CN111135845A - Preparation method of titanium dioxide/titanium sulfide carbide nano composite material - Google Patents
Preparation method of titanium dioxide/titanium sulfide carbide nano composite material Download PDFInfo
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- CN111135845A CN111135845A CN202010034560.4A CN202010034560A CN111135845A CN 111135845 A CN111135845 A CN 111135845A CN 202010034560 A CN202010034560 A CN 202010034560A CN 111135845 A CN111135845 A CN 111135845A
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- titanium
- composite material
- titanium dioxide
- porcelain boat
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 18
- 239000000463 material Substances 0.000 title claims abstract description 16
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- RCYJPSGNXVLIBO-UHFFFAOYSA-N sulfanylidenetitanium Chemical compound [S].[Ti] RCYJPSGNXVLIBO-UHFFFAOYSA-N 0.000 title claims description 5
- 239000010936 titanium Substances 0.000 claims abstract description 25
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 14
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000011593 sulfur Substances 0.000 claims abstract description 10
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 241000534944 Thia Species 0.000 claims abstract 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 8
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 8
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract 1
- 230000032900 absorption of visible light Effects 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 229910021389 graphene Inorganic materials 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 125000005842 heteroatom Chemical group 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a titanium dioxide/thia titanium carbide nano composite material, which mainly comprises the steps of sequentially adding a titanium source, a sulfur source and titanium carbide into a beaker according to a certain mass ratio, stirring for 10-30 minutes, putting the mixture into a porcelain boat, putting the porcelain boat into a tube furnace, and putting N into the tube furnace2Keeping the temperature of the porcelain boat at 300-800 ℃ for 2h in the atmosphere, and taking out the mixture after the porcelain boat is naturally cooled to room temperature, namely the titanium dioxide/sulfur hybrid titanium carbide composite material. The preparation method can realize the preparation of the titanium dioxide-based nano composite material by adopting a one-step method, has simple process, mild reaction conditions, no need of adding any surfactant and low cost, and the prepared titanium dioxide/titanium carbide sulfide composite material has good absorption of visible light, shows excellent photoelectrochemical properties and has important significance in the field of photoelectric conversion.
Description
Technical Field
The invention relates to a preparation method of a titanium dioxide/titanium sulfocarbide nano composite material.
Background
Among the numerous semiconductor materials, titanium dioxide (TiO)2) Because of high photoelectric conversion efficiency, stable photoelectric performance, no toxicity and low cost, the material is favored by experts and scholars and is always the hottest and most promising photocatalytic material. However, TiO2The photocatalyst has a wide forbidden band width at room temperature, has low sunlight absorption rate, cannot absorb visible light, and can only be effectively utilized4% ultraviolet light in sunlight; (2) the photon-generated carriers are easy to compound and have low quantum efficiency, and (3) the preparation method is complex and greatly limits the independent application of the photon-generated carriers. Thus, how to improve TiO2The absorption rate of sunlight to realize effective separation of photo-generated charges is an important subject of researchers. One of the solution strategies is to mix TiO2Compounding with other carrier materials.
Graphene is one of the research hotspots in the last decade as a two-dimensional nano material with good physicochemical properties. In the field of photocatalysis, a large number of documents report that graphene is introduced into TiO2The novel nano photocatalyst can effectively utilize the advantages of light transmittance, conductivity, large specific surface area and the like of graphene to obviously improve the photocatalytic effect of titanium dioxide. Heteroatom doping is also a very effective method in improving the conductivity and specific capacitance of graphene. For example: nitrogen atoms (N), boron atoms (B), sulfur atoms (S), chlorine atoms (Cl) and phosphorus atoms (P) have been successfully doped into graphene layers. Two or more heteroatoms co-doped with graphene increases asymmetry of charge and spin density of graphene and distortion of structure, which characteristics increase conductivity of graphene. The existence of the heteroatom not only improves the wettability of the surface of the graphene, but also increases the surface active sites of the graphene. The two-dimensional transition metal carbide or nitride (Mxene) is a graphene-like material, has a unique layered structure, is excellent in conductivity, high in electrochemical activity and large in specific surface area, and has great application potential in the fields of electrocatalysis and energy storage in recent years. Modification studies of the individual components thereof are a significant problem. Analogy studies show that for Mxene materials (such as Ti)3C2) Heteroatom doping can be expected to be an effective modification means.
Disclosure of Invention
The invention aims to overcome the defects of wider band gap of semiconductor titanium dioxide and low utilization rate of sunlight in the prior art, and provides a method for preparing a titanium dioxide/titanium sulfocarbide nano composite material in one step. The method is simple, the raw materials are easy to obtain, and the prepared material shows good visible light response.
A preparation method of a titanium dioxide/sulfur hybrid titanium carbide nano composite material comprises the steps of mixing a titanium source, a sulfur source and titanium carbide according to a certain mass ratio, stirring for 10-30 minutes, putting the mixture into a porcelain boat, placing the porcelain boat into a tube furnace, and adding N2Keeping the temperature of the porcelain boat at 300-800 ℃ for 2h in the atmosphere, and taking out the mixture after the porcelain boat is naturally cooled to room temperature, namely the titanium dioxide/sulfur hybrid titanium carbide composite material.
