CN107340367A - A kind of preparation method of three-dimensional rGO/In2O3 composite room temperature gas sensitive - Google Patents
A kind of preparation method of three-dimensional rGO/In2O3 composite room temperature gas sensitive Download PDFInfo
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- CN107340367A CN107340367A CN201710559471.XA CN201710559471A CN107340367A CN 107340367 A CN107340367 A CN 107340367A CN 201710559471 A CN201710559471 A CN 201710559471A CN 107340367 A CN107340367 A CN 107340367A
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- room temperature
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- 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
Abstract
The invention provides a kind of cube indium oxide of meso-hole structure to be grown in three-dimensional redox graphene（rGO）On composite room temperature gas sensitive preparation method.The preparation method specifically includes：With graphene oxide GO, four water inidum chlorides, urea are raw material, using trisodium citrate as surfactant and reducing agent, through hydro-thermal method, calcination processing, the cube indium oxide for obtaining meso-hole structure is evenly distributed on composite room temperature gas sensitive on the three-dimensional rGO carriers for being overlapped to form pore passage structure.This method simple production process, the cube indium oxide that meso-hole structure is made are evenly distributed on the three-dimensional rGO carriers for being overlapped to form pore passage structure, and obtain the air-sensitive detection material to front three amine gas at room temperature with sensitive property.
Description
Technical field
The present invention relates to a kind of three-dimensional rGO/In2O3Composite room temperature gas sensitive preparation method, belong to advanced nanometer material
Expect fabricating technology field.
Background technology
In recent years, food security enjoys people to pay attention to, and a large amount of TMAOs are contained in marine product, and they make in biology enzyme
Easily be decomposed into formaldehyde and dimethylamine with lower, and be also easy to produce under bacterial action bad smell trimethylamine (Trimethylamine,
TMA), they are all the precursor substances of carcinogenic substance nitroso-amines.Therefore, one of the chemical index of trimethylamine as fish freshness,
The safety and health, its air-sensitive Journal of Sex Research for being related to mankind itself are also increasingly taken seriously.Trimethylamine gas sensor at present
With TiO2, ZnO be main gas sensitive.But metal-oxide semiconductor (MOS) does not possess conductivity at room temperature, its carrier mobility
It is relatively low, reference area is smaller causes utilization rate low.Generally requiring heat at 70 ~ 250 DEG C to work.Therefore open
Generating transport factor is high, and specific surface area is big and the gas sensor that can work at room temperature is to break through semiconductor transducer development
A kind of feasible method of bottleneck.Three-dimensional rGO possesses more as a kind of carbon material with porous network structure than two-dimentional rGO
It big specific surface area and Geng Gao electron mobility and should not stack, be widely used in electronics, sensor, medicine and catalysis
Deng field, to overcome Semiconductor gas sensors material shortcoming to provide new thinking.Various countries expert is become since graphene is found
The focus of scholar's research, while the graphene that synthesizes of three-dimensional grapheme preferably improves sensor air-sensitive performance and provides new grind
Study carefully direction.
The form and structure of micro/nano structure functional material are also to influence the principal element of its air-sensitive performance, and many people are
Through being directed to controlling its form in preparation process and structure or developing new construction and realize the enhancing of performance, make its
Widely being paid close attention to using these unique properties in optics, electronics, magnetics, bionics and catalysis.Meso-hole structure
Cube indium oxide metal oxide nano-material have high specific surface area and it is regularly arranged be not susceptible to reunite receive
Rice structure, and storeroom electron mobility is improved by contact of the face with face, thus be considered as very promising air-sensitive
Material.China is the most abundant country of graphite resource, and big producer, but the deep processing to its high-tech is probed into still in just
The level stage.The research of three-dimensional rGO composites, which is concentrated mainly on, also has many problems to need to study recent years.Therefore, explore
There is the three-dimensional rGO composite air-sensitives material of high air-sensitive property energy to be one at room temperature to still need to solve the problems, such as.
