CN107099817A - A kind of preparation method of doped ferric oxide nanometer line ordered array light anode - Google Patents
A kind of preparation method of doped ferric oxide nanometer line ordered array light anode Download PDFInfo
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- CN107099817A CN107099817A CN201710240783.4A CN201710240783A CN107099817A CN 107099817 A CN107099817 A CN 107099817A CN 201710240783 A CN201710240783 A CN 201710240783A CN 107099817 A CN107099817 A CN 107099817A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
- C25B11/077—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25D1/00—Electroforming
- C25D1/006—Nanostructures, e.g. using aluminium anodic oxidation templates [AAO]
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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Abstract
The invention discloses a kind of preparation method of doped ferric oxide nanometer line ordered array light anode, belong to catalysis technical field.The present invention is prepared for the FeOOH nanometer line ordered array containing doped chemical using aluminum oxide ordered template and electrochemical method for synthesizing, and then carrying out calcination processing to sample again obtains ion doping iron oxide nano-wire oldered array.The doped ferric oxide nanometer line ordered array of preparation is polycrystalline structure, and arranged regular, size uniform, with preferable photocatalysis performance, can have broad application prospects as light anode in terms of following photolysis water hydrogen.
Description
Technical field
The present invention relates to photocatalysis technology field, more particularly to a kind of doped ferric oxide nanometer line ordered array light anode
Preparation method.
Background technology
Sunshine hydrogen production by water decomposition is by as a kind of effective way for providing clean energy resource.Photocatalytic water mainly has two kinds of differences
Mode：Photocatalysis and photoelectrocatalysis.Photocatalysis is some scattered photolytic activity catalysis materials in aqueous, during illumination, whole
Hydrogen and oxygen are produced in individual solution simultaneously.Photoelectrocatalysis is, as electrode, to constitute photoelectrochemical cell using light active material,
Occur oxidation reaction in anode and separate out O2, negative electrode generation reduction reaction precipitation H2, two electrodes are connected by aqueous electrolyte solution
And external circuit, form current loop.For photocatalysis, the advantage of photoelectrochemical cell is that it can be efficiently separated
And collect O2And H2。
TiO is utilized since Fujishima and Honda are reported first2Since optical electro-chemistry decomposition water, relevant light anode material
Research for solar hydrogen making is received more and more attention.Light anode material will typically meet some particular/special requirements：Partly lead
Body band gap is narrow；Conduction band positions are more negative than the reduction potential of water, and valence band is corrected than the oxidizing potential of water；Photo-generated carrier is to water decomposition
Stability height in product high conversion efficiency, liquid phase environment, cost are low.
Some light anode materials of greatest concern mainly include TiO both at home and abroad2、ZnS、α-Fe2O3、BiVO4、WO3Etc., but
All need further raising in terms of photoelectric properties, its improved method includes element doping, pattern control, surface modification and structure
Hetero-junctions etc..
The visible light-responded light anode material of development is the focus that current optical electro-chemistry decomposes wate research.Visible ray accounts for total
The 40% of solar energy, its scope shows that the band gap of semiconductor is proper in 1.56~3.12eV in 400~800nm.One
A little Fe sills (such as α-Fe2O3、CaFe2O4、ZnFe2O4Deng), Bi sills (such as BiVO4), Ta sills (such as Ta3N5), W bases
Material (such as WO3) and Cu2O etc. meets the requirement in band gap, and these materials all have excellent PhotoelectrochemicalProperties Properties, turned into
The important system of light anode material.
Due to α-Fe2O3It is widespread in nature, the features such as cheap, nontoxic so that α-Fe2O3As most
One of light anode material of potentiality.But the conductance of difference limits the transfer of electric charge, is bloodstone α-Fe2O3As light anode
One major limitation.Doping is considered as a kind of effective means for solving this problem.The element of electron donor is doped with, such as
Sn, Si, Ti etc., can significantly increase α-Fe2O3Donor density, so as to improve conductance.
