CN113198501A - Novel TiO (titanium dioxide)2Preparation method of/MXene composite material - Google Patents
Novel TiO (titanium dioxide)2Preparation method of/MXene composite material Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000004408 titanium dioxide Substances 0.000 title claims description 4
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000010936 titanium Substances 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910001495 sodium tetrafluoroborate Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 2
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- 230000035484 reaction time Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
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- 229910009819 Ti3C2 Inorganic materials 0.000 abstract description 37
- 239000013078 crystal Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000000707 layer-by-layer assembly Methods 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
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- 238000005215 recombination Methods 0.000 description 2
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- 229910052723 transition metal Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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- 239000000203 mixture Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research 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
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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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
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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Abstract
The invention discloses a novel TiO2MXene composite material and preparation method thereof, wherein MXene comprises Ti3C2、Ti2C, preparing TiO by adopting calcining method by using MXene as substrate2the/MXene composite material. The process is that firstly, a two-dimensional lamellar material MXene with good lamellar structure is prepared, the MXene is taken as a Ti source, and the MXene and NaBF are passed through4Fully grinding, and then calcining at high temperature to obtain mixed-phase TiO2the/MXene composite material. The preparation process adopted by the invention is simple, and the prepared mixed phase TiO2TiO in/MXene composite material2Anatase and rutile crystal forms appear and are distributed on the surface of the MXene sheet layer, and the charge separation efficiency of the composite material is enhanced. The novel TiO2the/MXene composite material can be used as a catalyst material and applied to the field of photoelectrocatalysis.
Description
Technical Field
The invention relates to a novel TiO2A preparation method of/MXene composite material.
Background
As the population grows, environmental pollution becomes a significant risk and challenge for people today. The excessive burning of fossil fuels increases carbon emissions, which in turn causes severe greenhouse effect, and is not conducive to sustainable development. The search for green and environment-friendly renewable energy sources with rich resources is urgent. Photocatalytic technology is considered to be an environmentally clean and sustainable process.
An ideal photovoltaic module would be one composed of low cost, high stability and moderate bandgap semiconductors to allow efficient use of solar energy. TiO 22The advantages of good stability, low price, moderate band gap position, simple preparation method and the like are widely concerned. Anatase, rutile and brookite are TiO2The three crystal phase structures of (1). Because of the band gap difference of different crystal phases, TiO with different crystal phase structures is mixed2It will be possible to increase the separation efficiency of the photo-generated electron pair.
MXene refers to a two-dimensional transition metal carbide or carbonitride having a graphene-like structure. It is prepared by stripping MAX phase, wherein M is transition metal element such as Ti, V, Ta; a is a group IIIA and IVA element, e.g. Al, Si; x is a C or N element. The surface of the prepared MXene is adsorbed with functional groups such as-O, -OH and-F, and the conductivity and the hydrophilicity of the MXene are influenced by different functional groups. Two-dimensional Ti3C2As one of MXene materials, the MXene materials have attracted wide attention due to excellent conductivity and simple preparation process, and have been studied in the aspects of photoelectrocatalysis, energy storage materials, antibiosis, bacteriostasis and the like. Ti3C2As a carbon material, it is widely known as a high-activity photocatalyst. Ti3C2The Ti atom on the film can be used as a bonding site to produce TiO2A natural platform is provided.
After organic pollutants are attached to the surface of a single semiconductor catalyst, strong oxidation is carried out to degrade the organic pollutants. But the degradation efficiency of pollutants is lower because the recombination speed of the generated electron-hole pairs is higher. Therefore, research has focused on constructing composite materials and tight interfaces to extend the time required for electron-hole pair recombination, such as anatase and rutile TiO formation2And a compact Z-type heterojunction is formed, and MXene has metal conductivity and can promote charge separation and storage, so that the catalytic efficiency of the wide-bandgap semiconductor is improved. Currently, there are few reports on MXene modified wide bandgap semiconductor materials, Low et al (. X. Low, L.Y. Zhang, T. Tong, B.J. Shen, J.G. Yu, TiO)2/MXene Ti3C2 composite with excellent photocatalytic CO2reduction activity, J.Catal., 361 (2018) 255-266) in CO2Under the protection of atmosphere, MXene is used as a titanium source to prepare TiO through high-temperature oxidation2the/MXene composite material can obtain reduced CO with high activity2The composite catalyst of (1). Zhuang et al (Y. Zhuang, Y.F. Liu, X.F. Meng, contamination of TiO)2 nanofibers/MXene Ti3C2 nanocomposites for photocatalytic H2evolution by electrostatic self-assembly, appl. surf. Sci., 496 (2019) 143647) by electrostatic self-assembly technique to achieve TiO2Compounding with MXene to obtain high-activity photocatalytic hydrogen-producing compound with hydrogen-producing rate up to 6.979 mmol h-1g-1. The MXene-doped wide-bandgap semiconductor compound has obvious effect on photocatalytic degradation.
