CN116789181A - Preparation method and application of perovskite type samarium ferrite - Google Patents

Preparation method and application of perovskite type samarium ferrite Download PDF

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CN116789181A
CN116789181A CN202310834610.0A CN202310834610A CN116789181A CN 116789181 A CN116789181 A CN 116789181A CN 202310834610 A CN202310834610 A CN 202310834610A CN 116789181 A CN116789181 A CN 116789181A
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samarium
precursor solution
perovskite type
ferrite material
hydrates
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张明
唐菲
赵龙凤
蔡勇
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Changsha Semiconductor Technology And Application Innovation Research Institute
Hunan University
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Changsha Semiconductor Technology And Application Innovation Research Institute
Hunan University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01G49/00—Compounds of iron
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • G—PHYSICS
    • G01—MEASURING; TESTING
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    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
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Abstract

Perovskite samarium ferrite (SmFeO) 3 ) The preparation method comprises the following steps: (1) Dissolving soluble ferric salt, soluble samarium salt and citric acid monohydrate in an aqueous solution to prepare a precursor solution; (2) Dropwise adding ammonia water into the precursor solution in the step (1) until the precursor solution is neutral, and magnetically stirring the precursor solution at room temperature until the precursor solution is uniform; (3) Freezing the precursor solution uniformly stirred in the step (2); (4) putting the mixture obtained in the step (3) into a freeze dryer for drying; (5) Transferring the dried material into a square boat, placing the square boat into a tube furnace, and air-drying at 1-10deg.C for min ‑1 And then the temperature is kept for 2 to 5 hours after the temperature is raised to 500 to 950 ℃. The freeze drying method is introduced into the samarium ferrite material for preparation, so that the agglomeration of the material is reducedThe phenomenon is that the surface area ratio of the obtained perovskite type samarium ferrite material is high, the oxygen adsorption quantity and reaction rate are improved, the working temperature is effectively reduced, the sensitivity is improved, the response-recovery time is shortened, and the application of acetylene low-concentration detection can be realized.

