CN110937625A - Preparation method of lanthanum titanate nanoparticles with defects - Google Patents
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- CN110937625A CN110937625A CN201911213330.8A CN201911213330A CN110937625A CN 110937625 A CN110937625 A CN 110937625A CN 201911213330 A CN201911213330 A CN 201911213330A CN 110937625 A CN110937625 A CN 110937625A
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Abstract
The invention relates to a preparation method of a defective lanthanum titanate nanoparticle, belonging to the field of improving the hydrogen production performance of a nano material. The method mainly comprises the steps of introducing defects on the surface of the small-size lanthanum titanate nanoparticles by a solid-phase thermal reduction method after the small-size lanthanum titanate nanoparticles are obtained by a sol-gel method, so that the photocatalytic hydrogen production activity is improved. After the defects are introduced, the absorption capacity and the charge carrier mobility of the lanthanum titanate nanoparticles in a visible light region are improved, so that the photocatalytic performance is improved. The method is simple and easy to operate, environment-friendly, low in cost and high in repeatability, and the prepared lanthanum titanate nanoparticles with defects have potential application value in the research aspect of photocatalytic hydrogen production materials.
Description
Technical Field
The invention belongs to the field of preparation of nano materials, and particularly relates to a preparation method of a defective lanthanum titanate nano particle.
Background
Because of the continuous development of industry in recent years, the environmental pollution is increasingly intensified, and how to reduce the problem of environmental pollution becomes the key of current research. According to investigation, the lanthanide titanate has good thermal stability, has proper forbidden band width, can effectively utilize sunlight, and has wide application prospect in the field of photocatalysis. Lanthanum titanate plays an important role in the aspect of photocatalytic hydrogen production as a compound with a monoclinic perovskite structure. However, the prepared lanthanum titanate reported in the literature has a relatively small specific surface area, a high electron-hole recombination rate, and a low mobility of a charge carrier of the lanthanum titanate in the monoclinic perovskite phase, which affects the photocatalytic activity. Therefore, how to increase the mobility of charge carriers of lanthanum titanate and reduce the size of lanthanum titanate crystal, thereby further improving its photocatalytic efficiency, becomes a major focus of current research.
This patent is earlier through the small-size lanthanum titanate nanoparticle that sol-gel method obtained, on this basis, introduces the defect on small-size lanthanum titanate nanoparticle surface, strengthens lanthanum titanate to the capture ability of electron to improve lanthanum titanate's charge carrier mobility, reinforcing photocatalysis hydrogen production activity.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing lanthanum titanate nanoparticles with defects, which is simple and easy to implement, high in accuracy and low in environmental pollution.
The purpose of the invention is realized as follows: the preparation of the lanthanum titanate nanoparticles having defects comprises the following steps:
step one, preparing small-size lanthanum titanate nanoparticles:
(1) adding 3g of polyethylene glycol (PEG-4000) into 16mL of deionized water, stirring for 30min at room temperature and the rotating speed of 300rpm, and completely dispersing to form a solution ①;
(2) adding 1.0825g of lanthanum nitrate hexahydrate solid into 16mL of glacial acetic acid, and stirring at room temperature for 30min at the rotating speed of 300rpm to fully dissolve the lanthanum nitrate hexahydrate solid to form a solution ②;
(3) dripping the solution ① into the solution ② to obtain a mixed solution A, and continuously stirring the mixed solution A at room temperature for 1h at the rotating speed of 300rpm to enable the mixed solution A to become clear to obtain a solution ③;
(4) adding 16mL of absolute ethyl alcohol into 1.7mL of tetrabutyl titanate (TBT) to obtain a mixed solution B, stirring at room temperature for 10min at the rotating speed of 300rpm, and fully mixing to obtain a solution ④;
(5) dripping the solution ③ into the solution ④, adjusting the pH to 1 with acetic acid to obtain a mixed solution C, and stirring the mixed solution C at 60 ℃ for 2 hours at the rotating speed of 300rpm to obtain a solution ⑤;
(6) transferring the solution ⑤ into an electric heating blast drying oven, drying for 48h at 60 ℃ to obtain lanthanum titanate gel, transferring the lanthanum titanate gel into a muffle furnace for high-temperature calcination treatment, heating to 900 ℃ at the speed of 2 ℃/min, preserving heat for 3h, and naturally cooling to room temperature to obtain the small-size lanthanum titanate nano-particles.
