CN114408963B - Method for preparing perovskite oxide nano material by microwave method - Google Patents
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Abstract
A method for preparing perovskite oxide nano material by using a microwave method comprises the following steps: according to the chemical formula La x Ba 1‑ x SnO 3 Adding barium nitrate, lanthanum nitrate and stannic chloride pentahydrate into water according to a medium metering ratio to obtain a clear solution; wherein x is more than or equal to 0 and less than or equal to 0.04; dropwise adding a sodium hydroxide solution into the clear solution to obtain a mixed solution; heating the mixed solution to obtain a precipitate; and calcining the precipitate to obtain the perovskite oxide nano material. The invention uses a microwave method to prepare doped perovskite oxide La for carbon dioxide reduction catalytic reaction x Ba 1‑x SnO 3 . According to the invention, the doped perovskite oxide nano material which has no impurity phase and is uniformly dispersed is prepared only under the alkaline condition without adding expensive complexing agents such as citric acid, ionic liquid and the like.
Description
Technical Field
The invention belongs to the field of preparation of electrocatalytic nano materials, and particularly relates to a method for preparing a perovskite oxide nano material by using a microwave method.
Background
Over the past centuries, rapid industrial development and population growth have led to excessive fossil fuel consumption, exacerbating the global energy crisis. At the same time, a large amount of CO is emitted from fossil fuel combustion 2 The air is continuously accumulated in the atmosphere, which brings important environmental problems of global warming and seriously threatens the sustainable development of the global society. To cope with this problem, a series of global deployments, developments and applications of climate change technology are required, including renewable energy technology and carbon capture, utilization and sequestration technology (CCUS). The CCUS technology can achieve the aims of carbon reduction and decarburization in industries difficult to reduce emission such as thermal power, cement, steel and the like. In recent years, electrocatalytic carbon dioxide reduction, as a potential CCUS solution, is emerging and is being used to address the carbon cycle problem of human society.
BaSnO 3 Is a wide band gap (3.1 eV) semiconductor perovskite structure oxideThe composite material has excellent optical performance, electrical performance, thermal stability and corrosion resistance, and has wide application prospect in the fields of transparent conductive films, thermally stable capacitors, electrocatalysis, solar cells and the like. BaSnO commonly used at present 3 The synthesis method of the nano material mainly comprises a high-temperature solid-phase method and a hydrothermal method, wherein the high-temperature solid-phase method causes the phenomenon of overlarge grain size due to high sintering temperature and long sintering time, and the hydrothermal method also has the problems of long time consumption and serious particle agglomeration.
Disclosure of Invention
The invention aims to provide a method for preparing a perovskite oxide nano material by using a microwave method, and compared with the traditional hydrothermal method, the method can not only accurately control the reaction temperature, reduce the influence caused by temperature difference, but also greatly shorten the reaction time, reduce agglomeration and reduce energy consumption.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing perovskite oxide nano material by using a microwave method comprises the following steps:
according to the chemical formula La x Ba 1-x SnO 3 Metering ratio, adding barium nitrate, lanthanum nitrate and stannic chloride pentahydrate into water to obtain a clear solution; wherein x is more than or equal to 0 and less than or equal to 0.04;
dropwise adding a sodium hydroxide solution into the clear solution to obtain a mixed solution;
heating the mixed solution by microwave for crystallization to obtain a precursor precipitate;
and calcining the precursor precipitate, and removing impurity phases to obtain the perovskite oxide nano material.
Furthermore, x is more than or equal to 0.01 and less than or equal to 0.04.
Further, the ratio of the dosage of the tin chloride pentahydrate to the dosage of the water is 1mmol:8 to 10mL.
Furthermore, the concentration of the sodium hydroxide solution is 1.5-2.5 mol/L.
Further, the ratio of the consumption of the tin chloride pentahydrate to the consumption of the sodium hydroxide solution is 1mmol:10 to 12mL.
Furthermore, the heating temperature is 150-180 ℃, and the time is 60-180 min.
