CN111892086A - Light absorbing material and method for producing the same - Google Patents
Light absorbing material and method for producing the same Download PDFInfo
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- CN111892086A CN111892086A CN202010785792.3A CN202010785792A CN111892086A CN 111892086 A CN111892086 A CN 111892086A CN 202010785792 A CN202010785792 A CN 202010785792A CN 111892086 A CN111892086 A CN 111892086A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 239000011358 absorbing material Substances 0.000 title claims description 30
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 73
- 239000000463 material Substances 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000843 powder Substances 0.000 claims abstract description 43
- 230000031700 light absorption Effects 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 48
- 238000005406 washing Methods 0.000 claims description 43
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- 239000008367 deionised water Substances 0.000 claims description 42
- 229910021641 deionized water Inorganic materials 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 40
- 238000001035 drying Methods 0.000 claims description 32
- 229910052720 vanadium Inorganic materials 0.000 claims description 28
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 28
- 239000002243 precursor Substances 0.000 claims description 21
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 16
- 235000006408 oxalic acid Nutrition 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 6
- 239000012043 crude product Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000007867 post-reaction treatment Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 41
- 238000000034 method Methods 0.000 abstract description 12
- 239000011941 photocatalyst Substances 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- 238000002329 infrared spectrum Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 238000006303 photolysis reaction Methods 0.000 abstract description 3
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract description 3
- 230000002265 prevention Effects 0.000 abstract description 3
- 230000005855 radiation Effects 0.000 abstract description 3
- 239000000809 air pollutant Substances 0.000 abstract description 2
- 231100001243 air pollutant Toxicity 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 238000001228 spectrum Methods 0.000 description 42
- 239000000047 product Substances 0.000 description 39
- 239000000203 mixture Substances 0.000 description 34
- 238000002441 X-ray diffraction Methods 0.000 description 22
- 239000013078 crystal Substances 0.000 description 18
- 238000001816 cooling Methods 0.000 description 17
- 230000001699 photocatalysis Effects 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 4
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 229910001935 vanadium oxide Inorganic materials 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910003206 NH4VO3 Inorganic materials 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229940073609 bismuth oxychloride Drugs 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002524 electron diffraction data Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229960003742 phenol Drugs 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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
- 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
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a light absorption material and a preparation method thereof, belonging to the technical field of functional materials. The invention aims to provide a novel light absorption material capable of efficiently capturing ultraviolet visible infrared spectrum, wherein the material is VOxPowder, wherein x is more than 2 and less than or equal to 2.5. The invention firstly proposes that the light absorption material is prepared by a hydrothermal synthesis method, the prepared powder has strong absorption to ultraviolet visible near-middle infrared light, the preparation conditions and the process are simple and easy to control, no pollution is caused to the environment, the raw material source is wide and cheap, and the large-scale production is facilitated. Prepared VOxThe photocatalyst has full absorption to sunlight, improves the utilization rate of solar energy, enhances the catalytic efficiency, can effectively degrade air pollutants, and is suitable for the fields of catalysts and hydrogen production by water photolysis. Furthermore, the VO producedxThe powder has high near-middle infrared absorption intensity, and can be applied to the fields of infrared absorption, infrared radiation prevention and the like.
Description
Technical Field
The invention relates to a light absorption material and a preparation method thereof, in particular to a novel ultraviolet-visible near-middle infrared light absorption material VOxAnd a preparation method thereof, belonging to the technical field of functional materials.
Background
The photocatalysis technology is a green technology with important application prospect in the field of energy and environment, and takes a semiconductor as a catalyst to carry out a series of oxidation-reduction reactions by absorbing external sunlight so as to achieve the effect of degrading pollutants. As a common pollutant degradation mode, the photocatalytic technology has attracted attention because it can effectively degrade organic pollutants such as rhodamine B, methyl orange, phenol, and the like. In addition, the photocatalysis technology can also utilize solar photocatalysis to crack water to generate hydrogen energy, and is expected to solve the energy crisis problem. The existing semiconductor catalyst can only utilize about 5 percent of ultraviolet light and about 46 percent of visible light in sunlight, and still about 49 percent of near-middle infrared light is not utilized, so that the utilization rate of the sunlight is greatly reduced. On the other hand, most semiconductor catalysts can only absorb and utilize part of light energy but not all solar energy, for example, titanium dioxide can only absorb and utilize ultraviolet light, iron oxide can only absorb and utilize visible light, and manganese oxide can only absorb and utilize near-infrared light. Therefore, how to find a photocatalyst capable of efficiently capturing ultraviolet, visible and infrared spectrums becomes a main way for improving the photocatalytic efficiency.
