CN110935483B - Semiconductor NbNO nano rod and preparation method and application thereof - Google Patents
Semiconductor NbNO nano rod and preparation method and application thereof Download PDFInfo
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- 239000002073 nanorod Substances 0.000 title claims abstract description 63
- 239000004065 semiconductor Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000001699 photocatalysis Effects 0.000 claims abstract description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000001257 hydrogen Substances 0.000 claims abstract description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 20
- 229910019804 NbCl5 Inorganic materials 0.000 claims abstract description 12
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 11
- 239000012298 atmosphere Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 238000000354 decomposition reaction Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000005286 illumination Methods 0.000 claims description 6
- 238000013032 photocatalytic reaction Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- 239000011941 photocatalyst Substances 0.000 abstract description 19
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 230000000694 effects Effects 0.000 description 5
- 239000010955 niobium Substances 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 229910052758 niobium Inorganic materials 0.000 description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 229910052724 xenon Inorganic materials 0.000 description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000004904 UV filter Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000006557 surface reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- -1 oxynitrides Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
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- 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
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B01J35/40—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1005—Arrangement or shape of catalyst
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
-
- 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 provides a semiconductor NbNO nanorod and a preparation method thereofThe preparation method and the application thereof comprise the following steps: providing NbCl5And calcining at the temperature of 700-900 ℃ to obtain NbO nanorods, and calcining the NbO nanorods in an ammonia atmosphere at the temperature of 700-900 ℃ to obtain the semiconductor NbNO nanorods. The preparation method of the NbNO semiconductor photocatalyst has the advantages of simple operation, wide applicability, good repeatability and wide application range, and provides a reliable scheme in the aspects of reducing the photocatalytic cost and producing hydrogen by photocatalysis.
Description
Technical Field
The invention relates to the field of catalysts, in particular to a semiconductor NbNO nanorod and a preparation method and application thereof.
Background
In order to solve the problems of energy crisis and environmental pollution, hydrogen has received much attention as an ideal substitute for fossil fuels. After the concept of photoelectrochemical water splitting was proposed in 1972 by Fujishima and Honda, researchers developed various photocatalysts including oxides, sulfides, nitrides, oxynitrides, carbides and composites thereof. However, it has its own disadvantages such as high electron-hole recombination rate, insufficient absorption of visible light, low specific surface area, few surface reaction activation sites, slow surface reaction kinetics, low oxidation ability, low charge mobility, and the like. In addition, the oxidation capability of the photogenerated holes can only oxidize water to generate oxygen, but not form non-selective hydroxyl radicals OH. This requires lowering the VB position of the semiconductor to enhance its water oxidizing ability. The above disadvantages greatly limit the photocatalytic performance.
At present, the modification strategy of the semiconductor photocatalyst is mainly developed around band gap engineering, defect control, morphology regulation, heterojunction construction, cocatalyst loading and the like. Wherein the semiconductor photocatalyst is mainly g-C3N4、TiO2CdS, etc., all of which have been well studied, g-C3N4Low degree of polymerization, poor activity, TiO2The visible light utilization rate of (2) is low, and the CdS is unstable and is heavy metal.
Disclosure of Invention
In view of the above disadvantages of the prior art, the present invention aims to provide a semiconductor photocatalyst NbNO nanorod, a preparation method and an application thereof, which are used for solving the problems of high preparation cost, low activity, instability, heavy metal content and the like of the photocatalyst in the prior art.
To achieve the above and other related objects, the present invention provides a method for manufacturing a semiconductor deviceThe preparation method of the semiconductor NbNO nanorod comprises the following steps: providing NbCl5And calcining to obtain the NbO nanorod, and calcining the NbO nanorod in an ammonia atmosphere to obtain the semiconductor NbNO nanorod.
Optionally calcining NbCl5The temperature may be 700 ℃ to 900 ℃, or 800 ℃ to 900 ℃, specifically 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃ and the like.
Optionally calcining NbCl5The time of (a) is 4-12h, 4-10h, 4-8h, specifically 4h, 5h, 6h, 7h, 8h, 9h, 10h, 11h, 12h, etc.
Optionally calcining NbCl5After that, the NbO nanorods are washed by water to obtain the cleaned NbO nanorods, and then the NbO nanorods are calcined in an ammonia atmosphere.
Optionally, the calcination temperature in the ammonia atmosphere may be 700-900 ℃, or may also be 700-800 ℃, specifically may be 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, and the like. Excessive temperatures may cause the catalyst to sinter.
Optionally, the calcination time in an ammonia atmosphere is 4-12h, 4-10h, or 4-8h, specifically 4h, 5h, 6h, 7h, 8h, 9h, 10h, 11h, 12h, and the like.
The invention also provides the semiconductor NbNO nanorod prepared by the method.
Optionally, the absorption band edge of the semiconductor NbNO nanorod is close to 886nm, and the corresponding energy bandwidth is 1.45 Ev.
