CN110563026A - preparation method of rGO composite indium oxide sheet with high gas-sensitive performance - Google Patents

preparation method of rGO composite indium oxide sheet with high gas-sensitive performance Download PDF

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CN110563026A
CN110563026A CN201910827324.5A CN201910827324A CN110563026A CN 110563026 A CN110563026 A CN 110563026A CN 201910827324 A CN201910827324 A CN 201910827324A CN 110563026 A CN110563026 A CN 110563026A
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宋鹏
田哲宾
王�琦
张敬群
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University of Jinan
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G15/00—Compounds of gallium, indium or thallium
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
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    • C01—INORGANIC CHEMISTRY
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    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM

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Abstract

the invention provides a preparation method of a rGO composite indium oxide sheet with high gas-sensitive performance. The preparation method specifically comprises the following steps: N-N dimethylformamide, terephthalic acid, graphene oxide sol, APTES and indium nitrate hydrate are used as raw materials, and the rGO composite indium oxide sheet is obtained through oil bath reaction, hydrothermal reaction and calcination treatment. The sheet structure has a larger surface area and can effectively adsorb more oxygen and target gas. The experiment does not use expensive surfactant, has lower cost and good gas-sensitive performance to formaldehyde gas, and thus has long-term application prospect in the aspect of formaldehyde gas detection.

