CN105870213A - Mesoporous <alpha>-Fe<2>O<3> and nanogold laminated photoelectrode and preparation method therefor - Google Patents
Mesoporous <alpha>-Fe<2>O<3> and nanogold laminated photoelectrode and preparation method therefor Download PDFInfo
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- CN105870213A CN105870213A CN201610230560.5A CN201610230560A CN105870213A CN 105870213 A CN105870213 A CN 105870213A CN 201610230560 A CN201610230560 A CN 201610230560A CN 105870213 A CN105870213 A CN 105870213A
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- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 19
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 14
- 239000010935 stainless steel Substances 0.000 claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 3
- 239000010931 gold Substances 0.000 claims description 45
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 39
- 229910052737 gold Inorganic materials 0.000 claims description 39
- 230000005693 optoelectronics Effects 0.000 claims description 31
- 238000003475 lamination Methods 0.000 claims description 29
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims description 27
- 229910000859 α-Fe Inorganic materials 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 19
- 239000002243 precursor Substances 0.000 claims description 17
- 239000002105 nanoparticle Substances 0.000 claims description 15
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 6
- 238000004528 spin coating Methods 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 229940055577 oleyl alcohol Drugs 0.000 claims description 3
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000031700 light absorption Effects 0.000 abstract 2
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910002588 FeOOH Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000000443 aerosol Substances 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000007792 gaseous phase Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000005622 photoelectricity Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The invention discloses a mesoporous <alpha>-Fe<2>O<3> and nanogold laminated photoelectrode and a preparation method therefor. The mesoporous <alpha>-Fe<2>O<3> and nanogold laminated photoelectrode is an efficient photoelectrode, wherein a stainless steel sheet is taken as the conductive substrate; a mesoporous nano <alpha>-Fe<2>O<3> layer is laminated with the nanogold layer to form a light absorption layer with the thickness of 600-800nm; and then the stainless steel sheet is uniformly coated with the light absorption layer. The preparation method for the mesoporous <alpha>-Fe<2>O<3> and nanogold laminated photoelectrode mainly relates to the steps of preparing the mesoporous nano <alpha>-Fe<2>O<3> layer by a gel-sol method, then enabling the mesoporous nano <alpha>-Fe<2>O<3> layer to be laminated with the nanogold layer, and carrying out high-temperature annealing on the mixture to obtain the mesoporous <alpha>-Fe<2>O<3> and nanogold laminated photoelectrode. The photoelectrode has the low-cost method and easily-available raw materials, rapid and convenient preparation process, and can realize large-batch preparation easily; and in addition, compared with the pure mesoporous <alpha>-Fe<2>O<3> photoelectrode, the light current of the obtained mesoporous <alpha>-Fe<2>O<3> and nanogold laminated photoelectrode is improved by 38%.
Description
Technical field
The present invention relates to a kind of mesoporous α-Fe2O3With nm of gold lamination optoelectronic pole and preparation method thereof.
Background technology
Along with becoming increasingly conspicuous of energy problem and the environmental problem that causes therefrom, solar energy is increasingly paid attention to by people as a kind of continuable clean energy resource, its trans-utilization.Photoelectrocatalysis process be utilize semiconductor absorber and conversion solar can after energy is stored as the process of chemical energy, it is to produce hydrogen by photoelectrolysis water, the raw material consumed during it only has water, the hydrogen produced as secondary energy sources, have cleaning, efficiently, safe, can store, the plurality of advantages such as can transport.At present, generally believe that the feature that excellent photochemical catalyst electrode should possess mainly has: good visible absorption performance, be stable in the aqueous solution, nontoxic, easily prepared and inexpensive etc..In existing photoelectrocatalysimaterial material, α-Fe2O3Because having good visible absorption performance (band gap ~ 2.1eV, the band of 40% in sunshine can be utilized), stability good under the conditions of neutral and alkalescence, the advantage such as nontoxic and cheap (rich reserves in Fe nature), and be considered most potential photoelectrocatalysimaterial material.