Therefore, MXene is expanded to be used as a Ti source, and mixed-phase TiO is precipitated by a thermal oxidation method2And is bonded with Ti3C2Under the combined action, the obtained photocatalyst has certain potential and prospect in the field of photodegradation. The invention obtains a catalytic material which is simple and easy to obtain and has certain potential for separating electron-hole pairs.
Disclosure of Invention
The invention aims to solve the technical problem of providing TiO2Mxene composite material and its preparing processThe absorption of the visible wave band is obviously enhanced, and the high-efficiency separation of electron-hole pairs is facilitated.
In order to achieve the purpose, the invention adopts the following technical scheme:
novel TiO (titanium dioxide)2The preparation method of the/MXene composite material comprises the following steps: the method comprises the following steps:
(1) preparing MXene: weighing a certain amount of MAX powder, etching by using an HF solution, cleaning by using clear water and absolute ethyl alcohol, and drying by using a vacuum oven to obtain MXene powder;
(2) preparation of TiO2the/MXene composite material: mixing MXene powder with NaBF4Fully grinding the solid; calcining at the temperature of 300-900 ℃, centrifuging, washing and drying the obtained sample to obtain MXene modified TiO2A composite material.
Further, the MAX powder is Ti3AlC2Or Ti2AlC。
Further, in the step (1), the mass fraction of the HF solution is 40-49%, and the mass ratio of MAX to HF is 10.75-5: 1.
further, the etching temperature in the step (1) is 60 ℃, and the reaction time is 24 h.
Further, MXene and NaBF4The mass ratio is 1: 0-4.95.
Further, the calcination temperature in the step (2) was 550 ℃.
Further, TiO obtained in the step (2)2The baking time of the/MXene composite material is 0-12 h.
The invention has the following advantages: the raw materials prepared by the method are common and easy to obtain, the cost is low, the preparation process is simple and convenient, the visible light response is obviously improved, and the method has potential application value in the field of environmental protection. In addition, the invention adopts a solvothermal method for two-step synthesis, and the experiment is easy to control.
Drawings
Fig. 1 is an SEM image of a sample: (a) MAX, (b) MXene, (c) 350 ℃ -TiO2/Ti3C2;（d）450℃-TiO2/Ti3C2;（e）550℃-TiO2/Ti3C2;（f）650℃-TiO2/Ti3C2。
FIG. 2 shows 550 ℃ to TiO2/Ti3C2EDS mapping plot of catalyst.
Fig. 3 is an XRD pattern of the sample: (a) MXene, (b) 350 ℃ -TiO2/Ti3C2; （c）450℃-TiO2/Ti3C2;（d）550℃-TiO2/Ti3C2;（e）650℃-TiO2/Ti3C2。
Fig. 4 is a graph of photocatalytic rate for samples: (a) 350-TiO2/Ti3C2; （b）450℃-TiO2/Ti3C2;（c）550℃-TiO2/Ti3C2;（d）650℃-TiO2/Ti3C2;。
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
Example 1
10mL of 49% HF solution was weighed into polytetrafluoroethylene, and 1g of Ti was weighed3AlC2Slowly adding the powder into an HF solution, fully stirring, putting the powder into an oven, heating to 60 ℃, reacting for 24 hours, washing the obtained powder with deionized water until the pH value is about 7, centrifugally washing with ethanol for three times, and finally drying the powder in a vacuum oven at 60 ℃ for 24 hours to obtain MXene powder.
