CN107159286A - A kind of Ti3C2/TiO2The preparation method of two-dimensional material - Google Patents
A kind of Ti3C2/TiO2The preparation method of two-dimensional material Download PDFInfo
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- CN107159286A CN107159286A CN201710354202.XA CN201710354202A CN107159286A CN 107159286 A CN107159286 A CN 107159286A CN 201710354202 A CN201710354202 A CN 201710354202A CN 107159286 A CN107159286 A CN 107159286A
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- 229910009819 Ti3C2 Inorganic materials 0.000 title claims abstract description 63
- 239000000463 material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000002131 composite material Substances 0.000 claims abstract description 31
- 238000011065 in-situ storage Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004900 laundering Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 4
- 239000010409 thin film Substances 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 description 8
- 239000004408 titanium dioxide Substances 0.000 description 5
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910019762 Nb4C3 Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910004472 Ta4C3 Inorganic materials 0.000 description 1
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
-
- B01J35/39—
-
- B01J35/60—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
Abstract
The invention discloses a kind of Ti3C2/TiO2The preparation method of two-dimensional material；The present invention is prepared for Ti3C2MXene thin-film materials, after heated oxide, interlamellar spacing becomes big, and in Ti3C2TiO is in situ generated on lamella2, obtain the Ti of two dimension3C2/TiO2Composite.The present invention is in Ti3C2Previous step growth in situ TiO2The Ti of two dimension is obtained3C2/TiO2Composite.Gained composite specific surface area is big, good conductivity, and with photo-generate electron-hole to the characteristics of, while Ti3C2With TiO2Xiao Te contacts are formed, its efficiency in terms of photocatalysis is improved.Present invention process is simple, and cost is low, is adapted to large-scale application, also, Ti3C2/TiO2Composite is highly suitable to be applied in the photocatalysis field present invention.
Description
Technical field
The present invention relates to technical field of material chemistry, more particularly to a kind of Ti3C2/TiO2The preparation method of two-dimensional material.
Background technology
Traditional catalytic science is that the mankind are made that particularly important contribution towards during to century, photocatalysis
The advantage for being probably one of all kinds of most promising new technologies of waste water of processing Photocatalysts is that technique is simple, cost is low
It is honest and clean, at normal temperatures and pressures can the constitutionally stable organic matter of oxidation Decomposition, utilize sunlight as light source, non-secondary pollution.Mesh
Before, in multiphase photocatalysis reacts applied semiconductor catalyst, TiO2 is so that its nontoxic, catalytic activity is high, stability it is good with
And oxidation resistance it is strong the advantages of and enjoy favor.
MXene is a kind of transition metal carbide with two-dimensional layered structure similar to graphene that be finding in recent years
Or nitride, a total of nearly 70 kinds, including Ti3C2, Ti2C, V2C, Nb2C, Nb4C3, Ta4C3 of the MXene having now been found that,
Ti4N3 etc..MXene is due to its good electric conductivity, big specific surface area and high intensity, in energy storage, electronics, composite wood
The fields such as material, sensor are with a wide range of applications.
In the world can be numerous as the material of photocatalyst, including titanium dioxide (TiO2), zinc oxide (ZnO), tin oxide
(SnO2), zirconium dioxide (ZrO2), many oxide sulfide semiconductor, wherein titanium dioxide such as cadmium sulfide (CdS)
(Titanium Dioxide) is strong because of its oxidability, and chemical property stablizes nontoxic, as most hot nano photocatalyst in the world
Catalytic material.It is also once more to use cadmium sulfide (CdS) and zinc oxide (ZnO) as photocatalyst material in early days, but be due to this
Both unstable chemcial properties, can be light-catalysed while occurring light dissolving, and the harmful metal ion of dissolution has certain
Bio-toxicity, therefore developed country has seldom been used them as civilian catalysis material at present.
Therefore, the prior art is defective, it is necessary to improve.
The content of the invention
The technical problems to be solved by the invention are：There is provided a kind of composite specific surface area big, good conductivity, and tool
There is Ti of the photo-generate electron-hole to feature3C2/TiO2The preparation method of two-dimensional material.