Description

preparation method of rGO composite indium oxide sheet with high gas-sensitive performance
Technical Field
the invention relates to a preparation method of rGO composite indium oxide sheet with high gas-sensitive performance, belonging to the technical field of advanced nano functional material preparation processes.
background
in daily life, people are seriously damaged by industrial production waste gas, automobile exhaust, PM2.5 and other gases when going out, and are influenced by toxic gases such as formaldehyde, benzene and the like when going home. Therefore, it is very important to research and develop a high-performance gas sensor, whether the gas sensor is needed for detecting environmental pollution gas or for ensuring quality of life and industrial safety. With the increasing attention of people to the environmental protection problem and the strict monitoring of the emission of toxic and harmful gases, various gas inspection and early warning devices with different functions are developed, and further, the industrialization and the commercialization are achieved. The semiconductor gas sensor has the characteristics of high detection sensitivity, quick response recovery, simple circuit, simplicity in operation, small element size, low price and the like, and is widely applied to various gas detection fields.
In2O3The high-sensitivity GaN-based light-emitting diode has the advantages of large forbidden band width, energy band gap close to GaN, low resistivity, high sensitivity, low working temperature, low light absorption rate, high infrared reflectivity and the like in a visible light region. Influence In2O3the main factor of the properties of nanomaterials is their structural morphology, so currently, many researchers are working on controlling In2O3The development of crystal morphology is studied in order to improve its properties in all respects. In recent years, the application of indium oxide nano materials in the field of photoelectric thin films is successively reported in developed countries in Europe and America. At present, researchers prepare one-dimensional, two-dimensional and three-dimensional In by using a nano material synthesis method of a gas phase method, a solid phase method and a liquid phase method2O3and (3) nano materials. The specific shapes of the nano-tube/nano-rod composite material comprise a nano-tube, a nano-wire, a nano-rod, a cube, an octahedron and the like, and the nano-tube/nano-rod composite material is widely applied to the fields of optics, magnetics, electronics, medical treatment and the like. In order to improve the recognition function, in addition to selecting a good matrix material and modifying the matrix material through doping, compounding and surface modification, designing and preparing porous and sheet-like structure materials with large specific surface area and high active site density are also interesting strategies. The graphene and indium oxide composite material prepared by the method has good permeability, can promote gas diffusion, and is beneficial to improvement of the utilization rate of a sensitive body. In addition, in order to improve the sensitivity of the semiconductor gas sensor, a method of increasing the surface area of the material is often employed,
graphene is a research hotspot in various fields in recent years due to the special specific surface area, and the surface area and the surface of a material are increased by compounding with graphenethe activity is greatly increased, so that the adsorption, desorption and redox reaction of the material on gas can be carried out at lower temperature, the working temperature is reduced, the response time is shortened, and the concentration range of gas detection is improved. For In China2O3the research on the nano material, particularly the structure and the appearance thereof, is in the beginning stage, but the preparation method has the defects of complex operation, high production cost and the like, so that the research result is difficult to be put into the actual industrial production in a large range. In addition, due to the restrictions of experimental facilities and production techniques, people are now dealing with In2O3the research of the nano material, especially the research of the gas-sensitive property is not very deep. Researchers are urgently required to study In a more systematic and comprehensive way2O3The structural morphology and the functional property of the nano material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of an rGO composite indium oxide sheet with high gas-sensitive performance. Has the characteristics of low cost, simple production process, high yield, no environmental pollution and easy industrialized large-scale production. The sensitivity of the obtained graphene and indium oxide composite material is greatly improved, and the graphene and indium oxide composite material can be used in the fields of gas sensors and the like. The technical scheme for realizing the purpose of the invention is as follows: a preparation method of rGO composite indium oxide sheet with high gas-sensitive performance is characterized by comprising the following steps: N-N dimethylformamide, terephthalic acid, graphene oxide sol, APTES and indium nitrate hydrate are used as raw materials, and the rGO composite indium oxide sheet is obtained through oil bath reaction, hydrothermal reaction and calcination treatment. The sheet structure has a larger surface area and can effectively adsorb more oxygen and target gas. The method has simple production process, does not use expensive surfactant, has lower cost, and the obtained indium oxide can be used as a gas-sensitive material and has long-term application prospect in the aspect of formaldehyde gas detection. The specific synthesis steps are as follows:
1. A preparation method of rGO composite indium oxide sheet with high gas-sensitive performance comprises the following specific synthesis steps:
(1) First, 160 mL of DMF was taken in 1 clean and dry 250 mL beaker with a measuring cylinder and placed in a clean magnetic rotor; accurately weighing 0.05-0.08 g of terephthalic acid and 0.05-0.08 g of indium nitrate hydrate by using an electronic analytical balance, pouring into a beaker filled with DMF, and putting the beaker on a magnetic stirrer for stirring;
