AU2021101632A4 - Preparation Method and Application of Li, C and N Ternary Co-Doped Titanium Dioxide Nanomaterials - Google Patents
Preparation Method and Application of Li, C and N Ternary Co-Doped Titanium Dioxide Nanomaterials Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/74—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by peak-intensities or a ratio thereof only
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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Abstract
A preparation method and application of Li, C and N ternary co-doped titanium dioxide (TiO2)
nanomaterials are disclosed in the invention. The preparation method comprises the following
steps of (1) mixture preparation. Dissolving lithium nitrate and urea in anhydrous ethanol, then
adding TiO2nanotubes and mixing them with magnetic stirring until the anhydrous ethanol is
completely volatilized; (2) preparation of TiO2nanomaterials. Placing that mixture from step
(1) in a crucible for calcination at a constant temperature under inert gas protection to obtain
the Li, C and N ternary co-doped TiO2 nanomaterials. The invention adopts TiO2 nanotubes as
the precursor, and prepares Li, C, and N ternary co-doped TiO2 nanomaterials in one step. The
process is simple and easy to industrialize. More importantly, the ternary co-doping is realized
at the same time when the precursor crystal structure and morphology are changed, and the
doped elements can be uniformly distributed in the TiO2 substrate, so that a TiO2 material with
fine structure and excellent performance can be prepared.
Description
Preparation Method and Application of Li, C and N Ternary Co-Doped Titanium
Dioxide Nanomaterials
The invention relates to the technical field of preparation and catalysis of nanomaterials,
and particularly describes a preparation method and an application of Li, C and N ternary
co-doped TiO2 nanomaterials.
TiO2 is a wide bandgap semiconductor. Under UV-irradiation, TiO2 can be used for
photocatalytic sterilization, effectively degrade harmful gases in the air and remove trace
amount of organic pollutants in water body. In order to utilize a large amount of visible
light in the solar spectrum, doping TiO2 is a widely reported method. For example, [Feng
C, Wang Y, Zhang J, Yu L, Li D, Yang J, et al. The effect ofinfrared light on visible light
photocatalytic activity: An intensive contrast between Pt-doped TiO2 and N-doped TiO2.
Appl Catal B Environ. 2012;113-114:61-71.]. Zhuang Weibin et al. prepared N-doped
TiO2 powder with excellent performance by depositing colloid on copper surface, and
then performing electro-thermal sintering [Reference: Zhuang Weibin, Liu Yue, Li
Heliang, Wu Bo, A preparationmethod ofN-doped TiO2 Powder, CN107670681A]. Pan
Xiaoyang et al. prepared a N-doped TiO-C material for catalyst of nitro reduction by sol
gel method with carbon nitride as template, carbon source and nitrogen source.
[Reference: Pan Xiaoyang, Long Peiqing, Yi Zhiguo, Preparation method and
application of N-doped TiO-C material, CN107983384A]. All of the above-mentioned
methods can expand the light absorption range of TiO 2 materials from ultraviolet light to visible light and demonstrates excellent activity of catalysing sand degrading organic pollutant by visible light. However, the above methods only realize one or two elements doping, and there is a problem that doped metal can not be uniformly distributed. Li ions with the smallest ion radius are relatively easy to dope. The introduction of non-metallic
C and N doping requires a relatively sophisticated preparation method.
The invention provides a preparation method and application of Li, C and N ternary co
doped TiO2nanomaterials. Dispersing dopants in situ on the inner and outer surfaces of
TiO2nanotubes, and then calcining at high temperature to prepare a Li, C and N co-doped
TiO2nanomaterial with visible light response.
The technical scheme for realizing the invention is as follows.
A preparation method of Li, C and N ternary co-doped TiO2nanomaterials comprises the
following steps.
(1) Mixture preparation. Dissolving lithium nitrate and urea in anhydrous ethanol, then
adding TiO2 nanotubes and mixing them with magnetic stirring until the anhydrous
ethanol is completely volatilized.
