CN115504507A - Preparation method of bismuth antimonate nano material - Google Patents
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Abstract
The invention discloses a preparation method of a bismuth antimonate nano material, which is characterized in that bismuth nitrate and antimony acetate are used as raw materials, citric acid is used as a precipitator, the bismuth antimonate nano material is prepared by adopting a coprecipitation method, the operation is simple, the cost is low, the phase and the size of a target product are controllable, and the prepared bismuth antimonate nano material has better application prospects in devices such as optics, electrics, electrochemistry and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of bismuth antimonate materials, and particularly relates to a preparation method of a bismuth antimonate nano material.
Background
The antimonate compound has good physical and chemical properties and stable physical and chemical properties, and has wide application in the fields of gas-sensitive sensing, photocatalysis, luminescent materials and the like. Common antimonates are sodium antimonate, meta-antimonate MSb 2 O 6 (M = Ca, sr, ba), ba of double perovskite structure 2 LnSbO 6 (Ln = Sc, Y and rare earth element), and the like. The prior preparation method of antimonate comprises the following steps: hydrothermal synthesis, high-temperature solid phase method, and the like. The invention discloses a preparation method of a self-supporting structure bismuth zinc antimonate self-assembled nanorod, a product and application thereof (patent number: ZL 201811620553.1), and the bismuth zinc antimonate self-assembled nanorod is synthesized by high-temperature calcination by taking sodium bismuthate, zinc acetate and antimony trichloride as raw materials. The operation of the proposal is complex and has the purpose ofThe phase and size of the target product are difficult to control effectively.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a bismuth antimonate nano material, which takes citric acid as a precipitator and adopts a coprecipitation method to prepare the bismuth antimonate nano material, so that the preparation method is simple to operate, low in cost and controllable in phase and size of a target product, and the prepared bismuth antimonate nano material has better application prospects in devices such as optics, electrics, electrochemistry and the like.
The invention provides the following technical scheme:
a preparation method of a bismuth antimonate nano material comprises the following steps:
s1, preparing a bismuth antimonate nano material by taking bismuth nitrate, antimony acetate, citric acid and deionized water as raw materials and adopting a coprecipitation method;
s2, dissolving citric acid in deionized water, and stirring by using a magnetic stirrer to prepare a citric acid solution with a certain concentration;
s3, simultaneously adding bismuth nitrate and antimony acetate into the citric acid solution prepared in the step S2 according to a certain molar ratio, stirring and standing for a period of time;
s4, filtering the precipitate obtained after the standing in the step S3, and repeatedly washing the precipitate with deionized water for a plurality of times;
s5, cleaning the precipitate, and drying the precipitate in a drying box at a certain temperature for a period of time;
and S6, carrying out heat preservation treatment on the precipitate dried in the step S5 at a certain temperature for a period of time to obtain the bismuth antimonate nano material.
Preferably, in step S2, the concentration of the citric acid solution is 1.7mol/L.
Preferably, in step S3, the molar ratio of bismuth nitrate to antimony acetate is 1.
Preferably, in step S3, the stirring time is 30min, and the standing time is 1h.
Preferably, in step S5, the drying oven temperature is 60 ℃, and the drying time is 4 hours.
Preferably, in the step S6, the muffle furnace temperature is 500-700 ℃, and the heat preservation treatment time is 1-4h.
Preferably, in step S6, a muffle furnace is used for heat preservation at a constant temperature.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the bismuth antimonate nano material, disclosed by the invention, the bismuth antimonate nano material is prepared by taking citric acid as a precipitator and adopting a coprecipitation method, the operation is simple, the cost is low, the phase and the size of a target product can be controlled, and the prepared bismuth antimonate nano material has a good application prospect in devices such as optics, electricity, electrochemistry and the like.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and that those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
FIG. 1 is a flow chart of the preparation method of the present invention.
FIG. 2 is an X-ray diffraction (XRD) pattern of the bismuth antimonate nano-material of the present invention.
Fig. 3 is a Scanning Electron Microscope (SEM) image of the bismuth antimonate nanomaterial of the present invention.
Fig. 4 is a Transmission Electron Microscope (TEM) image of the bismuth antimonate nanomaterial of the present invention.
