CN114538512B - Luminescent vanadium tetrasulfide and preparation method and application thereof - Google Patents
Luminescent vanadium tetrasulfide and preparation method and application thereof Download PDFInfo
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- CN114538512B CN114538512B CN202210025788.6A CN202210025788A CN114538512B CN 114538512 B CN114538512 B CN 114538512B CN 202210025788 A CN202210025788 A CN 202210025788A CN 114538512 B CN114538512 B CN 114538512B
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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
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- 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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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
- C09K11/691—Chalcogenides
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- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/77—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/78—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by stacking-plane distances or stacking sequences
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Abstract
The invention discloses a preparation method of luminescent vanadium tetrasulfide, which comprises the following steps: VS 4 Dispersing the powder in a high boiling point glycol solution to obtain a mixed solution A, carrying out ultrasonic vibration on the mixed solution A for 4-6 hours, heating to 70-100 ℃, stirring for 3-7 days at a stirring rate of 300-600r/s to obtain a mixed solution B, adding ethanol into the mixed solution B, centrifuging, washing and drying to obtain the luminescent vanadium tetrasulfide. The preparation method is simple and efficient. The invention also discloses the luminescent vanadium tetrasulfide prepared by the luminescent vanadium tetrasulfide preparation method. The vanadium tetrasulfide has higher catalytic performance and better luminescence characteristic. 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 and a preparation method and application thereof.
Background
The transition metal sulfide has unique physical and chemical properties and crystal structure, and can be widely applied to the field of energy, so that the transition metal sulfide 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 (VS 2) is of particular interest. VS with lamellar results has recently been reported 2 Quantum dots and nanoplatelets exhibit good luminescence properties and excellent photocatalytic contaminant degradation properties.
Up to now, vanadium disulfide powder with excellent performance is difficult to obtain by direct combination of elements, is mostly synthesized in organic solvent, has complex preparation method operation, requires expensive cost, and is difficult to control the valence state of vanadium in the vanadium disulfide powder, so that VS is difficult to obtain 2 This allows for the disulfide phaseThe preparation cost of the vanadium powder is greatly increased, and the large-scale production is difficult to realize.
VS compared to that with metallic band structure 2 Vanadium tetrasulfide (VS 4 ) Has a special one-dimensional chain structure and a semiconductor band gap structure. There is a great deal of attention in the battery electrode materials in view of their high theoretical specific capacity and excellent electrochemical reversibility. VS (virtual switch) 4 The single-dimensional chain-shaped semiconductor structure and multiple active sites are provided, which has great application prospect in flexible light-emitting devices and photocatalytic degradation pollution, but at present VS 4 Has little report on the luminescence and catalytic properties of (C).
The main difficulty facing today is VS 4 The band gap is about 1.0eV, and photocatalysis by visible light is not possible, and the band gap is also very narrow, so that light emission in the visible light region is not possible. VS (virtual switch) 4 The interlayer spacing between the one-dimensional atomic chains is larger (0.583 nm), the atomic chains are connected only through weak Van der Waals bonds, a loose one-dimensional stacked structure is provided, and the VS can be regulated by regulating the stacked structure of the V-S atomic chains 4 Microcosmic morphology and electron band structure. VS (virtual switch) 4 The change in the structure of the atomic chain can shift it from the indirect bandgap of the bulk towards the direct bandgap. Electrons in semiconductors having a direct band gap do not need to release or absorb phonons (i.e., lattice vibration) upon transition, thereby avoiding energy loss, exhibiting excellent light emission characteristics at short wavelengths such as the visible region, etc.; in addition, VS 4 The one-dimensional atomic chain structure of the catalyst is favorable for the migration of carriers, so that the stacking structure of the atomic chain is changed, the mobility of electrons/holes of the catalyst can be regulated and controlled, and the VS is reduced 4 The dimension and the specific surface area of the catalyst are increased, and the excellent photocatalytic activity can be obtained, so that the performance of photocatalytic degradation of pollutants is improved.