100 mg of MXene and 165 mg of NaBF were taken4Fully grinding, placing in a muffle furnace for high-temperature roasting to prepare TiO2the/MXene tablet compound is washed for three times by 25 mL of 1M HCl, repeatedly washed by acetone, deionized water and absolute ethyl alcohol, and then dried in an oven at 60 ℃.
The other steps are not changed, the roasting temperature is respectively controlled to be 350 ℃, 450 ℃, 550 ℃ and 650 ℃, and TiO is obtained2the/MXene composite photocatalyst is shown in the table 1.
Other steps are unchanged, the roasting time is respectively controlled to be 0 h, 4h, 8 h and 12h, and TiO is obtained2the/MXene composite photocatalyst is shown in the table 1.
The other steps are unchanged, the content of the additive NaBF4 is controlled to be 0mg, 165 mg, 330 mg and 495 mg respectively, and TiO is obtained2the/MXene composite photocatalyst is shown in the table 1.
Table 1 sample formulation table
Note: above T is the roasting temperature and T is the roasting time
Example 2
10mL of 49% HF solution was weighed into polytetrafluoroethylene, and 1g of Ti was weighed2Slowly adding AlC powder into an HF solution, fully stirring, putting the solution into an oven, heating to 60 ℃, reacting for 24 hours, washing the obtained powder with deionized water until the pH value is about 7, centrifugally washing with ethanol for three times, and finally drying the powder in a vacuum oven at 60 ℃ for 24 hours to obtain MXene powder.
Other steps are not changed, and the prepared TiO2/MXene composite photocatalyst.
Ti obtained in examples 1 to 23C2And TiO2/Ti3C2The composites were analyzed using a Field Emission Scanning Electron Microscope (FESEM), X-ray diffractometer (XRD), ultraviolet-visible spectrometer (UV-vis).
FIG. 1 is Ti3AlC2、Ti3C2、350-TiO2/Ti3C2、450-TiO2/Ti3C2、550-TiO2/Ti3C2And 650-TiO2/Ti3C2SEM image of the sample. As can be seen from FIG. 1 (a), Ti3AlC2Presenting a larger block shape. By the pair of Ti3AlC2The etching of (A) gives FIG. 1 (b), and it can be seen that there is a significant change in the morphology, from bulk Ti3AlC2Ti etched into potato-like chip3C2. In-situ control agent NaBF4In the presence of Ti and at higher reaction temperatures3C2The lamella is destroyed and nano-particle TiO is separated out on the surface2(FIG. 1 c). In FIGS. 1 c-f, the morphology does not change significantly at 350 deg.C-650 deg.C. Is noteworthy in the range of 650 ℃ to TiO2/Ti3C2Larger lumps appear.
FIG. 2 shows 550 ℃ to TiO2/Ti3C2EDS mapping map of (a). The elemental content and elemental surface distribution of the samples were analyzed by EDS spectrometer. As is clear from the figure, TiO2/Ti3C2Contains Ti, C and O elements, because of Ti3C2And TiO2Both contain Ti and O, so the surface of the material is full of Ti and O elements. Notably, at 550 ℃, TiO was prepared2/Ti3C2The compound does not contain F element.
FIG. 3 is Ti3C2、350-TiO2/Ti3C2、450-TiO2/Ti3C2、550-TiO2/Ti3C2And 650-TiO2/Ti3C2XRD pattern of the sample. It can be seen that Ti3C2Characteristic peaks appear at 9.58 °, 18.30 °, 27.43 °, 35.94 °, 41.74 °, 60.51 °, corresponding to the (002), (004), (101), (103), (105), (108), (109), (110) crystal planes, respectively. Anatase TiO2（TiO2(A) Characteristic peaks appear at 25.14 °, 37.55 °, 47.94 °, 54.83 °, 62.49 °, 75.03 °, corresponding to the (101), (004), (200), (105), (204), (215) crystal planes, respectively. Rutile TiO 22（TiO2(R)) has characteristic peaks at 27.45 degrees, 36.09 degrees, 39.18 degrees, 41.23 degrees, 44.05 degrees, 54.32 degrees, 56.64 degrees, 65.47 degrees, 69.01 degrees and 69.78 degrees, which respectively correspond to crystal planes of (110), (101), (200), (111), (211), (220), (221), (301) and (112). To Ti at different temperatures3C2All of which produce anatase TiO2Characteristic peak of (2). Due to Ti3C2Is partially oxidized to TiO2And in TiO2Has a strong characteristic peak, so that Ti3C2The characteristic peaks of (a) are difficult to be found. Notably, with increasing temperature, rutile TiO appeared at 27.45 °2Characteristic peak of (2).
