CN114538512A - Luminescent vanadium tetrasulfide, preparation method and application thereof - Google Patents
Luminescent vanadium tetrasulfide, preparation method and application thereof Download PDFInfo
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- CN114538512A CN114538512A CN202210025788.6A CN202210025788A CN114538512A CN 114538512 A CN114538512 A CN 114538512A CN 202210025788 A CN202210025788 A CN 202210025788A CN 114538512 A CN114538512 A CN 114538512A
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/69—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing vanadium
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Abstract
The invention discloses a preparation method of luminescent vanadium tetrasulfide, which comprises the following steps: will VS4Dispersing powder in a high-boiling point glycol solution to obtain a mixed solution A, ultrasonically vibrating the mixed solution A for 4-6h, heating to 70-100 ℃, stirring at the stirring speed of 300-600r/s for 3-7 days to obtain a mixed solution B, adding ethanol into the mixed solution B, centrifugally washing, and drying to obtain the luminescent vanadium tetrasulfide. The preparation method is simple and efficient. The invention also discloses luminescent vanadium tetrasulfide prepared by the preparation method of the luminescent vanadium tetrasulfide. The vanadium tetrasulfide has high catalytic performance and good luminescence property. The invention also discloses application of the luminescent vanadium tetrasulfide in degrading and purifying organic pollutants.
Description
Technical Field
The invention belongs to the field of luminescent materials, and particularly relates to luminescent vanadium tetrasulfide as well as a preparation method and application thereof.
Background
The transition metal sulfide has unique physical chemistryThe properties and the crystal structure can be widely applied to the field of energy sources, so that the material becomes a potential luminescent and catalytic material. For example, as lithium electrodes, catalysts, etc., are a very important class of materials. In particular, vanadium disulfide (VS2) is of particular interest. VS with lamellar results has recently been reported2The quantum dots and the nano-sheets show good luminescence characteristics and excellent photocatalytic pollutant degradation performance.
So far, vanadium disulfide powder with excellent performance is difficult to obtain by direct combination of elements, is mostly synthesized in an organic solvent, the preparation method is complex to operate, expensive cost is required, the valence state of vanadium in the vanadium is difficult to control, and VS is difficult to obtain2The preparation cost of the vanadium disulfide powder is greatly improved, and the large-scale production is difficult to realize.
VS metallic compared to band structure2Vanadium tetrasulfide (VS)4) Has a special one-dimensional chain structure and a semiconductor band gap structure. Has received much attention in battery electrode materials in view of its high theoretical specific capacity and excellent electrochemical reversibility. VS4Has a one-dimensional chain semiconductor structure and multiple active sites, which has great application prospect in flexible light-emitting devices and photocatalytic degradation pollution, but currently VS4The luminescence and catalytic properties of (A) are rarely reported.
The major difficulty facing today is VS4The band gap is about 1.0eV, and photocatalysis by visible light is impossible, and similarly, the band gap is narrow, and light emission in the visible light region cannot be realized. VS4The interlamellar spacing between the one-dimensional atomic chains is large (0.583nm), the atomic chains are only connected through weak van der Waals bonds to provide a loose one-dimensional stacking structure, and VS can be regulated and controlled by regulating and controlling the stacking structure of the V-S atomic chains4Micro-morphology and electronic band structure. VS4The change of the atomic chain structure can make the atomic chain structure change from the indirect band gap of the bulk to the direct band gap. The transition of electrons in a semiconductor having a direct band gap does not require release or absorption of phonons (i.e., lattice vibration), thereby avoiding energy loss, and exhibiting excellent light emission characteristics at short wavelengths such as a visible light region, etc.;furthermore, VS4The one-dimensional atomic chain structure is beneficial to the migration of carriers, so that the stacking structure of the atomic chain is changed, the electron/hole mobility of the atomic chain can be regulated and controlled, and the VS is reduced4The dimension and the specific surface area of the photocatalyst are increased, the active sites of the photocatalyst are increased, and excellent photocatalytic activity can be obtained, so that the performance of degrading pollutants by photocatalysis is improved.
