temperature
The TiO of high-sequential is obtained afterwards2Two-dimensional nano bowl array;Nano bowl array structure diameter 420nm, height about 210nm.
2nd, prepared by organic solar batteries.
1) ITO electro-conductive glass is put into beaker, is cleaned by ultrasonic 20 minutes with acetone, absolute ethyl alcohol, deionized water respectively,
Dried up after cleaning with nitrogen;
2) by obtained TiO2Colloidal sol is spin-coated on ITO surfaces, spin speed 3000rpm;Then TiO will be carried2Colloidal sol
ITO electro-conductive glass is calcined 2h with Muffle furnace under the conditions of 450 DEG C;After natural cooling cools to room temperature, you can be made on ITO
TiO2Film, the thickness of film is 40nm;
3) under room temperature condition, by donor material PCDTBT and acceptor material PCBM (mass ratioes 1:4) it is dissolved in organic solvent two
In chlorobenzene (Beijing lark prestige company), 7mg/mL solution is configured to, 48h is then stirred under 300rpm mixing speed, i.e.,
It can be configured to PCDTBT:PCBM mixed solution;
4) in TiO2Spin coating PCDTBT on film:PCBM mixed solutions, rotating speed 2000rpm;Then, sample is put into and filled
In the glove box of full argon gas, annealed 30 minutes with 70 DEG C in thermal station, so as in TiO2Active layer is made on film, thickness is
200nm;
5) sample of the active layer of spin coating is placed in nano hot stamping machine, using the TiO prepared2Two-dimensional nano bowl battle array
Row are used as masterplate, then set pressed temperature as 50 DEG C, pressurize temperature 70 C, 20 minutes dwell times, 30 DEG C of pressure release temperature, from
And two-dimensional nano bowl array is made on active layer;
6) sample is taken out, is 1 × 10 in pressure-5Under Pa, MoO is deposited on active layer3(Chinese medicines group chemical reagent has
Limit company) hole transmission layer, thickness 4nm, the speed of growth is
7) finally pressure be 1 × 10-5Ag (Chemical Reagent Co., Ltd., Sinopharm Group) electrode is deposited under Pa, thickness is
100nm, the speed of growth areAnd then the organic sun of two-dimensional nano bowl array light trapping structure of the present invention is prepared
Can battery.
Claims (3)
1. a kind of preparation method of the organic solar batteries with two-dimensional nano bowl array light trapping structure, its step are as follows:
1) ITO electro-conductive glass is put into beaker, is cleaned by ultrasonic 20~30 minutes with acetone, absolute ethyl alcohol, deionized water respectively,
Dried up after cleaning with nitrogen;
2) by TiO2Colloidal sol is spin-coated on ITO conductive glass surfaces, and spin speed is 3000~5000rpm;Then TiO will be carried2It is molten
The ITO electro-conductive glass Muffle furnace of glue is annealed 2~3h under the conditions of 350~500 DEG C;After natural cooling cools to room temperature, you can
TiO is made on ITO2Film;
3) under room temperature condition, by donor material PCDTBT and acceptor material PCBM in mass ratio 1:4 are dissolved in organic solvent dichloro-benzenes
In, 5~10mg/mL solution is configured to, 24~48h is then stirred under 100~400rpm mixing speed, you can be configured to
PCDTBT:PCBM mixed solution;
4) in TiO2Spin coating PCDTBT on film:PCBM mixed solutions, rotating speed are 1000~2500rpm;Then, sample is put into
In glove box full of argon gas, annealed 30~50 minutes with 70~100 DEG C in thermal station, so as in TiO2It is made on film
PCDTBT:PCBM active layers;
5) sample of the active layer of spin coating is placed in nano hot stamping machine, with TiO2Two-dimensional nano bowl array is masterplate, Ran Houshe
It is 50~70 DEG C to determine pressed temperature, 60~80 DEG C of pressurize temperature, 10~20 minutes dwell times, 30~60 DEG C of pressure release temperature, from
And in PCDTBT:The light trapping structure of two-dimensional nano bowl array is made in the surface of PCBM active layers;A diameter of the 350 of nano bowl~
450nm, it is highly 170~230nm;
6) again pressure be 1 × 10-4~1 × 10-5Under the conditions of Pa, on the active layer with two-dimensional nano bowl array light trapping structure
MoO is deposited3Hole transmission layer, thickness are 3~5nm, and the speed of growth is
7) finally pressure be 1 × 10-5~1 × 10-3In MoO under the conditions of Pa3Ag electrodes, thickness 80 are deposited on hole transmission layer
~120nm, the speed of growth areAnd then it is prepared with two-dimensional nano bowl array light trapping structure organic solar electricity
Pond.