(2) putting the beaker with the solute completely dissolved into an oil bath pan for oil bath heating, setting the conditions at 120 ℃, keeping the temperature for 30-50 min after the temperature is raised to 120 ℃, taking out the beaker immediately after the heating is finished, standing, cooling, and washing the precipitate;
(washing method comprises diluting the precipitate with deionized water or anhydrous ethanol in a beaker, subjecting the mixture to ultrasonic oscillation for 5 min until it is uniformly dispersed, pouring into a centrifuge tube, and centrifuging at a proper rotation speed for 7 min;
(3) uniformly dispersing the dried sample in a dry crucible, and then putting the crucible into a box ~ type muffle furnace for calcination, wherein the temperature is firstly controlled to be raised to 400 ~ 500 ℃ for 1 minute and one degree, and is kept for 3 hours, the temperature is lowered to 2 ~ 3 ℃/min, and the calcination is finished, so that a light yellow powdery sample can be obtained;
(4) Taking 1 cleaned and dried 50 mL beaker, measuring 25 mL absolute ethyl alcohol by using a measuring cylinder, pouring into the beaker, and accurately weighing 0.025-0.05 g of In by using an electronic analytical balance2O3Pouring the mixture into a beaker filled with absolute ethyl alcohol, putting a clean magnetic rotor, and putting the magnetic rotor on a magnetic stirrer to stir until the mixture is dissolved;
(5) And (3) carrying out ultrasonic treatment on the dissolved solution for 30min, then adding 0.25-0.5 mL of ATPES, and maintaining the temperature at 60 ℃. Stirring for 4 h, selecting a second 50 mL beaker, dispersing 3-60 mg GO into 40-80 mL deionized water in the beaker, and carrying out ultrasonic treatment for 30 min;
(6) adding the obtained powder into a second beaker, carrying out ultrasonic treatment, then putting the mixture into a reaction kettle, carrying out heat preservation at 120 ℃ for 14 hours, collecting the obtained black precipitate after the end of the heat preservation, washing for a plurality of times, and finally paying attention to treatment by deionized water;
(7) the obtained black precipitate was put into a refrigerator, frozen, and further dried using a freeze dryer.
Drawings
Fig. 1 is an SEM image of rGO compounded indium oxide sheets.
figure 2 is an EDS map of rGO compounded indium oxide sheets.
Fig. 3 is a raman plot of rGO compounded indium oxide sheets.
FIG. 4 is a graph of gas sensing performance of rGO composite indium oxide sheets as a function of valence full packet concentration (1-20 ppm).
Fig. 5 is a graph of the gas sensitivity to different gas selectivities of rGO-composited indium oxide sheets.
Detailed Description
the following is a detailed description of the embodiments of the present invention, which is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
example 1:
(1) First, 160 mL of DMF was taken in 1 clean and dry 250 mL beaker with a measuring cylinder and placed in a clean magnetic rotor; accurately weighing 0.07 g of terephthalic acid and 0.073 g of indium nitrate hydrate by using an electronic analytical balance, pouring into a beaker filled with DMF, and putting on a magnetic stirrer for stirring;
(2) putting the beaker with the solute completely dissolved into an oil bath pan for oil bath heating, setting the conditions at 120 ℃, keeping the temperature for 30min after the temperature is raised to 120 ℃, immediately taking out the beaker after heating, standing, cooling, and washing the precipitate;
(washing method comprises diluting the precipitate with deionized water or anhydrous ethanol in a beaker, subjecting the mixture to ultrasonic oscillation for 5 min until it is uniformly dispersed, pouring into a centrifuge tube, and centrifuging at a proper rotation speed for 7 min;
(3) And uniformly dispersing the dried sample in a dry crucible, and then putting the crucible into a box-type muffle furnace for calcining. Firstly, controlling the temperature rising rate to be 1 minute and one degree till 400 ℃, preserving the temperature for 3 hours, and finishing calcination to obtain a light yellow powdery sample, wherein the temperature lowering system is a rate of 3 ℃ per minute;
(4) 1 piece is taken and cleanedA dry 50 mL beaker, 25 mL absolute ethanol measured In a measuring cylinder and poured into the beaker, 0.025 g of In accurately weighed by an electronic analytical balance2O3Pouring the mixture into a beaker filled with absolute ethyl alcohol, putting a clean magnetic rotor, and putting the magnetic rotor on a magnetic stirrer to stir until the mixture is dissolved;
(5) The dissolved solution is subjected to ultrasonic treatment for 30min, and then 0.25 mL ATPES is added, and the temperature is maintained at 60 ℃. Stirring for 4 h, selecting a second 50 mL beaker, dispersing 10 mg GO into 40 mL deionized water in the beaker, and carrying out ultrasonic treatment for 30 min;
(6) Adding the obtained powder into a second beaker, carrying out ultrasonic treatment, then putting the mixture into a reaction kettle, carrying out heat preservation at 120 ℃ for 14 hours, collecting the obtained black precipitate after the end of the heat preservation, washing for a plurality of times, and finally paying attention to treatment by deionized water;
(7) The obtained black precipitate was put into a refrigerator, frozen, and further dried using a freeze dryer.
Example 2:
(1) first, 160 mL of DMF was taken in 1 clean and dry 250 mL beaker with a measuring cylinder and placed in a clean magnetic rotor; accurately weighing 0.07 g of terephthalic acid and 0.08 g of indium nitrate hydrate by using an electronic analytical balance, pouring into a beaker filled with DMF, and putting the beaker on a magnetic stirrer for stirring;
(2) Putting the beaker with the solute completely dissolved into an oil bath pan for oil bath heating, setting the conditions at 120 ℃, keeping the temperature for 40 min after the temperature is raised to 120 ℃, immediately taking out the beaker after the heating is finished, standing, cooling, and washing the precipitate;
(washing method comprises diluting the precipitate with deionized water or anhydrous ethanol in a beaker, subjecting the mixture to ultrasonic oscillation for 5 min until it is uniformly dispersed, pouring into a centrifuge tube, and centrifuging at a proper rotation speed for 7 min;
(3) And uniformly dispersing the dried sample in a dry crucible, and then putting the crucible into a box-type muffle furnace for calcining. Firstly, controlling the temperature rise rate to be 1 minute and one degree till 500 ℃, preserving the temperature for 3 hours, and finishing calcination to obtain a light yellow powdery sample, wherein the temperature drop system is the rate of 3 degrees/min;