Technical scheme is as follows：A kind of Ti3C2/TiO2The preparation method of two-dimensional material, S1：Ti3C2MXene system
It is standby；S11：Quantitatively weigh the Ti of MAX phases3AlC2, it is dissolved in the HF that concentration is 50%, it is reacted 18-24h under agitation；
S12：Dry, that is, obtain after the reaction solution filtering in step S11 and massive laundering solid, then under 40 degree of -60 degree
Ti3C2MXene powder；S2：Ti3C2/TiO2The preparation of composite；S21：Quantitatively weigh Ti3C2MXene powder, is dissolved in
100ml 0.1M HNO3In the aqueous solution, magnetic agitation 30min, and the ultrasound 15min under 100w；S22：By in step S21
Solution adds hydro-thermal axe, and the hydro-thermal reaction 12h under 160 degree, makes in Ti3C2Upper growth in situ TiO2；S22：By step S22's
Reaction solution is filtered, and 300 degree of lower heating 1-2h obtain Ti3C2/TiO2Composite.
Applied to above-mentioned technical proposal, in described preparation method, in step S11,1g MAX phases are quantitatively weighed
Ti3AlC2；Also, in step S21：Quantitatively weigh 1g Ti3C2MXene powder.
Using such scheme, the present invention is prepared for Ti3C2MXene thin-film materials, after heated oxide, interlamellar spacing becomes big,
And in Ti3C2TiO is in situ generated on MXen lamellas2, obtain the Ti of two dimension3C2/TiO2Composite.TiO2There is provided efficient
Photo-generate electron-hole pair, Ti3C2Material has high-specific surface area, good electric conductivity, and both yet forms both schottky junction.
Therefore, Ti3C2/TiO2Composite is highly suitable to be applied in photocatalysis field.
Brief description of the drawings
Fig. 1 a are Ti3C2Surface sweeping sem image figure；
Fig. 1 b are Ti3C2/TiO2The scanning electron microscope image figure of composite；
Fig. 2 a are Ti3C2Images of transmissive electron microscope figure；
Fig. 2 b are Ti3C2/TiO2Sem image figure is retouched in the transmission of composite；
Fig. 3 is Ti3C2And Ti3C2/TiO2The XRD picture figure of composite；
Fig. 4 is Ti3C2/TiO2The XPS image graphs one of composite；
Fig. 5 is Ti3C2/TiO2The XPS image graphs two of composite.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Present embodiments provide a kind of Ti3C2/TiO2The preparation method of two-dimensional material, the preparation method is in Ti3C2On MXene
Growth in situ TiO2The Ti of two dimension is obtained3C2/TiO2Composite, two-dimentional Ti3C2/TiO2Composite not only has concurrently
Ti3C2MXene and TiO2Advantage, and Ti3C2With TiO2Xiao Tejie is formd, composite is greatly improved and is led in photocatalysis
The efficiency in domain.
Ti3C2/TiO2The preparation method of two-dimensional material comprises the following steps, first, step S1：Ti3C2MXene preparation；
Specifically, step S11：Quantitatively weigh the Ti of 1g MAX phases3AlC2, by the Ti of MAX phases3AlC2It is dissolved in the HF that concentration is 50%
In, it is reacted 18-24h under agitation；Then, step S12：After stirring reaction, the reaction solution in step S11 is filtered,
And after massive laundering solid, then the drying under 40 degree of -60 degree, that is, obtain Ti3C2MXene powder.
Then step S2 is carried out：Ti3C2/TiO2The preparation of composite；Specifically step S21：Quantitatively weigh 1g's
Ti3C2MXene powder, by the Ti weighed3C2MXene powder is dissolved in 100ml 0.1M HNO3In the aqueous solution, wherein, M for mole
Concentration, then carries out magnetic agitation 30min, and the ultrasound 15min under 100w；Then step S22：After ultrasound, by step S21
Solution add hydro-thermal axe, and make under 160 degree its progress hydro-thermal reaction 12h, in hydrothermal reaction process, make in Ti3C2Upper original
Position growth TiO2；Final step S22：Make in Ti3C2Upper growth in situ TiO2Afterwards, step S22 reaction solution is filtered,
Solid matter after filtering is heated into 1-2h under 300 degree and obtains Ti3C2/TiO2Composite.