Optionally, the flat band potential of the semiconductor NbNO nanorod is-0.49 eV, and the corresponding conduction band potential and valence band potential are-0.69 eV and 0.86eV respectively.
The invention also provides the application of the semiconductor NbNO nanorod in preparing a catalyst for photocatalytic reaction.
Optionally, the photocatalytic reaction is photocatalytic decomposition of water to produce hydrogen.
The invention also provides a method for generating hydrogen by using the semiconductor NbNO nanorod to carry out photocatalytic water decomposition, which comprises the following steps: and mixing the NbNO nanorods with a sacrificial agent and water, placing the mixture under an anaerobic condition, providing illumination, and reacting to obtain hydrogen.
Optionally, the volume of the sacrificial agent is 10% of the total volume of the water and sacrificial agent.
Optionally, the sacrificial agent is selected from methanol.
Optionally, the illumination intensity is 160mV cm-2。
Alternatively, the wavelength λ of the light source is >420nm, which is typically obtained by mounting a UV filter on the light source.
Optionally, the ratio of the niobium oxynitride semiconductor photocatalyst to the total volume of the sacrificial agent and water is 50 mg: 80 mL.
Alternatively, the anaerobic conditions are nitrogen atmosphere, although other inert gases may be used.
Alternatively, the light source providing illumination is a xenon lamp, a Xe arc lamp, or a high pressure mercury lamp.
Optionally, the power of a light source providing illumination is 300-350W.
As described above, the present invention has the following advantageous effects:
the semiconductor NbNO nanorod can be effectively applied to a photocatalytic reaction system, and particularly can play a high-efficiency catalytic role in a system for producing hydrogen by photocatalytic water decomposition. The preparation method of the NbNO semiconductor photocatalyst has the advantages of simple operation, wide applicability, good repeatability and wide application range, and provides a reliable scheme in the aspects of reducing the photocatalytic cost and producing hydrogen by photocatalysis.
Drawings
Figure 1 is a TEM image of the NbNO catalyst prepared.
Figure 2 is an XRD pattern of the NbNO catalyst prepared and the comparative example.
Figure 3 is a graph of the ultraviolet absorption of the NbNO catalyst prepared.
FIG. 4 is a diagram of the prepared NbNO catalyzed Mott-Schottky.
FIG. 5 is a graph showing the performance of the prepared NbNO catalyst in photolysis of water to produce hydrogen.
Detailed Description
The invention is further described with reference to the drawings and the following detailed description, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
So far, no report is available about nitride and niobium-based semiconductor photocatalysts, and the invention can widen the research range of photocatalysts by developing niobium-based nitride for photocatalytic research. Therefore, the design of the novel niobium-based nitride semiconductor photocatalyst is particularly important in the practical significance of photocatalytic decomposition of hydrogen produced by water.
The NbNO nanorod semiconductor photocatalyst is prepared for the first time and is used for producing hydrogen by photocatalytic decomposition of water. The prepared NbNO nanorod semiconductor photocatalyst has proper position of a valence band and a conduction band, and can meet the thermodynamic requirement of photolysis for producing hydrogen from water. The mechanism of the prepared NbNO nanorod semiconductor photocatalyst for photocatalytic decomposition of aquatic hydrogen can be explained as follows: the NbNO nanorods are used as an n-type semiconductor and have a band gap of 1.45eV, so the NbNO nanorods can be excited to generate photo-generated electrons and holes under the irradiation of visible light. Next, the photogenerated electrons will jump from the valence band of NbNO to the NbNO conduction band, while the holes remain on its VB. The photo-generated electrons are combined with water on a conduction band of NbNO to generate reduction reaction to generate hydrogen, and meanwhile, a hole left on a valence band reacts with methanol to finish the hydrogen production by water decomposition through photocatalysis.
The nanorod semiconductor photocatalyst prepared by the embodiment of the invention can also be applied to hydrogen production by photocatalytic decomposition of water. And relative to extensively studied g-C3N4The activity of the photocatalyst is obviously superior to that of g-C3N4。
The experimental steps for producing hydrogen by photocatalytic water decomposition are as follows: (a) adding the NbNO prepared by the invention, a sacrificial agent and water into a photocatalytic reactor; (b) ultrasonically dispersing the photocatalyst and introducing nitrogen to remove air light; (c) irradiating the reactor with a xenon lamp; (d) online analysis was performed using gas chromatography.
Preferably, the light source is a 300W xenon lamp, an optical filter is used for filtering ultraviolet light, and the lambda in the reaction system is more than 420 nm.
The sacrificial agent is methanol, and the volume concentration of the sacrificial agent is 10%.
In the following examples, NbCl5Graphene oxide was purchased from Shanghai Michelin Biochemical technology, Inc.
Example 1
The preparation method of the NbNO nanorod in the embodiment is as follows:
(1) preparing NbO nano-rod from NbCl5Calcining the mixture for 6 hours in a muffle furnace at 800 ℃, and washing the obtained sample with water for three times to obtain the NbO nanorod.