Therefore, development of regulatory VS4An effective preparation method of a stacking mode of a one-dimensional chain structure is a key problem to be solved at present. At present, few stripping methods are used for low-dimensional materials, wherein a solvent dispersion method is simple and efficient, and shows a good effect. At present, the method for dispersing and stripping one-dimensional sulfide and selenide can only realize the regulation and control of micro-nano scale, and the method does not realize obvious atom-level local stacking
Disclosure of Invention
The invention provides a preparation method of luminescent vanadium tetrasulfide, which is simple and efficient, and the prepared vanadium tetrasulfide has high catalytic performance and good luminescent property.
A preparation method of luminescent vanadium tetrasulfide comprises the following steps: will VS4Dispersing powder in a high-boiling point glycol solution to obtain a mixed solution A, ultrasonically vibrating the mixed solution A for 4-6h, heating to 70-100 ℃, stirring at the stirring speed of 300-600r/s for 3-7 days to obtain a mixed solution B, adding ethanol into the mixed solution B, centrifugally washing, and drying to obtain the luminescent vanadium tetrasulfide.
Because of VS4The crystal is relatively stable, and the chemical bond in the crystal is very difficult to break. Therefore, high temperature of 70-100 ℃ is adopted to ensure that glycol molecules in high boiling point solvent are infiltrated into VS4Is expanded and then broken by ultrasonic vibration and long-term stirring (3-7) days4Van der Waals force between the medium V-S atomic chains, so that regulation and control of a V-S atomic chain stacking structure are realized, and the luminescent vanadium tetrasulfide is obtained and has high catalytic performance.
The required heating temperature is not too low or too high, and the stirring time is not too short. The dispersing effect is not obvious when the temperature is too low and the stirring time is too short, and the dispersion is easy to damage when the temperature is too highVS4The structure of the atomic chain and the initiation of other chemical reactions.
The dispersion temperature of the high-boiling point glycol solution is 70-120 ℃.
The VS4The mass/solution ratio of the powder to the high boiling point ethylene glycol is 0.1-0.3 g/L.
The centrifugal washing parameters are as follows: the centrifugal washing speed is 4000-8000r/s, and the centrifugal washing time is 4-8 min.
The drying parameters are as follows: the drying temperature is 40-60 deg.C, and the drying time is 8-12 h.
The luminescent vanadium tetrasulfide prepared by the preparation method has a V-S atomic chain bending stacking structure.
The luminous vanadium tetrasulfide has 002 or 011 crystal faces and 0.4-0.8nm crystal face spacing.
The luminescent vanadium tetrasulfide has a luminescent peak in a visible light range with the wavelength of 390-500 nm.
The luminescent vanadium tetrasulfide is applied to degrading and purifying organic pollutants.
The organic pollutant is rhodamine, and is completely degraded within 4-8 h.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the luminescent vanadium tetrasulfide provided by the invention utilizes a stirring mode with higher temperature and higher strength to permeate ethylene glycol into the vanadium tetrasulfide and change the chain structure of the vanadium tetrasulfide to form a stacked curved chain structure, so that the vanadium tetrasulfide prepared by the preparation method provided by the invention can emit light in a visible light range with the wavelength of 390-500nm, has better photocatalytic performance, can be applied to aspects such as flexible light-emitting devices, photocatalysts and the like, and is simple and easy to edit, low in cost and capable of realizing under the normal pressure condition.
Drawings
FIG. 1 is a graph showing comparative example 1 (VS)4-0), comparative example 2 (VS)4-1), example 1 (VS)4-2), example 2 (VS)4-3) preparation of VS4Wherein FIG. 1(a) is an XRD pattern of 10 to 40 degrees in diffraction angleXRD pattern, FIG. 1(b) is XRD pattern with diffraction angle of 15-17.5 degrees.
FIG. 2 is VS prepared in comparative example 1, and example 24In which FIG. 2(a) is a comparative example 1 (VS)4HRTEM image of-0), FIG. 2(b) is example 1 (VS)4HRTEM image of-2), FIGS. 2(c) and (d) are example 2 (VS)4HRTEM image of-3).
