CN114232025B - Ce-Co 3 O 4 /α-Fe 2 O 3 Preparation method of nanorod array and application of nanorod array in photo-anode - Google Patents
Ce-Co 3 O 4 /α-Fe 2 O 3 Preparation method of nanorod array and application of nanorod array in photo-anode Download PDFInfo
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- CN114232025B CN114232025B CN202111441198.3A CN202111441198A CN114232025B CN 114232025 B CN114232025 B CN 114232025B CN 202111441198 A CN202111441198 A CN 202111441198A CN 114232025 B CN114232025 B CN 114232025B
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Abstract
The invention relates to the field of photoelectrode materials, and discloses a Ce-Co 3 O 4 /α‑Fe 2 O 3 Preparation method of nanorod array and application of nanorod array in photo anode, pouring mixed aqueous solution obtained by mixing sodium nitrate and ferric trichloride into a reaction kettle with FTO, washing with a large amount of deionized water after hydrothermal reaction, drying and calcining to obtain alpha-Fe 2 O 3 A nanorod array; ce-Co deposition method under three-electrode system 3 O 4 Loaded to alpha-Fe 2 O 3 A nanorod array; the electrolyte is a mixed aqueous solution of cobalt nitrate hexahydrate and cerium nitrate hexahydrate; calcining at 200-420 ℃ for 1-3h to obtain Ce-Co 3 O 4 /α‑Fe 2 O 3 Optoelectronic material of the nanorod array. The invention uses the electrodeposition method to deposit Ce-Co 3 O 4 Loaded on alpha-Fe 2 O 3 On the nanorod array, the prepared photoelectric material has good photoelectric response, low cost and environmental friendliness.
Description
Technical Field
The invention relates to the technical field of preparation of nano composite photoelectrode materials, in particular to a Ce-Co 3 O 4 /α-Fe 2 O 3 A preparation method of a nano rod array and application of the nano rod array in a photo anode.
Background
α-Fe 2 O 3 Is a natural compound and has wide application in the fields of catalysis, steel manufacturing, gas sensing, photoelectrons and the like. Because of the advantages of small forbidden bandwidth, low cost, easy acquisition, environmental friendliness, high light stability and the like, the material is often used as a photo-anode material for photoelectrochemical decomposition of water. The document reports that the photocurrent density of the ferric oxide photoanode can reach 12.6 mA/cm theoretically 2 However, the photocurrent density achieved so far is far below the theoretical level due to the short lifetime of the iron oxide photogenerated carriers and the high number of surface oxygen vacancy defect states on the surface.
Disclosure of Invention
The invention aims to: aiming at the problems existing in the prior art, the invention provides a Ce-Co 3 O 4 /α-Fe 2 O 3 Preparation method of nanorod array and application of nanorod array in photo-anode, and Ce-Co is prepared by electrodeposition method 3 O 4 Loaded on alpha-Fe 2 O 3 On the nanorod array, the prepared photoelectric material has good photoelectric response, and the preparation method is simple, low in cost and environment-friendly.
The technical scheme is as follows: the invention provides a Ce-Co 3 O 4 /α-Fe 2 O 3 The preparation method of the nanorod array comprises the following steps: mixing sodium nitrate and ferric trichloride to obtain a mixed aqueous solution, pouring the mixed aqueous solution into a reaction kettle filled with FTO, reacting for 10-15 hours under the hydrothermal condition of 80-120 ℃, then flushing with a large amount of deionized water, drying and calcining to obtain alpha-Fe 2 O 3 A nanorod array; ce-Co deposition method under three-electrode system 3 O 4 Loaded to alpha-Fe 2 O 3 A nanorod array; the electrolyte is Co (NO) 3 ) 2 ·6H 2 O and Ce (NO) 3 ) 3 ·6H 2 A mixed aqueous solution of O; electrodepositing for 0-600 s and then drying; calcining at 200-420 ℃ for 1-3h to finally obtain Ce-Co 3 O 4 /α-Fe 2 O 3 Optoelectronic material of the nanorod array.