A Chinese patent with the application number of 201811030034.X discloses a full-spectrum response carbon dioxide reduction composite photocatalyst and a preparation method thereof, wherein the composite photocatalyst is Cu2In2ZnS5/Gd2O2Tb complex, Gd2O2Tb dispersed in Cu2In2ZnS5Upper, Cu2In2ZnS5Is a two-dimensional sheet structure of Gd2O2Tb is Gd2O2S, Tb nano-sheet is agglomerated. The Chinese invention patent with application number of 201811124607.5 discloses a preparation method of a black titanium dioxide nano composite material with an imitation moth-eye nano structure, which takes carbon cloth as a substrate material to provide a good diffusion channel for the dispersion of solar energy steam; the titanium dioxide nano composite material with the moth-eye-imitated nano structure introduces oxygen vacancies and a surface disordered structure on the surface of the carbon cloth through the reduction reaction of a reducing agent. The invention patent with the application number of 201710213349.7 discloses a high-efficiency full-spectral response CuS/graphene composite photocatalyst and a preparation method thereof, wherein the composite photocatalyst is formed by attaching CuS microspheres on graphene sheets, the graphene is of a two-dimensional sheet structure, and the CuS microspheres are assembled by CuS nanoparticles. The invention patent with application number 201010247518.7 discloses a preparation method and application of a photocatalytic material with ultraviolet visible full spectrum.The material is a nano material which takes bismuth oxychloride as a substrate and is doped with one or two elements of bromine and iodine.
Therefore, the full-spectrum photocatalytic material has less research, the preparation method is more complex, the cost is higher, and the large-scale industrial application cannot be realized.
Disclosure of Invention
Aiming at the defects, the first technical problem solved by the invention is to provide a novel light absorption material capable of efficiently capturing ultraviolet visible infrared spectra, and the material is simple in preparation method and low in cost.
The light absorbing material of the invention is VOxPowder, wherein x is more than 2 and less than or equal to 2.5.
Preferably, the material absorbs ultraviolet, visible and near-mid infrared light.
Preferably, the material is prepared by carrying out hydrothermal reaction on a vanadium-containing precursor and oxalic acid, wherein the temperature of the hydrothermal reaction is 220-250 ℃, and the molar ratio of vanadium in the vanadium-containing precursor to carbon in the oxalic acid is 1 (1.5-3.5).
Preferably, the vanadium-containing precursor includes any one of vanadium pentoxide and ammonium metavanadate.
Preferably, the reaction time of the hydrothermal reaction is 24 to 72 hours.
The second technical problem solved by the invention is to provide a preparation method of the light absorption material.
The preparation method of the light absorption material comprises the following steps:
1) mixing materials: mixing the oxalic acid solution and the vanadium-containing precursor, and fully stirring to obtain sol; wherein the molar ratio of vanadium in the vanadium-containing precursor to carbon in the oxalic acid is 1 (1.5-3.5); the vanadium-containing precursor comprises any one of vanadium pentoxide and ammonium metavanadate;
2) hydrothermal reaction: reacting the sol obtained in the step 1) at 220-250 ℃ for 24-72 hours to obtain a crude product;
3) and (3) post-reaction treatment: and washing and drying the crude product to obtain the light absorption material.
Preferably, in the step 1), the concentration of the oxalic acid solution is 0.2-1 mol/L.
Preferably, in the step 3), the washing is centrifugal washing with deionized water and absolute ethyl alcohol alternately.
Preferably, in the step 3), the drying temperature is 50-150 ℃ and the drying time is 6-24 hours.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for preparing a novel ultraviolet visible infrared light absorbing material VO by a hydrothermal synthesis methodxThe powder prepared has strong absorption to ultraviolet visible near-middle infrared light.
The method has the advantages of simple and easily-controlled preparation conditions and process, no environmental pollution, wide and cheap raw material sources and contribution to large-scale production. Preparation of VO by hydrothermal methodxThe powder is finished in liquid phase at one time, the product has uniform granularity, and impurities are not easy to be mixed. Prepared VOxThe photocatalyst has full absorption to sunlight, improves the utilization rate of solar energy, enhances the catalytic efficiency, can effectively degrade air pollutants, and is suitable for the fields of catalysts and hydrogen production by water photolysis. Furthermore, the VO producedxThe powder has high near-middle infrared absorption intensity, and can be applied to the fields of infrared absorption, infrared radiation prevention and the like.
