CN115069248A - Silver niobate nano material and preparation method and application thereof - Google Patents

Silver niobate nano material and preparation method and application thereof Download PDF

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CN115069248A
CN115069248A CN202210818030.8A CN202210818030A CN115069248A CN 115069248 A CN115069248 A CN 115069248A CN 202210818030 A CN202210818030 A CN 202210818030A CN 115069248 A CN115069248 A CN 115069248A
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silver
silver niobate
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nano material
niobate
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高爽
郑小铭
李琦
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Southwest Jiaotong University
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    • B01J23/66—Silver or gold
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    • B01J37/08—Heat treatment
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
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Abstract

The invention discloses a silver niobate nano material and a preparation method and application thereof, and belongs to the technical field of nano material preparation, solar energy utilization and environmental protection. The preparation of the pure-phase silver niobate with the grain size of nanometer level is realized by combining the technical means of ion coordination complexing and ultrasonic spray pyrolysis, the difficult problems that the silver niobate nanometer material prepared by the traditional solid phase synthesis method is easy to generate impure phase and needs a high-oxygen environment are solved, the size of the prepared silver niobate nanometer grain is less than 100nm, the prepared silver niobate nanometer grain can absorb sunlight in a visible light wave band, and the silver niobate nanometer grain can be used as a photocatalytic material applied to CO 2 Reduction and purification of organic pollutants in the environment.