(2) Preparation of TiO2nanomaterials. Placing that mixture from step (1) in a crucible for
calcination at a constant temperature under inert gas protection to prepare the Li, C and N
ternary co-doped TiO2nanomaterials.
The preparation method of TiO2nanotubes in step (1) is detailed by mixing TiO2 and
alkali solution in a polytetrafluoroethylene reactor, magnetically stirring for reaction,
filtering, washing to neutrality and drying.
The alkali solution is NaOH solution with a concentration of 8-20mol-L', and the
magnetic stirring is carried out at temperature of 100-150°C for 20-30h.
The mass ratio of lithium nitrate to TiO2nanotubes in step (1) is (0.06-0.6): 1.
The calcination temperature in step (2) is 300-700°C and the calcination time is 1-6h.
The invention further includes the application of prepared ternary co-doped TiO2
nanomaterials in catalysis and degradation of visible light.
The method has following beneficial effects. TiO2 nanotubes are used as the precursor,
and Li, C, and N ternary co-doped TiO2 nanomaterials are prepared in one step. The
process is simple and easy to industrialize. More importantly, the ternary co-doping is
realized at the same time when the precursor crystal structure and morphology are
changed, and the doped elements can be uniformly distributed in the TiO2 substrate, so
that a TiO2 material with fine structure and excellent performance can be prepared.
In order to explain the embodiments of the present invention or the technical scheme in
the prior art more clearly, the figures required in the embodiments or the description of
the prior art will be briefly introduced below. Obviously, the figures in the following
description are only some embodiments of the present invention, and other figures can be
obtained according to these figures for ordinary technicians in the field without paying
creative labour.
Figure 1 is an electron micrograph of TiO2 nanotube in Embodiment 1 of the present
invention.
Figure 2 is an XRD pattern (X-ray diffraction pattern) of TiO2 nanotube in Embodiment 1
of the present invention.
Figure 3 is an XRD pattern of Li, C and N ternary co-doped TiO2 nanomaterials prepared
in Embodiment 4 of the present invention.
Figure 4 is an electron micrograph of ternary co-doped TiO2 nanomaterials prepared in
Embodiment 4 of the present invention.
The following will clearly and completely describe the technical scheme of the present
invention in combination with embodiments of the present invention. Obviously, the
described embodiments are only part of the embodiments of the present invention, not all
of them. Based on the embodiments of the present invention, all other embodiments
obtained by ordinary technicians in the field without paying creative labour belong to the
protection scope of the present invention.
Embodiment 1
A preparation method of Li, C and N ternary co-doped TiO2 nanomaterials comprises the
following steps.
(1) Weighing 100mL- 1 l0mol-L-1 NaOH solution and mixing it with TiO2 in a
polytetrafluoroethylene reactor. Controlling the temperature to 120°C and magnetically
stirring it for 25h. After naturally cooling it to room temperature, filtering and washing it
until the pH is neutral. At last, drying it to obtain TiO2 nanotubes.
(2) Weighing 0.5g of lithium nitrate and Ig of urea and dissolving them anhydrous
ethanol, then adding 5g of TiO2nanotubes and mixing them with magnetic stirring until
the anhydrous ethanol is completely volatilized.
(3) Placing that mixture from step (2) in a crucible for calcination at 300°C under inert
gas protection for 2h. Then naturally cooling it to room temperature to prepare the Li, C
and N ternary co-doped TiO2 nanomaterials.
Fig. 1 is an electron micrograph of TiO2nanotubes prepared in step (1). It can be seen
that the prepared material is one-dimensional nanotube, with a diameter of about 6nm and
a tube length of hundreds of nanometres. The tubular structure enables a large specific
surface area of TiO2nanotube so that both the inner and outer walls can adsorb lithium
nitrate and urea.
Fig. 2 is an XRD pattern of TiO2 nanotubes prepared in step (1). There is an obvious
characteristic diffraction peak of TiO2 nanotubes at 9, which belongs to orthorhombic
crystal system.
Embodiment 2
The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials is different
from that in Embodiment 1 that the calcination temperature in step (3) is 400°C.
