CN114715950A - Preparation method of nanorod iron trioxide/niobium dioxide/graphene oxide composite material - Google Patents
Preparation method of nanorod iron trioxide/niobium dioxide/graphene oxide composite material Download PDFInfo
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- HFLAMWCKUFHSAZ-UHFFFAOYSA-N niobium dioxide Chemical compound O=[Nb]=O HFLAMWCKUFHSAZ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002073 nanorod Substances 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 4
- 229910021389 graphene Inorganic materials 0.000 title abstract description 4
- 230000001699 photocatalysis Effects 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 12
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004202 carbamide Substances 0.000 claims abstract description 9
- 230000005496 eutectics Effects 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 13
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000000197 pyrolysis Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 229910019804 NbCl5 Inorganic materials 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013478 data encryption standard Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 niobium chloride-niobium chloride Chemical compound 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 1
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8472—Vanadium
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B01J35/33—Electric or magnetic properties
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- C01B32/00—Carbon; Compounds thereof
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Abstract
The invention discloses a preparation method of a nanorod iron trioxide/niobium dioxide/graphene oxide composite material. Fe of the invention2O3/NbO2Preparation of/GO composites, includingThe following steps: 1) mixing ferric chloride, niobium chloride and urea to prepare a eutectic solvent; 2) roasting the eutectic solvent to obtain the Fe2O3/NbO2a/GO composite material. The invention prepares the nano-rod Fe by one-step pyrolysis oxidation of the designed eutectic solvent2O3/NbO2The preparation method of the/GO composite material is simple to operate, low in preparation cost and easy to realize industrial production, and the obtained nano rod Fe2O3/NbO2the/GO composite material has regular shape and better crystal form; nanorod Fe2O3/NbO2the/GO has excellent photoelectrocatalysis performance and can be applied to photocatalytic water decomposition hydrogen production.
Description
Technical Field
The invention belongs to the technical field of photoelectrocatalysis, and particularly relates to a nanorod Fe2O3/NbO2A preparation method of a/GO composite material.
Background
With the increasing prominence of energy crisis and environmental pollution problems, the development of renewable clean energy to replace traditional fossil energy becomes a hotspot and challenge for researchers. Nowadays, there is an increasing interest in producing hydrogen from water, which is considered to be an effective means of solar energy conversion. As a clean and environment-friendly energy source, hydrogen is usually produced by adopting the traditional electrolysis technology, but the hydrogen cannot be economically compared with solar photocatalytic decomposition water. Therefore, in the past decades, various materials including organic or inorganic systems and metallic or non-metallic systems have been generally developed as semiconductor photocatalysts for decomposing water to generate visible light driven secondary energy, hydrogen energy. However, due to the limitation of high recombination rate of photo-generated electron/hole pairs, the quantum efficiency of the single-phase photocatalyst is severely limited, resulting in low photocatalytic activity. Therefore, the construction of heterojunction photocatalysts in combination with other semiconductors is considered as an important strategy to improve their photocatalytic performance. Because the energy levels of the conduction band and the valence band are different between the two semiconductors, the photo-generated electron/hole pairs can be effectively separated and transferred, and the photocatalytic activity is greatly improved. However, it is limited by instability of materials and complicated preparation processes, and thus it is very necessary to develop a good heterostructure photocatalyst having a simple method and excellent stability.
Hematite (alpha-Fe)2O3) The solar energy is a visible light driven transition metal oxide, has a direct band gap of 2.2eV, and can absorb and utilize solar energy up to 600 nm. The relatively low valence band edge (2.48eV) makes it a promising catalyst for photochemical reactions. A number of studies have demonstrated that alpha-Fe2O3Makes it a good candidate for coupling with other semiconductors to build heterojunctions with higher photocatalytic performance. However, at present, alpha-Fe is synthesized2O3The composite material method is relatively complicated.
Disclosure of Invention
The invention aims to provide a preparation method of a nanorod iron trioxide/niobium dioxide/graphene oxide composite material, which is used for preparing Fe in one step by using a designed eutectic solvent2O3/NbO2the/GO composite material has the advantages of simple preparation process, mild conditions, low preparation cost, industrial production and no environmental pollution; the obtained nano rod Fe2O3/NbO2the/GO has excellent photoelectric catalytic performance.
In a first aspect, the invention provides Fe2O3/NbO2The preparation method of the/GO composite material comprises the following steps:
1) mixing ferric chloride, niobium chloride and urea to prepare a eutectic solvent;
2) roasting the eutectic solvent to obtain the Fe2O3/NbO2a/GO composite material.