Drawings
FIG. 1 shows VO prepared in example 1 of the present inventionxScanning electron micrographs of the powder.
FIG. 2 shows VO prepared in example 1 of the present inventionxXRD pattern of the powder.
FIG. 3 shows VO prepared in example 1 of the present inventionxAnd (3) selecting an electronic diffraction pattern of the powder.
FIG. 4 shows VO prepared in example 1 of the present inventionxEDS spectrum of powder.
FIG. 5 shows VO prepared in example 1 of the present inventionxThe powder has an X-ray photoelectron spectrum (V2p 3/2).
FIG. 6 shows VO prepared in example 1 of the present inventionxReflection spectrum of the powder.
FIG. 7 shows VO prepared in example 2 of the present inventionxXRD pattern of the powder.
FIG. 8 shows an embodiment of the present inventionExample 2 preparation of VOxReflection spectrum of the powder.
FIG. 9 shows VO prepared in example 7 of the present inventionxXRD pattern of the powder.
FIG. 10 shows VO prepared in example 9 of the present inventionxReflection spectrum of the powder.
FIG. 11 shows VO prepared in example 10 of the present inventionxReflection spectrum of the powder.
FIG. 12 shows VO prepared in example 13 of the present inventionxXRD pattern of the powder.
FIG. 13 shows VO prepared in example 13 of the present inventionxReflection spectrum of the powder.
FIG. 14 shows VO prepared in example 14 of the present inventionxReflection spectrum of the powder.
FIG. 15 shows VO prepared in example 16 of the present inventionxXRD pattern of the powder.
FIG. 16 shows VO prepared in example 17 of the present invention2XRD pattern of the powder.
Detailed Description
The light absorbing material of the invention is VOxPowder, wherein x is more than 2 and less than or equal to 2.5.
The light absorption material can absorb ultraviolet light, visible light and near-mid infrared light. The material has strong absorption to ultraviolet visible near-middle infrared light, and can be used in the fields of photocatalyst, hydrogen production by water photolysis, infrared light absorption, infrared radiation prevention and the like.
The light absorption material is prepared from a vanadium-containing precursor and oxalic acid through a hydrothermal reaction, wherein the temperature of the hydrothermal reaction is 220-250 ℃, and the molar ratio of vanadium in the vanadium-containing precursor to carbon in the oxalic acid is 1 (1.5-3.5).
Wherein, different from the common hydrothermal method for reducing pentavalent vanadium compounds, the reaction temperature of the light absorption material of the invention is higher, and the chemical mixture ratio of the raw materials and the reaction temperature are controlled, so as to obtain a brand new vanadium oxide VOxComparison of existing phase database, VOxIs a novel artificially synthesized vanadium oxide. On the other hand, when the reaction temperature is lowered, VO having excellent light absorption properties according to the present invention cannot be producedxAnd (3) powder.
Common vanadium-containing precursors are suitable for the present invention, and preferably, the vanadium-containing precursor includes any one of vanadium pentoxide and ammonium metavanadate.
Preferably, the reaction time of the hydrothermal reaction is 24 to 72 hours.
The preparation method of the light absorption material comprises the following steps:
1) mixing materials: mixing the oxalic acid solution and the vanadium-containing precursor, and fully stirring to obtain sol; wherein the molar ratio of vanadium in the vanadium-containing precursor to carbon in the oxalic acid is 1 (1.5-3.5); the vanadium-containing precursor comprises any one of vanadium pentoxide and ammonium metavanadate;
2) hydrothermal reaction: reacting the sol obtained in the step 1) at 220-250 ℃ for 24-72 hours to obtain a crude product;
3) and (3) post-reaction treatment: and washing and drying the crude product to obtain the light absorption material.
The method of the invention is to add oxalic acid (H) according to the preset V: C molar ratio2C2O4) Adding a vanadium-containing precursor into the deionized water solution, uniformly stirring to obtain sol, and transferring the sol into a hydrothermal kettle for hydrothermal reaction to obtain a hydrothermal product; the hydrothermal product is cooled, washed to neutrality by water and ethanol, and dried to obtain the required material with full spectrum high absorption to ultraviolet light, visible light and near-mid infrared light. The method has the advantages of simple and easily-controlled preparation conditions and process, no environmental pollution, wide and cheap raw material sources, and is beneficial to large-scale production. And the reaction is finished in a liquid phase at one time, the product has uniform granularity, and impurities are not easy to mix.
