CN107215890A - A kind of preparation method of cubic nanostructures indium oxide gas sensitive - Google Patents
A kind of preparation method of cubic nanostructures indium oxide gas sensitive Download PDFInfo
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- CN107215890A CN107215890A CN201710504899.4A CN201710504899A CN107215890A CN 107215890 A CN107215890 A CN 107215890A CN 201710504899 A CN201710504899 A CN 201710504899A CN 107215890 A CN107215890 A CN 107215890A
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- C01G15/00—Compounds of gallium, indium or thallium
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Abstract
The invention provides a kind of preparation method of cubic nanostructures indium oxide gas sensitive.The preparation method is specifically included:Using four trichloride hydrate indiums and Isosorbide-5-Nitrae butanediamine as raw material, through hydro-thermal reaction, calcination processing, the indium oxide cube with loose structure is obtained.This method simple production process, without using any surfactant, synthesis cost is low, experimental implementation is simple, gained indium oxide can be as gas sensitive, and it has good air-sensitive performance to front three amine gas, therefore can be used widely in front three amine gas context of detection.
Description
Technical field
The present invention relates to a kind of preparation method of cubic nanostructures indium oxide gas sensitive, belong to advanced nano functional
Material preparation process technical 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, trimethylamine is as one of chemical index of fish freshness,
It is related to the safety and health of mankind itself, its air-sensitive Journal of Sex Research is also increasingly taken seriously.Current trimethylamine gas sensor
With TiO2, ZnO be main gas sensitive.Japanese Scientists Egashira etc. is with doped precious metal ruthenium, the TiO of indium2For material
First TMA gas sensor has been made, but its response recovery time is longer(Makoto E, Yasuhiro S, Yuji T.
Trimethylamine sensor based semiconductive metal oxides for detection of fish
freshness [J]. Sens. Actuators B, 1990, 1: 108-112).On this basis, although Zhang Zhongxiao etc. contracts
Short response recovery time, but its less stable(Zhang Zhongxiao, Meng Alan, Li Houfu, wait to measure the trimethylamine of seafood degree
[(CH3)3N] metal oxide semiconductor sensing element development [J] sensor technologies, 1995, (3): 31-34).Therefore,
Exploration has high sensitivity, shorter response recovery time, the good metal semiconductor of long-time stability with straightforward procedure synthesis
Gas sensitive and study its air-sensitive performance very it is necessary therefore.
In2O3Be it is a kind of study the gas sensitive started late, because its operating temperature is relatively low, low-resistivity, sensitivity
It is high and have the advantages that response to multiple gases and be increasingly subject to the concern of people.In2O3It is a kind of new Semiconductor gas sensors material
Material, no matter its composition is pure phase, also or is doped with the compound of certain element or oxide, poisonous in air is detected to have
Have in terms of evil gas and be widely applied very much, particularly to NO2、H2S、H2, CO and alcohol gas show preferable gas sensing property
Energy.In gas detection process, be mainly concerned with gas diffusion into the surface and gas and Surface Oxygen between redox phase
Interaction.Therefore, the gas sensitive material of high-specific surface area is very beneficial for realizing hypersensitivity of the material to reducibility gas.
In order to improve identification function, except selecting good matrix material, it is modified outside by doping, compound and surface modification, if
Meter and preparation are also the strategy attracted attention with bigger serface, the porous structure material of high activity site density.The present invention
The indium oxide cube prepared has loose structure, with good permeability, can promote gas diffusion, is conducive to improving
The utilization rate of gas sensitive.Further, since the restriction of experimental facilities and production technology, current people are for In2O3Nano material
It is not also very deep to probe into probing into terms of especially air-sensitive performance.Researcher is urgently ground with the comprehensive angle of more system
Study carefully In2O3The structure and morphology feature and functional character feature of nano material.