In the above preparation method, in step 1), the ratio of the ferric chloride, the niobium chloride and the urea may be any ratio to form DESs, and the molar ratio of the ferric chloride, the niobium chloride and the urea may be 1: (0.2-0.5): 10, specifically 1: 0.5: 10 or 1: 0.2: 10.
the ferric chloride may be added in the form of ferric chloride or its hydrate, such as FeCl3·6H2O；
The niobium chloride may specifically be niobium chloride or a niobium chloride-niobium chloride mixtureAddition in the form of hydrates, e.g. NbCl5；
The mixing may be carried out at 40 to 90 ℃, such as 70 ℃.
The mixing was carried out under stirring until a homogeneous solution was formed.
In the preparation method, step 2), the roasting procedure is as follows: heating to 550 ℃ at the speed of 2-10 ℃/min, preserving heat for 4h, heating to 750-950 ℃ at the speed of 2-10 ℃/min, and preserving heat for 4 h.
The roasting procedure can be specifically any one of the following a1) -a 3):
a1) heating to 550 ℃ at a speed of 5 ℃/min, preserving heat for 4h, heating to 850-950 ℃ at a speed of 5 ℃/min, and preserving heat for 4 h;
a2) heating to 550 ℃ at a speed of 5 ℃/min, preserving heat for 4h, heating to 850 ℃ at a speed of 5 ℃/min, and preserving heat for 4 h;
a3) heating to 550 deg.C at 5 deg.C/min, maintaining for 4 hr, heating to 950 deg.C at 5 deg.C/min, and maintaining for 4 hr.
The firing may be performed in an air atmosphere.
The method also comprises the following steps after the baking and sintering process: cooling along with the furnace, washing the sample by deionized water and ethanol, and drying.
In a second aspect, the invention provides Fe prepared by any one of the above preparation methods2O3/NbO2a/GO composite material.
Said Fe2O3/NbO2The shape of the/GO composite material is a nano rod.
In a third aspect, the invention provides Fe2O3/NbO2The application of the/GO composite material in photocatalytic water decomposition hydrogen production.
The invention has the following beneficial effects:
the invention prepares the nano-rod Fe by one-step pyrolysis oxidation of the designed eutectic solvent2O3/NbO2The preparation method of the/GO composite material is simple to operate, low in preparation cost and easy to realize industrial production, and the obtained nano rod Fe2O3/NbO2the/GO composite material has regular shape and better performanceA crystalline form of (a); nanorod Fe2O3/NbO2the/GO has excellent photoelectrocatalysis performance and can be applied to photocatalytic water decomposition hydrogen production.
Drawings
FIG. 1 shows Fe prepared in example 1 of the present invention2O3/NbO2SEM photograph of/GO composite;
FIG. 2 shows Fe prepared in example 1 of the present invention2O3/NbO2XRD spectrum of GO composite material;
FIG. 3 shows Fe prepared in example 1 of the present invention2O3/NbO2Raman spectrum of/GO composite;
FIG. 4 shows Fe prepared in examples 1 to 3 of the present invention2O3/NbO2The photocatalytic hydrogen evolution performance curve of the/GO composite material; case 1-example 1; case 2-example 2; case 3-example 3.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention. The examples provided below serve as a guide for further modifications by a person skilled in the art and do not constitute a limitation of the invention in any way.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are commercially available unless otherwise specified.
The firing in the following examples is carried out in air unless otherwise specified.
Example 1 preparation of nanorod Fe2O3/NbO2/GO
Accurately weighing 0.01mol FeCl3·6H2O、0.005mol NbCl5And 0.1mol of urea, placing the mixture into an oil bath kettle, and stirring the mixture at 70 ℃ to form uniform solutions (DESS); and (3) placing the synthesized DESS in a muffle furnace, heating to 550 ℃ at the speed of 5 ℃/min, preserving heat for 4h, heating to 850 ℃ at the speed of 5 ℃/min, and preserving heat for 4 h. After the procedure is finished, cooling along with the furnace, and passing through deionized waterAnd washing the sample with ethanol for 3 times, and drying.
Example 2 preparation of nanorod Fe2O3/NbO2/GO
Accurately weighing 0.01mol FeCl3·6H2O、0.002mol NbCl5And 0.1mol of urea, placing the mixture into an oil bath kettle, and stirring the mixture at 70 ℃ to form uniform solutions (DESS); and (3) placing the synthesized DESS in a muffle furnace, heating to 550 ℃ at the speed of 5 ℃/min, preserving heat for 4h, heating to 850 ℃ at the speed of 5 ℃/min, and preserving heat for 4 h. After the procedure was completed, the sample was cooled down with the furnace, washed 3 times with deionized water and ethanol, and dried.