Preferably, in the step 1), the concentration of the oxalic acid solution is 0.2-1 mol/L.
Washing methods commonly used in the art are suitable for the present invention, and preferably, in step 3), the washing is centrifugal washing with deionized water and absolute ethyl alcohol alternately for several times.
The method has no special requirement on drying, and as an optimal scheme, in the step 3), the drying temperature is 50-150 ℃, and the drying time is 6-24 hours.
In some embodiments of the invention, the invention employs the following specific process:
(1) configuration H2C2O4Solution: weighing a certain amount of H2C2O4Putting the blocky solid in a beaker, weighing a certain volume of deionized water by using a measuring cylinder, pouring the deionized water into the beaker, and putting the beaker on a magnetic stirrer for stirring;
(2) weighing a certain amount of vanadium-containing precursor (V) according to a preset V to C molar ratio2O5Or NH4VO3) Pouring a certain volume of the solution prepared in the step 1) and putting the solution in a magnetic stirrer for fully stirring to obtain the required sol; the preferable proportion of the raw materials is as follows: the molar ratio of V to C is 1: (1.5-3.5);
(3) washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, and pouring the sol prepared in the step 2) into the inner container of the hydrothermal reaction kettle;
(4) the inner container is put into a reaction kettle to be sealed, and is put into a drying box to be set at a certain temperature and time for hydrothermal reaction; the temperature of the hydrothermal reaction is 220-250 ℃, and the time is 24-72 hours;
(5) taking out the reactant from the inner container after the reaction is finished, alternately centrifugally cleaning for a plurality of times by using deionized water and absolute ethyl alcohol, and finally drying in a drying oven for a certain time to obtain a required product; the drying temperature is 50-150 ℃, and the drying time is 6-24 hours.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention. Chemical raw material H used in examples2C2O4，V2O5And NH4VO3All are analytically pure.
Example 1
(1) Preparing sol: take 30mmol of H2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 10mmol of V is taken2O5Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle by using deionized water and absolute ethyl alcohol, and pouring the sol prepared in the step 1) into the hydrothermal reaction kettleReacting for 48 hours in an inner container of a 100mL hydrothermal reaction kettle at 240 ℃, cooling to room temperature, alternately washing the product for 3 times by using water and absolute ethyl alcohol, and drying for 10 hours in an oven at 100 ℃ to obtain a black product VOxA powdered light absorbing material.
VO produced in this examplexThe scanning electron micrograph of the powder is shown in FIG. 1, which shows that the morphology of the sample is similar to a spherical structure. The XRD pattern of the sample is shown in FIG. 2, and the sample is novel VO through detection of a databasexA crystal structure. The selected region electron diffraction pattern of the sample is shown in FIG. 3, indicating that the sample has a hexagonal symmetric crystal structure. EDS spectrum of the sample is shown in FIG. 4, which shows that the sample is vanadium oxide VOx. FIG. 5 is an X-ray photoelectron spectrum of a sample (V2 p)3/2) Shows that the valence of vanadium in the sample is +4 and +5, and the molecular formula is VOx(ii) a The binding peak area was further analyzed by fitting the data and the value of x was 2.1. Fig. 6 is an optical reflection spectrum of a sample, demonstrating that the sample has very strong absorption in uv, visible, and near-mid ir, and is an excellent full spectrum absorbing material.
Example 2
(1) Preparing sol: take 30mmol of H2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 20mmol of NH are taken4VO3Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 48 hours at 240 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 150 ℃ for 6 hours to obtain a black product VOxA powdered light absorbing material.
The VOxThe XRD pattern of the powder is shown in FIG. 7, which is similar to FIG. 2 and shows the novel VO of the inventionxA crystal structure. The reflection spectrum is shown in fig. 8, which proves that the material has very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 3
(1) Preparing sol: take 30mmol of H2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; taking 15mmol of V2O5Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 48 hours at 240 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in a 100 ℃ oven for 10 hours to obtain a black product VOxA powdered light absorbing material.
The VOxXRD pattern of powder is similar to that of FIG. 2, showing novel VO of the inventionxA crystal structure. The reflection spectrum is similar to that of fig. 6, and the material is proved to have very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 4
(1) Preparing sol: take 30mmol of H2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 30mmol of NH are taken4VO3Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 48 hours at 240 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 100 ℃ for 15 hours to obtain a black product VOxA powdered light absorbing material.