The content of the invention
It is an object of the present invention to overcome the deficiencies in the prior art, there is provided a kind of cubic nanostructures indium oxide air-sensitive
The preparation method of material.Low with cost, simple production process, yield is high, the characteristics of non-environmental-pollution.Gained has porous knot
The sensitivity of the indium oxide gas sensitive of structure is largely increased, available for fields such as gas sensors.Realize the object of the invention
Technical scheme be:A kind of preparation method of cubic nanostructures indium oxide gas sensitive.The preparation method is specifically included:With
Four trichloride hydrate indiums and Putriscine are raw material, through hydro-thermal reaction, calcination processing, obtain the indium oxide with loose structure
Cube.This method simple production process, without using any surfactant, synthesis cost is low, and experimental implementation is simple, gained
Indium oxide can be as gas sensitive, and it has good air-sensitive performance to front three amine gas, therefore in front three amine gas detection side
Face can be used widely.Specific synthesis step is as follows:
(1)A certain amount of four trichloride hydrates indium, Putriscine are weighed, is dissolved in 40 mL deionized waters, wherein four hydrations three
The concentration of inidum chloride is 0.02-0.05 mol/L, and the concentration of Putriscine is 0.02-0.05 mol/L, and controls four to be hydrated
The mol ratio of indium trichloride and Putriscine is 1:(1-2);
(2)By step(1)Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180-200 DEG C
At a temperature of, carry out hydro-thermal reaction 8-24 h, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and spend from
Sub- water and ethanol are repeatedly washed to gained solid product;
(3)By step(2)Gained solid product is positioned in drying box, 60 DEG C of dryings, is subsequently placed in alumina crucible and is put into horse
Not stove, is heat-treated 3 h at 400-550 DEG C, obtains the cube indium oxide powder with loose structure.
Brief description of the drawings
Fig. 1 is the XRD spectrum of cubic nanostructures indium oxide.
Fig. 2 schemes for the SEM of cubic nanostructures indium oxide.
Fig. 3 schemes for the TEM of cubic nanostructures indium oxide.
Fig. 4 is the N of cubic nanostructures indium oxide2Suction-desorption figure.
Fig. 5 is sensitivity curve of the cubic nanostructures indium oxide gas sensor to 10-1000ppm front three amine gas
Figure.
Fig. 6 is the response recovery curve figure of cubic nanostructures indium oxide gas sensor under optimum operating voltage.
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 implementations
Example.
Embodiment 1
(1)A certain amount of four trichloride hydrates indium, Putriscine are weighed, is dissolved in 40 mL deionized waters, wherein four hydrations three
The concentration of inidum chloride is 0.025 mol/L, and the concentration of Putriscine is 0.025 mol/L, and controls four trichloride hydrate indiums
Mol ratio with Putriscine is 1:1;
(2)By step(1)Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 180 DEG C of temperature
Under, carry out the h of hydro-thermal reaction 8, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and with deionized water with
Ethanol is repeatedly washed to gained solid product;
(3)By step(2)Gained solid product is positioned in drying box, 60 DEG C of dryings, is subsequently placed in alumina crucible and is put into horse
Not stove, is heat-treated 3 h at 500 DEG C, obtains the cube indium oxide powder with loose structure.
Embodiment 2
(1)A certain amount of four trichloride hydrates indium, Putriscine are weighed, is dissolved in 40 mL deionized waters, wherein four hydrations three
The concentration of inidum chloride is 0.025 mol/L, and the concentration of Putriscine is 0.025 mol/L, and controls four trichloride hydrate indiums
Mol ratio with Putriscine is 1:1;
(2)By step(1)Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 180 DEG C of temperature
Under, carry out the h of hydro-thermal reaction 12, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and with deionized water with
Ethanol is repeatedly washed to gained solid product;
(3)By step(2)Gained solid product is positioned in drying box, 60 DEG C of dryings, is subsequently placed in alumina crucible and is put into horse
Not stove, is heat-treated 3 h at 500 DEG C, obtains the cube indium oxide powder with loose structure.
Embodiment 3
(1)A certain amount of four trichloride hydrates indium, Putriscine are weighed, is dissolved in 40 mL deionized waters, wherein four hydrations three
The concentration of inidum chloride is 0.025 mol/L, and the concentration of Putriscine is 0.025 mol/L, and controls four trichloride hydrate indiums
Mol ratio with Putriscine is 1:1;
(2)By step(1)Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 180 DEG C of temperature
Under, carry out the h of hydro-thermal reaction 20, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and with deionized water with
Ethanol is repeatedly washed to gained solid product;
(3)By step(2)Gained solid product is positioned in drying box, 60 DEG C of dryings, is subsequently placed in alumina crucible and is put into horse
Not stove, is heat-treated 3 h at 500 DEG C, obtains the cube indium oxide powder with loose structure.