Embodiment 3
The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials is different
from that in Embodiment 1 that the calcination temperature in step (3) is 500°C.
Embodiment 4
The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials is different
from that in Embodiment 1 that the calcination temperature in step (3) is 600°C.
Fig. 3 is an XRD pattern of Li, C and N ternary co-doped TiO2 nanomaterials prepared in
Embodiment 4. After calcination at high temperature, the orthorhombic crystal structure
of TiO2 nanotubes changed, and the crystal structure of the prepared material is mainly
anatase TiO2. The diffraction peaks of Li salt appear at 18 and 33, which indicates that
Li ions are well dispersed in Li, C and N ternary co-doped TiO2 nanomaterials.
Fig. 4 is an electron micrograph of Li, C and N ternary co-doped TiO2 nanomaterials
prepared in Embodiment 4. It can be seen that the morphology of TiO2 nanotubes has
changed from tubular to nanoparticle, with a particle size of 3050nm.
Embodiment 5
The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials is different
from that in Embodiment 1 that the calcination temperature in step (3) is 700°C.
Embodiment 6
The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials is different
from that in Embodiment 1 that the calcination time in step (3) is 3h.
Embodiment 7
The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials is different
from that in Embodiment 1 that the calcination time in step (3) is 4h.
Embodiment 8
The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials is different
from that in Embodiment 1 that the calcination time in step (3) is 5h.
Embodiment 9
The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials is different
from that in Embodiment 1 that the calcination time in step (3) is 6h.
The foregoing is only preferred embodiments of the present invention and is not intended
to limit the present invention. Any modifications, equivalent substitutions, improvements,
etc. made within the spirit and principles of the present invention shall be included in the
protection scope of the present invention.
Claims (6)
1. A preparation method of Li, C and N ternary co-doped TiO2 nanomaterials,
characterized by comprising the following steps.
(1) Mixture preparation. Dissolving lithium nitrate and urea in anhydrous ethanol, then
adding TiO2 nanotubes and mixing them with magnetic stirring until the anhydrous
ethanol is completely volatilized.
(2) Preparation of TiO2 nanomaterials. Placing that mixture from step (1) in a crucible for
calcination at a constant temperature under inert gas protection to prepare the Li, C and N
ternary co-doped TiO2 nanomaterials.
2. The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials as stated
in Claim 1, characterized in that the preparation method of TiO2nanotubes in step (1) is
detailed by mixing TiO2 and alkali solution in a polytetrafluoroethylene reactor,
magnetically stirring for reaction, filtering, washing to neutrality and drying.
3. The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials as stated
in Claim 2, characterized in that the alkali solution is NaOH solution with a concentration
of 8-20mol-L-1, and the magnetic stirring is carried out at temperature of 100-150°C for
-30h.
4. The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials as stated
in Claim 1, characterized in that the mass ratio of lithium nitrate to TiO2nanotubes in step
(1) is (0.06-0.6): 1.
5. The preparation method of Li, C and N ternary co-doped TiO2 nanomaterials as stated
in Claim 1, characterized in that the calcination temperature in step (2) is 300-700°C and
the calcination time is 1-6h.
6. Application of ternary co-doped TiO2 nanomaterials prepared according to any one of
Claims 1 to 6 in catalysis and degradation of visible light.
FIGURES
1/2 2021101632
Figure 1 An electron micrograph of TiO2 nanotube in Embodiment 1 of the present
invention.
Figure 2 An XRD pattern (X-ray diffraction pattern) of TiO2 nanotube in Embodiment 1
of the present invention.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE1029032B1 (en) * | 2021-06-03 | 2022-08-16 | Univ Henan | Fabrication process and application of Li, C, N ternary co-doped titanium dioxide nanomaterials |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| BE1029032B1 (en) * | 2021-06-03 | 2022-08-16 | Univ Henan | Fabrication process and application of Li, C, N ternary co-doped titanium dioxide nanomaterials |
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