Fig. 5 is a High Resolution Transmission Electron Microscope (HRTEM) image of the bismuth antimonate nanomaterial of the present invention.
FIG. 6 is a flow chart of a CALYPSO method of the present invention.
FIG. 7 is an X-ray powder diffraction pattern of the bismuth antimonate nano-material of the present invention under different pressures.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described in detail and completely with reference to the accompanying drawings. It is to be understood that the described embodiments are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Thus, the following detailed description of the embodiments of the present invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Referring to fig. 1-5, a method for preparing a bismuth antimonate nano material includes the following steps:
s1, preparing a bismuth antimonate nano material by taking bismuth nitrate, antimony acetate, citric acid and deionized water as raw materials and adopting a coprecipitation method;
s2, dissolving citric acid in deionized water, and stirring by using a magnetic stirrer to prepare a citric acid solution with a certain concentration;
s3, simultaneously adding bismuth nitrate and antimony acetate into the citric acid solution prepared in the step S2 according to a certain molar ratio, stirring and standing for a period of time;
s4, filtering the precipitate obtained after the standing in the step S3, and repeatedly washing the precipitate with deionized water for a plurality of times;
s5, cleaning the precipitate, and drying the precipitate in a drying box at a certain temperature for a period of time;
and S6, carrying out heat preservation treatment on the precipitate dried in the step S5 at a certain temperature for a period of time by using a muffle furnace to obtain the bismuth antimonate nano material.
The bismuth antimonate nano material is prepared by taking citric acid as a precipitator and adopting a coprecipitation method, so that the operation is simple, the cost is low, the phase and the size of a target product can be controlled, and the prepared bismuth antimonate nano material has a good application prospect in devices such as optics, electricity, electrochemistry and the like.
Further, as a specific embodiment, in the step S2, the concentration of the citric acid solution is 1.7mol/L.
Further, as a specific embodiment, in step S3, the molar ratio of bismuth nitrate to antimony acetate is 1.
Further, as a specific embodiment, in step S3, the stirring time is 30min, and the standing time is 1h.
Further, as a specific embodiment, in step S5, the drying oven temperature is 60 ℃, and the drying time is 4h.
Further, in the step S6, the muffle furnace temperature is 500-700 ℃, and the heat preservation treatment time is 1-4h.
FIG. 2 is an X-ray diffraction (XRD) pattern of the bismuth antimonate nano-material prepared by the invention.
FIG. 2 is an XRD pattern of a bismuth antimonate nano material, the calcination temperature is 600 ℃, the heat preservation time is 2h, and compared with a PDF (No. 44-0198) standard card, the peaks of 27.94 degrees, 31.71 degrees, 32.69 degrees, 46.89 degrees, 54.24 degrees and 55.49 degrees in a doped sample are corresponding to Bi 7.89 Sb 0.11 O 12.0+x (PDF No. 44-0198) (201), (002), (220), (222), (203), and (421) crystal planes. This result indicates that the product is composed of tetragonal Bi 7.89 Sb 0.11 O 12.0+x (PDF No. 44-0198), the diffraction peaks in the product are sharp, which indicates that the crystallinity is high, and the diffraction peaks of other impurities are not detected from the product, which indicates that the product has high purity.
Fig. 3 is a Scanning Electron Microscope (SEM) image of the bismuth antimonate nanomaterial prepared by the present invention. And (3) observing the structure and the morphology of the bismuth antimonate nano material by using a field emission electron scanning microscope (FE-SEM), wherein the calcining temperature is 600 ℃, and the heat preservation time is 2 hours, as shown in figure 3. The bismuth antimonate nano material is formed by stacking irregular nano sheets, and the nano sheets are vertically interpenetrated with the nano sheets. The morphology has larger specific surface area, and provides possibility for improving the performance of the material.
Fig. 4 is a Transmission Electron Microscope (TEM) image of the bismuth antimonate nanomaterial prepared by the present invention. The obtained product is a nano-sheet, the surface is smooth, and the shape of the nano-sheet is angular.
Fig. 5 is a High Resolution Transmission Electron Microscope (HRTEM) image of the bismuth antimonate nanomaterial prepared according to the present invention. The regular lattice fringes of the resulting bismuth antimonate nanoplatelets can be seen in the figure, indicating that such nanoplatelets consist of single crystals.
