CN113385200B - Full-spectrum oxygen production CeF without sacrificial agent3alpha-FeOOH photocatalyst and preparation method thereof - Google Patents
Full-spectrum oxygen production CeF without sacrificial agent3alpha-FeOOH photocatalyst and preparation method thereof Download PDFInfo
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000001301 oxygen Substances 0.000 title claims abstract description 60
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 60
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 37
- 238000001228 spectrum Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910002588 FeOOH Inorganic materials 0.000 title description 8
- 229910006540 α-FeOOH Inorganic materials 0.000 claims abstract description 65
- 229910020187 CeF3 Inorganic materials 0.000 claims abstract description 37
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 14
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 6
- 238000013032 photocatalytic reaction Methods 0.000 abstract description 2
- 230000005012 migration Effects 0.000 abstract 1
- 238000013508 migration Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 229910052724 xenon Inorganic materials 0.000 description 7
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 7
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000004098 selected area electron diffraction Methods 0.000 description 2
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- 229910017676 MgTiO3 Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002524 electron diffraction data Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000008177 pharmaceutical agent Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 229910000161 silver phosphate Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Images
Classifications
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/12—Fluorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/02—Preparation of oxygen
- C01B13/0203—Preparation of oxygen from inorganic compounds
- C01B13/0207—Water
-
- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a full-spectrum oxygen production CeF without a sacrificial agent3alpha-FeOOH photocatalyst, preparation method and preparation method thereofThe method comprises the steps of completely dissolving cerium nitrate, ferric nitrate and ammonium fluoride in water to obtain a mixed solution, carrying out high-temperature hydrothermal reaction at 200-280 ℃ to obtain the full-spectrum oxygen production CeF without a sacrificial agent3a/alpha-FeOOH photocatalyst. The obtained photocatalyst is crystalline CeF3And amorphous alpha-FeOOH, crystalline CeF3And the interface of the amorphous alpha-FeOOH is shown as a gold-like semi-contact. Wherein the alpha-FeOOH has a high degree of amorphous and crystalline CeF3Form amorphous state-crystalline state interface contact similar to Schottky junction, facilitate separation and migration of electrons, promote the progress of photocatalytic reaction. Meanwhile, the amorphous alpha-FeOOH can store electrons, so that water can be decomposed to generate oxygen without additionally adding a sacrificial agent in the full-spectrum photocatalytic oxygen generation process. The invention has simple operation, and the CeF3the/alpha-FeOOH photocatalyst has good oxygen production performance and good stability.
Description
Technical Field
The invention belongs to the technical field of semiconductor photocatalytic water decomposition, and particularly relates to full-spectrum oxygen production CeF without a sacrificial agent3a/alpha-FeOOH photocatalyst and a preparation method thereof.
Background
The semiconductor photocatalysis decomposition water to generate hydrogen and oxygen is one of the key research directions for solving the energy crisis and providing clean energy. In pursuit of high hydrogen or oxygen production efficiency, various sacrificial agents are used in the water splitting process to reduce the energy barrier that the photocatalytic direct water splitting needs to overcome. Co, Ni and Fe-based transition metal semiconductor compounds are widely concerned and developed in the field of hydrogen production and oxygen production through photocatalytic water splitting, and particularly, Co, Ni and Fe-based oxyhydroxide has excellent performance in the field of water electrolysis due to excellent electron conduction property, and is gradually used for hydrogen production or oxygen production through photocatalytic water splitting combined with a traditional photocatalyst.
The use of a sacrificial agent to decompose water to produce hydrogen or oxygen has not been considered to be a complete water decomposition process. In recent years, some hydrogen or oxygen producing materials without sacrifice have been reported. Xu et al synthesized an Ag3PO4the/MXene compound utilizes two-dimensional MXene as an electron pool to realize oxygen generation without a sacrificial agent. Guan et al synthesized similar Si/MgTiO3The heterojunction catalyst, Si, can store certain electrons, and can be used in pure waterCan produce hydrogen independently without sacrifice agent. Similar materials for the cell part are based on conductive materials with a layered structure, which are compounded by complicated methods. The research provides a thought for the hydrogen or oxygen production material under the condition of no sacrifice agent. CeF prepared by the invention3the/alpha-FeOOH photocatalyst has high oxygen production efficiency and simple preparation method, and provides a material basis for efficiently decomposing water to produce oxygen without a sacrificial agent.