The present embodiment product will use laser Raman spectrometer (laser Raman spectrometer), X-ray diffraction
(XRD), SEM (SEM), electrochemical workstation (Electrochemical workstation) characterize production
Product.Wherein Raman can characterize the characteristic peak and the number of plies of sample, and SEM can observe the sight pattern of product, and XRD can enter to product
Row Crystalline form analysis, electrochemical workstation can be with the chemical property of test product.Specific test data is as follows：
Fig. 1 a are Ti3C2Surface sweeping sem image, Fig. 2 b be Ti3C2/TiO2The scanning electron microscope image of composite.It can see
To after hydro-thermal reaction and high-temperature process, in Ti3C2Growth in situ TiO on lamella2Form Two-dimensional Composites.
Fig. 2 a are Ti3C2Images of transmissive electron microscope, Fig. 2 b be Ti3C2/TiO2Sem image is retouched in the transmission of composite.Can be with
See after hydro-thermal reaction and high-temperature process, in Ti3C2Growth in situ TiO on lamella2Form Two-dimensional Composites.
Fig. 3 is Ti3C2And Ti3C2/TiO2The XRD picture of composite.After hydrothermal reduction is heated, TiO2It is grown in
Ti3C2Upper formation composite.
Fig. 4 and Fig. 5 are Ti3C2/TiO2The XPS images of composite.It can be seen that after hydro-thermal reaction and heating,
Ti-O keys are generated.
The present invention is in Ti3C2MXene previous step growth in situ TiO2The Ti of two dimension is obtained3C2/TiO2Composite.Gained
Composite specific surface area is big, good conductivity, and with photo-generate electron-hole to the characteristics of, while Ti3C2With TiO2Form Xiao
Spy's contact, improves its efficiency in terms of photocatalysis.Present invention process is simple, and cost is low, is adapted to large-scale application.
These are only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Any modifications, equivalent substitutions and improvements made within principle etc., should be included in the scope of the protection.
Claims (2)
1. a kind of Ti3C2/TiO2The preparation method of two-dimensional material, it is characterised in that：
S1：Ti3C2MXene preparation；
S11：Quantitatively weigh the Ti of MAX phases3AlC2, it is dissolved in the HF that concentration is 50%, it is reacted 18- under agitation
24h；
S12：Dry, that is, obtain after the reaction solution filtering in step S11 and massive laundering solid, then under 40 degree of -60 degree
Ti3C2MXene powder；
S2：Ti3C2/TiO2The preparation of composite；
S21：Quantitatively weigh Ti3C2MXene powder, is dissolved in 100ml 0.1M HNO3In the aqueous solution, magnetic agitation 30min,
And under 100w ultrasound 15min；
S22：Solution in step S21 is added into hydro-thermal axe, and the hydro-thermal reaction 12h under 160 degree, made in Ti3C2Upper growth in situ
TiO2；
S22：Step S22 reaction solution is filtered, 300 degree of lower heating 1-2h obtain Ti3C2/TiO2Composite.
2. preparation method according to claim 1, it is characterised in that：In step S11,1g MAX phases are quantitatively weighed
Ti3AlC2；Also, in step S21：Quantitatively weigh 1g Ti3C2MXene powder.
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| CN107537323A (en) * | 2017-10-24 | 2018-01-05 | 中国地质大学（北京） | A kind of MXene nano wire composite electrospun tunica fibrosas for photo-thermal desalination |
| CN108525700A (en) * | 2018-05-14 | 2018-09-14 | 燕山大学 | A kind of composite photo-catalyst and the preparation method and application thereof |
| CN108565471A (en) * | 2018-05-30 | 2018-09-21 | 广东工业大学 | The preparation method and photo-thermal biology anode of a kind of photo-thermal biology anode and its application |
| CN108641779A (en) * | 2018-04-25 | 2018-10-12 | 青岛大学 | A kind of TiO2Nano particle coats the preparation method of carbon-coating electric current change composite material |
| CN108855167A (en) * | 2018-07-13 | 2018-11-23 | 吉林大学 | A kind of carbon doping TiO2Nanometer hierarchical structural material and its application |
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