It is combined and enhancing visible absorption to be prevented effectively from photo-generated carrier, photoelectrode structure reasonable in design is to improving
PhotoelectrochemicalProperties Properties are extremely important.Compared with block materials, one-dimensional nano structure semi-conducting material can more effectively separate photoproduction
Electronics and hole.Therefore, α-Fe2O3One-dimensional nanotube, nanometer rods or nano-wire array is preferable material structure system.
The formal design of material carried out based on this thinking of the invention, utilizes aluminum oxide ordered template and electrochemistry formated side
Method is prepared for the FeOOH nanometer line ordered array containing doped chemical, then again to sample carry out calcination processing obtain from
Sub- doped ferric oxide nanometer line ordered array.The doped ferric oxide nanometer line ordered array of preparation is polycrystalline structure, arranged regular,
Size uniform, with preferable photocatalysis performance, can there is wide application as light anode in terms of following photolysis water hydrogen
Prospect.
The content of the invention
Prepare ion using aluminum oxide ordered template and electrochemical method for synthesizing it is an object of the invention to provide one kind and mix
The method of miscellaneous iron oxide nano-wire oldered array.
A kind of element doping iron oxide nano-wire oldered array light anode material proposed by the present invention, its pattern arrangement rule
Whole, size uniform, its a diameter of 20~100nm, its length is 1~100 μm；Including α-Fe2O3:M nanometer line ordered arrays, its
Middle doped chemical M is at least one of Ti, Sn, Al, Be, Cu, Mg, Si；Doped chemical M has in element doping iron oxide nano-wire
The content of sequence array photo-anode material is 1-10%.
The invention provides a kind of preparation method of doped ferric oxide nanometer line ordered array light anode, including following step
Suddenly：
(1) layer of metal is deposited as conductive substrate in the one side at one with the porous alumina formwork of through hole, spends
Ionized water cleaned standby seam；
(2) prepared with deionized water and contain FeCl3·6H2O and (NH4)2C2O4·H2O mixed liquor, the concentration of mixed liquor
For 0.1~0.7mol/L, FeCl3·6H2O and (NH4)2C2O4·H2O mol ratio is 1：2~5；Then 0.05- is added
The villaumite ethanol solution of 0.5mol/L doped chemicals obtains depositing the villaumite ethanol of liquid, mixed liquor and doped chemical into mixed liquor
The volume ratio of solution is 20:1~10:1；
(3) the deposition liquid for obtaining step (2) is put into dislodger, is sunk using bipolar electrode AC electrochemical method
Porous alumina formwork, using the carbon of high-purity as to electrode, is handed over as electrode after product, the evaporation obtained using step (1)
The frequency of stream electricity is 60Hz, and the voltage of alternating current is 15V, and sedimentation time is 5~60min；
(4) the deposition rear oxidation aluminum alloy pattern plate that step (3) is obtained is taken out, is cleaned up with deionized water, then heat to 500
~700 DEG C, calcine 1~3h；
(5) material removes alumina formwork with 0.2~0.5mol/L NaOH aqueous solution after the calcining for obtaining step (4)
Obtain element doping iron oxide nano-wire oldered array light anode material.
The beneficial effects of the invention are as follows：α-the Fe prepared2O3One-dimensional nano line array structure, one is entered by element doping
Step improves its photoelectric characteristic, is conducive to improving photolysis water hydrogen efficiency, positive for promoting the development of solar hydrogen making technology to have
Meaning.
Brief description of the drawings
Fig. 1 is the gained α-Fe of the embodiment of the present invention 12O3:The shape appearance figure of Ti nanometer line ordered arrays；Wherein (a) be α-
Fe2O3:The SEM photograph of Ti nanometer line ordered arrays；(b) it is α-Fe2O3:The TEM photos of Ti nanometer line ordered arrays.
Fig. 2 is the gained α-Fe of the embodiment of the present invention 12O3:The XRD of Ti nanometer line ordered arrays.