Further, a titanium source and a sulfur source are titanium sulfate, and the mass ratio of the titanium sulfate to the titanium carbide is (10-50): 1.
further, the temperature in the porcelain boat is programmed to rise at 1-5 ℃/min.
Has the advantages that:
(1) the invention provides a method for preparing TiO in one step2Ti sulfide3C2The preparation method of the nano composite material has simple steps, simple and easily obtained raw materials, and is very beneficial to industrialization;
(2) TiO prepared by the invention2Ti sulfide3C2Nanocomposite, compared to TiO alone2The utilization rate of visible light is obviously improved, and the method can be expected to have better application prospect in the field of energy.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a scheme for preparing TiO2Ti sulfide3C2XPS full spectrum and high power resolution spectrum of S2P of the nanocomposite;
FIG. 2 is TiO2And TiO2Ti sulfide3C2Ultraviolet absorption spectrum of the nanocomposite.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1
TiO2Ti sulfide3C2The preparation steps are as follows: 1mL of Ti was measured out3C2Aqueous dispersion (Ti in dispersion)3C2The concentration of (1 mg/mL), adding 20mg of titanium sulfate, uniformly mixing by ultrasonic waves, pouring into a ceramic crucible, and adding into N2Performing heat treatment in a tube furnace under the atmosphere, raising the temperature by a program of 1 ℃/min, and keeping the temperature at 300 ℃ for 2 h.
Example 2
TiO2Ti sulfide3C2The preparation steps are as follows: 3mL of Ti was measured out3C2Aqueous dispersion (Ti in dispersion)3C2Is 1mg/mL), adding 150mg of titanium sulfate, uniformly mixing by ultrasonic wave, pouring into a ceramic crucible, and adding into N2Performing heat treatment in a tube furnace under the atmosphere, heating at 3 ℃/min, and keeping at 500 ℃ for 2 h.
Example 3
TiO2Ti sulfide3C2The preparation steps are as follows: 5mL of Ti was measured out3C2Aqueous dispersion (Ti in dispersion)3C2Is 1mg/mL), adding 50mg of titanium sulfate, ultrasonically mixing uniformly, pouring into a ceramic crucible, and adding into N2Performing heat treatment in a tube furnace under the atmosphere, raising the temperature by a program of 5 ℃/min, and keeping the temperature at 800 ℃ for 2 h.
FIG. 1 shows the TiO prepared in example 32Ti sulfide3C2X-ray photoelectron spectroscopy (XPS) of (A), wherein FIG. 1(a) is a prepared TiO2Ti sulfide3C2The XPS full spectrum scan of (1) shows that characteristic peaks of S, C, Ti and O appear at electron binding energies of 170eV, 280eV, 460eV and 530eV respectively; fig. 1(b) is a high-resolution map of S2P, and the detection of S element confirms the successful doping of sulfur in the composite material.
FIG. 2 shows the TiO prepared in example 32Ti sulfide3C2The ultraviolet absorption spectrum of (2) clearly shows that the absorption of the composite material in the visible light region is obviously enhanced after the titanium sulfide heterocarbide is introduced.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A preparation method of a titanium dioxide/thia titanium carbide nano composite material is characterized in that a titanium source, a sulfur source and titanium carbide are mixed according to a certain mass ratio, then the mixture is stirred for 10-30 minutes, then the mixture is placed into a porcelain boat and placed into a tube furnace, and N is added into the porcelain boat2Keeping the temperature of the porcelain boat at 300-800 ℃ for 2h in the atmosphere, and taking out the mixture after the porcelain boat is naturally cooled to room temperature, namely the titanium dioxide/sulfur hybrid titanium carbide composite material.
2. The method for preparing the titanium dioxide/titanium sulfide carbide nanocomposite as claimed in claim 1, wherein the titanium source and the sulfur source are titanium sulfate, and the mass ratio of the titanium sulfate to the titanium carbide is 10-50: 1.
3. the method for preparing titanium dioxide/thia titanium carbide nano composite material according to claim 1, wherein the temperature in the porcelain boat is programmed to 1-5 ℃/min.
4. The method for preparing titanium dioxide/titanium sulfide carbide nanocomposite as claimed in claim 1, wherein the titanium sulfate and the titanium carbide are uniformly mixed by using ultrasound with a frequency of 260W to 340W.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010034560.4A CN111135845A (en) | 2020-01-14 | 2020-01-14 | Preparation method of titanium dioxide/titanium sulfide carbide nano composite material |
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| CN202010034560.4A CN111135845A (en) | 2020-01-14 | 2020-01-14 | Preparation method of titanium dioxide/titanium sulfide carbide nano composite material |
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| CN111135845A true CN111135845A (en) | 2020-05-12 |
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| CN202010034560.4A Withdrawn CN111135845A (en) | 2020-01-14 | 2020-01-14 | Preparation method of titanium dioxide/titanium sulfide carbide nano composite material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114527176A (en) * | 2022-02-18 | 2022-05-24 | 常州大学 | Construction method of photoelectrochemical self-powered sensor for sensitive detection of microcystin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114527176A (en) * | 2022-02-18 | 2022-05-24 | 常州大学 | Construction method of photoelectrochemical self-powered sensor for sensitive detection of microcystin |
| CN114527176B (en) * | 2022-02-18 | 2024-10-01 | 常州大学 | Construction method of photoelectrochemistry self-powered sensor for sensitively detecting microcystin |
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Application publication date: 20200512 |