Disclosure of Invention
The invention aims to provide a full spectrum oxygen generation CeF without a sacrificial agent3The obtained photocatalyst can efficiently decompose water to produce oxygen without a sacrificial agent under full-spectrum illumination.
The invention adopts the following specific technical scheme:
in a first aspect, the present invention provides a full spectrum oxygen production CeF without a sacrificial agent3The photocatalyst is crystalline CeF3And amorphous alpha-FeOOH, crystalline CeF3And the interface of the amorphous alpha-FeOOH is shown as a gold-like semi-contact.
Preferably, the photocatalyst can generate oxygen without a sacrificial agent under full-spectrum light irradiation, and meanwhile, no other gas except oxygen is generated.
In a second aspect, the invention provides a full spectrum oxygen production CeF without a sacrificial agent3The preparation method of the/alpha-FeOOH photocatalyst comprises the following specific steps:
completely dissolving cerium nitrate, ferric nitrate and ammonium fluoride in water to obtain a mixed solution, and carrying out high-temperature hydrothermal reaction at 200-280 ℃ to obtain full-spectrum oxygen production CeF without a sacrificial agent3a/alpha-FeOOH photocatalyst.
Preferably, the mixing molar ratio of the cerium nitrate to the ammonium fluoride is 1: (4-8).
Preferably, Ce is contained in the mixed solution3+And Fe3+In a molar ratio of 1: (4.0 to 8.0X 10-3)。
Preferably, the reaction time of the high-temperature hydrothermal reaction is at least 10 h.
Preferably, the reaction temperature of the high-temperature hydrothermal reaction is 200 ℃ and the reaction time is 10 h.
Compared with the prior art, the invention has the following beneficial effects:
1) the method adopts a high-temperature hydrothermal reaction with a temperature (200-280 ℃) higher than that of a common hydrothermal reaction, and generates CeF in one step through self-assembly3a/alpha-FeOOH photocatalyst. When the temperature of the hydrothermal reaction is lower than 200 ℃, the white CeF3And the red alpha-FeOOH product appeared clearly delaminated, CeF3And alpha-FeOOH, cannot self-assemble, and the resulting material cannot decompose water and generate oxygen without a sacrificial agent.
2) The invention is realized by mixing Fe of solution in the preparation process3+The content is controlled, and the oxygen production performance of the photocatalyst can be effectively regulated and controlled.
3)CeF3In the/alpha-FeOOH photocatalyst, alpha-FeOOH has high amorphous state and crystalline state CeF3Form amorphous-crystalline interface contact similar to Schottky junction, and facilitate electrons to pass through crystalline CeF3Transferring to amorphous alpha-FeOOH to promote the photocatalytic reaction. If the crystallinity of the alpha-FeOOH is improved, the alpha-FeOOH is combined with the crystalline CeF3The structure will not show the property of Schottky junction, but will be converted into p-n heterojunction, and the photocatalytic oxygen-generating capability of the material will be greatly reduced.
4)CeF3In the/alpha-FeOOH photocatalyst, amorphous alpha-FeOOH plays a role similar to metal and can store electrons, so that water can be decomposed to generate oxygen without adding a sacrificial agent in the full-spectrum photocatalytic oxygen generation process.
5) The preparation method of the invention has simple operation, and the obtained CeF3The alpha-FeOOH photocatalyst has good oxygen production performance and good stability.
Drawings
FIG. 1 shows CeF synthesized in examples 1 to 43XRD pattern of/alpha-FeOOH photocatalyst;
FIG. 2 shows CeF synthesized in examples 1 to 43FTIR profile for the/α -FeOOH photocatalyst;
FIG. 3 shows CeF synthesized in examples 1 to 43Method for preparing/alpha-FeOOH photocatalystTEM picture in which (a) is CeF30.008 of/alpha-FeOOH and (b) is CeF3The (c) is CeF3The (d) is CeF3/α-FeOOH-0.06；
FIG. 4 shows CeF synthesized in examples 1 to 43A selected area electron diffraction pattern diagram of the/alpha-FeOOH photocatalyst, wherein (a) is CeF30.008 of/alpha-FeOOH and (b) is CeF3The (c) is CeF3The (d) is CeF3/α-FeOOH-0.06；
FIG. 5 shows CeF synthesized in examples 1 to 43A test result chart of the full spectrum photocatalysis oxygen production performance of the/alpha-FeOOH photocatalyst.