Step two, preparing the lanthanum titanate nano particles with defects:
uniformly mixing 0.6g of the small-size lanthanum titanate nanoparticles obtained in the step one with 0.3g of sodium borohydride, grinding for 30min to obtain a mixed sample, heating the mixed sample to 400 ℃ at a speed of 10 ℃/min by using a tube furnace under the protection of argon, preserving heat for 15 min to obtain a primary lanthanum titanate nanoparticle product with defects, loading the primary lanthanum titanate particle product into a 50mL centrifuge tube, adding 25mL deionized water, and standing for 48 hours to allow the primary lanthanum titanate particle product to react fully; centrifuging the reacted initial product at the centrifugal speed of 5000rpm for 5min, discarding the supernatant to obtain a precipitate, washing the precipitate with deionized water and ultrasonically treating for 4min, repeating the centrifuging and deionized water washing processes twice, and draining the precipitate under natural conditions to obtain a final product: lanthanum titanate nanoparticles having defects.
The invention has the following advantages and positive effects:
1. the lanthanum titanate nano particles with defects synthesized by the method have high purity, the synthesis process is simple and advanced, and the defects are introduced on the surface of the small-size lanthanum titanate nano particles, so that the photocatalytic hydrogen production activity is improved.
2. The method of the invention has the advantages of simple and easy operation, low cost, high repetition rate, stable property, environmental protection and no pollution.
Drawings
Fig. 1 is an X-ray diffraction (XRD) pattern of lanthanum titanate nanoparticles having defects according to the present invention;
FIG. 2 is a graph of the ultraviolet diffuse reflectance spectrum (UV-VisDRS) of a lanthanum titanate nanoparticle solid with defects according to the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) image of lanthanum titanate nanoparticles having defects according to the present invention;
FIG. 4 is a graph of hydrogen production performance of lanthanum titanate nanoparticles having defects according to the present invention.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
The preparation of the lanthanum titanate nanoparticle catalyst having defects includes the following steps:
step one, preparing small-size lanthanum titanate nanoparticles:
(1) adding 3g of polyethylene glycol (PEG-4000) into 16mL of deionized water, stirring for 30min at room temperature and the rotating speed of 300rpm, and completely dispersing to form a solution ①;
(2) adding 1.0825g of lanthanum nitrate hexahydrate solid into 16mL of glacial acetic acid, and stirring at room temperature for 30min at the rotating speed of 300rpm to fully dissolve the lanthanum nitrate hexahydrate solid to form a solution ②;
(3) dripping the solution ① into the solution ② to obtain a mixed solution A, and continuously stirring the mixed solution A at room temperature for 1h at the rotating speed of 300rpm to enable the mixed solution A to become clear to obtain a solution ③;
(4) adding 16mL of absolute ethyl alcohol into 1.7mL of tetrabutyl titanate (TBT) to obtain a mixed solution B, stirring at room temperature for 10min at the rotating speed of 300rpm, and fully mixing to obtain a solution ④;
(5) dripping the solution ③ into the solution ④, adjusting the pH to 1 with acetic acid to obtain a mixed solution C, and stirring the mixed solution C at 60 ℃ for 2 hours at the rotating speed of 300rpm to obtain a solution ⑤;
(6) transferring the solution ⑤ into an electric heating blast drying oven, drying for 48h at 60 ℃ to obtain lanthanum titanate gel, transferring the lanthanum titanate gel into a muffle furnace for high-temperature calcination treatment, heating to 900 ℃ at the speed of 2 ℃/min, preserving heat for 3h, and naturally cooling to room temperature to obtain the small-size lanthanum titanate nano-particles.
Step two, preparing the lanthanum titanate nano particles with defects:
uniformly mixing 0.6g of the small-size lanthanum titanate nanoparticles obtained in the step one with 0.3g of sodium borohydride, grinding for 30min to obtain a mixed sample, heating the mixed sample to 400 ℃ at a speed of 10 ℃/min by using a tube furnace under the protection of argon, preserving heat for 15 min to obtain a primary lanthanum titanate nanoparticle product with defects, loading the primary lanthanum titanate particle product into a 50mL centrifuge tube, adding 25mL deionized water, and standing for 48 hours to allow the primary lanthanum titanate particle product to react fully; centrifuging the reacted initial product at the centrifugal speed of 5000rpm for 5min, discarding the supernatant to obtain a precipitate, washing the precipitate with deionized water and ultrasonically treating for 4min, repeating the centrifuging and deionized water washing processes twice, and draining the precipitate under natural conditions to obtain a final product: lanthanum titanate nanoparticles having defects.