Furthermore, the calcining temperature is 750-850 ℃ and the time is 2h.
A perovskite oxide nano material prepared according to the method is a nano rod-shaped material with the diameter of 500 nm-1 mu m and the length of 3-7 mu m.
Compared with the prior art, the invention has the beneficial effects that:
microwaves are a form of energy that can be converted to heat in a medium. When heated by microwaves, the microwave energy is converted to heat energy by the microwave absorber. In the process, heat is generated from the inside of the material instead of absorbing a heat source from the outside, the whole material is heated at the same time, the heat energy utilization rate is high, and the temperature gradient of the whole material is small, so that the method is different from other conventional heating modes such as heating of a reaction kettle. Compared with traditional synthesis methods such as a high-temperature solid phase method, a hydrothermal method and the like, the microwave method shortens the reaction time and the subsequent sintering time, and the synthesized perovskite oxide nano material has better crystallinity and higher phase purity, saves energy to a certain extent, and improves the efficiency. Therefore, the invention prepares the doped perovskite oxide La for the carbon dioxide reduction catalytic reaction by using a microwave method x Ba 1-x SnO 3 (x is more than or equal to 0 and less than or equal to 0.04). According to the invention, under the condition that expensive complexing agents such as citric acid, ionic liquid and the like are not added, the doped perovskite oxide nano material which has no impurity phase and is uniformly dispersed is prepared only under the alkaline condition, and the defects of long reaction time consumption, nonuniform doping and expensive reagents in the traditional method are overcome.
Further, in the preparation process, the alkali concentration, the microwave reaction temperature and time and the calcination temperature are opposite to the La x Ba 1-x SnO 3 (x is more than or equal to 0 and less than or equal to 0.04) has obvious influence on crystallization and phase purity; la doping content x vs CO 2 The current density of the electro-catalytic reduction has a significant influence, CO 2 The electrocatalytic reduction performance improves as the La doping content x increases, and an optimal La doping amount exists.
Drawings
FIG. 1 is La prepared according to example 1 of the present invention x Ba 1-x SnO 3 (0≤x≤0.04) X-ray diffraction pattern (XRD) of the powder material.
FIG. 2 is La prepared according to example 1 of the present invention x Ba 1-x SnO 3 (x is more than or equal to 0 and less than or equal to 0.04) and a field emission Scanning Electron Microscope (SEM) and an EDS mapping (EDS mapping) picture of the powder material. Wherein, (a) is BaSnO 3 Low power SEM image of (a), (b) is BSO: 2-high magnification SEM image of La, (c) Ba element mapping image of correspondence map (b), (d) Sn element mapping image of correspondence map (b), (e) La element mapping image of correspondence map (b), and (f) O element mapping image of correspondence map (b).
FIG. 3 is La prepared according to example 1 of the present invention x Ba 1-x SnO 3 (x is more than or equal to 0 and less than or equal to 0.04) linear scanning voltammetry curve of the nano material. Wherein, (a) is BSO with different doping concentrations and La catalyst sample in CO 2 Linear sweep voltammograms in saturated electrolyte; (b) 2% for BSO La catalyst samples saturated in He and CO, respectively 2 Linear sweep voltammogram in saturated electrolyte.
Detailed Description
The invention will be further described in connection with embodiments of the invention and the accompanying drawings in order to better illustrate the advantages of the invention.
A method for preparing perovskite oxide for carbon dioxide reduction catalytic reaction by using a microwave method comprises the following steps:
(1) According to the chemical formula La x Ba 1-x SnO 3 Weighing barium nitrate, lanthanum nitrate and stannic chloride pentahydrate according to the molar ratio of the elements, wherein the molar ratio of the sum of the barium nitrate and the lanthanum nitrate to the stannic chloride pentahydrate is 1: x is more than or equal to 1,0 and less than or equal to 0.04.