Example 2
The difference from the embodiment 1 is that citric acid is dissolved in deionized water, then a magnetic stirrer is used for stirring, bismuth nitrate and antimony acetate are added simultaneously after dissolution, stirring is carried out for 30min, standing is carried out for 1h, the obtained precipitate is filtered and repeatedly washed by deionized water for a plurality of times, after washing, the precipitate is dried in a drying oven at 60 ℃ for 4h, and finally the sample is subjected to heat preservation treatment at 500 ℃ for 2h by using a muffle furnace. Wherein the molar ratio of the bismuth nitrate to the antimony acetate is 1.
Example 3
The difference from the embodiment 1 is that citric acid is dissolved in deionized water, then a magnetic stirrer is used for stirring, bismuth nitrate and antimony acetate are added simultaneously after dissolution, stirring is carried out for 30min, standing is carried out for 1h, the obtained precipitate is filtered and repeatedly washed by deionized water for a plurality of times, after washing, the precipitate is dried in a drying oven at 60 ℃ for 4h, and finally the sample is subjected to heat preservation treatment at 700 ℃ for 2h by using a muffle furnace. Wherein the molar ratio of the bismuth nitrate to the antimony acetate is 1.
Example 4
The difference from the embodiment 1 is that citric acid is dissolved in deionized water, then a magnetic stirrer is used for stirring, bismuth nitrate and antimony acetate are added simultaneously after dissolution, stirring is carried out for 30min, standing is carried out for 1h, the obtained precipitate is filtered and repeatedly washed by deionized water for a plurality of times, after washing, the precipitate is dried in a drying oven at 60 ℃ for 4h, and finally the sample is subjected to heat preservation treatment at 600 ℃ for 1h by using a muffle furnace. Wherein the molar ratio of the bismuth nitrate to the antimony acetate is 1.
Example 5
The difference from the embodiment 1 is that citric acid is dissolved in deionized water, then a magnetic stirrer is used for stirring, bismuth nitrate and antimony acetate are added simultaneously after dissolution, stirring is carried out for 30min, standing is carried out for 1h, the obtained precipitate is filtered and repeatedly washed by deionized water for a plurality of times, after washing, the precipitate is dried in a drying oven at 60 ℃ for 4h, and finally the sample is subjected to heat preservation treatment at 600 ℃ for 4h by using a muffle furnace. Wherein the molar ratio of the bismuth nitrate to the antimony acetate is 1.
Example 6
The difference from the embodiment 1 is that citric acid is dissolved in deionized water, then a magnetic stirrer is used for stirring, bismuth nitrate and antimony acetate are added simultaneously after dissolution, stirring is carried out for 30min, standing is carried out for 1h, the obtained precipitate is filtered and repeatedly washed by deionized water for a plurality of times, after washing, the precipitate is dried in a drying oven at 60 ℃ for 4h, and finally the sample is subjected to heat preservation treatment at 500 ℃ for 4h by using a muffle furnace. Wherein the molar ratio of the bismuth nitrate to the antimony acetate is 1.
Example 7
The difference from example 1 is that citric acid is dissolved in deionized water, then a magnetic stirrer is used for stirring, bismuth nitrate and antimony acetate are added simultaneously after dissolution, stirring is carried out for 30min, standing is carried out for 1h, the obtained precipitate is filtered and washed repeatedly with deionized water for a plurality of times, after washing, the precipitate is dried in a drying oven at 60 ℃ for 4h, and finally the sample is subjected to heat preservation treatment at 700 ℃ for 4h by using a muffle furnace. Wherein the molar ratio of the bismuth nitrate to the antimony acetate is 1.
Example 8
The difference from example 1 is that citric acid is dissolved in deionized water, then a magnetic stirrer is used for stirring, bismuth nitrate and antimony acetate are added simultaneously after dissolution, stirring is carried out for 30min, standing is carried out for 1h, the obtained precipitate is filtered and washed repeatedly with deionized water for a plurality of times, after washing, the precipitate is dried in a drying oven at 60 ℃ for 4h, and finally the sample is subjected to heat preservation treatment at 700 ℃ for 1h by using a muffle furnace. Wherein the molar ratio of the bismuth nitrate to the antimony acetate is 1.