A kind of 2. preparation side of the organic solar batteries with two-dimensional nano bowl array light trapping structure as claimed in claim 1
Method, it is characterised in that:TiO2The preparation process of two-dimensional nano bowl array is as follows,
1) preparation of PS beads template
First, the water and ethanol of mass fraction 5wt%~10wt% a diameter of 300~500nm polystyrene PS beads are prepared
Single dispersing liquid;Secondly, deionized water is added in culture dish, and the water and ethanol of PS beads are slowly added to deionized water surface
Single dispersing liquid, PS beads scatter in the water surface, continuously add dispersion liquid until PS beads are paved with the whole water surface;Then, dripped to the water surface
Enter 2wt%~5wt% C12H25NaO4The S aqueous solution adjusts the surface tension of the water surface, makes the arrangement of PS beads close, and then control and adjust
Save the PS bead sizes of space;Subsequently, the glass substrate after cleaning treatment is inserted in water at a slant and slowly lifted, make arrangement
Close PS bead monodisperse layers are transferred in glass substrate;Finally, the glass substrate of PS bead monodisperse layers will be loaded with horse
Not in stove under the conditions of 90 DEG C~150 DEG C dry 15~30 minutes remove solvent, so as to glass substrate surface obtain close-packed arrays,
The orderly small ball arrays of two-dimentional PS;
2)TiO2The preparation of two-dimensional nano bowl array
First, the glass substrate covered with the small ball arrays of PS step 1) obtained is vertically slowly immersed in TiO23 in sol solution
~5 minutes, make TiO2Colloidal sol fills up the gap of PS bead templates;Then, will be from TiO2The glass substrate taken out in sol solution exists
Annealed 1.5~2.5 hours under the conditions of 350~500 DEG C in Muffle furnace, naturally cool to after room temperature and obtain height on a glass substrate
Orderly TiO2Two-dimensional nano bowl array.
A kind of 3. system of the organic solar batteries with two-dimensional nano bowl array light trapping structure as claimed in claim 1 or 2
Preparation Method, it is characterised in that:TiO2The preparation of colloidal sol is 5~20mL of addition into 30~60mL absolute ethyl alcohol
C16H36O4Ti, stir 50~90 minutes;5~20mL glacial acetic acid and 10~30mL absolute ethyl alcohols are added, is stirred 20~40 minutes;Add
Enter 5~20mL acetylacetone,2,4-pentanediones and 10~30mL absolute ethyl alcohols, stir 20~40 minutes;Add 5~20mL deionized waters and 10~
30mL absolute ethyl alcohols, stir 15~30h;2~4 days are stood, obtains TiO2Colloidal sol.
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CN106356425B (en) * | 2016-11-03 | 2018-03-13 | 西安交通大学 | A kind of preparation method of the open-type silicon thin film spherical shell array structure of light absorbs enhancing |
CN108063187B (en) * | 2017-12-18 | 2021-01-26 | 苏州大学 | Aluminum nanoparticle array, preparation method and application thereof |
CN110212096B (en) * | 2019-06-21 | 2021-05-18 | 福州大学 | Organic solar cell based on molybdenum trioxide hole transport layer with light trapping structure and preparation method thereof |
CN111017867B (en) * | 2019-11-21 | 2023-03-17 | 厦门大学 | Preparation method and application of network structure silicon-based lattice |
CN111272612B (en) * | 2020-03-03 | 2022-01-28 | 西南石油大学 | Primary screening method of demulsifier |
CN112853279A (en) * | 2021-02-06 | 2021-05-28 | 郝云霞 | Preparation method of long-acting bactericidal aluminum or aluminum alloy material |
CN112831758A (en) * | 2021-02-06 | 2021-05-25 | 郝云霞 | Aluminum or aluminum alloy antibacterial material |
CN113161153B (en) * | 2021-03-25 | 2022-03-22 | 中国人民解放军国防科技大学 | Preparation method of visible light multi-band resonant photo-anode |
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