Detailed Description
The invention will be further elucidated and described with reference to the drawings and the detailed description. The technical features of the embodiments of the present invention can be combined correspondingly without mutual conflict. The processes referred to in the examples are, unless otherwise specified, conventional processes or procedures, and the pharmaceutical agents used are commercially available unless otherwise specified.
Example 1
2mmol of Ce (NO)3)3、8mmol NH4F、0.008mmol Fe(NO3)3Dissolving in 15ml deionized water, and carrying out hydrothermal reaction at 200 ℃ for 10h to obtain the full spectrum oxygen production CeF without sacrificial agent3the/alpha-FeOOH photocatalyst is noted as CeF3/α-FeOOH-0.008。
In pure water, a 300W xenon lamp (filter: lambda) was used>400nm) irradiation of the resulting CeF3The result of 1h of the/alpha-FeOOH photocatalyst is that CeF is found3The oxygen production rate of the/alpha-FeOOH photocatalyst is 2970 mu mol g-1h-1Thus showing excellent visible light oxygen generating activity.
Example 2
2mmol of Ce (NO)3)3、8mmol NH4F、0.02mmol Fe(NO3)3Dissolving in 15ml deionized water, and carrying out hydrothermal reaction at 200 ℃ for 10h to obtain the full spectrum oxygen production CeF without sacrificial agent3the/alpha-FeOOH photocatalyst is noted as CeF3/α-FeOOH-0.02。
In pure water, a 300W xenon lamp (filter: lambda) was used>400nm) irradiation of the resulting CeF3The result of 1h of the/alpha-FeOOH photocatalyst is that CeF is found3The oxygen production rate of the/alpha-FeOOH photocatalyst is 3465 mu mol g-1h-1Thus showing excellent visible light oxygen generating activity.
Example 3
2mmol of Ce (NO)3)3、8mmol NH4F、0.04mmol Fe(NO3)3Dissolving in 15ml deionized water, and carrying out hydrothermal reaction at 200 ℃ for 10h to obtain the full spectrum oxygen production CeF without sacrificial agent3the/alpha-FeOOH photocatalyst is noted as CeF3/α-FeOOH-0.04。
In pure water, a 300W xenon lamp (filter: lambda) was used>400nm) irradiation of the resulting CeF3The result of 1h of the/alpha-FeOOH photocatalyst is that CeF is found3The oxygen production rate of the/alpha-FeOOH photocatalyst is 4702.5 mu mol g-1h-1Thus showing excellent visible light oxygen generating activity.
Example 4
2mmol of Ce (NO)3)3、8mmol NH4F、0.06mmol Fe(NO3)3Dissolving in 15ml deionized water, and carrying out hydrothermal reaction at 200 ℃ for 10h to obtain the full spectrum oxygen production CeF without sacrificial agent3the/alpha-FeOOH photocatalyst is noted as CeF3/α-FeOOH-0.06。
In pure water, a 300W xenon lamp (filter: lambda) was used>400nm) irradiation of the resulting CeF3The result of 1h of the/alpha-FeOOH photocatalyst is that CeF is found3The oxygen production rate of the/alpha-FeOOH photocatalyst is 2745 mu mol g-1h-1Thus showing excellent visible light oxygen generating activity.
Example 5
2mmol of Ce (NO)3)3、8mmol NH4F、0.06mmol Fe(NO3)3Dissolving in 15ml deionized water, and carrying out high-temperature hydrothermal reaction at 280 ℃ for 10h to obtain the full-spectrum oxygen-producing CeF without a sacrificial agent3a/alpha-FeOOH photocatalyst.
In pure water, a 300W xenon lamp (filter: lambda) was used>400nm) irradiationThe resultant CeF3The result of 1h of the/alpha-FeOOH photocatalyst is that CeF3The oxygen production rate of the/alpha-FeOOH photocatalyst is 1032 mu mol g-1h-1Thus showing excellent visible light oxygen generating activity.
Example 6
2mmol of Ce (NO)3)3、8mmol NH4F、0.04mmol Fe(NO3)3Dissolving in 15ml deionized water, and carrying out hydrothermal reaction at high temperature of 240 ℃ for 10h to obtain the full spectrum oxygen production CeF without sacrificial agent3a/alpha-FeOOH photocatalyst.
In pure water, a 300W xenon lamp (filter: lambda) was used>400nm) irradiation of the resulting CeF3The result of 1h of the/alpha-FeOOH photocatalyst is that CeF is found3The oxygen production rate of the/alpha-FeOOH photocatalyst is 1755 mu mol g-1h-1Thus showing excellent visible light oxygen generating activity.