Description

Silver niobate nano material and preparation method and application thereof
Technical Field
The invention relates to the technical field of nano material preparation, solar energy utilization and environmental protection, in particular to a silver niobate nano material and a preparation method and application thereof.
Background
With the development of human society and the rapid development of industry, the consumption of fossil fuels is rapidly increased, and environmental pollution and the shortage of renewable energy resources become two major problems facing the world. Therefore, developing environmentally friendly, clean, safe, and sustainable technologies to face environmental and energy issues is one of the most pressing challenges facing researchers today. The semiconductor photocatalysis technology can realize the purposes of degrading pollutants, decomposing water to prepare hydrogen, reducing carbon dioxide and the like, and the technical core of the semiconductor photocatalysis technology lies in the design and synthesis of high-efficiency semiconductor photocatalysis materials. The silver niobate material with the perovskite structure has natural polarity characteristics, and the special property of the 4d orbit of Ag of the noble metal Ag element on the A site brings the uniqueness of the catalytic performance. In addition, the energy band structure of the silver niobate is matched with the spectrum of sunlight, the solar energy utilization rate is high, the sufficient reduction capability is kept, and the strong oxidation capability is also kept, so that the silver niobate is an ideal photocatalytic material.
However, the current method for preparing silver niobate is mainly a solid-phase sintering method, namely, a silver source (containing Ag) 2 O、AgNO 3 Etc.) and Nb 2 O 5 As raw material, grinding and then adding into O 2 Synthesis of AgNbO in an atmosphere 3 And (3) powder. The solid-phase reaction method has the following defects: (1) during the mixed sintering at high temperature, due to Ag 2 The existence of a hetero phase in the product due to the thermodynamic instability of O; (2) the reaction is required to be carried out in a high-oxygen environment; (3) the crystal size is large and difficult to control. The grain size and specific surface area of the photocatalytic material directly affect the photocatalytic activity and efficiency, so the existing preparation method is not enough to meet the design requirement of the silver niobate material with high photocatalytic activity. Development of grain sizeThe preparation process of the silver niobate material with fully exposed surface catalytic sites at the nanometer level is particularly important for the development of semiconductor photocatalysis technology and related semiconductor technology.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method and application of a silver niobate nano material, particularly, the preparation of pure-phase silver niobate with a grain size of nano grade is realized by combining ion coordination and complexation with an ultrasonic spray pyrolysis technical means, the problems that the silver niobate nano material prepared by the traditional solid phase synthesis method is easy to generate impure phase and needs a high-oxygen environment are solved, the size of the prepared silver niobate nano grain is less than 100nm, the prepared silver niobate nano grain can absorb sunlight in a visible light wave band, and the silver niobate nano grain can be used as a photocatalytic material applied to CO 2 Reduction and purification of organic pollutants in the environment
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the perovskite structure silver niobate nano material is characterized in that the prepared silver niobate nano crystal grain size is less than 100nm, the forbidden bandwidth is 2.9-3.2eV, and the silver niobate nano material can absorb ultraviolet and partial visible wave band light energy in solar spectrum.
The material is prepared by adopting an ion coordination complexing and spray pyrolysis process.
The preparation method of the silver niobate photocatalytic material is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a precursor solution by ion coordination and complexation: dissolving niobium hydroxide in ammonium bifluoride (NH) 4 HF 2 ) Obtaining solution A in the solution; weighing a proper amount of silver salt to prepare a silver ion solution to obtain a solution B; adding the solution B into the solution A, stirring uniformly, and adding hydrogen peroxide for coordination complexing to obtain a precursor solution;
(2) spray pyrolysis: and putting the precursor solution into an ultrasonic atomizer for atomization to generate liquid drops, carrying out pyrolysis on the liquid drops by adopting airflow to convey at the temperature of 700-1000 ℃, collecting the obtained powder, washing the powder for 3-5 times by using deionized water, and then carrying out vacuum drying for 8-24h at the temperature of 50-80 ℃ to obtain the silver niobate nano material.
The preparation method of the silver niobate nano material is characterized by comprising the following steps: in the step (1), niobium hydroxide and NH 4 HF 2 The molar ratio of the silver acetate to the niobium hydroxide to the hydrogen peroxide is 1:3-1:4, and the molar ratio of the silver acetate to the niobium hydroxide to the hydrogen peroxide is 1:1 (500-2000).
The preparation method of the silver niobate nano material is characterized by comprising the following steps: in the step (2), the ultrasonic frequency range of the ultrasonic atomizer is 1-2 MHz.
The silver niobate nano material is characterized in that: the silver niobate nano material is directly applied to CO under illumination 2 Reduction and degradation of organic matter.
The design idea of the invention is as follows:
the traditional solid phase sintering method has higher requirement on atmosphere, the prepared silver niobate is accompanied with impurity phases, and the solid phase sintering method also has the problems of overhigh required temperature and overlarge grain size. The grain size and specific surface area of the photocatalytic material directly affect the photocatalytic activity and efficiency, so the existing preparation method is not enough to meet the design requirement of the silver niobate material with high photocatalytic activity. The invention adopts a process method of ion coordination complexing combined with ultrasonic spray pyrolysis to prepare silver niobate nano powder. The core concept is that precursor solution containing silver salt and niobium salt with certain concentration is prepared and added with hydrogen peroxide for coordination and complexation, the precursor solution is atomized into liquid drops from a liquid phase to form aerosol through an ultrasonic atomization process, and the aerosol is pyrolyzed and synthesized in a tubular furnace under the transportation of carrier gas to finally form the silver niobate.
The invention has the advantages that:
1. the silver niobate synthesized by the method has good crystallinity and high purity.
2. The invention controls the appearance and the crystal size of the nano particles through the size of liquid drops formed by ultrasonic atomization.
3. The invention carries out coordination complexing on niobium salt and silver salt by adding hydrogen peroxide.
4. The silver niobate synthesized by the method has smaller crystal size, larger specific surface area and higher adsorption performance.
5. The silver niobate has the forbidden band width of about 2.7-3.2eV and has the optical response of visible light.
6. The silver niobate nano material prepared by the invention can be directly applied to CO under illumination 2 Reduction and degradation of organic matter.
Drawings
FIG. 1 is a graph comparing the results of X-ray diffraction of the silver niobate photocatalytic material prepared in example 1 and the heterogeneous phase-containing silver niobate prepared in comparative example 1; wherein: (a) x-ray diffraction pattern of silver niobate crystals prepared in example 1; (b) x-ray diffraction pattern of the silver niobate crystal containing a hetero-phase prepared in comparative example 1.
Fig. 2 is a uv-vis absorption curve of nano silver niobate prepared in example 1.
FIG. 3 is the graph of the absorption curve of RhB light in the photocatalytic degradation of silver niobate material in example 1.
FIG. 4 shows the photocatalytic reduction of CO by the silver niobate material in example 1 2 A map of methanol yield was generated.
FIG. 5 is a schematic view of the structure of a spray pyrolysis apparatus.
The specific implementation mode is as follows:
the invention is described in detail below with reference to the figures and examples.
In the following examples, the concentration of hydrogen peroxide used was 30 wt%; NH (NH) 4 HF 2 The niobium hydroxide is completely dissolved in a stirring mode, and the silver acetate is completely dissolved in an ultrasonic mode; NH (NH) 4 HF 2 Silver acetate, and niobium hydroxide contained 20 wt% water, and no crystal water.
The invention is carried out by adopting spray pyrolysis equipment when preparing silver niobate powder, as shown in figure 5, the spray pyrolysis equipment comprises an ultrasonic sprayer, a high-temperature tube furnace and a collector, wherein: the fog outlet of the ultrasonic sprayer is connected with the inlet end of the high-temperature tube furnace through a pipeline, and the outlet end of the high-temperature tube furnace is connected with the collector; the mist outlet of the ultrasonic sprayer is also connected with an air compressor for delivering compressed air to the mist outlet. When the device is used, precursor solutions of silver salt and niobium salt are atomized by an ultrasonic atomizer to generate liquid drops, the liquid drops are input into a high-temperature tube furnace by compressed air input by an air compressor, and finally, the obtained powder is collected by a collector; finally, washing the collected powder with deionized water for 3-5 times, and then drying the washed powder in vacuum for 8-24h at 50-80 ℃ to obtain the silver niobate nano material.
Example 1
The preparation process of the silver niobate nano material of the embodiment is as follows:
(1) preparing a precursor solution by ion coordination and complexation: 125mg of niobium hydroxide were dissolved in 60ml of 0.0675mol/L ammonium hydrogen fluoride (NH) 4 HF 2 ) Obtaining a niobate solution in an aqueous solution; weighing 112.6mg of silver acetate, dissolving the silver acetate in 60ml of deionized water to prepare a silver ion solution, and obtaining a silver salt solution; adding a silver salt solution into a niobium salt solution, uniformly stirring, and adding 11.8ml of hydrogen peroxide for coordination complexing to obtain a precursor solution;
(2) spray pyrolysis: and putting the precursor solution into an ultrasonic atomizer for atomization to generate liquid drops, carrying out pyrolysis on the liquid drops by adopting airflow to convey the liquid drops at the temperature of 800 ℃, collecting the obtained powder, washing the powder for 3 to 5 times by using deionized water, and then carrying out vacuum drying at the temperature of 60 ℃ for 24 hours to obtain the silver niobate nano material.
Comparative example 1
The preparation process of the silver niobate nano material comprises the following steps:
(1) 166.91mg of silver acetate, Nb are weighed 2 O 5 132.9mg of the powder was mixed in a mortar and ground, mixed uniformly and then placed in a crucible, calcined in a muffle furnace for 4 hours, ground, and further calcined at 900 ℃ for 5 hours.
(2) Washing and drying: and (2) putting the powder obtained in the step (1) into deionized water, then carrying out centrifugal separation, washing the separated powder for 3-5 times by using secondary deionized water, and drying the washed powder for 8-24 hours at the temperature of 50-80 ℃ to obtain a solid-phase sintered silver niobate sample.
As shown in fig. 1, comparing the XRD results of example 1 and comparative example 1, it is evident that pure phase silver niobate is synthesized by the spray pyrolysis process, whereas impurity phase-containing silver niobate is synthesized by the conventional solid phase sintering.
Fig. 2 is a uv-vis absorption curve of the nano silver niobate prepared in example 1, and it can be seen that the light absorption edge is about 420 nm.
Example 2
The photocatalytic material prepared in the example 1 is used for photocatalytic degradation of rhodamine B, and the specific process is as follows:
(1) 10mg of the powder obtained in example 1 was ultrasonically dispersed in 20mL of an aqueous solution of rhodamine b (rhb) of 10ppm to obtain a suspension. Transferring the suspension into a photocatalytic reactor, stirring for 30min in the dark with a magnetic stirrer, and irradiating the suspension with light under a 300W xenon lamp source with a visible spectrum and intensity of 45mW/cm 2 And (5) visible light illumination for 2 h.
(2) After the light irradiation is finished, supernatant is taken to determine the concentration of remaining rhodamine B (RhB) in the solution.
FIG. 3 is the graph of the absorption curve of RhB light in the photocatalytic degradation of silver niobate material in example 1.
Example 3
The photocatalytic material prepared in example 1 is used for photocatalytic reduction of carbon dioxide, and the specific process is as follows:
1. 50mg of the silver niobate nano material prepared in the embodiment 1 is added into 50ml of deionized water, and then ultrasonic dispersion is carried out for 15min, so as to prepare reaction liquid.
2. Adding the prepared reaction solution into a photocatalytic reactor, introducing carbon dioxide at the flow rate of 50-80ml/min for 30min, adsorbing for 30min in dark light (without illumination condition), and irradiating the reaction solution for 24h by using a xenon lamp.
FIG. 4 shows the photocatalytic reduction of CO by the silver niobate material in example 1 2 A map of methanol yield was generated.