For photoelectrolysis material, preparation process and the preparation condition thereof of semi-conducting material have critically important impact to material photoelectrochemical property.Traditional α-Fe2O3Light anode preparation method has electrodeposition process, aerosol high temperature decomposition, chemical gaseous phase deposition etc..Electrodeposition process mainly in the precursor liquid containing Fe ion by the way of electro-deposition by FeOOH thin film deposition to substrate, then the calcining of FeOOH film is obtained α-Fe2O3Film.Aerosol high temperature decomposition is to utilize Fe3+α-Fe is prepared in the oxidation environment that oxygen exists2O3Semiconductive thin film.Chemical gaseous phase deposition is with Fe (CO)5α-Fe is deposited as presoma2O3Semiconductive thin film is as light anode.But, conventional method the α-Fe prepared2O3Generally there is the shortcomings such as extinction efficiency is low, photo-generated carrier diffusion length is short in light anode, causes light utilization efficiency the highest.
Summary of the invention
An object of the present invention is to provide a kind of mesoporous α-Fe2O3With nm of gold lamination optoelectronic pole.
The two of the purpose of the present invention are to provide the preparation method of this optoelectronic pole a kind of.The present invention is by adding nm of gold, with α-Fe2O3The layer structure superimposed with gold nano layer can make photoelectric current improve 38%.This is because nm of gold has absorption and the scattering of surface plasma resonance effect, beneficially light, the diffusion velocity of photo-generated carrier can be accelerated simultaneously, greatly improve α-Fe2O3Light utilization efficiency.
For achieving the above object, the technical scheme is that
A kind of mesoporous α-Fe2O3With nm of gold lamination optoelectronic pole, it is characterised in that this optoelectronic pole is that alternately superposition is coated with mesoporous shape nanometer α-Fe in conductive substrates2O3The light absorbing zone that layer is formed with nano gold layer, the thickness of this optoelectronic pole layer is 600 ~ 800nm, its intermediary hole shape nanometer α-Fe2O3Layer is 1.8~2.2 times of nano gold layer thickness, encapsulated after obtain mesoporous α-Fe2O3With nm of gold lamination optoelectronic pole.
Above-mentioned conductive substrates is: stainless steel substrates or FTO electro-conductive glass.
A kind of prepare above-mentioned mesoporous α-Fe2O3Method with nm of gold lamination optoelectronic pole, it is characterised in that concretely comprising the following steps of the method:
A. nanometer α-Fe is prepared2O3Precursor liquid;
B. alternative stacked coating α-Fe2O3Precursor liquid and nano-Au solution;
C. annealing forms mesoporous α-Fe2O3With nm of gold lamination;
D. mesoporous α-Fe is encapsulated2O3With nm of gold lamination optoelectronic pole.
Above-mentioned step a method particularly includes: under inert gas shielding; ferric acetyl acetonade and oleyl alcohol are stirred by the molal volume ratio of 2:100 ~ 3:100; until after ferric acetyl acetonade all dissolves; low whipping speed is 700 ~ 900r/min; under conditions of temperature is 260 ~ 300 DEG C of reactions; reaction 1 ~ 1.5h, the most respectively with acetone and ethanol purge, then obtains magnetic Fe by centrifugal3O4Nano particle, is eventually adding chloroform and prepares magnetic 14mg/mLFe3O4The collosol and gel precursor liquid of nano particle.
Above-mentioned step b method particularly includes: by above-mentioned magnetic Fe3O4The mode of the collosol and gel precursor liquid spin coating of nano particle is evenly applied in conductive substrates, and then this conductive substrates is placed in heating plate preheating 3 ~ 5 minutes;Naturally cool to after room temperature one layer of 1mg/mL nano-Au solution of spin coating again, then this conductive substrates is placed preheat 3 ~ 5 minutes on hot plate;The most alternately and repeatedly superposition coating magnetic Fe3O4The collosol and gel precursor liquid of nano particle and nano-Au solution are until light absorbing zone reaches 600 ~ 700nm.
Above-mentioned step c method particularly includes: the conductive substrates having coated light absorbing zone is calcined 30 ~ 60min at 500 ~ 600 DEG C, forms mesoporous α-Fe2O3With nm of gold lamination optoelectronic pole.
Compared with the conventional method, the invention have the characteristics that:
(1) the mesoporous α-Fe that the present invention provides2O3With nm of gold lamination optoelectronic pole, improved the nanometer α-Fe of mesoporous shape by the surface plasma resonance effect of nanogold particle2O3Utilization rate to sunshine, with the nanometer α-Fe of simple mesoporous shape2O3The photoelectric current that compares increases 38%.
(2) the mesoporous α-Fe that the present invention provides2O3Mesoporous α-Fe can be passed through with nm of gold lamination optoelectronic pole preparation method2O3The number of plies is superposed to control light absorbing zone thickness with nm of gold.