(2) Sequentially dissolving the barium nitrate, the lanthanum nitrate and the stannic chloride pentahydrate obtained in the step (1) in 8-10 mL of deionized water, and continuously stirring for 10min to obtain a clear solution; the amount of tin chloride pentahydrate was 1mmol.
(3) Slowly dripping 10-12 mL of 1.5-2.5 mol/L sodium hydroxide solution into the clear solution obtained in the step (2), and continuously stirring for 30min to obtain a mixed solution;
(4) Placing the mixed solution obtained in the step (3) in a microwave reaction chamber, controlling the infrared heating temperature to be 150-180 ℃, and heating for 60-180 min to obtain a precipitate;
(5) Washing the precipitate obtained in the step (4) with deionized water for 4-5 times until the pH value is 7, and performing centrifugal filtration;
(6) Drying the precipitate obtained in the step (5) in an oven at 80 ℃ for 8-10 h to obtain solid powder;
(7) And (5) calcining the solid powder obtained in the step (6) in a muffle furnace at the temperature of 750-850 ℃ for 2h to obtain the required perovskite oxide.
The perovskite oxide nano material is applied to the preparation of an electrocatalyst.
Example 1
A method for preparing perovskite oxide for carbon dioxide reduction catalytic reaction by using a microwave method comprises the following steps:
(1) Adding 9mL of deionized water into a beaker, starting stirring, sequentially adding weighed 1mmol of barium nitrate (x = 0.01), 0mmol of lanthanum nitrate and 1mmol of stannic chloride pentahydrate, and stirring for 10min until the barium nitrate, the lanthanum nitrate and the stannic chloride pentahydrate are completely dissolved;
(2) Preparing 2mol/L sodium hydroxide solution, dropwise adding 12mL of the prepared sodium hydroxide solution into the solution obtained in the step (1), and continuously stirring for 30min;
(3) Transferring the solution obtained in the step (2) into a microwave reaction tube, and adjusting the infrared reaction temperature to 170 ℃ and the reaction time to 60min;
(4) And (4) washing the precipitate obtained in the step (3) for 4-5 times by a high-speed centrifuge to be neutral, and adjusting the rotating speed of the centrifuge to be 9800r/min for 3min.
(5) And (5) drying the water-washed precipitate obtained in the step (4) in an oven for 10 hours, and adjusting the temperature of the oven to 80 ℃.
(6) Calcining the dried precipitate obtained in the step (5) in a muffle furnace at 800 ℃ for 2h to obtain the perovskite oxide prepared by the microwave method, and marking the perovskite oxide as BaSnO 3 。
(7) And (3) weighing 5mg of the perovskite oxide obtained in the step (6), uniformly dispersing the perovskite oxide into 1mL of 0.05 wt% Nafion solution, and ultrasonically dispersing for 30min to obtain a catalyst dispersion liquid.
(8) And (4) measuring 2 mu L of the dispersion liquid obtained in the step (7) by using a liquid transfer gun, dripping the dispersion liquid on a glassy carbon electrode with the diameter of 6mm, and drying for later use.
(9) Placing the glassy carbon electrode loaded with the catalyst obtained in the step (8) as a working electrode in an H-shaped electrolytic cell with a Nafion 117 proton exchange membrane, taking Ag/AgCl as a reference electrode and a Pt sheet as a counter electrode, and before reaction, taking KHCO as the counter electrode 3 Continuously introducing high-purity CO into (0.5 mol/L) electrolyte 2 Until saturation (at least 30 min), and then carrying out linear sweep voltammetry curve test in the range of 0 to-1.5V vs. Ag/AgCl, with the sweep speed of 50mV s -1 。
Example 2
The difference from the example is that x =0.01, and the other processes are the same as example 1.
Example 3
The difference from the example is that x =0.02, and the other processes are the same as example 1.
Example 4
The difference from the example is that x =0.04, and the other processes are the same as example 1.