Claims (7)

1. A silver niobate nano material is characterized in that: the silver niobate nano material is of a perovskite structure and is prepared by combining an ion coordination complexing and spray pyrolysis process.
2. The method for preparing a silver niobate nanomaterial according to claim 1, characterized in that: the method comprises the following steps:
(1) ion(s)Preparing a precursor solution by coordination and complexation: dissolving niobium hydroxide in ammonium bifluoride (NH) 4 HF 2 ) Obtaining a solution A in the solution; weighing a proper amount of silver salt to prepare a silver ion solution to obtain a solution B; adding the solution B into the solution A, stirring uniformly, and adding hydrogen peroxide for coordination complexing to obtain a precursor solution;
(2) spray pyrolysis: and putting the precursor solution into an ultrasonic atomizer for atomization to generate liquid drops, carrying out pyrolysis on the liquid drops by adopting airflow to convey at the temperature of 700-1000 ℃, collecting the obtained powder, washing the powder for 3-5 times by using deionized water, and then carrying out vacuum drying for 8-24h at the temperature of 50-80 ℃ to obtain the silver niobate nano material.
3. The method for preparing a silver niobate nanomaterial according to claim 2, characterized in that: in the step (1), the ammonium hydrogen fluoride (NH) 4 HF 2 ) The molar ratio of the niobium hydroxide to the niobium hydroxide is 1:3-1: 4.
4. The method for preparing a silver niobate nanomaterial according to claim 2, characterized in that: in the precursor solution, the molar ratio of niobium hydroxide, silver acetate to hydrogen peroxide is 1:1: (500-2000).
5. Silver niobate nanomaterial obtained according to claims 2 to 4, characterized in that: the silver niobate nano material has the grain size of 10-100nm and the forbidden band width of 2.7-3.2eV, and can absorb the light energy of ultraviolet and visible light wave bands in the solar spectrum.
6. The use of the silver niobate nanomaterial of claims 1 to 5, wherein: the silver niobate nano material is directly applied to CO under illumination 2 Reduction and degradation of organic matter.
7. The use of the silver niobate nano-material according to claim 6, characterized in that: the application process of the silver niobate nano material is as follows: dispersing the material in an aqueous solution containing carbon dioxide, and reducing carbon dioxide molecules into single-carbon and multi-carbon products under the illumination condition; in the organic matter-reducing water, the organic matter can be oxidatively decomposed into carbon dioxide and water.
CN202210818030.8A 2022-07-12 2022-07-12 Silver niobate nano material and preparation method and application thereof Pending CN115069248A (en)

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