(3) the mesoporous α-Fe that the present invention provides2O3Have simple to operate with nm of gold lamination optoelectronic pole preparation method, low cost, it is easy to the advantages such as batch production.
Accompanying drawing explanation
Fig. 1 is for prepare mesoporous α-Fe2O3Schematic flow sheet with nm of gold lamination optoelectronic pole.
Fig. 2 is to obtain mesoporous α-Fe in embodiment 12O3Surface Electronic Speculum figure with nm of gold lamination optoelectronic pole.
Fig. 3 is the mesoporous α-Fe obtained in embodiment 12O3Photoelectric properties figure with nm of gold lamination optoelectronic pole.
Fig. 4 is the mesoporous shape nanometer α-Fe obtained in embodiment 22O3The photoelectric properties figure of optoelectronic pole.
Detailed description of the invention
Embodiment 1: see Fig. 1, in a nitrogen atmosphere, is sufficiently stirred for 3mmol ferric acetyl acetonade and 35mL oleyl alcohol, until ferric acetyl acetonade all dissolves.Afterwards, solution is 700r/min at rotating speed, and temperature is to react one hour at 260 DEG C, obtains containing magnetic Fe3O4The viscous liquid of nano particle.Naturally, after cooling, pour 50mL acetone into and clean this and contain magnetic Fe3O4The viscous liquid of nano particle, then obtain magnetic Fe with centrifuge with the rotating speed of 10000r/min3O4Nano particle, then with the ethanol purge of 50mL, be centrifuged with same rotating speed and obtain clean magnetic Fe3O4Nano particle, is eventually adding 30mL chloroform and prepares magnetic Fe3O4The collosol and gel precursor liquid of nano particle.With 2000r/min rotating speed, precursor liquid is uniformly spun on stainless steel substrates (1cm*1.5cm) by sol evenning machine, then the stainless steel substrates that spin coating is good is placed in the heating plate of 300 DEG C preheating 5 minutes.After stainless steel substrates cools down naturally, then one layer of gold nano grain is spin-coated on the stainless steel substrates of existing precursor liquid with 1000r/min, then stainless steel substrates is placed in the heating plate of 300 DEG C and preheats 5 minutes, then by magnetic Fe3O4The collosol and gel precursor liquid of nano particle is spin-coated in nano gold layer, then is placed in by stainless steel substrates in the heating plate of 300 DEG C and preheats 5 minutes, repeats mesoporous α-Fe2O3With nm of gold lamination, light absorbing zone thickness is 600nm heretofore, finally goes to stainless steel substrates to reach and calcines 30min in the tube furnace air atmosphere of 550 DEG C, finally obtains the nanometer α-Fe coating mesoporous shape2O3With nm of gold lamination stainless steel substrates.As in figure 2 it is shown, it can clearly be observed that the nanometer α-Fe of the mesoporous shape being made up of the elongated particle of 60 ~ 80nm under ESEM2O3.With epoxy encapsulation mesoporous α-Fe2O3With nm of gold lamination stainless steel substrates, seal all current-carrying parts, form mesoporous α-Fe2O3With nm of gold lamination optoelectronic pole.With mesoporous α-Fe2O3With nm of gold lamination optoelectronic pole as working electrode, platinum electrode is counterelectrode, AgCl/Ag electrode is reference electrode, it is placed in 1MNaOH electrolyte, it is 0-0.65V in sweep limits, light source is under the test condition of solar simulator AM1.5, obtains photoelectricity flow graph as shown in Figure 3, with simple mesoporous shape α-Fe2O3Optoelectronic pole is compared photoelectric current and is increased 38%.
Embodiment 2: prepare simple mesoporous shape α-Fe2O3Mesoporous α-Fe in optoelectronic pole, with embodiment 12O3Compare with nm of gold lamination optoelectronic pole.Identical with step in embodiment 1, first prepare magnetic Fe3O4The collosol and gel precursor liquid of nano particle, then superposition spin coating precursor liquid, until light absorbing zone reaches 600-700nm, finally go to stainless steel substrates to reach and calcine 30min in the tube furnace air atmosphere of 550 DEG C, and finally encapsulation obtains the nanometer α-Fe of simple mesoporous shape2O3Optoelectronic pole.Nanometer α-Fe with mesoporous shape2O3Photoelectricity extremely working electrode, under test condition same as in Example 1, obtains photoelectricity flow graph as shown in Figure 4.