Thus, the development of regulatory VS 4 An effective preparation method of a one-dimensional chain structure stacking mode is a key problem to be solved at present. At present, the stripping method for the low-dimensional material is less, wherein the solvent dispersion method is simpler and more efficient, and good effect is shown. At present, the dispersion and stripping method for one-dimensional sulfides and selenides can only realize micro-nano scale regulation and control, and no display is realizedLocal stacking at atomic level
Disclosure of Invention
The invention provides a preparation method of luminescent vanadium tetrasulfide, which is simple and efficient, and the prepared vanadium tetrasulfide has higher catalytic performance and better luminescent characteristic.
A method for preparing luminescent vanadium tetrasulfide, comprising: VS 4 Dispersing the powder in a high boiling point glycol solution to obtain a mixed solution A, carrying out ultrasonic vibration on the mixed solution A for 4-6 hours, heating to 70-100 ℃, stirring for 3-7 days at a stirring rate of 300-600r/s to obtain a mixed solution B, adding ethanol into the mixed solution B, centrifuging, washing and drying to obtain the luminescent vanadium tetrasulfide.
Because of VS 4 The crystals are relatively stable and breaking chemical bonds in the crystals is very difficult. Thus, the high boiling point solvent glycol molecules penetrate into VS by adopting high temperature of 70-100 DEG C 4 Is expanded and then broken by ultrasonic vibration and long-term stirring (3-7 days) 4 Van der Waals force between the V-S atomic chains is achieved, and therefore regulation and control of the V-S atomic chain stacking structure are achieved, and luminescent vanadium tetrasulfide is obtained and has high catalytic performance.
The required heating temperature is not too low nor too high, and the stirring time is not too short. Too low a temperature and too short a stirring time, the dispersing effect is not obvious, and too high a temperature is easy to destroy VS 4 The atomic chain structure and other chemical reactions are initiated.
The dispersion temperature of the high-boiling point glycol solution is 70-120 ℃.
The VS 4 The mass/solution ratio of the powder to the high boiling point glycol is 0.1-0.3g/L.
The centrifugal washing parameters are as follows: the centrifugal washing speed is 4000-8000r/s, and the centrifugal washing time is 4-8min.
The drying parameters are as follows: the drying temperature is 40-60 ℃ and the drying time is 8-12h.
The luminescent vanadium tetrasulfide prepared by the preparation method of the luminescent vanadium tetrasulfide has a V-S atomic chain bending stacking structure.
The luminescent vanadium tetrasulfide has 002 or 011 crystal faces with the interplanar spacing of 0.4-0.8nm.
The luminescent vanadium tetrasulfide has a luminescence peak in a visible light range with the wavelength of 390-500 nm.
The application of the luminescent vanadium tetrasulfide in degrading and purifying organic pollutants.
The organic pollutant is rhodamine and is completely degraded for 4-8 hours.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the luminous vanadium tetrasulfide provided by the invention utilizes a stirring mode with higher temperature and higher strength to infiltrate ethylene glycol into the vanadium tetrasulfide, and changes the chain structure of the vanadium tetrasulfide to form a stacked and bent chain structure, so that the vanadium tetrasulfide prepared by the preparation method of the invention emits light in the visible light range with the wavelength of 390-500nm, has better photocatalytic performance, can be applied to the aspects of flexible light emitting devices, photocatalysts and the like, and the preparation method provided by the invention is simple, easy to edit, low in cost and can be realized under normal pressure conditions.
Drawings
FIG. 1 is comparative example 1 (VS 4 -0), comparative example 2 (VS 4 -1), example 1 (VS 4 -2), example 2 (VS 4 -3) prepared VS 4 Wherein FIG. 1 (a) is an XRD pattern having a diffraction angle of 10 to 40 degrees and FIG. 1 (b) is an XRD pattern having a diffraction angle of 15 to 17.5 degrees.
FIG. 2 shows VS prepared in comparative example 1, example 2 4 Wherein FIG. 2 (a) is a graph of comparative example 1 (VS 4 -0), FIG. 2 (b) is example 1 (VS) 4 -2) HRTEM images, fig. 2 (c) and (d) are example 2 (VS 4 -3) HRTEM diagram.
FIG. 3 shows the VS prepared in comparative example 1 and example 2 4 -3.
FIG. 4 is a VS prepared in example 2 4 -rhodamine degradation ultraviolet absorbance map of 3.