(4) Taking 1 cleaned and dried 50 mL beaker, measuring 25 mL absolute ethyl alcohol by using a measuring cylinder, pouring into the beaker, and accurately weighing 0.05 g In by using an electronic analytical balance2O3Pouring the mixture into a beaker filled with absolute ethyl alcohol, putting a clean magnetic rotor, and putting the magnetic rotor on a magnetic stirrer to stir until the mixture is dissolved;
(5) the dissolved solution is subjected to ultrasonic treatment for 30min, and then 0.4 mL of ATPES is added, and the temperature is maintained at 60 ℃. Stirring for 4 h, selecting a second 50 mL beaker, dispersing 30 mg GO into 80 mL deionized water in the beaker, and carrying out ultrasonic treatment for 30 min;
(6) adding the obtained powder into a second beaker, carrying out ultrasonic treatment, then putting the mixture into a reaction kettle, carrying out heat preservation at 120 ℃ for 14 hours, collecting the obtained black precipitate after the end of the heat preservation, washing for a plurality of times, and finally paying attention to treatment by deionized water;
(7) the obtained black precipitate was put into a refrigerator, frozen, and further dried using a freeze dryer.
Example 3:
(1) first, 160 mL of DMF was taken in 1 clean and dry 250 mL beaker with a measuring cylinder and placed in a clean magnetic rotor; accurately weighing 0.08 g of terephthalic acid and 0.06 g of indium nitrate hydrate by using an electronic analytical balance, pouring into a beaker filled with DMF, and putting the beaker on a magnetic stirrer for stirring;
(2) Putting the beaker with the solute completely dissolved into an oil bath pan for oil bath heating, setting the conditions at 120 ℃, keeping the temperature for 50 min after the temperature is raised to 120 ℃, immediately taking out the beaker after heating, standing, cooling, and washing the precipitate;
(washing method comprises diluting the precipitate with deionized water or anhydrous ethanol in a beaker, subjecting the mixture to ultrasonic oscillation for 5 min until it is uniformly dispersed, pouring into a centrifuge tube, and centrifuging at a proper rotation speed for 7 min;
(3) and uniformly dispersing the dried sample in a dry crucible, and then putting the crucible into a box-type muffle furnace for calcining. Firstly, controlling the temperature rise rate to be 1 minute and one degree till 500 ℃, preserving the temperature for 3 hours, and finishing calcination to obtain a light yellow powdery sample, wherein the temperature drop system is the rate of 3 degrees/min;
(4) Taking 1 cleaned and dried 50 mL beaker, measuring 25 mL absolute ethyl alcohol by using a measuring cylinder, pouring into the beaker, and accurately weighing 0.05 g In by using an electronic analytical balance2O3pouring the mixture into a beaker filled with absolute ethyl alcohol, putting a clean magnetic rotor, and putting the magnetic rotor on a magnetic stirrer to stir until the mixture is dissolved;
(5) and (3) carrying out ultrasonic treatment on the dissolved solution for 30min, then adding 0.25-0.5 mL of ATPES, and maintaining the temperature at 60 ℃. Stirring for 4 h, selecting a second 50 mL beaker, dispersing 60 mg GO into 80 mL deionized water in the beaker, and carrying out ultrasonic treatment for 30 min;
(6) adding the obtained powder into a second beaker, carrying out ultrasonic treatment, then putting the mixture into a reaction kettle, carrying out heat preservation at 120 ℃ for 14 hours, collecting the obtained black precipitate after the end of the heat preservation, washing for a plurality of times, and finally paying attention to treatment by deionized water;
(7) the obtained black precipitate was put into a refrigerator, frozen, and further dried using a freeze dryer.
Example 4:
(1) first, 160 mL of DMF was taken in 1 clean and dry 250 mL beaker with a measuring cylinder and placed in a clean magnetic rotor; accurately weighing 0.06 g of terephthalic acid and 0.048 g of indium nitrate hydrate by using an electronic analytical balance, pouring into a beaker filled with DMF, and putting the beaker on a magnetic stirrer for stirring;
(2) putting the beaker with the solute completely dissolved into an oil bath pan for oil bath heating, setting the conditions at 120 ℃, keeping the temperature for 40 min after the temperature is raised to 120 ℃, immediately taking out the beaker after the heating is finished, standing, cooling, and washing the precipitate;
(washing method comprises diluting the precipitate with deionized water or anhydrous ethanol in a beaker, subjecting the mixture to ultrasonic oscillation for 5 min until it is uniformly dispersed, pouring into a centrifuge tube, and centrifuging at a proper rotation speed for 7 min;
(3) and uniformly dispersing the dried sample in a dry crucible, and then putting the crucible into a box-type muffle furnace for calcining. Firstly, controlling the heating rate to be 1 minute and one degree till 400-500 ℃, preserving the heat for 3 hours, and controlling the cooling system to be 2 ℃ per minute, and obtaining a light yellow powdery sample after the calcination is finished;
(4) taking 1 cleaned and dried 50 mL beaker, measuring 25 mL absolute ethyl alcohol by using a measuring cylinder, pouring into the beaker, and accurately weighing 0.035 g In by using an electronic analytical balance2O3Pouring the mixture into a beaker filled with absolute ethyl alcohol, putting a clean magnetic rotor, and putting the magnetic rotor on a magnetic stirrer to stir until the mixture is dissolved;
(5) the dissolved solution is subjected to ultrasonic treatment for 30min, and then 0.35 mL of ATPES is added, and the temperature is maintained at 60 ℃. Stirring for 4 h, selecting a second 50 mL beaker, dispersing 40 mg GO into 40-80 mL deionized water in the beaker, and carrying out ultrasonic treatment for 30 min;
(6) adding the obtained powder into a second beaker, carrying out ultrasonic treatment, then putting the mixture into a reaction kettle, carrying out heat preservation at 120 ℃ for 14 hours, collecting the obtained black precipitate after the end of the heat preservation, washing for a plurality of times, and finally paying attention to treatment by deionized water;
(7) the obtained black precipitate was put into a refrigerator, frozen, and further dried using a freeze dryer.

