CN109019673A - A kind of SnO2-In2O3The preparation method of nanocomposite - Google Patents
A kind of SnO2-In2O3The preparation method of nanocomposite Download PDFInfo
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- CN109019673A CN109019673A CN201810862948.6A CN201810862948A CN109019673A CN 109019673 A CN109019673 A CN 109019673A CN 201810862948 A CN201810862948 A CN 201810862948A CN 109019673 A CN109019673 A CN 109019673A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01G15/00—Compounds of gallium, indium or thallium
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
Abstract
The present invention provides a kind of SnO2‑In2O3The preparation method of nanocomposite.The preparation method specifically includes: with four trichloride hydrate indiums, urea, trisodium citrate hydrate obtains cube indium oxide through hydro-thermal reaction for raw material after calcination processing；And then with stannic chloride, sodium hydroxide is raw material, in indium oxide cube face composite particles shape tin oxide, finally obtains SnO2‑In2O3Nanocomposite.This method simple production process, the n-n hetero-junctions that there is gained gas sensitive indium oxide and tin oxide to constitute, it shows higher sensitivity and quickly response, recovery to triethylamine, can be used for Triethylamine gas sensor field, to obtain highly sensitive novel gas sensitive.
Description
Technical field
The present invention relates to a kind of SnO2-In2O3The preparation method of nanocomposite belongs to advanced nano-functional material system
Standby technology field.
Background technique
With the aggravation of environmental pollution, the qualitative and quantitative detection of toxic and harmful gas is become more and more important.It is existing
Nowadays, to the analysis of these gases generally use be all it is some test time-consuming and expensive test equipment, such as spectrum
Analysis, chromatography.Due to metal oxide semiconductor gas sensor have highly sensitive, highly selective, quick response and
The advantages that cheap, therefore future can detect the ideal of toxic and harmful gas, and have the substitution of application prospect
Product.In these metal oxide semiconductors, In2O3It is a kind of novel gas sensitive, with ZnO, Fe2O3Deng traditional air-sensitive material
Material is compared, and has many advantages, such as wider forbidden bandwidth, lesser resistivity and higher catalytic activity.Although one-component
The potentiality of the application prospect of the gas sensor of indium oxide nanostructure, but still there is poor selectivity, work in practical applications
Make the disadvantages of temperature is high.In order to improve the air-sensitive performance of indium oxide, the pattern and structure for controlling micro/nano structure functional material are
Influence the principal element of its application performance, many people have been directed to the pattern for controlling material during the preparation process and structure or
It is the enhancing for developing new construction to realize performance.
For the air-sensitive performance of material, we can make to be formed between the semiconductor material of different band gap and energy level heterogeneous
Junction structure.Heterojunction structure is constructed while controlling material morphology, is improved air-sensitive performance.However, such a
The method of important raising material air-sensitive performance obtains sufficient investigation and research not yet.Tin oxide is a kind of good n type
Semiconductor, it is widely used in catalyst, electrode, biosensor and magnetic material etc..In recent years, also someone studies
About SnO2The project of hetero-junctions, such as Zhou J Y (Zhou J Y, Bai J L, Zhao H, et al. Gas
sensing enhancing mechanism via doping-induced oxygen vacancies for gas
sensors based on indium tin oxide nanotubes[J]. Sensors & Actuators B
Chemical, 2018,265:273-284.) it is prepared for the nanocomposite of tin oxide and indium oxide, and composite material
The air-sensitive performance of triethylamine has been obtained significantly increasing.It can thus be seen that indium oxide and the oxidation of design and synthesis
The compound gas sensitive of nickel will be with important science and practice significance.However, as far as we know, indium oxide is compound with tin oxide
Gas sensitive be reported it is also seldom.Therefore during this investigation it turned out, we prepare indium oxide nanocube by hydro-thermal method
And n-n heterojunction structure is formed and to its microstructure and air-sensitive performance with granular ruthenium-oxide modification indium oxide nanosphere
System research is carried out.