Detailed Description
The invention is further illustrated by the following examples, which are given by way of illustration only and are not to be construed as limiting the scope of the invention.
Comparative example 1
1g of ammonium metavanadate (NaVO) was weighed out 3 ) And 3.6g Thioacetamide (TAA) in 60ml deionized water; dropwise adding the prepared 3mol/L hydrochloric acid in the stirring process to adjust the pH value to 3; stirring for 40 min, pouring into polytetrafluoroethylene lining, loading into a hydrothermal reaction kettle, preserving heat for 24h at 180 ℃ in an oven, 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, ultrasonically oscillating, centrifuging at 8000r/s for 3min, removing supernatant, adding ethanol, ultrasonically oscillating, centrifuging, repeating the steps for 3 times, drying in oven at 60deg.C for 18 hr, taking out, and grinding to obtain VS 4 Powder precursor, denoted as VS 4 -0. As shown in FIGS. 1 (a) and 1 (b), VS of XRD 4 The-0 diffraction peak can correspond to VS 4 PDF card 21-1434 of (f). As shown in FIG. 2c, the high resolution electron microscope results indicate VS 4 The-0 interplanar spacing is 0.310nm, which is attributed to the 301 lattice plane.
Comparative example 2
The ultrasonic treatment method by stirring at normal temperature comprises the following steps: weigh 20mg VS 4 Placing the powder precursor into a single-neck flask, pouring 40ml of acetone into the single-neck flask, taking out the single-neck flask after ultrasonic treatment for 3 days by an ultrasonic cleaning machine, centrifuging for 4min at the rotation speed of 6000r/s by a centrifuge, removing supernatant, pouring ethanol into the single-neck flask, continuously centrifuging for 3 times, finally pouring the supernatant, placing the supernatant into a drying oven, drying at 60 ℃ for 18h, taking out the supernatant, and preserving the supernatant at room temperature to obtain VS 4 Powder, designated VS-1. As shown in FIGS. 1 (a) and 1 (b), the diffraction peaks of XRD may correspond to VS 4 PDF card 87-0603 of (f). With VS 4 -0 VS 4 The diffraction peak angle of-1 is unchanged.
Example 1
High-temperature stirring treatment method 1: weigh 15mg VS 4 -0 placing the powder precursor into a single-neck flask, pouring 120ml of glycol, heating to 100deg.C with a magnetic stirrer, stirring for 6 days at a stirring rate of 300r/s, and preserving at room temperature to obtain a sample, denoted as VS 4 -2. As shown in FIGS. 1 (a) and 1 (b), the diffraction peak of XRD was shifted 0.15 degrees to a low angle, compared with VS 4 -1 is larger than the interplanar spacing, VS 4 -2 the 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 that there was a unique lattice bending distortion phenomenon. However VS 4 No significant change in the-0 lattice occurs as shown in fig. 2 (a). The above results indicate that the van der Waals forces between vanadium and sulfur atom chains are destroyed after the ethylene glycol solvent is treated at 100 ℃, resulting in significant lattice distortion.
Example 2
High-temperature stirring treatment method 2: unlike example 1, 15mg of VS was weighed 4 -0 placing the powder precursor into a single-neck flask, pouring 50ml of ethylene glycol into the single-neck flask, heating to 70 ℃ by using a magnetic stirrer, and stirring for 3 days at a stirring speed of 500r/s; adding ethanol, centrifuging with a centrifuge 8000r/s for 4min, removing supernatant, adding ethanol, centrifuging for 3 times, pouring supernatant, drying at 60deg.C for 18 hr, and storing at room temperature to obtain sample (VS) 4 -3. As shown in FIGS. 1 (a) and 1 (b), the diffraction peak of XRD was shifted to a low angle by 0.18 degrees, compared with VS 4 -1 is significantly broader than the lattice spacing. As shown in fig. 2c and 2d, the high resolution electron microscope showed that the interplanar spacing was 0.568nm, which is assigned to the 011 plane, and that there was a unique lattice bending distortion structure and an irregular chain-like stacking structure. The results show that after the ethylene glycol solvent is treated at 70 ℃, van der Waals force among vanadium and sulfur atom chains is destroyed, so that the crystal lattice is obviously distorted. With VS 4 -2 VS 4 The local lattice distortion of-3 is more pronounced and is therefore considered as a next step in luminescence and catalytic performance studies.