Embodiment 3: using FTO electro-conductive glass is conductive substrates, specific experiment step, with embodiment 1, prepares the mesoporous α-Fe with FTO as conductive substrates2O3With nm of gold lamination optoelectronic pole.
Claims (6)
1. a mesoporous α-Fe2O3With nm of gold lamination optoelectronic pole, it is characterised in that this optoelectronic pole is that alternately superposition is coated with mesoporous shape nanometer α-Fe in conductive substrates2O3The light absorbing zone that layer is formed with nano gold layer, the thickness of this optoelectronic pole layer is 600 ~ 800nm, its intermediary hole shape nanometer α-Fe2O3Layer thickness is 1.8~2.2 times of nano gold layer thickness, encapsulated after obtain mesoporous α-Fe2O3With nm of gold lamination optoelectronic pole.
Mesoporous α-Fe the most according to claim 12O3With nm of gold lamination optoelectronic pole, it is characterised in that described conductive substrates is: stainless steel substrates or FTO electro-conductive glass.
3. prepare mesoporous α-Fe according to claim 1 and 2 for one kind2O3Method with nm of gold lamination optoelectronic pole, it is characterised in that concretely comprising the following steps of the method:
A. nanometer α-Fe is prepared2O3Precursor liquid;
B. alternative stacked coating α-Fe2O3Precursor liquid and nano-Au solution;
C. annealing forms mesoporous α-Fe2O3With nm of gold lamination;
D. mesoporous α-Fe is encapsulated2O3With nm of gold lamination optoelectronic pole.
Method the most according to claim 3; it is characterized in that described step a method particularly includes: under inert gas shielding; ferric acetyl acetonade and oleyl alcohol are stirred by the molal volume ratio of 2:100 ~ 3:100; until after ferric acetyl acetonade all dissolves; low whipping speed is 700 ~ 900r/min, under conditions of temperature is 260 ~ 300 DEG C of reactions, reacts 1 ~ 1.5h; the most respectively with acetone and ethanol purge, then obtain magnetic Fe by centrifugal3O4Nano particle, is eventually adding chloroform and prepares 14mg/mL magnetic Fe3O4The collosol and gel precursor liquid of nano particle.
Method the most according to claim 3, it is characterised in that described step b method particularly includes: by above-mentioned magnetic Fe3O4The mode of the collosol and gel precursor liquid spin coating of nano particle is evenly applied in conductive substrates, and then this conductive substrates is placed in heating plate preheating 3 ~ 5 minutes;Naturally cool to after room temperature one layer of 1mg/mL nano-Au solution of spin coating again, then this conductive substrates is placed preheat 3 ~ 5 minutes on hot plate;The most alternately and repeatedly superposition coating magnetic Fe3O4The collosol and gel precursor liquid of nano particle and nano-Au solution are until light absorbing zone reaches 600 ~ 700nm.
Method the most according to claim 3, it is characterised in that described step c method particularly includes: the conductive substrates having coated light absorbing zone is calcined 30 ~ 60min at 500 ~ 600 DEG C, forms mesoporous α-Fe2O3With nm of gold lamination optoelectronic pole.
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CN109110820A (en) * | 2018-10-08 | 2019-01-01 | 五邑大学 | A kind of biomimetic features two-stage hole Fe2O3Film and preparation method thereof |
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CN102951687A (en) * | 2012-03-01 | 2013-03-06 | 纳米籽有限公司 | Ferric oxide mesoporous microsphere and preparation method thereof |
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ELIJAH THIMSEN,ET.AL: "Influence of Plasmonic Au Nanoparticles on", 《NANO LETTERS》 * |
HANWEI GAO,ET.AL: "Plasmon-Enhanced Photocatalytic", 《ASC NANO》 * |
JUE WANG,ET.AL: "Gold Nanorod-Enhanced Light Absorption and Photoelectrochemical", 《THE JOURNAL OF PHYSICAL CHEMISTRY C》 * |
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CN109110820A (en) * | 2018-10-08 | 2019-01-01 | 五邑大学 | A kind of biomimetic features two-stage hole Fe2O3Film and preparation method thereof |
CN109110820B (en) * | 2018-10-08 | 2020-07-17 | 五邑大学 | Bionic structure two-stage hole Fe2O3Film and preparation method thereof |
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