FIG. 1 shows CeF prepared in examples 1 to 43XRD diffractogram of the/alpha-FeOOH photocatalyst, in which peaks at 24.4 DEG, 25.1 DEG, 27.9 DEG, 44.1 DEG, 45.2 DEG, 51.0 DEG, 53.0 DEG, 65.0 DEG, 68.9 DEG, 69.7 DEG, 69.9 DEG and 71.3 DEG are CeF3Standard peak of (JCPDS No.: 08-0045). The peak at 21.2 ° is assigned to α -FeOOH, the intensity with Fe3+The ion content increases. However, because α -FeOOH has low crystallinity and is predominantly amorphous, the peaks of α -FeOOH in XRD are not apparent and need to be analyzed in conjunction with FTIR testing for the presence of α -FeOOH.
FIG. 2 shows CeF prepared in examples 1 to 43FTIR chart of/alpha-FeOOH photocatalyst, 879cm in the chart-1And 796cm-1Bending vibrations at wavenumber ascribed to Fe-O-H of alpha-FeOOH, 590cm-1The stretching vibration at wave number is attributed to Fe-O of alpha-FeOOH, further illustrating CeF3Successful preparation of/alpha-FeOOH nanoparticles.
FIG. 3 shows CeF prepared in examples 1 to 43TEM image of/alpha-FeOOH photocatalyst, FIG. 4 is CeF prepared in examples 1-43A selected area electron diffraction pattern of the/alpha-FeOOH photocatalyst. As can be seen from the figure, the selected region electron diffraction pattern shows a distinct amorphous ring, indicating the amorphous state of α -FeOOH.
FIG. 5 shows CeF prepared in examples 1 to 43The result of the test on the full spectrum photocatalytic oxygen production performance of the/alpha-FeOOH photocatalyst can be seen from the figure that all materials have excellent photocatalytic activity under the simulated sunlight irradiation of a xenon lamp.
According to the experimental results and the combination of the examples 1-4, the invention can be known by mixing Fe in the solution in the preparation process3+The content is controlled, and the oxygen production performance of the photocatalyst can be effectively regulated and controlled.
The above-described embodiments are merely preferred embodiments of the present invention, which should not be construed as limiting the invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, the technical solutions obtained by means of equivalent substitution or equivalent transformation all fall within the protection scope of the present invention.
Claims (4)
1. Full spectrum oxygen production CeF without sacrificial agent3the/alpha-FeOOH photocatalyst is characterized in that the photocatalyst is crystalline CeF3And amorphous alpha-FeOOH, crystalline CeF3The interface of the amorphous alpha-FeOOH is in Schottky contact;
full spectrum oxygen production CeF without sacrificial agent3The preparation method of the/alpha-FeOOH photocatalyst comprises the following specific steps:
completely dissolving cerous nitrate, ferric nitrate and ammonium fluoride in water to obtain a mixed solution, carrying out high-temperature hydrothermal reaction at 200 ℃ for 10 hours to obtain full-spectrum oxygen production CeF without a sacrificial agent3a/alpha-FeOOH photocatalyst; ce in the mixed solution3+And Fe3+In a molar ratio of 1: (4.0X 10)-3~8.0×10-3）。
2. The full spectrum oxygen generating CeF without sacrificial agent of claim 13the/alpha-FeOOH photocatalyst is characterized in that the photocatalyst can generate oxygen without a sacrificial agent under the irradiation of full-spectrum light, and other gases except oxygen are not generated.
3. Full spectrum oxygen production CeF without sacrificial agent3The preparation method of the/alpha-FeOOH photocatalyst is characterized by comprising the following steps:
completely dissolving cerous nitrate, ferric nitrate and ammonium fluoride in water to obtain a mixed solution, carrying out high-temperature hydrothermal reaction at 200 ℃ for 10 hours to obtain full-spectrum oxygen production CeF without a sacrificial agent3a/alpha-FeOOH photocatalyst; ce in the mixed solution3+And Fe3+In a molar ratio of 1: (4.0X 10)-3~8.0×10-3）。
4. The full spectrum oxygen generating CeF without sacrificial agent of claim 33The preparation method of the/alpha-FeOOH photocatalyst is characterized in that the mixing molar ratio of the cerium nitrate to the ammonium fluoride is 1: (4-8).
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