Summary of the invention
It is an object of the present invention to overcome the deficiencies of the prior art and provide a kind of SnO2-In2O3The system of nanocomposite
Preparation Method.With the characteristics of at low cost, simple production process, yield is high, non-environmental-pollution.Gained indium oxide and nickel oxide are compound
The sensitivity of gas sensitive obtain a degree of raising compared to pure zirconia indium oxide, can be used for the neck such as gas sensor
Domain.Realizing the technical solution of the object of the invention is: a kind of SnO2-In2O3The preparation method of nanocomposite, it is characterised in that:
With four trichloride hydrate indiums, urea, trisodium citrate hydrate obtains cube after calcination processing through hydro-thermal reaction for raw material
Indium oxide；And then with stannic chloride, sodium hydroxide is raw material, final to obtain in indium oxide cube face composite particles shape tin oxide
To SnO2-In2O3Nanocomposite.There is indium oxide and tin oxide to constitute for this method simple production process, gained gas sensitive
N-n hetero-junctions, to triethylamine show higher sensitivity and quickly response, restore, can be used for Triethylamine gas biography
Sensor field, to obtain highly sensitive novel gas sensitive.Specific synthesis step is as follows:
(1) it weighs a certain amount of inidum chloride, trisodium citrate and urea to be dissolved in dehydrated alcohol, wherein the concentration of inidum chloride is
0.020 mol/L, the concentration of trisodium citrate are 0.120 mol/L, and the concentration of urea is 0.099 mol/L.And control chlorination
The molar ratio of indium and trisodium citrate is 1:(1 ~ 6)；
(2) gained mixed solution in step (1) is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 120 ~ 160 DEG C
At a temperature of, carry out 2 ~ 6 h of hydro-thermal reaction, then the product utilization centrifuge after hydro-thermal reaction be separated by solid-liquid separation, and spend from
Sub- water and ethyl alcohol repeatedly wash obtained solid product, and obtained solid product is placed in drying box, 60 DEG C of dryings,
It is subsequently placed in alumina crucible and is put into Muffle furnace, 3 h are heat-treated at 400 ~ 550 DEG C, obtain indium oxide powder；
(3) it disperses step (2) resulting indium oxide powder in 50 mL deionized waters, weighs a certain amount of stannic chloride hydration
Object is dissolved in above-mentioned solution 0.0018 mol/L of concentration for making stannic chloride, and stirs evenly.Na (OH), which is added, makes its concentration
For 0.024 mol/L.Gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 160 ~ 200 DEG C of temperature
Under degree, hydro-thermal reaction 4-8 h is carried out, then the product utilization centrifuge after hydro-thermal reaction is separated by solid-liquid separation, and use deionization
Water and ethyl alcohol repeatedly wash obtained solid product, and obtained solid product is placed in drying box, 60 DEG C of dryings, so
It is placed on alumina crucible and is put into Muffle furnace, 3 h are heat-treated at 400 ~ 550 DEG C, obtain indium oxide powder；
(4) step (3) obtained solid product is heat-treated at 400-600 DEG C 2 ~ 4 h, SnO can be obtained2-In2O3Nanometer is multiple
Condensation material.
Fig. 1 is SnO2-In2O3The XRD diagram of nanocomposite.
Fig. 2 is SnO2-In2O3The FESEM of nanocomposite schemes.
Fig. 3 is SnO2-In2O3The EDS of nanocomposite schemes.
Fig. 4 is SnO2-In2O3The TEM of nanocomposite schemes.
Fig. 5 is SnO under optimum operating voltage2-In2The sound of O nanocomposite gas sensor and pure zirconia indium gas sensor
Recovery curve is answered to compare.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
(1) it weighs a certain amount of inidum chloride, trisodium citrate and urea to be dissolved in dehydrated alcohol, wherein the concentration of inidum chloride is
0.020 mol/L, the concentration of trisodium citrate are 0.120 mol/L, and the concentration of urea is 0.099 mol/L.And control chlorination
The molar ratio of indium and trisodium citrate is 1:6；
(2) gained mixed solution in step (1) is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 140 DEG C of temperature
Under, carry out 4 h of hydro-thermal reaction, then the product utilization centrifuge after hydro-thermal reaction be separated by solid-liquid separation, and with deionized water with
Ethyl alcohol repeatedly washs obtained solid product, and obtained solid product is placed in drying box, then 60 DEG C of dryings are set
It is put into Muffle furnace in alumina crucible, 3 h are heat-treated at 500 DEG C, obtains indium oxide powder；
(3) it disperses step (2) resulting indium oxide powder in 50 mL deionized waters, weighs a certain amount of stannic chloride hydration
Object is dissolved in above-mentioned solution 0.0018 mol/L of concentration for making stannic chloride, and stirs evenly.Na (OH), which is added, makes its concentration
For 0.024 mol/L.Gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 180 DEG C of temperature
Under, carry out 6 h of hydro-thermal reaction, then the product utilization centrifuge after hydro-thermal reaction be separated by solid-liquid separation, and with deionized water with
Ethyl alcohol repeatedly washs obtained solid product, and obtained solid product is placed in drying box, then 60 DEG C of dryings are set
It is put into Muffle furnace in alumina crucible, 3 h are heat-treated at 500 DEG C, obtains indium oxide powder；
(4) step (3) obtained solid product is heat-treated at 600 DEG C 4 h, SnO can be obtained2-In2O3Nano combined material
Material.