As can be seen from FIG. 1, la prepared by the microwave method x Ba 1-x SnO 3 (x is more than or equal to 0 and less than or equal to 0.04) the nano material is matched with the main diffraction peak of a standard card (PDF # 15-0708) and no miscellaneous peak is formed, which shows that La is x Ba 1-x SnO 3 (x is more than or equal to 0 and less than or equal to 0.04), uniform doping and good crystallinity.
As can be seen from (a) to (f) in FIG. 2, la prepared by the microwave method x Ba 1-x SnO 3 (x is more than or equal to 0 and less than or equal to 0.04) the shape of the nano material is a nano rod shape with the diameter of 500nm to 1 mu m and the length of 3 to 7 mu m, and the constituent elements are uniformly dispersed.
As can be seen from (a) and (b) of FIG. 3, la with different doping concentrations was prepared by the microwave method x Ba 1-x SnO 3 (x is more than or equal to 0 and less than or equal to 0.04) the nano material is in CO 2 Under the condition of saturated electrolyte linear sweep voltammetry test, BSO:2% of La 3+ The current density of (2) is the maximum, indicating that the sample has the optimal CO 2 Reducing power, and the reduction reaction is initiatedThe potential was about-0.7v vs. ag/AgCl, significantly less than the reduction onset potential (-0.9V) in a saturated He electrolyte. This result demonstrates that saturated CO is compared to the hydrogen evolution reaction that occurs in saturated He solutions 2 The reduction process of the solution requires less overpotential and higher current density with CO 2 Potential application of electrocatalytic reduction.
Example 5
(1) Adding 9ml of deionized water into a beaker, starting stirring, sequentially adding weighed (1-x) mmol of barium nitrate (x = 0.01), x mmol of lanthanum nitrate and 1mmol of stannic chloride pentahydrate, and stirring for 10min until the barium nitrate, the lanthanum nitrate and the stannic chloride pentahydrate are completely dissolved;
(2) Preparing 1.5mol/L sodium hydroxide solution, dropwise adding 10mL of the prepared sodium hydroxide solution into the solution obtained in the step (1), and continuously stirring for 30min;
(3) Transferring the solution obtained in the step (2) into a microwave reaction tube, and adjusting the infrared reaction temperature to 170 ℃ and the reaction time to 60min;
(4) And (4) washing the precipitate obtained in the step (3) for 4-5 times by a high-speed centrifuge to be neutral, adjusting the rotating speed of the centrifuge to be 9800r/min, and keeping the rotating speed for 3min.
(5) And (5) drying the water-washed precipitate obtained in the step (4) in an oven for 8 hours, and adjusting the temperature of the oven to 80 ℃.
(6) Calcining the dried precipitate obtained in the step (5) in a muffle furnace at 800 ℃ for 2h to obtain the perovskite oxide prepared by the microwave method, and marking the perovskite oxide as La x Ba 1-x SnO 3 。
Example 6
(1) Adding 9ml of deionized water into a beaker, starting stirring, sequentially adding weighed (1-x) mmol of barium nitrate (x = 0.01), x mmol of lanthanum nitrate and 1mmol of stannic chloride pentahydrate, and stirring for 10min until complete dissolution;
(2) Preparing 2.5mol/L sodium hydroxide solution, dropwise adding 12mL of the prepared sodium hydroxide solution into the solution obtained in the step (1), and continuously stirring for 30min;
(3) Transferring the solution obtained in the step (2) into a microwave reaction tube, and adjusting the infrared reaction temperature to 180 ℃ and the reaction time to 60min;
(4) And (4) washing the precipitate obtained in the step (3) for 4-5 times by a high-speed centrifuge to be neutral, and adjusting the rotating speed of the centrifuge to be 9800r/min for 3min.
(5) And (5) drying the water-washed precipitate obtained in the step (4) in an oven for 9 hours, and adjusting the temperature of the oven to 80 ℃.