The content of the invention
A kind of it is an object of the present invention to overcome the deficiencies in the prior art, there is provided the cube indium oxide life of meso-hole structure
Grow in three-dimensional redox graphene（rGO）On composite room temperature gas sensitive preparation method.With simple production process, nothing
Environmental pollution, it is easy to the characteristics of industrialization mass produces.Gained three-dimensional rGO/In2O3Gas sensing property obtains gas sensitive at room temperature
To greatly improving.Realizing the technical scheme of the object of the invention is：A kind of three-dimensional rGO/In2O3Room temperature gas sensitive preparation method,
It is characterized in that：With graphene oxide GO, four water inidum chlorides, urea is raw material, using trisodium citrate as surfactant and also
Former agent, through hydro-thermal method, calcination processing, the cube indium oxide for obtaining meso-hole structure is evenly distributed on and is overlapped to form the three of pore passage structure
Tie up the composite room temperature gas sensitive on rGO carriers.This method simple production process, the holey knot using three-dimensional rGO as carrier
Structure, gained indium oxide are cube meso-hole structure, and three-dimensional rGO/ In are obtained by hydro-thermal reaction2O3Composite, obtain in room
The lower new gas sensitive with higher sensitivity of temperature.Specific synthesis step is as follows：
Weigh 100-350 mg GO and be distributed in 20-100 ml deionized water simultaneously 30 min of ultrasound, then by 0.01-0.1
Mol/l four water inidum chlorides and 0.01-0.5 mol/l trisodium citrate and 0.01-0.1 mol/l urea add above-mentioned
In mixed liquor, the 120-160 DEG C of insulation 24-38h in insulating box is placed in reactor, gained solid product is collected by centrifugation, is used in combination
Deionized water and absolute ethyl alcohol washing for several times, are put into -50 degree in freeze drying box and dry 2-72 hours, then in tube furnace,
High-temperature calcination is carried out under Ar atmosphere protections, calcining heat is 400-600 DEG C, and soaking time is 2-4 hours, obtains rGO/In2O3It is multiple
Close room temperature gas sensitive.It is 1 to control the mol ratio of four water inidum chlorides and trisodium citrate:2-8, four water inidum chlorides and urea
Mol ratio be 1:0.1-2.
Brief description of the drawings
Fig. 1 is three-dimensional rGO/In2O3FESEM figure.
Fig. 2 is three-dimensional rGO/In2O3XRD spectrum.
Fig. 3 is three-dimensional rGO/In2O3TEM figure.
Fig. 4 is three-dimensional rGO/In at room temperature2O3Sensitive writing music of the gas sensor to 100-1000ppm front three amine gas
Line chart.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
（1）240mg graphene oxide GO is weighed, by its ultrasonic disperse in 30 mL deionized waters, obtains GO colloidal solution,
Wherein GO concentration is 8 mg/mL；
（2）0.027mol/l four water inidum chlorides, 0.16mol/l trisodium citrates and 0.013mol/l urea are weighed, dissolves in step
Suddenly（1）Gained GO colloidal solution, stir 1 hour at room temperature, and it is 1 to control the mol ratio of four water inidum chlorides and trisodium citrate:
5.9, the mol ratio of four water inidum chlorides and urea is 1：0.48；
（3）By step（2）Gained mixed solution is placed in reactor 140 DEG C of insulation 24h in insulating box, and it is solid that gained is collected by centrifugation
Body product, and washed for several times with deionized water and absolute ethyl alcohol, it is put into -50 degree in freeze drying box and dries 24 hours, Ran Hou
In tube furnace, high-temperature calcination is carried out under Ar atmosphere protections, calcining heat is 500 DEG C, and soaking time is 2 hours, obtains rGO/
In2O3Compound composite room temperature gas sensitive control；
Embodiment 2
（1）150mg graphene oxide GO is weighed, by its ultrasonic disperse in 30 mL deionized waters, obtains GO colloidal solution,
Wherein GO concentration is 5 mg/mL；
（2）0.02mol/l four water inidum chlorides, 0.1mol/l trisodium citrates and 0.01mol/l urea are weighed, dissolves in step
（1）Gained GO colloidal solution, stir 1 hour at room temperature, and it is 1 to control the mol ratio of four water inidum chlorides and trisodium citrate:5,
The mol ratio of four water inidum chlorides and urea is 1：0.5；
（3）By step（2）Gained mixed solution is placed in reactor 160 DEG C of insulation 20h in insulating box, and it is solid that gained is collected by centrifugation
Body product, and washed for several times with deionized water and absolute ethyl alcohol, it is put into -50 degree in freeze drying box and dries 30 hours, Ran Hou
In tube furnace, high-temperature calcination is carried out under Ar atmosphere protections, calcining heat is 600 DEG C, and soaking time is 3 hours, obtains rGO/
In2O3Compound composite room temperature gas sensitive control；
Embodiment 3
（1）300mg graphene oxide GO is weighed, by its ultrasonic disperse in 30 mL deionized waters, obtains GO colloidal solution,
Wherein GO concentration is 10 mg/mL；
（2）0.025mol/l four water inidum chlorides, 0.15mol/l trisodium citrates and 0.015mol/l urea are weighed, dissolves in step
Suddenly（1）Gained GO colloidal solution, stir 1 hour at room temperature, and it is 1 to control the mol ratio of four water inidum chlorides and trisodium citrate:
6, the mol ratio of four water inidum chlorides and urea is 1：0.6；
（3）By step（2）Gained mixed solution is placed in reactor 150 DEG C of insulation 28h in insulating box, and it is solid that gained is collected by centrifugation
Body product, and washed for several times with deionized water and absolute ethyl alcohol, it is put into -50 degree in freeze drying box and dries 38 hours, Ran Hou
In tube furnace, high-temperature calcination is carried out under Ar atmosphere protections, calcining heat is 550 DEG C, and soaking time is 2.5 hours, obtains rGO/
In2O3Compound composite room temperature gas sensitive control.