Embodiment
A kind of element doping iron oxide nano-wire oldered array light anode material proposed by the present invention, its pattern arrangement rule
Whole, size uniform, its a diameter of 20~100nm, its length is 1~100 μm；Including α-Fe2O3:M nanometer line ordered arrays, its
Middle doped chemical M is at least one of Ti, Sn, Al, Be, Cu, Mg, Si；Doped chemical M has in element doping iron oxide nano-wire
The molar content of sequence array photo-anode material is 1-10%.
The invention provides a kind of preparation method of doped ferric oxide nanometer line ordered array light anode, including following step
Suddenly：
(1) layer of metal is deposited as conductive substrate in the one side at one with the porous alumina formwork of through hole, spends
Ionized water cleaned standby seam；
(2) prepared with deionized water and contain FeCl3·6H2O and (NH4)2C2O4·H2O mixed liquor, the concentration of mixed liquor
For 0.1~0.7mol/L, FeCl3·6H2O and (NH4)2C2O4·H2O mol ratio is 1：2~5；Then 0.05- is added
The villaumite ethanol solution of 0.5mol/L doped chemicals obtains depositing the villaumite ethanol of liquid, mixed liquor and doped chemical into mixed liquor
The volume ratio of solution is 20:1~10:1；
(3) the deposition liquid for obtaining step (2) is put into dislodger, is sunk using bipolar electrode AC electrochemical method
Porous alumina formwork, using the carbon of high-purity as to electrode, is handed over as electrode after product, the evaporation obtained using step (1)
The frequency of stream electricity is 60Hz, and the voltage of alternating current is 15V, and sedimentation time is 5~60min；
(4) the deposition rear oxidation aluminum alloy pattern plate that step (3) is obtained is taken out, is cleaned up with deionized water, then heat to 500
~700 DEG C, calcine 1~3h；
(5) material removes alumina formwork with 0.2~0.5mol/L NaOH aqueous solution after the calcining for obtaining step (4)
Obtain element doping iron oxide nano-wire oldered array light anode material.
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
The invention provides a kind of preparation method of doped ferric oxide nanometer line ordered array light anode, including following step
Suddenly：
(1) porous alumina formwork with through hole is voluntarily prepared using anodizing, its aperture is 70nm, with
The porous alumina formwork evaporation layer of metal of through hole is used as conductive substrate, deionized water cleaned standby seam；
(2) prepared with deionized water and contain FeCl3·6H2O and (NH4)2C2O4·H2O mixed liquor, the concentration of mixed liquor
For 0.5mol/L, FeCl3·6H2O and (NH4)2C2O4·H2O mol ratio is 1：3；Then 0.5mol/L TiCl are added4Second
Alcoholic solution obtains depositing liquid into mixed liquor, and the volume ratio of the villaumite ethanol solution of mixed liquor and doped chemical is 20:1；
(3) the deposition liquid for obtaining step (2) is put into dislodger, is sunk using bipolar electrode AC electrochemical method
Porous alumina formwork, using the carbon of high-purity as to electrode, is handed over as electrode after product, the evaporation obtained using step (1)
The frequency of stream electricity is 60Hz, and the voltage of alternating current is 15V, and sedimentation time is 10min；
(4) the deposition rear oxidation aluminum alloy pattern plate that step (3) is obtained is taken out, is cleaned up with deionized water, then heat to 600
DEG C, calcine 2h；
(5) material removes alumina formwork with the 0.5mol/L NaOH aqueous solution and obtains member after the calcining for obtaining step (4)
Plain doped ferric oxide nanometer line ordered array light anode material, i.e. α-Fe2O3:Ti nanometer line ordered arrays, wherein Ti contents are
5%, its a diameter of 40~60nm, length are 20 μm, and its pattern is as shown in figure 1, its XRD curve is as shown in Figure 2.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (4)
1. a kind of element doping iron oxide nano-wire oldered array light anode material, it is characterised in that including α-Fe2O3:M nanometers
Line oldered array, wherein doped chemical M are at least one of Ti, Sn, Al, Be, Cu, Mg, Si.