FIG. 3 is VS prepared in comparative example 1 and example 24-3 luminescence map.
FIG. 4 is VS prepared in example 24-3 rhodamine degradation ultraviolet absorption map.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary of the invention and are not intended to be limiting thereof.
Comparative example 1
1g of ammonium metavanadate (NaVO) was weighed3) Mixing with 3.6g Thioacetamide (TAA), and stirring in 60ml deionized water; dropwise adding prepared 3mol/L hydrochloric acid in the stirring process to adjust the pH value to 3; stirring for 40 min, pouring into polytetrafluoroethylene lining, placing into a hydrothermal reaction kettle, keeping the temperature at 180 ℃ in an oven for 24h, and taking out after cooling to room temperature. Pouring a sample in the hydrothermal reaction kettle into a centrifuge tube sample; adding ethanol into the solution, performing ultrasonic oscillation uniformly, centrifuging at 8000r/s for 3min, removing supernatant, adding ethanol, performing ultrasonic oscillation uniformly, centrifuging, repeating the step for 3 times, drying in oven at 60 deg.C for 18h, taking out, and grinding to obtain VS4Powder precursor, noted VS4-0. VS by XRD as shown in FIGS. 1(a) and 1(b)4The-0 diffraction peak may correspond to VS421-1434 of a PDF card. As shown in FIG. 2c, the high resolution electron microscopy results show VS4The spacing between the-0 planes is 0.310nm and is assigned to the 301 plane.
Comparative example 2
The normal-temperature stirring ultrasonic treatment method comprises the following steps: weighing 20mg VS4-0 powder precursor is put into a single-neck flask, 40ml of acetone is poured into the single-neck flask, the mixture is taken out after being subjected to ultrasonic treatment for 3 days by an ultrasonic cleaning machine, the mixture is centrifuged for 4min at the rotating speed of 6000r/s by a centrifuge, ethanol is poured into the mixture after supernatant fluid is removed, the mixture is continuously centrifuged for 3 times, finally the supernatant fluid is poured out, and the mixture is put into a drying oven to be driedDrying at 60 deg.C for 18h, and storing at room temperature to obtain VS4Powder, designated VS-1. As shown in FIGS. 1(a) and 1(b), the diffraction peak of XRD corresponds to VS4PDF card 87-0603. And VS4Comparison of-0, VS4The diffraction peak angle of-1 did not change.
Example 1
High-temperature stirring treatment method 1: weighing 15mg VS4-0 powder precursor into a single-neck flask and 120ml ethylene glycol was poured into the flask and stirred for 6 days by heating to 100 ℃ with a magnetic stirrer at a stirring rate of 300r/s, and the sample obtained, designated VS, was stored at room temperature4-2. As shown in FIGS. 1(a) and 1(b), the diffraction peak of XRD is shifted to a low angle by 0.15 degrees, which is related to VS4Larger interplanar spacing, VS, than 14-2 lattice spacing is significantly broadened. As shown in FIG. 2(b), the high resolution electron microscope showed that the interplanar spacing was 0.607nm, which was attributed to the 002 plane, and a unique phenomenon of lattice bending distortion was present. However VS4The-0 lattice does not change significantly as shown in FIG. 2 (a). The above results show that van der waals forces between vanadium sulfur atom chains are destroyed by the glycol solvent treatment at 100 ℃, resulting in significant lattice distortion.