Claims (1)
- A kind of 1. three-dimensional rGO/In2O3Composite room temperature gas sensitive preparation method：Specific synthesis step is as follows：（1）Graphene oxide GO prepared by a certain amount of improvement Hummers methods is weighed, its ultrasonic disperse is gone in 10-100 mL In ionized water, GO colloidal solution is obtained, wherein GO concentration is 2-15 mg/mL；（2）A certain amount of four water inidum chloride, trisodium citrate and urea are weighed, dissolves in step（1）Gained GO colloidal solution, room temperature Lower stirring 1 hour, wherein the concentration of four water inidum chlorides is 0.01-0.1mol/l, the concentration of trisodium citrate is 0.01-0.5 Mol/l, the concentration of urea is 0.01-0.1mol/l, and it is 1 to control the mol ratio of four water inidum chlorides and trisodium citrate:2-8, The mol ratio of four water inidum chlorides and urea is 1：0.1-2；（3）By step（2）Gained mixed solution is placed in reactor 120-160 DEG C of insulation 24-38h, centrifugation in insulating box and received Collection gained solid product, and washed for several times with deionized water and absolute ethyl alcohol, it is put into -50 degree in freeze drying box and dries 24-72 Hour, then in tube furnace, high-temperature calcination is carried out under Ar atmosphere protections, calcining heat is 500-600 DEG C, soaking time 2- 6 hours, obtain rGO/In2O3Compound composite room temperature gas sensitive control.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108445049A (en) * | 2018-05-08 | 2018-08-24 | 公安部天津消防研究所 | A kind of preparation method of the composite metal oxide gas-sensing material of graphene oxide modification |
| CN109019673A (en) * | 2018-08-01 | 2018-12-18 | 济南大学 | A kind of SnO2-In2O3The preparation method of nanocomposite |
| CN109455706A (en) * | 2018-12-13 | 2019-03-12 | 东莞理工学院 | A kind of preparation method of sulfonated graphene load indium oxide gas sensitive |
| CN109709184A (en) * | 2019-01-24 | 2019-05-03 | 吉林大学 | One kind being based on In2O3The NO of carbon dots compound2Sensor and preparation method thereof |
| CN112394091A (en) * | 2020-10-27 | 2021-02-23 | 盐城工学院 | Indium oxide dimethylamine gas-sensitive sensor material with hierarchical structure and preparation method and application thereof |
| CN112649477A (en) * | 2019-10-12 | 2021-04-13 | 中国科学院大连化学物理研究所 | With rGO/In2O3Self-generating gas sensor as electrode material |
| CN113686928A (en) * | 2021-08-24 | 2021-11-23 | 华北电力大学 | GO/In2O3Composite nano material and preparation and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108445049A (en) * | 2018-05-08 | 2018-08-24 | 公安部天津消防研究所 | A kind of preparation method of the composite metal oxide gas-sensing material of graphene oxide modification |
| CN109019673A (en) * | 2018-08-01 | 2018-12-18 | 济南大学 | A kind of SnO2-In2O3The preparation method of nanocomposite |
| CN109455706A (en) * | 2018-12-13 | 2019-03-12 | 东莞理工学院 | A kind of preparation method of sulfonated graphene load indium oxide gas sensitive |
| CN109709184A (en) * | 2019-01-24 | 2019-05-03 | 吉林大学 | One kind being based on In2O3The NO of carbon dots compound2Sensor and preparation method thereof |
| CN109709184B (en) * | 2019-01-24 | 2020-12-01 | 吉林大学 | In-based2O3NO of carbon dot complexes2Sensor and preparation method thereof |
| CN112649477A (en) * | 2019-10-12 | 2021-04-13 | 中国科学院大连化学物理研究所 | With rGO/In2O3Self-generating gas sensor as electrode material |
| CN112394091A (en) * | 2020-10-27 | 2021-02-23 | 盐城工学院 | Indium oxide dimethylamine gas-sensitive sensor material with hierarchical structure and preparation method and application thereof |
| CN112394091B (en) * | 2020-10-27 | 2023-01-10 | 盐城工学院 | Indium oxide dimethylamine gas-sensitive sensor material with hierarchical structure and preparation method and application thereof |
| CN113686928A (en) * | 2021-08-24 | 2021-11-23 | 华北电力大学 | GO/In2O3Composite nano material and preparation and application thereof |
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Application publication date: 20171110 |