Embodiment 2
(1) it weighs a certain amount of inidum chloride, trisodium citrate and urea to be dissolved in dehydrated alcohol, wherein the concentration of inidum chloride is
0.020 mol/L, the concentration of trisodium citrate are 0.100 mol/L, and the concentration of urea is 0.099 mol/L.And control chlorination
The molar ratio of indium and trisodium citrate is 1:5；
(2) gained mixed solution in step (1) is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 140 DEG C of temperature
Under, carry out 4 h of hydro-thermal reaction, then the product utilization centrifuge after hydro-thermal reaction be separated by solid-liquid separation, and with deionized water with
Ethyl alcohol repeatedly washs obtained solid product, and obtained solid product is placed in drying box, then 60 DEG C of dryings are set
It is put into Muffle furnace in alumina crucible, 3 h are heat-treated at 500 DEG C, obtains indium oxide powder；
(3) it disperses step (2) resulting indium oxide powder in 50 mL deionized waters, weighs a certain amount of stannic chloride hydration
Object is dissolved in above-mentioned solution 0.0018 mol/L of concentration for making stannic chloride, and stirs evenly.Na (OH), which is added, makes its concentration
For 0.024 mol/L.Gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 180 DEG C of temperature
Under, carry out 6 h of hydro-thermal reaction, then the product utilization centrifuge after hydro-thermal reaction be separated by solid-liquid separation, and with deionized water with
Ethyl alcohol repeatedly washs obtained solid product, and obtained solid product is placed in drying box, then 60 DEG C of dryings are set
It is put into Muffle furnace in alumina crucible, 3 h are heat-treated at 500 DEG C, obtains indium oxide powder；
(4) step (3) obtained solid product is heat-treated at 500 DEG C 2 h, SnO can be obtained2-In2O3Nano combined material
Material.
Embodiment 3
(1) it weighs a certain amount of inidum chloride, trisodium citrate and urea to be dissolved in dehydrated alcohol, wherein the concentration of inidum chloride is
0.020 mol/L, the concentration of trisodium citrate are 0.060 mol/L, and the concentration of urea is 0.099 mol/L.And control chlorination
The molar ratio of indium and trisodium citrate is 1:3；
(2) gained mixed solution in step (1) is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 140 DEG C of temperature
Under, carry out 4 h of hydro-thermal reaction, then the product utilization centrifuge after hydro-thermal reaction be separated by solid-liquid separation, and with deionized water with
Ethyl alcohol repeatedly washs obtained solid product, and obtained solid product is placed in drying box, then 60 DEG C of dryings are set
It is put into Muffle furnace in alumina crucible, 3 h are heat-treated at 500 DEG C, obtains indium oxide powder；
(3) it disperses step (2) resulting indium oxide powder in 50 mL deionized waters, weighs a certain amount of stannic chloride hydration
Object is dissolved in above-mentioned solution 0.0018 mol/L of concentration for making stannic chloride, and stirs evenly.Na (OH), which is added, makes its concentration
For 0.024 mol/L.Gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 160 DEG C of temperature
Under, carry out 6 h of hydro-thermal reaction, then the product utilization centrifuge after hydro-thermal reaction be separated by solid-liquid separation, and with deionized water with
Ethyl alcohol repeatedly washs obtained solid product, and obtained solid product is placed in drying box, then 60 DEG C of dryings are set
It is put into Muffle furnace in alumina crucible, 3 h are heat-treated at 500 DEG C, obtains indium oxide powder；
(4) step (3) obtained solid product is heat-treated at 600 DEG C 3 h, SnO can be obtained2-In2O3Nano combined material
Material.
Embodiment 4
(1) it weighs a certain amount of inidum chloride, trisodium citrate and urea to be dissolved in dehydrated alcohol, wherein the concentration of inidum chloride is
0.020 mol/L, the concentration of trisodium citrate are 0.120 mol/L, and the concentration of urea is 0.099 mol/L.And control chlorination
The molar ratio of indium and trisodium citrate is 1:6；
(2) gained mixed solution in step (1) is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 140 DEG C of temperature
Under, carry out 4 h of hydro-thermal reaction, then the product utilization centrifuge after hydro-thermal reaction be separated by solid-liquid separation, and with deionized water with
Ethyl alcohol repeatedly washs obtained solid product, and obtained solid product is placed in drying box, then 60 DEG C of dryings are set
It is put into Muffle furnace in alumina crucible, 3 h are heat-treated at 500 DEG C, obtains indium oxide powder；
(3) it disperses step (2) resulting indium oxide powder in 50 mL deionized waters, weighs a certain amount of stannic chloride hydration
Object is dissolved in above-mentioned solution 0.0018 mol/L of concentration for making stannic chloride, and stirs evenly.Na (OH), which is added, makes its concentration
For 0.024 mol/L.Gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 200 DEG C of temperature
Under, carry out 6 h of hydro-thermal reaction, then the product utilization centrifuge after hydro-thermal reaction be separated by solid-liquid separation, and with deionized water with
Ethyl alcohol repeatedly washs obtained solid product, and obtained solid product is placed in drying box, then 60 DEG C of dryings are set
It is put into Muffle furnace in alumina crucible, 3 h are heat-treated at 500 DEG C, obtains indium oxide powder.