Description

Preparation method and application of perovskite type samarium ferrite
Technical Field
The invention belongs to the field of semiconductor gas sensors, and particularly relates to a preparation method of a simple perovskite samarium ferrite (SmFeO 3) material and application thereof in detection of low-concentration acetylene gas.
Background
With the rapid development of industry and technology, production safety and environmental problems are increasingly highlighted while the material wealth is greatly enriched. Some inflammable and explosive and toxic harmful gases can cause threat to the health and life of people once generated or leaked. Therefore, it is necessary to develop a gas sensor having high responsiveness. Acetylene is both an important fuel and raw material and a flammable and explosive gas, and is often used in metal cutting and welding and organic material synthesis. When the leaked acetylene reaches a certain concentration, the acetylene is extremely easy to explode when meeting open fire, and threatens the life and property safety of people. If an alarm is given when the initial concentration of acetylene leakage is below the explosion limit, serious losses can be effectively avoided. Therefore, the development of the acetylene gas sensor with high responsiveness, low detection lower limit and high response speed has important summary of the invention.
In order to improve the performance index of the acetylene sensor, the invention patent with the application number of 201910396898.1 proposes that a TiO2 doped ZnO composite nanomaterial is used as a sensitive material, the sensitivity of the acetylene sensor to 200ppm is 9.9 at the working temperature of 280 ℃, and the response recovery time is faster. Furthermore, 16 pages 19635-19643 published in journal CERAMICS INTERNATIONAL, journal volume 45, were prepared by hydrothermal method. It utilizes the p-n heterojunction and the high catalytic activity of NiO, and the response of NiO-ZnO (5%) to 50ppm C2H2 reaches 15.23 at 200 ℃. Most of the research on the modification of acetylene sensors is based on the conventional materials such as SnO2, znO, etc. for oxide or noble metal doping, while little research on the detection of low concentration of acetylene is performed.
Perovskite-type oxides have been widely studied in the fields of anode materials, cathode materials, and the like of solid oxide fuel cells. Perovskite oxide LnFeO3 (ln=lanthanide series compound) has been regarded as a promising sensor material for detecting reducing/oxidizing gases due to its excellent properties such as catalytic activity, electrical conductivity, and oxygen absorption.
It is well known that good gas-sensitive properties are closely related to the large number of oxygen adsorption sites on the surface of the material. The perovskite oxide prepared by the traditional sol-gel method is generally low in specific surface area, and low-concentration detection of hazardous gas cannot be realized. Therefore, the sensor which is provided with the synthetic material and has simple process and can detect the harmful gas with low concentration has very important scientific research significance and application value.
Disclosure of Invention
The invention provides a preparation method of perovskite type samarium ferrite material, which introduces a freeze drying method into the preparation of the samarium ferrite material, and reduces the aggregation phenomenon of the material, so that the surface area ratio of the obtained perovskite type samarium ferrite material is high, the oxygen adsorption quantity and the reaction rate are improved, the working temperature is effectively reduced, the sensitivity is improved, the response-recovery time is shortened, and the application of acetylene low-concentration detection can be realized.
The invention solves the technical problems and adopts the following technical scheme:
a preparation method of perovskite type samarium ferrite material comprises the following steps:
(1) Dissolving soluble ferric salt, soluble samarium salt and citric acid monohydrate in an aqueous solution to prepare a precursor solution;
(2) Dropwise adding ammonia water into the precursor solution in the step (1) until the precursor solution is neutral, and magnetically stirring the precursor solution at room temperature until the precursor solution is uniform;
(3) Freezing the precursor solution uniformly stirred in the step (2);
(4) Drying the mixture in the step (3) in a freeze dryer;
(5) Transferring the dried material into a square boat, placing the square boat into a tube furnace, and air-drying at 1-10deg.C for min -1 And then the temperature is kept for 2 to 5 hours after the temperature is raised to 500 to 950 ℃.
Further, the soluble iron salt is: iron acetate (C) 4 H 6 O 4 Fe), iron acetylacetonate (C) 15 H 21 FeO 6 ) Iron nitrate and its hydrates, iron chloride and its hydrates, iron sulfate and its hydrates.
Further, the soluble samarium salt is: samarium acetate (C) 4 H 6 O 4 Sm), samarium acetylacetonate (C) 15 H 21 SmO 6 ) Samarium nitrate and its hydrate, samarium chloride and its hydrate, samarium sulfate and its hydrate.
Further, the mole ratio of the soluble iron salt, the soluble samarium salt and the citric acid monohydrate is (0.9-1.3):
(0.85～1.3)：(1.9～2.4)。
further, the aqueous solution is: deionized water, distilled water, hydrochloric acid solution or nitric acid solution.
Further, in the step (2), the magnetic stirring time is 5-10h.
The perovskite type samarium ferrite material is applied, and is characterized in that: the perovskite type samarium ferrite material is used as an acetylene sensitive material of a semiconductor type acetylene gas sensor.
The invention has the technical characteristics and effects as follows:
(1) The method for preparing the perovskite type samarium ferrite material is simple, only soluble ferric salt, soluble samarium salt, citric acid monohydrate and a proper amount of ammonia water are dissolved in deionized water to prepare a precursor solution, simple freezing and drying treatment are carried out, and the dried material is calcined in a tube furnace for one step to obtain the samarium ferrite material; the synthetic material disclosed by the invention is simple in process, better keeps the morphology, and forms the detection material with higher surface area ratio.
(2) The invention is applied to the detection of low-concentration acetylene gas, and has extremely low detection lower limit, lower working temperature and higher sensitivity.
Drawings
FIG. 1 is an SEM image of a perovskite type samarium ferrite material prepared by a freeze-drying method of example 1.
FIG. 2 is an XRD pattern of a perovskite type samarium ferrite material prepared by the freeze-drying method of example 1.
FIG. 3 is an SEM image of a perovskite type samarium ferrite material prepared by a sol-gel method according to comparative example 1.
FIG. 4 (d) is the nitrogen adsorption/desorption curve of example 1, and 4 (f) is the nitrogen adsorption/desorption curve of comparative example 1.
FIG. 5 is a response curve of example 1 at low concentrations of 300ppb, 400ppb, and 500 ppb.
Fig. 6 is a graph showing the response of comparative example 1 and comparative example 1 at the same time, temperature, humidity, and concentration.
Detailed Description
The present invention is further illustrated by, but not limited to, the following examples.