Example 2
High-temperature stirring treatment method 2: in contrast to example 1, 15mg of VS was weighed out4-0 powder precursor is put into a single-neck flask, 50ml of ethylene glycol is poured into the single-neck flask, and the mixture is heated to 70 ℃ by a magnetic stirrer and stirred for 3 days at a stirring speed of 500 r/s; adding ethanol, centrifuging at 8000r/s for 4min, removing supernatant, adding ethanol, centrifuging for 3 times, removing supernatant, drying at 60 deg.C for 18 hr, storing at room temperature to obtain sample designated as VS4-3. As shown in FIGS. 1(a) and 1(b), the diffraction peak of XRD is shifted to a low angle of 0.18 degrees, in relation to VS4The-1 crystal face spacing becomes larger and the lattice spacing becomes significantly wider. As shown in FIGS. 2c and 2d, the high resolution electron microscope shows that the interplanar spacing is 0.568nm, which belongs to 011 planes, and a unique crystal lattice bending distortion structure and an irregular chain-shaped stacking structure exist. The results show that the van der Waals force between vanadium and sulfur atom chains is destroyed after the treatment at 70 ℃ by the glycol solvent, resulting in the destructionThe crystal lattice is significantly distorted. And VS 42 comparison, VS4Local lattice distortion of-3 is more pronounced and therefore is investigated as a step in luminescence and catalytic performance.
Characterization of luminescence Properties
Respectively weighing VS4-0 and VS 43 fluorescence spectra of 2mg each, as shown in FIG. 3, finding VS4-3 a distinct luminescence peak in the visible range of 390-500nm, whereas the untreated VS 40 has no light emission characteristic.
Application example
Testing VS4-3 photocatalytic rhodamine (RhB) degradation: weighing 0.5mg of VS4And 3, dispersing the rhodamine in an aqueous solution of rhodamine with the concentration of 0.005g/L, and irradiating the rhodamine aqueous solution for 8 hours by using a simulated solar light source, wherein the pink completely disappears, and the absorption peak intensity is close to zero, which indicates that the rhodamine is completely degraded, and is shown in FIG. 4. The results show that VS4-3 has good photocatalytic performance for degrading pollutants under the irradiation of sunlight.
Claims (9)
1. A preparation method of luminescent vanadium tetrasulfide is characterized by comprising the following steps: will VS4Dispersing powder in a high-boiling point glycol solution to obtain a mixed solution A, ultrasonically vibrating the mixed solution A for 4-6h, heating to 70-100 ℃, stirring at the stirring speed of 300-600r/s for 3-7 days to obtain a mixed solution B, adding ethanol into the mixed solution B, centrifugally washing, and drying to obtain the luminescent vanadium tetrasulfide.
2. The method of claim 1, wherein the dispersion temperature of the high boiling point glycol solution is 70-100 ℃.
3. The method of claim 1, wherein said VS is provided by4The mass/solution ratio of the powder to the high boiling point ethylene glycol is 0.1-0.3 g/L.
4. The method of claim 1, wherein the centrifugal washing parameters are: the centrifugal washing speed is 4000-8000r/s, and the centrifugal washing time is 4-8 min.
5. The luminescent vanadium tetrasulfide prepared by the method for preparing the luminescent vanadium tetrasulfide according to any one of claims 1 to 4, characterized in that the luminescent vanadium tetrasulfide has a V-S atomic chain bent stacking structure.
6. The luminescent vanadium tetrasulfide prepared by the preparation method of the luminescent vanadium tetrasulfide of claim 5, characterized in that the luminescent vanadium tetrasulfide is 002 or 011 crystal planes, and the spacing between the crystal planes is 0.4-0.8 nm.
7. The luminescent vanadium tetrasulfide prepared by the preparation method of the luminescent vanadium tetrasulfide as claimed in claim 5, characterized in that the luminescent vanadium tetrasulfide has a luminescence peak in the wavelength range of 390-500nm visible light.
8. The application of the luminescent vanadium tetrasulfide prepared by the preparation method of the luminescent vanadium tetrasulfide according to claim 5 in degrading and purifying organic pollutants.
9. The application of the luminescent vanadium tetrasulfide prepared by the preparation method of the luminescent vanadium tetrasulfide according to claim 8 in degrading and purifying organic pollutants, characterized in that the organic pollutants are rhodamine, and the degradation time is 4-8 h.
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CN115215421A (en) * | 2022-08-16 | 2022-10-21 | 南华大学 | Application of vanadium tetrasulfide in degradation of organic pollutants |
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