Claims (1)

1. A preparation method of rGO composite indium oxide sheet with high gas-sensitive performance comprises the following specific synthesis steps:
(1) First, 160 mL of DMF was taken in 1 clean and dry 250 mL beaker with a measuring cylinder and placed in a clean magnetic rotor; accurately weighing 0.05-0.08 g of terephthalic acid and 0.05-0.08 g of indium nitrate hydrate by using an electronic analytical balance, pouring into a beaker filled with DMF, and putting the beaker on a magnetic stirrer for stirring;
(2) putting the beaker with the solute completely dissolved into an oil bath pan for oil bath heating, setting the conditions at 120 ℃, keeping the temperature for 30-50 min after the temperature is raised to 120 ℃, taking out the beaker immediately after the heating is finished, standing, cooling, and washing the precipitate;
(washing method comprises diluting the precipitate with deionized water or anhydrous ethanol in a beaker, subjecting the mixture to ultrasonic oscillation for 5 min until it is uniformly dispersed, pouring into a centrifuge tube, and centrifuging at a proper rotation speed for 7 min;
(3) uniformly dispersing the dried sample in a dry crucible, and then putting the crucible into a box ~ type muffle furnace for calcination, wherein the temperature rise rate is controlled to be 1 minute and one degree till 400 ~ 500 ℃, the temperature is kept for 3 hours, the temperature reduction system is controlled to be 2 ~ 3 ℃ per minute, and the calcination is finished to obtain a light yellow powdery sample;
(4) taking 1 cleaned and dried 50 mL beaker, measuring 25 mL absolute ethyl alcohol by using a measuring cylinder, pouring into the beaker, and accurately weighing 0.025-0.05 g of In by using an electronic analytical balance2O3pouring the mixture into a beaker filled with absolute ethyl alcohol, putting a clean magnetic rotor, and putting the magnetic rotor on a magnetic stirrer to stir until the mixture is dissolved;
(5) Performing ultrasonic treatment on the dissolved solution for 30min, adding 0.25-0.5 mL ATPES, stirring for 4 h under the condition of maintaining 60 ℃, selecting a second 50 mL beaker, dispersing 3-60 mg GO into 40-80 mL deionized water in the beaker, and performing ultrasonic treatment for 30 min;
(6) adding the obtained powder into a second beaker, carrying out ultrasonic treatment, then putting the mixture into a reaction kettle, carrying out heat preservation at 120 ℃ for 14 hours, collecting the obtained black precipitate after the end of the heat preservation, washing for a plurality of times, and finally paying attention to treatment by deionized water;
(7) the obtained black precipitate was put into a refrigerator, frozen, and further dried using a freeze dryer.
CN201910827324.5A 2019-09-03 2019-09-03 preparation method of rGO composite indium oxide sheet with high gas-sensitive performance Pending CN110563026A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105668612A (en) * 2016-03-15 2016-06-15 济南大学 Preparation method of hexagonal-tube-shaped indium oxide with complex as precursor
CN107381622A (en) * 2017-06-28 2017-11-24 济南大学 A kind of rGO In2O3The preparation method of nanoparticle composite
CN108663417A (en) * 2018-06-22 2018-10-16 山东大学 One kind being directed to low concentration of NO2The novel I n of gas2O3/Sb2O3Composite hollow nanotube gas sensitive
CN109019672A (en) * 2018-08-01 2018-12-18 济南大学 A kind of porous oxidation indium micro-pipe preparation method with unique morphology

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105668612A (en) * 2016-03-15 2016-06-15 济南大学 Preparation method of hexagonal-tube-shaped indium oxide with complex as precursor
CN107381622A (en) * 2017-06-28 2017-11-24 济南大学 A kind of rGO In2O3The preparation method of nanoparticle composite
CN108663417A (en) * 2018-06-22 2018-10-16 山东大学 One kind being directed to low concentration of NO2The novel I n of gas2O3/Sb2O3Composite hollow nanotube gas sensitive
CN109019672A (en) * 2018-08-01 2018-12-18 济南大学 A kind of porous oxidation indium micro-pipe preparation method with unique morphology

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