The VOxXRD pattern of powder is similar to that of FIG. 2, showing novel VO of the inventionxA crystal structure. The reflection spectrum is similar to that of fig. 6, and the material is proved to have very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 5
(1) System for makingPreparing sol: take 30mmol of H2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; taking 15mmol of V2O5Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 48 hours at 220 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 100 ℃ for 20 hours to obtain a black product VOxA powdered light absorbing material.
The VOxXRD pattern of powder is similar to that of FIG. 2, showing novel VO of the inventionxA crystal structure. The reflection spectrum is similar to that of fig. 6, and the material is proved to have very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 6
(1) Preparing sol: take 30mmol of H2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 30mmol of NH are taken4VO3Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 48 hours at 220 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 140 ℃ for 6 hours to obtain a black product VOxA powdered light absorbing material.
The VOxXRD pattern of powder is similar to that of FIG. 2, showing novel VO of the inventionxA crystal structure. The reflection spectrum is similar to that of fig. 6, and the material is proved to have very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 7
(1) Preparing sol: take 30mmol of H2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 20mmol of V is taken2O5Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 48 hours at 240 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 130 ℃ for 24 hours to obtain a black product VOxA powdered light absorbing material.
The VOxThe XRD pattern of the powder is shown in FIG. 9, which is similar to FIG. 2 and shows the novel VO of the inventionxA crystal structure. The reflection spectrum is similar to that of fig. 6, and the material is proved to have very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 8
(1) Preparing sol: take 30mmol of H2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 40mmol of NH are taken4VO3Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 48 hours at 240 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in a 110 ℃ oven for 24 hours to obtain a black product VOxA powdered light absorbing material.
The VOxXRD pattern of powder is similar to that of FIG. 2, showing novel VO of the inventionxA crystal structure. The reflection spectrum is similar to that of fig. 6, and the material is proved to have very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 9
(1) Preparing sol: 60mmol of H are taken2C2O4Added into 80mL of deionized water,uniformly stirring until the mixture is completely dissolved; then 24mmol of V is taken2O5Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 36 hours at 250 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 100 ℃ for 24 hours to obtain a black product VOxA powdered light absorbing material.
The VOxXRD pattern of powder is similar to that of FIG. 2, showing novel VO of the inventionxA crystal structure. The reflection spectrum is shown in fig. 10, which proves that the material has very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 10
(1) Preparing sol: 60mmol of H are taken2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 48mmol of NH are taken4VO3Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 36 hours at 250 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 140 ℃ for 6 hours to obtain a black product VOxA powdered light absorbing material.
The VOxXRD pattern of powder is similar to that of FIG. 2, showing novel VO of the inventionxA crystal structure. The reflection spectrum is shown in fig. 11, which proves that the material has very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 11
(1) Preparing sol: 60mmol of H are taken2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; taking 17.1mmol of V2O5Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 36 hours at 250 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 100 ℃ for 24 hours to obtain a black product VOxA powdered light absorbing material.
The VOxXRD pattern of powder is similar to that of FIG. 2, showing novel VO of the inventionxA crystal structure. The reflection spectrum is similar to that of fig. 6, and the material is proved to have very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 12
(1) Preparing sol: 60mmol of H are taken2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 34.3mmol of NH are taken4VO3Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 24 hours at 250 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 140 ℃ for 6 hours to obtain a black product VOxA powdered light absorbing material.
The VOxXRD pattern of powder is similar to that of FIG. 2, showing novel VO of the inventionxA crystal structure. The reflection spectrum is similar to that of fig. 6, and the material is proved to have very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 13
(1) Preparing sol: 80mmol of H are taken2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 32mmol of V is taken2O5Dissolving in the above solution, and stirring to completeDissolving to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 72 hours at 220 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 100 ℃ for 24 hours to obtain a black product VOxA powdered light absorbing material.
The VOxThe XRD pattern of the powder is shown in FIG. 12, which is similar to FIG. 2 and shows the novel VO of the inventionxA crystal structure. The reflection spectrum is shown in fig. 13, which proves that the material has very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 14
(1) Preparing sol: 80mmol of H are taken2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 64mmol of NH are taken4VO3Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 72 hours at 220 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 140 ℃ for 6 hours to obtain a black product VOxA powdered light absorbing material.