Characterization of luminescence properties
Respectively weigh VS 4 -0 and VS 4 -3 each 2mg test fluorescence spectrum, as shown in FIG. 3, found VS 4 -3 has a distinct luminescence peak in the visible range of 390-500nm, whereas untreated VS 4 -0 has no luminescence properties.
Application example
Testing VS 4 -3 photocatalytic rhodamine (RhB) degradation performance: 0.5mg of VS was weighed out 4 -3, dispersed in an aqueous rhodamine solution at a concentration of 0.005g/L, using a dieThe quasi-solar light source irradiates for 8 hours, the pink completely disappears, and the absorption peak intensity is close to zero, which indicates that rhodamine is completely degraded, as shown in figure 4. The results indicate VS 4 3 has good photocatalytic performance for degrading pollutants under the irradiation of sunlight.
Claims (9)
1. A method for preparing luminescent vanadium tetrasulfide, comprising: VS 4 Dispersing the powder in a high boiling point glycol solution to obtain a mixed solution A, carrying out ultrasonic vibration on the mixed solution A for 4-6 hours, heating to 70-100 ℃, stirring for 3-7 days at a stirring rate of 300-600r/s to obtain a mixed solution B, adding ethanol into the mixed solution B, centrifuging, washing and drying to obtain the luminescent vanadium tetrasulfide.
2. The method for preparing luminescent vanadium tetrasulfide according to claim 1, wherein the dispersion temperature of the high boiling point ethylene glycol solution is 70-100 ℃.
3. The method for preparing luminescent vanadium tetrasulfide according to claim 1, wherein the VS 4 The mass/solution ratio of the powder to the high boiling point glycol is 0.1-0.3g/L.
4. The method for preparing luminescent vanadium tetrasulfide according to claim 1, wherein the centrifugal washing parameters are as follows: the centrifugal washing speed is 4000-8000r/s, and the centrifugal washing time is 4-8min.
5. The luminescent vanadium tetrasulfide produced by the process for producing luminescent vanadium tetrasulfide according to any one of claims 1-4, wherein the luminescent vanadium tetrasulfide has a V-S atomic chain curved stacking structure.
6. The luminescent vanadium tetrasulfide prepared by the preparation method of luminescent vanadium tetrasulfide according to claim 5, wherein the luminescent vanadium tetrasulfide has 002 or 011 crystal faces with a interplanar spacing of 0.4-0.8nm.
7. The luminescent vanadium tetrasulfide produced by the process for producing luminescent vanadium tetrasulfide according to claim 5, wherein the luminescent vanadium tetrasulfide has a luminescence peak in the visible light range having a wavelength of 390 to 500 nm.
8. The method for preparing luminescent vanadium tetrasulfide according to claim 5, wherein the luminescent vanadium tetrasulfide is used for degrading and purifying organic pollutants.
9. The application of the luminescent vanadium tetrasulfide prepared by the preparation method of the luminescent vanadium tetrasulfide in degrading and purifying organic pollutants, which is characterized in that the organic pollutant is rhodamine, and the degradation time is 4-8 hours.
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| CN107381636A (en) * | 2017-07-11 | 2017-11-24 | 陕西科技大学 | A kind of vanadic sulfide powder of nano-particles self assemble three dimensional micron cauliflower-shaped four and its preparation method and application |
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| CN107381636A (en) * | 2017-07-11 | 2017-11-24 | 陕西科技大学 | A kind of vanadic sulfide powder of nano-particles self assemble three dimensional micron cauliflower-shaped four and its preparation method and application |
| CN108862381A (en) * | 2018-06-26 | 2018-11-23 | 中国科学院宁波材料技术与工程研究所 | Four vanadic sulfide electrode materials of one kind and its preparation method and application |
| CN110180556A (en) * | 2019-05-28 | 2019-08-30 | 广州大学 | A kind of four vanadic sulfide fenton catalyst of modification and its preparation method and application |
| AU2020101299A4 (en) * | 2020-06-08 | 2020-08-20 | Qilu University Of Technology | Vanadium tetrasulfide-nitrogen-doped carbon tube composite and preparation method and use thereof |
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