Example 1
(1) 1mmol Fe (NO) 3 ) 3 ·9H 2 O，1mmol SmN 3 O 9 ·6H 2 O,2mmol citric acid monohydrate is dissolved in deionized water to prepare a precursor solution;
(2) Slowly dripping ammonia water into the precursor solution in the step (1) until the solution is neutral, and magnetically stirring for 6 hours;
(3) Freezing the fully stirred precursor solution in the step (2);
(4) Drying the mixture in the step (3) in a freeze dryer;
(5) Transferring the dried material into a square boat, placing the square boat into a tube furnace, and preserving the temperature at 700 ℃ for 2 hours in an air atmosphere, wherein the temperature rising rate is 2 ℃ for min -1 The method comprises the steps of carrying out a first treatment on the surface of the And collecting a target product to obtain the perovskite type samarium ferrite material.
SEM and XRD tests are carried out on the obtained material, and the particle size of the perovskite type samarium ferrite material obtained in the example 1 is 17-50 nm as shown in an SEM image (a) image and a b) image of the example 1 under different magnifications, wherein a is 6K times and b) is 80K times; the particles are uniform in size, and gaps and holes exist among the particles. As is apparent from the XRD pattern of FIG. 2, the annealed material at 700 ℃ is perovskite samarium ferrite material. As can be seen from BET plot d) of FIG. 4, the specific surface area is 7.706m 2 /g。
Example 2
(1) 1mmol FeCl 3 ·6H 2 O，1mmol SmN 3 O 9 ·6H 2 O,2mmol citric acid monohydrate is dissolved in deionized water to prepare a precursor solution;
(2) Slowly dripping ammonia water into the precursor solution in the step (1) until the solution is neutral, and magnetically stirring for 6 hours;
(3) Placing the precursor solution fully stirred in the step (2) into a refrigerator for freezing;
(4) Drying the mixture in the step (3) in a freeze dryer;
(5) Transferring the dried material into a square boat, placing the square boat into a tube furnace, and preserving heat at 550 ℃ for 5h under air atmosphere at a heating rate of 10 ℃ for min -1 The method comprises the steps of carrying out a first treatment on the surface of the And collecting a target product to obtain the perovskite type samarium ferrite nano material.
Example 3
(1) 1mmol Fe (NO) 3 ) 3 ·9H 2 O，1mmol C 6 H 9 O 6 Preparing a precursor solution from Sm,2mmol citric acid monohydrate and deionized water;
(2) Slowly dripping ammonia water into the precursor solution in the step (1) until the solution is neutral, and magnetically stirring for 6 hours;
(3) Placing the precursor solution fully stirred in the step (2) into a refrigerator for freezing;
(4) Drying the mixture in the step (3) in a freeze dryer;
(5) Transferring the dried material into a square boat, placing the square boat into a tube furnace, and preserving the temperature at 700 ℃ for 2 hours in an air atmosphere, wherein the temperature rising rate is 2 ℃ for min -1 The method comprises the steps of carrying out a first treatment on the surface of the And collecting a target product to obtain the perovskite type samarium ferrite material.
Example 4
(1) 1mmol FeCl 3 ·6H 2 O，1mmol SmCl 3 ·6H 2 O,2mmol citric acid monohydrate is dissolved in deionized water to prepare a precursor solution;
(2) Slowly dripping ammonia water into the precursor solution in the step (1) until the solution is neutral, and magnetically stirring for 6 hours;
(3) Placing the precursor solution fully stirred in the step (2) into a refrigerator for freezing;
(4) Drying the mixture in the step (3) in a freeze dryer;
(5) Transferring the dried material into a square boat, placing the square boat into a tube furnace, and preserving the temperature at 700 ℃ for 2 hours in an air atmosphere, wherein the temperature rising rate is 2 ℃ for min -1 The method comprises the steps of carrying out a first treatment on the surface of the And collecting a target product to obtain the perovskite type samarium ferrite material.
Comparative example 1
(1) 1mmol Fe (NO) 3 ) 3 ·9H 2 O，1mmol SmN 3 O 9 ·6H 2 O,2mmol citric acid monohydrate and 2mmol glycol are dissolved in deionized water to prepare a precursor solution;
(2) Stirring the precursor solution in the step (1) in a water bath kettle at 80 ℃ for 4 hours to form colloid;
(3) Heating the fully stirred precursor in the step (2) for 10 hours at 150 ℃;
(4) Grinding the sample in the step (3) in a grinding pot;
(5) Transferring the dried material into a square boat, placing the square boat into a tube furnace, and preserving the temperature at 700 ℃ for 2 hours in an air atmosphere, wherein the temperature rising rate is 2 ℃ for min -1 The method comprises the steps of carrying out a first treatment on the surface of the And collecting a target product to obtain the perovskite type samarium ferrite material.
As can be seen from the SEM image of FIG. 3, the particle size of comparative example 1 is 2.5-87.5. Mu.m; the size of comparative example 1 is much larger than the particle size of the material of the examples (17 to 50nm in the particle size of example 1), and the specific surface area is 1.217m as can be seen from FIG. 4 e) 2 And/g, the surface area ratio is clearly smaller than in example 1.
Gas sensitivity performance test for perovskite type samarium ferrite materials of example 1 and comparative example 1:
in order to test that the perovskite type samarium ferrite material provided by the invention has gas-sensitive property and can be used for low-concentration acetylene detection, the perovskite type samarium ferrite material obtained in the example 1 and the comparative example 1 is adopted to prepare a semiconductor type gas sensor, and the method comprises the following steps:
(1) Alternately ultrasonically cleaning the ceramic tube and the sensor base by using acetone and deionized water to remove surface impurities;
(2) Putting 0.3 g-0.5 g of samarium ferrite nano material into an agate mortar, grinding for 0.5-1 hour, adding terpineol, and fully grinding to prepare pasty sensitive material;
(3) Uniformly coating a sensitive material on the outer surface of a ceramic tube core, completely covering a gold electrode, naturally drying in the shade after the coating is finished or putting the ceramic tube core into a drying oven for drying, placing the ceramic tube core into a muffle furnace for calcining at 350 ℃ for 0.5-1h after the ceramic tube core is dried, and removing organic matters in the material;
(4) A nickel-chromium heating wire passes through a ceramic tube and is welded with a platinum lead wire on a sensor base respectively, an aging table with the voltage of 3.7V is placed on the sensor base for aging for 0 to 30 days after an outer cover is installed, so that a gas sensor taking perovskite type samarium ferrite nano material as a sensitive material is obtained; aging enables the sensor to have better repeatability and stability in the experimental process;
example 1 the test results are shown in figure 5. It can be seen from fig. 5 that the lowest detection limit of the sensor obtained by welding is 300ppb, and the response value thereof is 1.81.
The results of the tests of example 1 and comparative example 1 are shown in fig. 6, and it can be seen from fig. 6 that the comparative example has no significant change in response at low concentrations, except that the temperature change at aeration causes a change in resistance.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