(6) Calcining the dried precipitate obtained in the step (5) in a muffle furnace at 850 ℃ for 2h to obtain the perovskite oxide prepared by the microwave method, and marking the perovskite oxide as La x Ba 1-x SnO 3 。
Example 7
(1) Adding 10ml of deionized water into a beaker, starting stirring, sequentially adding weighed (1-x) mmol of barium nitrate (x = 0.01), x mmol of lanthanum nitrate and 1mmol of stannic chloride pentahydrate, and stirring for 10min until the barium nitrate, the lanthanum nitrate and the stannic chloride pentahydrate are completely dissolved;
(2) Preparing 2mol/L sodium hydroxide solution, dropwise adding 12mL of the prepared sodium hydroxide solution into the solution obtained in the step (1), and continuously stirring for 30min;
(3) Transferring the solution obtained in the step (2) into a microwave reaction tube, and adjusting the infrared reaction temperature to 160 ℃ and the reaction time to 120min;
(4) And (4) washing the precipitate obtained in the step (3) for 4-5 times by a high-speed centrifuge to be neutral, and adjusting the rotating speed of the centrifuge to be 9800r/min for 3min.
(5) And (5) drying the water-washed precipitate obtained in the step (4) in an oven for 10 hours, and adjusting the temperature of the oven to 80 ℃.
(6) Calcining the dried precipitate obtained in the step (5) in a muffle furnace at 750 ℃ for 2h to obtain the perovskite oxide prepared by the microwave method, and marking the perovskite oxide as La x Ba 1-x SnO 3 。
Claims (4)
1. The application of the perovskite oxide nano material prepared by the microwave method in the carbon dioxide reduction catalytic reaction is characterized by comprising the following steps:
the nano material is in CO 2 Can react to CO in saturated electrolyte 2 Electrocatalytic reduction;
the perovskite oxide nano material prepared by the microwave method is prepared by the following steps: according to the chemical formula La x Ba 1-x SnO 3 Metering ratio, adding barium nitrate, lanthanum nitrate and stannic chloride pentahydrate into water to obtain a clear solution; wherein x is more than 0 and less than or equal to 0.04;
dropwise adding a sodium hydroxide solution into the clear solution to obtain a mixed solution;
heating the mixed solution by microwave for crystallization to obtain a precursor precipitate; wherein the heating temperature is 150 to 180 ℃, and the time is 60 to 180 min;
calcining the precursor precipitate, and removing impurity phases to obtain the perovskite oxide nano material; wherein the calcining temperature is 750 to 850 ℃, and the time is 2 hours.
2. The application of the perovskite oxide nano-material prepared by the microwave method in the carbon dioxide reduction catalytic reaction as claimed in claim 1, wherein the ratio of the consumption of tin chloride pentahydrate to the consumption of water is 1mmol:8 to 10mL.
3. The perovskite oxide nano material prepared by the microwave method and applied to the carbon dioxide reduction catalytic reaction according to claim 1, wherein the concentration of the sodium hydroxide solution is 1.5 to 2.5mol/L.
4. The use of the perovskite oxide nanomaterial prepared by the microwave method in the carbon dioxide reduction catalytic reaction as claimed in claim 3, wherein the ratio of the amount of tin chloride pentahydrate to the amount of sodium hydroxide solution is 1mmol:10 to 12mL.
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| KR101804173B1 (en) * | 2016-04-04 | 2017-12-05 | 한국화학연구원 | BaSnO3 film, and method of low- temperature manufacturing the same |
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| CN111298784A (en) * | 2020-02-03 | 2020-06-19 | 天津大学 | Catalyst for preparing oxalic acid by electrocatalytic reduction of carbon dioxide and preparation method thereof |
| CN112442760A (en) * | 2020-11-24 | 2021-03-05 | 内蒙古工业大学 | Orthorhombic phase P doped La2Co2O5Perovskite nanofiber, electrocatalyst formed by perovskite nanofiber and preparation method of perovskite nanofiber |
| CN112981454A (en) * | 2021-02-03 | 2021-06-18 | 山东大学 | Manganese dioxide ultra-long nanowire catalyst with oxygen vacancy as well as preparation method and application thereof |
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