FIG. 4 is 350 ℃ to TiO2/Ti3C2、450℃-TiO2/Ti3C2、550℃-TiO2/Ti3C2And 650 deg.C-TiO2/Ti3C2The photocatalytic rate of (a); 50mL of 20mg/L RhB solution was degraded from 20mg of sample under visible light conditions. 550-TiO2/Ti3C2The degradation effect is optimal, and the degradation effect on rhodamine B is up to 90.7 percent in 120 min. And 350 ℃ to TiO2/Ti3C2、450℃-TiO2/Ti3C2And 650 deg.C-TiO2/Ti3C2The degradation at 120min was 82.0%, 86.0%, 67.2%, respectively.
From the above characterization, it can be concluded that: ti3C2Surface precipitation of TiO2The photocatalytic performance of the system is enhanced. And the degradation rate of the organic pollutants after modification is greatly improved.
Although specific embodiments of the invention have been described above, it will be understood by those skilled in the art that the specific embodiments described are illustrative only and are not limiting upon the scope of the invention, and that equivalent modifications and variations can be made by those skilled in the art without departing from the spirit of the invention, which is to be limited only by the appended claims.
Claims (8)
1. Novel TiO (titanium dioxide)2The preparation method of the/MXene composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing MXene: weighing a certain amount of MAX powder, etching by using an HF solution, cleaning by using clear water and absolute ethyl alcohol, and drying by using a vacuum oven to obtain MXene powder;
(2) preparation of TiO2the/MXene composite material: will be provided withMXene powder and NaBF4Fully grinding the solid, then calcining for 0-12h at the temperature of 300-900 ℃ to destroy the layered structure of MXene, and precipitating nano-particle TiO on the surface2Centrifuging, washing and drying the obtained sample to obtain MXene modified TiO2A composite material.
2. The novel TiO of claim 12The preparation method of the/MXene composite material is characterized by comprising the following steps: the MAX powder is Ti3AlC2Or Ti2AlC。
3. The novel TiO of claim 12The preparation method of the/MXene composite material is characterized by comprising the following steps: in the step (1), the mass fraction of the HF solution is 40-49%, and the mass ratio of MAX to HF is 10.75-5: 1.
4. the novel TiO of claim 12The preparation method of the/MXene composite material is characterized by comprising the following steps: the etching temperature in the step (1) is 60 ℃, and the reaction time is 24 h.
5. The novel TiO of claim 12The preparation method of the/MXene composite material is characterized by comprising the following steps: the MXene and NaBF4The mass ratio is 1: 0-4.95.
6. The novel TiO of claim 12The preparation method of the/MXene composite material is characterized by comprising the following steps: the calcination temperature in step (2) was 550 ℃.
7. The novel TiO of claim 12The preparation method of the/MXene composite material is characterized by comprising the following steps: TiO obtained in step (2)2The baking time of the/MXene composite material is 0-12 h.
8. A novel TiO according to any one of claims 1 to 52Preparation of/MXene composite materialTiO prepared by the method2the/MXene composite material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113578296A (en) * | 2021-08-13 | 2021-11-02 | 哈尔滨理工大学 | Lamellar gray TiO2 photocatalytic material and preparation method thereof |
| CN114229845A (en) * | 2021-11-18 | 2022-03-25 | 华南理工大学 | Preparation method of MXene |
| CN114481195A (en) * | 2022-01-24 | 2022-05-13 | 辽宁大学 | TiO2-MXene/IL modified electrode and its application in electrocatalysis of N2Conversion to NH3In (1) |
| CN116586084A (en) * | 2022-09-08 | 2023-08-15 | 河南工业大学 | Sc (Sc) 2 O 3 MXene-derived TiO 2 Photocatalytic material and preparation method thereof |
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| CN116586084A (en) * | 2022-09-08 | 2023-08-15 | 河南工业大学 | Sc (Sc) 2 O 3 MXene-derived TiO 2 Photocatalytic material and preparation method thereof |
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