Example 3 preparation of nanorod Fe2O3/NbO2/GO
Accurately weighing 0.01mol FeCl3·6H2O、0.002mol NbCl5And 0.1mol of urea, placing the mixture into an oil bath kettle, and stirring the mixture at 70 ℃ to form uniform solutions (DESS); and (3) placing the synthesized DESS in a muffle furnace, heating to 550 ℃ at the speed of 5 ℃/min, preserving heat for 4h, then heating to 950 ℃ at the speed of 5 ℃/min, and preserving heat for 4 h. After the procedure was completed, the sample was cooled down with the furnace, washed 3 times with deionized water and ethanol, and dried.
Example 4 characterization
The product obtained in example 1 was topographically characterized. Wherein the product morphology is observed by SEM and the product composition and crystal form are identified by XRD.
FIG. 1 shows Fe prepared in example 1 of the present invention2O3/NbO2SEM photograph of/GO composite material, from which it can be seen that the prepared material is composed of nano rods;
FIG. 2 shows Fe prepared in example 1 of the present invention2O3/NbO2The XRD spectrum of the/GO composite material can be seen, and XRD diffraction peaks of all samples can be classified into Fe2O3(PDF #33-0664) and NbO2(PDF#19-0859)；
FIG. 3 shows Fe prepared in example 1 of the present invention2O3/NbO2The Raman spectrum of the/GO composite material can analyze that GO is contained in a sample from a D peak and a G peak in the Raman spectrum.
Example 5, Performance test
The photocatalytic hydrogen analysis reaction by water decomposition is carried out on an on-line analysis system of the photocatalytic reaction of the gold source in Beijing. The specific operating conditions were as follows: 50mg of the synthesized catalyst is accurately weighed and is added with 90mL of deionized water for uniform ultrasonic dispersion. Then 10mL of methanol was added and the mixture was again dispersed by sonication to homogeneity. Transferring the mixture into a photocatalytic reactor, connecting a photocatalytic reaction system, and vacuumizing for 30 min. The light source was then turned on and the system extracted the hydrogen produced every 30min for quantitative analysis.
FIG. 4 shows Fe prepared in examples 1 to 3 of the present invention2O3/NbO2The photocatalytic hydrogen evolution performance diagram of/GO can be seen, and the synthesized FeVO4the/GO composite material has excellent photocatalytic hydrogen evolution performance.
The present invention has been described in detail above. It will be apparent to those skilled in the art that the invention can be practiced in a wide range of equivalent parameters, concentrations, and conditions without departing from the spirit and scope of the invention and without undue experimentation. While the invention has been described with reference to specific embodiments, it will be appreciated that the invention can be further modified. In general, this application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. The use of some of the essential features is possible within the scope of the appended claims.
Claims (9)
1. Fe2O3/NbO2The preparation method of the/GO composite material comprises the following steps:
1) mixing ferric chloride, niobium chloride and urea to prepare a eutectic solvent;
2) roasting the eutectic solvent to obtain the Fe2O3/NbO2a/GO composite material.
2. The method of claim 1, wherein: in the step 1), the molar ratio of the ferric chloride to the niobium chloride to the urea is 1: (0.2-0.5): 10.
3. the production method according to claim 1 or 2, characterized in that: in the step 1), the niobium chloride is niobium pentachloride.
4. The production method according to any one of claims 1 to 3, characterized in that: in the step 1), the mixing is carried out at 40-90 ℃.
5. The production method according to any one of claims 1 to 4, characterized in that: in the step 2), the roasting procedure is as follows: heating to 550 ℃ at the speed of 2-10 ℃/min, preserving heat for 4h, heating to 750-950 ℃ at the speed of 2-10 ℃/min, and preserving heat for 4 h.
6. The production method according to any one of claims 1 to 5, characterized in that: in the step 2), the roasting is performed in an air atmosphere.
7. Fe prepared by the method of any one of claims 1 to 62O3/NbO2a/GO composite material.
8. Fe of claim 72O3/NbO2the/GO composite material is characterized in that: said Fe2O3/NbO2The shape of the/GO composite material is a nano rod.
9. Fe as claimed in claim 7 or 82O3/NbO2The application of the/GO composite material in photocatalytic water decomposition hydrogen production.
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| CN116641066A (en) * | 2023-07-26 | 2023-08-25 | 四川大学 | Photoelectrocatalysis material and preparation method thereof |
Citations (4)
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| CN116641066B (en) * | 2023-07-26 | 2023-10-17 | 四川大学 | Photoelectrocatalysis material and preparation method thereof |
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