(2) And (2) preparing the NbNO nanorod, calcining the NbO nanorod prepared in the step (1) for 6 hours at 700 ℃ in an ammonia atmosphere, and cooling to room temperature to obtain a sample, namely the NbNO nanorod.
As can be seen from FIG. 1, the NbNO nanorods have a very clear structure, and the diameter of the visible nanorods is obviously less than 100nm, which shows that the nanorods are nano materials.
From fig. 2, it can be seen that NbNO nanorods correspond one-to-one to the standard XRD card peaks, from which it can be seen that, in moles, Nb: n: o ═ 3.49: 4.56: 0.44.
as can be seen from FIG. 3, the absorption band edge of the NbNO nanorod is close to 886nm, and the corresponding energy bandwidth is 1.45 Ev.
As can be seen from FIG. 4, the flat band potential of NbNO nanorods is-0.49 eV, and the corresponding conduction band potential and valence band potential are-0.69 eV and 0.86eV, respectively.
Photocatalytic activity
The reaction apparatus was a 150mL quartz reactor. The xenon lamp with 300W light source is provided with a UV filter (lambda) in front of the lamp cap>420nm), the light intensity of the position where the quartz reactor is located is 160mV cm-2. 50mg of the sample prepared in the above example was charged into a quartz reactor containing a mixed solution of methanol and deionized water, wherein the mixed solution contained 72mL of deionized water and 8mL of methanol. The suspension was sonicated for 30 minutes before testing for light, followed by nitrogen gas in the quartz reactor for 30 minutes to ensure that the reaction test was performed under anaerobic conditions. After 1 hour of illumination, 1mL of sample is introducedThe reactor was purged with 0.4mL of gas from the quartz reactor and analyzed by GC-9500 gas chromatography (Ar as a carrier gas).
As can be seen from FIG. 5, the photocatalytic decomposition of nanorods resulted in a hydrogen production activity of 4.6. mu. mol. h-1*g-1。
Example 2
The preparation method of the NbNO nanorod in the embodiment is as follows:
(1) preparing NbO nano-rod from NbCl5Calcining the mixture for 12 hours at 700 ℃ in a muffle furnace, and washing the obtained sample with water for three times to obtain the NbO nanorod.
(2) And (2) preparing the NbNO nanorod, putting the NbO nanorod prepared in the step (1) in an ammonia atmosphere, calcining for 4 hours at 800 ℃, and cooling to room temperature to obtain a sample, namely the NbNO nanorod.
Example 3
The preparation method of the NbNO nanorod in the embodiment is as follows:
(1) preparing NbO nano-rod from NbCl5Calcining the mixture for 4 hours at 900 ℃ in a muffle furnace, and washing the obtained sample with water for three times to obtain the NbO nanorod.
(2) And (2) preparing the NbNO nanorod, putting the NbO nanorod prepared in the step (1) in an ammonia atmosphere, calcining for 12h at 900 ℃, and cooling to room temperature to obtain a sample, namely the NbNO nanorod.
The physicochemical properties of the NbNO nanorods prepared in example 2 and example 3 were similar to those of example 1.
In conclusion, the NbNO nanorod semiconductor photocatalyst can be effectively applied to a photocatalytic reaction system, and particularly can play a high-efficiency catalytic role in a system for producing hydrogen by photocatalytic water decomposition. The preparation method of the NbNO semiconductor photocatalyst has the advantages of simple operation, wide applicability, good repeatability and wide application range, and provides a reliable scheme in the aspects of reducing the photocatalytic cost and producing hydrogen by photocatalysis.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A preparation method of a semiconductor NbNO nanorod is characterized by comprising the following steps: providing NbCl5And calcining at 900 ℃ of 800-.
2. The method of claim 1, wherein: calcination of NbCl5The time of (a) is 4-12 h.
3. The method of claim 1, wherein: calcination of NbCl5After that, the NbO nanorods are washed by water to obtain the cleaned NbO nanorods, and then the NbO nanorods are calcined in an ammonia atmosphere.
4. The method of claim 1, wherein: the calcination temperature under the ammonia atmosphere is 700-800 ℃.
5. The method of claim 1, wherein: the calcination time under the ammonia atmosphere is 4-12 h.
6. The semiconductor NbO nanorods prepared by the preparation method according to any one of claims 1-5.
7. The use of the semiconducting NbNO nanorod of claim 6 in the preparation of a catalyst for photocatalytic reactions.
8. Use according to claim 7, characterized in that: the photocatalytic reaction is photocatalytic decomposition of water to produce hydrogen.
9. The method for producing hydrogen by photocatalytic water splitting by using the semiconductor NbNO nanorod of claim 6, is characterized by comprising the following steps of: and mixing the semiconductor NbNO nanorod with a sacrificial agent and water, placing the mixture under an anaerobic condition, providing illumination, and reacting to obtain hydrogen.
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