Preferably, in the S1, in the mixed aqueous solution of sodium nitrate and ferric trichloride, the mass ratio of the sodium nitrate to the ferric trichloride is 8.5:4.
preferably, in S1, the conditions of calcination are as follows: calcining at 100 ℃ for 2 hours.
Preferably, in S2, the Co (NO 3 ) 2 ·6H 2 The concentration of O is 0.005-0.10M.
Preferably, in S2, the Ce (NO 3 ) 3 ·6H 2 The concentration of O is 0.0005-0.02M.
Preferably, in S2, the Co (NO 3 ) 2 ·6H 2 O and Ce (NO) 3 ) 3 ·6H 2 In the mixed aqueous solution obtained by mixing O, co (NO 3 ) 2 ·6H 2 O and Ce (NO) 3 ) 3 ·6H 2 The ratio of the mass concentration of O to the mass concentration of O is 10:1-5:1.
Preferably, the Co (NO 3 ) 2 ·6H 2 O and Ce (NO) 3 ) 3 ·6H 2 In the mixed aqueous solution obtained by mixing O, co (NO 3 ) 2 ·6H 2 O and Ce (NO) 3 ) 3 ·6H 2 The ratio of the mass concentration of O is 9:1.
preferably, in S2, the electrodeposition time is 60S.
The invention also provides the Ce-Co prepared by the method 3 O 4 /α-Fe 2 O 3 Use of an array of nanorods in a photoanode.
The beneficial effects are that: the invention uses simple hydrothermal method to make alpha-Fe 2 O 3 The nano rod array grows on the FTO substrate, and then the Ce-Co is electrodeposited 3 O 4 Loaded to alpha-Fe 2 O 3 On the nano rod array, finally obtaining Ce-Co 3 O 4 /α-Fe 2 O 3 An array of nanorods. Ce-Co 3 O 4 The load of the (C) is formed into the construction of a p-n heterojunction, thereby forming the charge transfer of gradient flow direction, promoting the separation and transmission of photo-generated carriers and prolonging the service lifeThe lifetime of the photogenerated carriers is prolonged. Ce-Co 3 O 4 The introduction of the catalyst also provides more oxygen evolution reaction active sites, which is beneficial to the efficient performance of water oxidation reaction of photoelectrically decomposed water. The method has simple synthesis steps, no pollution and convenient industrialization.
Drawings
FIG. 1 is alpha-Fe 2 O 3 Nanorod array and Ce-Co 3 O 4 /α-Fe 2 O 3 XRD pattern of the nanorod array;
FIG. 2 is alpha-Fe 2 O 3 SEM images of nanorod arrays and different electrodeposition times, wherein (a) is alpha-Fe 2 O 3 SEM image of nanorod arrays; (b) Is Ce-Co 3 O 4 /α-Fe 2 O 3 SEM image of nanorod arrays.
FIG. 3 is a view of alpha-Fe 2 O 3 Nanorod array and Ce-Co 3 O 4 /α-Fe 2 O 3 I-V graph for nanorod arrays.
FIG. 4 is a view of alpha-Fe 2 O 3 Nanorod array and Ce-Co 3 O 4 /α-Fe 2 O 3 Impedance spectrum of the nanorod array.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Embodiment 1:
mixing 8.5g of sodium nitrate and 4.0g of ferric trichloride to obtain a mixed aqueous solution, stirring, and fixing the volume in a 100mL volumetric flask; transferring the solution into a reaction kettle with FTO, and carrying out hydrothermal reaction at 100 ℃ for 12h; then washing with a large amount of deionized water, finally drying and calcining for 2 hours at 100 ℃ to obtain alpha-Fe 2 O 3 An array of nanorods.