Embodiment 4
(1)A certain amount of four trichloride hydrates indium, Putriscine are weighed, is dissolved in 40 mL deionized waters, wherein four hydrations three
The concentration of inidum chloride is 0.025 mol/L, and the concentration of Putriscine is 0.05 mol/L, and four trichloride hydrate indiums of control with
The mol ratio of Putriscine is 1:2;
(2)By step(1)Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 200 DEG C of temperature
Under, carry out the h of hydro-thermal reaction 12, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and with deionized water with
Ethanol is repeatedly washed to gained solid product;
(3)By step(2)Gained solid product is positioned in drying box, 60 DEG C of dryings, is subsequently placed in alumina crucible and is put into horse
Not stove, is heat-treated 3 h at 500 DEG C, obtains the cube indium oxide powder with loose structure.
Embodiment 5
(1)A certain amount of four trichloride hydrates indium, Putriscine are weighed, is dissolved in 40 mL deionized waters, wherein four hydrations three
The concentration of inidum chloride is 0.025 mol/L, and the concentration of Putriscine is 0.025 mol/L, and controls four trichloride hydrate indiums
Mol ratio with Putriscine is 1:1;
(2)By step(1)Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), in 200 DEG C of temperature
Under, carry out the h of hydro-thermal reaction 24, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and with deionized water with
Ethanol is repeatedly washed to gained solid product;
(3)By step(2)Gained solid product is positioned in drying box, 60 DEG C of dryings, is subsequently placed in alumina crucible and is put into horse
Not stove, is heat-treated 3 h at 500 DEG C, obtains the cube indium oxide powder with loose structure.
Claims (1)
1. a kind of preparation method of cubic nanostructures indium oxide gas sensitive, specific synthesis step is as follows:
(1)A certain amount of four trichloride hydrates indium, Putriscine are weighed, is dissolved in 40 mL deionized waters, wherein four hydrations three
The concentration of inidum chloride is 0.02-0.05 mol/L, and the concentration of Putriscine is 0.02-0.05 mol/L, and controls four to be hydrated
The mol ratio of indium trichloride and Putriscine is 1:(1-2);
(2)By step(1)Middle gained mixed solution is moved in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), at 180-200 DEG C
At a temperature of, carry out hydro-thermal reaction 8-24 h, then by after hydro-thermal reaction product utilization centrifuge carry out separation of solid and liquid, and spend from
Sub- water and ethanol are repeatedly washed to gained solid product;
(3)By step(2)Gained solid product is positioned in drying box, 60 DEG C of dryings, is subsequently placed in alumina crucible and is put into horse
Not stove, is heat-treated 3 h at 400-550 DEG C, obtains the cube indium oxide powder with loose structure.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110386620A (en) * | 2019-08-01 | 2019-10-29 | 刘骞 | Indium oxide gas sensitive and preparation method and application for ppb grades of ethyl alcohol detections |
CN111735857A (en) * | 2020-07-07 | 2020-10-02 | 华准科技(绍兴)有限公司 | In supporting Ru2O3Nano material and preparation method and application thereof |
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CN102963922A (en) * | 2012-10-26 | 2013-03-13 | 河南圣玛斯光电科技有限公司 | Hydrothermal synthesis method for indium oxide with cubic crystal structure |
CN106006719A (en) * | 2016-07-20 | 2016-10-12 | 济南大学 | Method for preparing indium oxide micro-spheres which comprise nanometer particles and are of classification structures |
CN106186048A (en) * | 2016-07-20 | 2016-12-07 | 济南大学 | A kind of preparation method of the hierarchy Indium sesquioxide. microsphere of cube composition |
CN107215889A (en) * | 2017-06-28 | 2017-09-29 | 济南大学 | A kind of preparation method of loose structure indium oxide cube gas sensitive |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102963922A (en) * | 2012-10-26 | 2013-03-13 | 河南圣玛斯光电科技有限公司 | Hydrothermal synthesis method for indium oxide with cubic crystal structure |
CN106006719A (en) * | 2016-07-20 | 2016-10-12 | 济南大学 | Method for preparing indium oxide micro-spheres which comprise nanometer particles and are of classification structures |
CN106186048A (en) * | 2016-07-20 | 2016-12-07 | 济南大学 | A kind of preparation method of the hierarchy Indium sesquioxide. microsphere of cube composition |
CN107215889A (en) * | 2017-06-28 | 2017-09-29 | 济南大学 | A kind of preparation method of loose structure indium oxide cube gas sensitive |
Non-Patent Citations (2)
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110386620A (en) * | 2019-08-01 | 2019-10-29 | 刘骞 | Indium oxide gas sensitive and preparation method and application for ppb grades of ethyl alcohol detections |
CN111735857A (en) * | 2020-07-07 | 2020-10-02 | 华准科技(绍兴)有限公司 | In supporting Ru2O3Nano material and preparation method and application thereof |
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