Claims (1)
1. a kind of SnO2-In2O3The preparation method of nanocomposite, specific synthesis step are as follows:
(1) it weighs a certain amount of inidum chloride, trisodium citrate and urea to be dissolved in dehydrated alcohol, wherein the concentration of inidum chloride is
0.020 mol/L, the concentration of trisodium citrate are 0.120 mol/L, and the concentration of urea is 0.099 mol/L, and controls chlorination
The molar ratio of indium and trisodium citrate is 1:(1 ~ 6)；
(2) gained mixed solution in step (1) is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 120 ~ 160 DEG C
At a temperature of, carry out 2 ~ 6 h of hydro-thermal reaction, then the product utilization centrifuge after hydro-thermal reaction be separated by solid-liquid separation, and spend from
Sub- water and ethyl alcohol repeatedly wash obtained solid product, and obtained solid product is placed in drying box, 60 DEG C of dryings,
It is subsequently placed in alumina crucible and is put into Muffle furnace, 3 h are heat-treated at 400 ~ 550 DEG C, obtain indium oxide powder；
(3) it disperses step (2) resulting indium oxide powder in 50 mL deionized waters, weighs a certain amount of stannic chloride hydration
Object is dissolved in above-mentioned solution 0.0018 mol/L of concentration for making stannic chloride, and stirs evenly, and Na (OH), which is added, makes its concentration
For 0.024 mol/L, gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 160 ~ 200 DEG C of temperature
Under degree, 4 ~ 8 h of hydro-thermal reaction is carried out, then the product utilization centrifuge after hydro-thermal reaction is separated by solid-liquid separation, and use deionization
Water and ethyl alcohol repeatedly wash obtained solid product, and obtained solid product is placed in drying box, 60 DEG C of dryings, so
It is placed on alumina crucible and is put into Muffle furnace, 3 h are heat-treated at 400 ~ 550 DEG C, obtain indium oxide powder；
(4) step (3) obtained solid product is heat-treated at 400 ~ 600 DEG C 2 ~ 4 h, SnO can be obtained2-In2O3Nanometer is multiple
Condensation material.
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Cited By (4)
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|---|---|---|---|---|
| CN109632893A (en) * | 2019-01-11 | 2019-04-16 | 东北大学 | One kind being based on p-n heterojunction structure NiO-In2O3The gas sensor of composite Nano ball |
| CN111579600A (en) * | 2020-06-28 | 2020-08-25 | 郑州轻工业大学 | Camellia flower-shaped ZnO/SnO-SnO2Composite material and preparation method and application thereof |
| CN113562719A (en) * | 2021-06-25 | 2021-10-29 | 鞍钢化学科技有限公司 | Nano SnO2Preparation method of water-soluble asphalt carbon composite electrode negative electrode material |
| CN114229885A (en) * | 2021-12-29 | 2022-03-25 | 吉林大学 | CdO/SnO2Composite nanocube gas-sensitive material, preparation method and application thereof in hydrogen detection |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109632893A (en) * | 2019-01-11 | 2019-04-16 | 东北大学 | One kind being based on p-n heterojunction structure NiO-In2O3The gas sensor of composite Nano ball |
| CN109632893B (en) * | 2019-01-11 | 2022-02-25 | 东北大学 | NiO-In based on p-n heterojunction structure2O3Composite nanosphere gas sensor |
| CN111579600A (en) * | 2020-06-28 | 2020-08-25 | 郑州轻工业大学 | Camellia flower-shaped ZnO/SnO-SnO2Composite material and preparation method and application thereof |
| CN111579600B (en) * | 2020-06-28 | 2022-11-22 | 郑州轻工业大学 | Camellia flower-shaped ZnO/SnO-SnO 2 Composite material and preparation method and application thereof |
| CN113562719A (en) * | 2021-06-25 | 2021-10-29 | 鞍钢化学科技有限公司 | Nano SnO2Preparation method of water-soluble asphalt carbon composite electrode negative electrode material |
| CN114229885A (en) * | 2021-12-29 | 2022-03-25 | 吉林大学 | CdO/SnO2Composite nanocube gas-sensitive material, preparation method and application thereof in hydrogen detection |
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