The VOxXRD pattern of powder is similar to that of FIG. 2, showing novel VO of the inventionxA crystal structure. The reflection spectrum is shown in fig. 14, which proves that the material has very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 15
(1) Preparing sol: 80mmol of H are taken2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 22.8mmol of V is taken2O5Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 72 hours at 220 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 100 ℃ for 24 hours to obtain a black product VOxA powdered light absorbing material.
The VOxXRD pattern of powder is similar to that of FIG. 2, showing novel VO of the inventionxA crystal structure. The reflection spectrum is similar to that of fig. 6, and the material is proved to have very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Example 16
(1) Preparing sol: 80mmol of H are taken2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 45.7mmol of NH are taken4VO3Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: washing the inner container of the hydrothermal reaction kettle with deionized water and absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 72 hours at 220 ℃, cooling to room temperature, alternately washing the product for 3 times with water and absolute ethyl alcohol, and drying in an oven at 140 ℃ for 6 hours to obtain a black product VOxA powdered light absorbing material.
The VOxThe XRD pattern of the powder is shown in FIG. 15, which is similar to FIG. 2 and shows the novel VO of the inventionxA crystal structure. The reflection spectrum is similar to that of fig. 6, and the material is proved to have very strong absorption in ultraviolet light, visible light and near-mid infrared light, and is an excellent full-spectrum absorption material.
Comparative example 1
(1) Preparing sol: take 30mmol of H2C2O4Adding the mixture into 80mL of deionized water, and uniformly stirring until the mixture is completely dissolved; then 30mmol of V is taken2O5Dissolving in the solution, and uniformly stirring until the solution is completely dissolved to obtain sol.
(2) Hydrothermal reaction: with deionized water andcleaning the inner container of the hydrothermal reaction kettle by absolute ethyl alcohol, pouring the sol prepared in the step 1) into a 100mL inner container of the hydrothermal reaction kettle, reacting for 48 hours at 180 ℃, cooling to room temperature, alternately washing the product for 3 times by using water and absolute ethyl alcohol, and drying for 24 hours in an oven at 80 ℃ to obtain a black product VO2The XRD of the powder material is shown in figure 16, which shows that the structure is VO2A crystal structure.
Claims (9)
1. A light absorbing material characterized by: the material is VOxPowder, wherein x is more than 2 and less than or equal to 2.5.
2. A light-absorbing material in accordance with claim 1, wherein: the material can absorb ultraviolet light, visible light and near-mid infrared light.
3. A light-absorbing material in accordance with claim 1 or 2, wherein: the material is prepared from a vanadium-containing precursor and oxalic acid through a hydrothermal reaction, wherein the temperature of the hydrothermal reaction is 220-250 ℃, and the molar ratio of vanadium in the vanadium-containing precursor to carbon in the oxalic acid is 1 (1.5-3.5).
4. A light-absorbing material in accordance with claim 3, wherein: the vanadium-containing precursor comprises any one of vanadium pentoxide and ammonium metavanadate.
5. A light-absorbing material in accordance with claim 3 or 4, wherein: the reaction time of the hydrothermal reaction is 24-72 hours.
6. The preparation method of the light absorption material is characterized by comprising the following steps:
1) mixing materials: mixing the oxalic acid solution and the vanadium-containing precursor, and fully stirring to obtain sol; wherein the molar ratio of vanadium in the vanadium-containing precursor to carbon in the oxalic acid is 1 (1.5-3.5); the vanadium-containing precursor comprises any one of vanadium pentoxide and ammonium metavanadate;
2) hydrothermal reaction: reacting the sol obtained in the step 1) at 220-250 ℃ for 24-72 hours to obtain a crude product;
3) and (3) post-reaction treatment: and washing and drying the crude product to obtain the light absorption material.
7. The method for producing a light-absorbing material according to claim 6, wherein: in the step 1), the concentration of the oxalic acid solution is 0.2-1 mol/L.
8. The method for producing a light-absorbing material according to claim 6 or 7, characterized in that: in the step 3), the washing is alternately centrifugal cleaning by using deionized water and absolute ethyl alcohol.
9. The method for producing a light-absorbing material according to any one of claims 6 to 8, wherein: in the step 3), the drying temperature is 50-150 ℃, and the drying time is 6-24 hours.
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| CN114873641A (en) * | 2022-05-23 | 2022-08-09 | 陕西科技大学 | Square VO2 nanosheet and preparation method and application thereof |
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| CN102294247A (en) * | 2011-07-15 | 2011-12-28 | 上海华明高技术（集团）有限公司 | Visible light responsive composite photocatalyst and preparation method thereof |
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