Claims (7)

1. A preparation method of perovskite type samarium ferrite material comprises the following steps:
(1) Dissolving soluble ferric salt, soluble samarium salt and citric acid monohydrate in an aqueous solution to prepare a precursor solution;
(2) Dropwise adding ammonia water into the precursor solution in the step (1) until the precursor solution is neutral, and magnetically stirring the precursor solution at room temperature until the precursor solution is uniform;
(3) Freezing the precursor solution uniformly stirred in the step (2);
(4) Putting the step (3) into a freeze dryer for drying;
(5) Transferring the dried material in the step (4) into a ark, and transferringPlacing the ark in a tube furnace at 1-10deg.C for min under air atmosphere -1 And then the temperature is kept for 2 to 5 hours after the temperature is raised to 500 to 950 ℃.
2. The method for preparing the perovskite type samarium ferrite material according to claim 1, characterized in that the soluble ferric salt is: iron acetate, iron acetylacetonate, iron nitrate and hydrates thereof, iron chloride and hydrates thereof, and iron sulfate and hydrates thereof.
3. The method for preparing the perovskite type samarium ferrite material according to claim 1, characterized in that the soluble samarium salt is: samarium acetate, samarium acetylacetonate, samarium nitrate, hydrates thereof, samarium chloride, hydrates thereof, and samarium sulfate, hydrates thereof.
4. The method for preparing the perovskite type samarium ferrite material according to claim 1, wherein the mole ratio of the soluble ferric salt, the soluble samarium salt and the citric acid monohydrate is (0.9-1.3): (0.85-1.3): (1.9-2.4).
5. The method for preparing the perovskite type samarium ferrite material according to claim 1, characterized in that the aqueous solution is: deionized water, distilled water, hydrochloric acid solution or nitric acid solution.
6. The method for preparing a perovskite type samarium ferrite material according to claim 1, wherein in the step (2), the magnetic stirring time is 5-10 hours.
7. Use of the perovskite type samarium ferrite material according to any one of claims 1 to 6, characterized in that: the perovskite type samarium ferrite material is used as an acetylene sensitive material of a semiconductor type acetylene gas sensor.
CN202310834610.0A 2023-07-07 2023-07-07 Preparation method and application of perovskite type samarium ferrite Pending CN116789181A (en)

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