Example 9
The difference from the embodiment 1 is that citric acid is dissolved in deionized water, then a magnetic stirrer is used for stirring, bismuth nitrate and antimony acetate are added simultaneously after dissolution, stirring is carried out for 30min, standing is carried out for 1h, the obtained precipitate is filtered and washed repeatedly for a plurality of times by deionized water, after washing, the precipitate is dried in a drying oven at 60 ℃ for 4h, and finally the sample is subjected to heat preservation treatment at 500 ℃ for 1h by using a muffle furnace. Wherein the molar ratio of the bismuth nitrate to the antimony acetate is 1.
Example 10
Referring to fig. 6, based on embodiment 1, a step S7 is further included, and a caliypso method is used to perform structure prediction on the bismuth antimonate nanomaterial prepared in step S6 under a certain high pressure.
In step S7, the specific implementation of the callposo method includes the steps of:
s71, firstly, randomly generating a certain number of initial structures as first generation structures under the condition of symmetry limitation;
s72, after the structure is generated, performing fingerprint characterization on the structure through the key-forming characteristic matrix, and further performing similarity judgment on the generated structure so as to eliminate the similar structure;
s73, carrying out local optimization on the generated structure by using a method based on a first linear principle or a force field;
s74, selecting a part of structures with high fitness (for example, 60% of the whole population) and generating a new structure by using a swarm intelligence algorithm (a particle swarm optimization algorithm), wherein the rest of structures (for example, 40% of the whole population) are generated by a random method (in this way, a random structure is introduced in the structure evolution process, so that the diversity of the population can be effectively increased, the algorithm is prevented from converging to a certain local minimum value point, and the global search capability of the CALYPSO method is enhanced);
and S75, judging whether the program is converged, and if so, ending the whole program.
The structure prediction of the bismuth antimonate nano material under high pressure is carried out based on CALYPSO method. And (3) calculating the total energy of the system by adopting a plane wave basis set CAStep module based on a density functional theory. The exchange relation is selected based on a generalized gradient approximation Perew-Burke-Ernzerhof (PBE) functional, and the pseudopotential is full electronic projection-augmented plane wave (PAW) pseudopotential based on freezing nuclear approximation. The full electron projection-enhanced wave PAW pseudopotentials for bismuth and antimony are 6s26p3 and 5s25p3, respectively. The truncation energy is set to 600 ev and the appropriate k-point grid density for brillouin zone sampling is selected with an energy accuracy of less than 1meV/atom.
The high-voltage synchrotron radiation X-ray experiment is respectively completed by a synchrotron radiation light source 15U1 experiment line station of a physical research institute and a synchrotron radiation light source 4W2 high-voltage experiment line station of a Beijing high-energy institute in Shanghai. The wavelengths of the X-rays of the two light sources are both
In the experiment, bismuth antimonate powder (Alfa Aesar, purity 99.99%) and a small piece of ruby were loaded into a diamond anvil chamber. Silicone oil is used as a pressure-transmitting medium. CeO is used as the distance between the sample and the detector and as the parameter of the detector 2 The standard is calibrated. The Bragg diffraction image was integrated using FIT2D software to generate a diffraction spectrum of intensity versus diffraction angle 2-theta.
In-situ resistivity and hall effect measurements are made at high voltage using a current inversion method to avoid thermoelectric offsets. The measurement procedure is performed automatically using the Van der Pauw method. For temperature dependent resistivity measurements, liquid nitrogen was used to obtain low temperatures of 85 to 275K. The hall effect measurements were performed in a magnetic field of 1.5T.