The obtained alpha-Fe 2 O 3 The nano rod array is subjected to constant potential deposition reaction for 15s under a three-electrode system, and the electrolyte is 0.05M Co (NO) 3 ) 2 ·6H 2 O and 0.005M Ce (NO) 3 ) 3 ·6H 2 A mixed aqueous solution of O; washing and drying the FTO, and calcining at 200 ℃ for 1h to obtain Ce-Co 3 O 4 /α-Fe 2 O 3 Is provided.
Embodiment 2:
mixing 8.5g of sodium nitrate and 4.0g of ferric trichloride to obtain a mixed aqueous solution, stirring, and fixing the volume in a 100mL volumetric flask; transferring the solution into a reaction kettle with FTO, and performing hydrothermal reaction for 12 hours at 100 ℃; then washing with a large amount of deionized water, finally drying and calcining for 2 hours at 100 ℃ to obtain alpha-Fe 2 O 3 An array of nanorods.
The obtained alpha-Fe 2 O 3 The nano rod array is subjected to constant potential deposition reaction for 60s under a three-electrode system, and the electrolyte is 0.09M Co (NO) 3 ) 2 ·6H 2 O and 0.01M Ce (NO) 3 ) 3 ·6H 2 A mixed aqueous solution of O; washing and drying the FTO, and finally calcining at 400 ℃ for 2 hours to obtain Ce-Co 3 O 4 /α-Fe 2 O 3 Is provided.
Embodiment 3:
mixing 8.5g of sodium nitrate and 4.0g of ferric trichloride to obtain a mixed aqueous solution, stirring, and fixing the volume in a 100mL volumetric flask; transferring the solution into a reaction kettle with FTO, and performing hydrothermal reaction for 12 hours at 100 ℃; then washing with a large amount of deionized water, finally drying and calcining for 2 hours at 100 ℃ to obtain alpha-Fe 2 O 3 An array of nanorods.
The obtained alpha-Fe 2 O 3 The nano rod array is subjected to constant potential deposition reaction for 600s under a three-electrode system, and the electrolyte is 0.1M Co (NO) 3 ) 2 ·6H 2 O and 0.02M Ce (NO) 3 ) 3 ·6H 2 A mixed aqueous solution of O; washing and drying the FTO, and finally calcining at 420 ℃ for 3 hours to obtain Ce-Co 3 O 4 /α-Fe 2 O 3 Is provided.
For Ce-Co obtained in the above embodiment 2 3 O 4 /α-Fe 2 O 3 The performance of the nanorod arrays was analyzed as follows:
FIG. 1 is alpha-Fe 2 O 3 Nanorod array and Ce-Co 3 O 4 /α-Fe 2 O 3 XRD patterns of nanorod arrays, in which pure alpha-Fe 2 O 3 Ce-Co 3 O 4 /α-Fe 2 O 3 Does not significantly change the diffraction peak of (C), probably because of Ce-Co 3 O 4 Too little content was not detected.
FIG. 2 is alpha-Fe 2 O 3 Nanorod array and Ce-Co 3 O 4 /α-Fe 2 O 3 SEM of nanorod array, FIG. a is a pure alpha-Fe 2 O 3 The appearance of the nanorod array can obviously show that the sample is in a rod-shaped structure; FIG. b is Ce-Co 3 O 4 /α-Fe 2 O 3 The nanorod array can be seen from the figure that the sample successfully supported a lamellar structure on a rod-like structure.
FIG. 3 is alpha-Fe 2 O 3 Nanorod array and Ce-Co 3 O 4 /α-Fe 2 O 3 I-V graph of nanorod array, from which it is apparent that pure alpha-Fe 2 O 3 The current density of (C) is weak, and Ce-Co 3 O 4 /α-Fe 2 O 3 The current density is obviously enhanced, which illustrates that Ce-Co 3 O 4 Is improved by the load of pure alpha-Fe 2 O 3 Is used for the photocatalytic performance of the catalyst.