2. element doping iron oxide nano-wire oldered array light anode material according to claim 1, it is characterised in that doping
Element M is 1-10% in the molar content of element doping iron oxide nano-wire oldered array light anode material.
3. element doping iron oxide nano-wire oldered array light anode material according to claim 1, it is characterised in that its shape
Looks are arranged regular, size uniform, and its a diameter of 20~100nm, its length is 1~100 μm.
4. a kind of preparation of the element doping iron oxide nano-wire oldered array light anode material as described in claim any one of 1-3
Method, it is characterised in that comprise the following steps：
(1) layer of metal is deposited as conductive substrate in the one side at one with the porous alumina formwork of through hole, uses deionization
Water cleaned standby seam；
(2) prepared with deionized water and contain FeCl3·6H2O and (NH4)2C2O4·H2O mixed liquor, the concentration of mixed liquor is 0.1
~0.7mol/L, FeCl3·6H2O and (NH4)2C2O4·H2O mol ratio is 1：2~5；Then addition 0.05-0.5mol/L mixes
The villaumite ethanol solution of miscellaneous element obtains depositing liquid, the volume of the villaumite ethanol solution of mixed liquor and doped chemical into mixed liquor
Than for 20:1~10:1；
(3) the deposition liquid for obtaining step (2) is put into dislodger, is deposited, adopted using bipolar electrode AC electrochemical method
Porous alumina formwork is as electrode after the evaporation obtained with step (1), using the carbon of high-purity as to electrode, alternating current
Frequency is 60Hz, and the voltage of alternating current is 15V, and sedimentation time is 5~60min；
(4) step (3) obtained deposition rear oxidation aluminum alloy pattern plate is taken out, is cleaned up with deionized water, then heat to 500~
700 DEG C, calcine 1~3h；
(5) material is obtained with 0.2~0.5mol/L NaOH aqueous solution removal alumina formwork after the calcining for obtaining step (4)
Element doping iron oxide nano-wire oldered array light anode material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107641817A (en) * | 2017-09-12 | 2018-01-30 | 苏州大学 | A kind of light anode preparation method and gained light anode structure for improving photocatalytic water performance |
| CN109534413A (en) * | 2018-11-01 | 2019-03-29 | 南京理工大学 | A kind of Fe2O3The preparation method of NiO nanowire |
| CN111346641A (en) * | 2020-04-14 | 2020-06-30 | 天津大学 | Doped α -ferric oxide, preparation method thereof and application thereof in hydrogenation reaction |
| CN113106484A (en) * | 2021-04-07 | 2021-07-13 | 西南大学 | Hydrothermal preparation method of novel photo-anode based on alpha-type iron oxide vermicular nano-structure array, product and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107641817A (en) * | 2017-09-12 | 2018-01-30 | 苏州大学 | A kind of light anode preparation method and gained light anode structure for improving photocatalytic water performance |
| CN107641817B (en) * | 2017-09-12 | 2019-04-05 | 苏州大学 | A kind of light anode preparation method and gained light anode structure improving photocatalytic water performance |
| CN109534413A (en) * | 2018-11-01 | 2019-03-29 | 南京理工大学 | A kind of Fe2O3The preparation method of NiO nanowire |
| CN109534413B (en) * | 2018-11-01 | 2021-06-11 | 南京理工大学 | Fe2O3Preparation method of-NiO nanowire |
| CN111346641A (en) * | 2020-04-14 | 2020-06-30 | 天津大学 | Doped α -ferric oxide, preparation method thereof and application thereof in hydrogenation reaction |
| CN113106484A (en) * | 2021-04-07 | 2021-07-13 | 西南大学 | Hydrothermal preparation method of novel photo-anode based on alpha-type iron oxide vermicular nano-structure array, product and application thereof |
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