An in-situ high-pressure synchrotron radiation X-ray experiment was performed on bismuth antimonate using a diamond anvil cell. As figure 7 (a) increases with pressure, all diffraction peaks move to higher angles. The diffraction peak of the bismuth antimonate has no obvious change from the normal pressure condition to 3.2 GPa. At pressures close to 4.2GPa, new diffraction peaks suddenly appear near 12.4 and 13.0 °, which clearly indicates the onset of structural phase transformation. The intensity of this new peak rapidly increases, becoming the strongest peak of the high-pressure phase. Within a narrow range of 4.2-8.5GPa, two phases of alpha-bismuth antimonate and beta-bismuth antimonate coexist. When the pressure is higher than 8.5GPa, the diffraction peak only has the diffraction peak of a beta-bismuth antimonate phase, and the phase change is completed. At 20.3GPa, new characteristic peaks appeared at 9.4 and 17.1 °, the β -bismuth antimonate started to convert to a new γ -bismuth antimonate and no further conversion was observed over the pressure range tested. The high-voltage structure of the bismuth antimonate is revealed through experiments. FIG. 7 (b) shows the results of Fullprof refinement of the R3m, I4/mcm and Pm-3m phases at 0.9 (. Alpha. -bismuth antimonate), 11.3 (. Beta. -bismuth antimonate) and 20.3GPa (. Gamma. -bismuth antimonate). Experiments show that the bismuth antimonate nano material prepared by taking citric acid as a precipitator and adopting a coprecipitation method has stronger compression resistance and better stability than the bismuth antimonate nano material prepared by the existing method.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art; 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 (10)
1. The preparation method of the bismuth antimonate nano material is characterized by comprising the following steps of:
s1, preparing a bismuth antimonate nano material by taking bismuth nitrate, antimony acetate, citric acid and deionized water as raw materials and adopting a coprecipitation method;
s2, dissolving citric acid in deionized water, and stirring by using a magnetic stirrer to prepare a citric acid solution with a certain concentration;
s3, simultaneously adding bismuth nitrate and antimony acetate into the citric acid solution prepared in the step S2 according to a certain molar ratio, stirring and standing for a period of time;
s4, filtering the precipitate obtained after the standing in the step S3, and repeatedly washing the precipitate with deionized water for a plurality of times;
s5, cleaning the precipitate, and then drying the precipitate for a period of time at a certain temperature in a drying box;
and S6, carrying out heat preservation treatment on the precipitate dried in the step S5 at a certain temperature for a period of time to obtain the bismuth antimonate nano material.
2. The method for preparing bismuth antimonate nano-material according to claim 1, wherein in step S2, the concentration of the citric acid solution is 1.7mol/L.
3. The method for preparing bismuth antimonate nano-material according to claim 1, wherein in step S3, the molar ratio of bismuth nitrate to antimony acetate is 1.
4. The method for preparing the bismuth antimonate nano-material according to claim 1, wherein in the step S3, the stirring time is 30min, and the standing time is 1h.
5. The method for preparing bismuth antimonate nano-material according to claim 1, wherein in step S5, the temperature of the drying oven is 60 ℃, and the drying time is 4h.
6. The method for preparing the bismuth antimonate nano material as claimed in claim 1, wherein in the step S6, the temperature of the muffle furnace is 500-700 ℃, and the duration of the heat preservation treatment is 1-4h.
7. The method for preparing the bismuth antimonate nano-material according to claim 1, wherein in the step S6, a muffle furnace is adopted for heat preservation treatment at a certain temperature.
8. The method for preparing the bismuth antimonate nano material according to claim 1, characterized by further comprising the step S7: and (4) performing structure prediction on the bismuth antimonate nano material prepared in the step (S6) under high pressure by adopting a CALYPSO method.
9. The method for preparing bismuth antimonate nano-material according to claim 8, wherein in the step S7, the implementation of the CALYPSO method includes the following steps:
s71, randomly generating a certain number of initial structures as first generation structures under the condition of symmetry limitation;
s72, after the structure is generated, performing fingerprint representation on the structure through the key-forming feature matrix, and further performing similarity judgment on the generated structure so as to eliminate the similar structure;
s73, carrying out local optimization on the generated structure by using a method based on a first linear principle or a force field;
s74, selecting a part of structure with high fitness to generate a new structure by using a crowd sourcing algorithm, wherein the rest part of structure is generated by a random method;
and S75, judging whether convergence occurs or not, and ending if convergence occurs.
10. The method for preparing the bismuth antimonate nano material according to claim 9, wherein the part of the structure with high adaptability accounts for 60% of the whole population; the swarm intelligence algorithm is a particle swarm optimization algorithm.
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