The lanthanum titanate nanoparticles with defects prepared by the method are characterized by X-ray diffraction (XRD), a solid ultraviolet diffuse reflectance spectrum (UV-VisDRS) diagram and a Scanning Electron Microscope (SEM).
From the XRD image of fig. 1, it can be seen that all the diffraction peak positions of the defective lanthanum titanate nanoparticles correspond to the diffraction peak positions of lanthanum titanate (JCPDS:28-0517), and there is no impurity peak, which proves that the lanthanum titanate nanoparticles prepared by the present invention have high purity.
As can be seen from the solid ultraviolet diffuse reflectance spectrum (UV-VisDRS) graph of fig. 2, the prepared lanthanum titanate nanoparticles having defects have improved absorption capacity in the visible region.
As can be seen from the SEM of fig. 3, the size of the lanthanum titanate nanoparticles having defects was about 30 nm.
Fig. 4 is a diagram of hydrogen production performance of the lanthanum titanate nanoparticles with defects, and it can be seen that the hydrogen production performance of the lanthanum titanate nanoparticles with defects is improved by about 13 times.
1. The reagent dosage in the first step can be amplified proportionally.
2. The reagents in the first step and the second step are analytically pure and are not further processed.
Claims (1)
1. A method for preparing a lanthanum titanate nanoparticle having defects, comprising the steps of:
step one, preparing small-size lanthanum titanate nanoparticles:
(1) adding 3g of polyethylene glycol (PEG-4000) into 16mL of deionized water, stirring for 30min at room temperature and the rotating speed of 300rpm, and completely dispersing to form a solution ①;
(2) adding 1.0825g of lanthanum nitrate hexahydrate solid into 16mL of glacial acetic acid, and stirring at room temperature for 30min at the rotating speed of 300rpm to fully dissolve the lanthanum nitrate hexahydrate solid to form a solution ②;
(3) dripping the solution ① into the solution ② to obtain a mixed solution A, and continuously stirring the mixed solution A at room temperature for 1h at the rotating speed of 300rpm to enable the mixed solution A to become clear to obtain a solution ③;
(4) adding 16mL of absolute ethyl alcohol into 1.7mL of tetrabutyl titanate (TBT) to obtain a mixed solution B, stirring at room temperature for 10min at the rotating speed of 300rpm, and fully mixing to obtain a solution ④;
(5) dripping solution ③ into solution ④, adjusting pH to 1 with acetic acid to obtain mixed solution C, and dissolving the mixed solution C at 60oStirring for 2 hours at the rotating speed of 300rpm under the condition of C to obtain a solution ⑤;
(6) the solution ⑤ was transferred to an electric hot air drying oven 60oDrying for 48 hours under the condition of C to obtain lanthanum titanate gel; transferring the lanthanum titanate gel into a muffle furnace for high-temperature calcination treatment to obtain a product with the purity of 2oHeating to 900 deg.C/minoC, preserving heat for 3 hours, and naturally cooling to room temperature to obtain small-size lanthanum titanate nanoparticles;
step two, preparing the lanthanum titanate nano particles with defects:
uniformly mixing 0.6g of the small-size lanthanum titanate nanoparticles obtained in the step one with 0.3g of sodium borohydride, grinding for 30min to obtain a mixed sample, and using a tube furnace to perform grinding for 10min under the protection of argon gasoThe temperature is raised to 400 ℃ at the rate of C/minoC, preserving the temperature for 15 minutes to obtain a primary product of the lanthanum titanate nanoparticles with defects, filling the primary product into a 50mL centrifuge tube, and adding 25mL of the primary productIonized water is placed for 48 hours to fully react; centrifuging the reacted initial product at the centrifugal speed of 5000rpm for 5min, discarding the supernatant to obtain a precipitate, washing the precipitate with deionized water and ultrasonically treating for 4min, repeating the centrifuging and deionized water washing processes twice, and draining the precipitate under natural conditions to obtain a final product: lanthanum titanate nanoparticles having defects.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111790366A (en) * | 2020-07-08 | 2020-10-20 | 齐鲁工业大学 | Defective lithium strontium titanate visible-light-driven photocatalyst, preparation method and application |
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