FIG. 4 shows that Ce-Co 3 O 4 /α-Fe 2 O 3 Impedance semicircle of the nanorod array is minimum, which indicates Ce-Co 3 O 4 The load facilitates photogenerated charge transport.
The foregoing embodiments are merely illustrative of the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and to implement the same, not to limit the scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of the present invention.
Claims (8)
1. Ce-Co 3 O 4 /α-Fe 2 O 3 The preparation method of the nanorod array is characterized by comprising the following steps of:
S1：mixing sodium nitrate and ferric trichloride to obtain a mixed aqueous solution, pouring the mixed aqueous solution into a reaction kettle filled with FTO, reacting for 10-15 hours under the hydrothermal condition of 80-120 ℃, then flushing with a large amount of deionized water, drying and calcining to obtain alpha-Fe 2 O 3 A nanorod array;
s2: ce-Co deposition method under three-electrode system 3 O 4 Loaded to alpha-Fe 2 O 3 A nanorod array; the electrolyte is Co (NO) 3 ) 2 ·6H 2 O and Ce (NO) 3 ) 3 ·6H 2 A mixed aqueous solution of O; electrodepositing for 15-600 s and then drying;
s3: calcining at 200-420 ℃ for 1-3h to finally obtain Ce-Co 3 O 4 /α-Fe 2 O 3 Photoelectric material of the nanorod array;
the Ce-Co 3 O 4 /α-Fe 2 O 3 The nanorod array is applied to a photo-anode material.
2. Ce-Co according to claim 1 3 O 4 /α-Fe 2 O 3 The preparation method of the nanorod array is characterized in that in S1, in a mixed aqueous solution of sodium nitrate and ferric trichloride, the mass ratio of the sodium nitrate to the ferric trichloride is 8.5:4.
3. Ce-Co according to claim 1 3 O 4 /α-Fe 2 O 3 The preparation method of the nanorod array is characterized in that in S1, the calcination conditions are as follows: calcination was carried out at 100℃for 2h.
4. Ce-Co according to claim 1 3 O 4 /α-Fe 2 O 3 A method for preparing a nanorod array is characterized in that in S2, co (NO 3 ) 2 ·6H 2 The concentration of O is 0.005-0.10M.
5. The Ce-Co according to claim 4 3 O 4 /α-Fe 2 O 3 Fabrication of nanorod arraysThe preparation method is characterized in that in S2, the Ce (NO 3 ) 2 ·6H 2 The concentration of O is 0.0005-0.02M.
6. Ce-Co according to claim 5 3 O 4 /α-Fe 2 O 3 A method for preparing a nanorod array is characterized in that in S2, co (NO 3 ) 2 ·6H 2 O and Ce (NO) 3 ) 3 ·6H 2 In the mixed aqueous solution obtained by mixing O, co (NO 3 ) 2 ·6H 2 O and Ce (NO) 3 ) 3 ·6H 2 The ratio of the amounts of O to the substance is 10:1-5:1.
7. The Ce-Co according to claim 6 3 O 4 /α-Fe 2 O 3 A method for producing a nanorod array, characterized in that Co (NO 3 ) 2 ·6H 2 O and Ce (NO) 3 ) 3 ·6H 2 In the mixed aqueous solution obtained by mixing O, co (NO 3 ) 2 ·6H 2 O and Ce (NO) 3 ) 3 ·6H 2 The ratio of the amounts of O: 1.
8. Ce-Co according to any one of claims 1 to 7 3 O 4 /α-Fe 2 O 3 The preparation method of the nanorod array is characterized in that in S2, the electrodeposition time is 60S.
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| CN108751736A (en) * | 2018-05-21 | 2018-11-06 | 济南大学 | A kind of synthetic method of porous bloodstone nanometer stick array |
| CN110424022A (en) * | 2019-06-26 | 2019-11-08 | 武汉科技大学 | Compound MIL-101 hetero-junctions light anode of nanometer rods alpha-ferric oxide and preparation method thereof |
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