CN106986375A - A kind of preparation method of nano indium oxide to n-butanol hypersensitivity - Google Patents
A kind of preparation method of nano indium oxide to n-butanol hypersensitivity Download PDFInfo
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- CN106986375A CN106986375A CN201710300240.7A CN201710300240A CN106986375A CN 106986375 A CN106986375 A CN 106986375A CN 201710300240 A CN201710300240 A CN 201710300240A CN 106986375 A CN106986375 A CN 106986375A
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- Prior art keywords
- indium
- butanol
- ethanol
- ethylene glycol
- indium oxide
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
The invention provides a kind of preparation method of the nano indium oxide to n-butanol hypersensitivity.The preparation method is specifically included：Using indium nitrate, ethanol, ethylene glycol and monoethanolamine as raw material, through solvent thermal reaction, calcination processing obtains the oxidation indium nanometer particle with special appearance.This method simple production process, without using expensive surfactant, cost is than relatively low.The nano indium oxide of gained has good air-sensitive performance to n-butanol gas as gas sensitive, therefore, is had a good application prospect in n-butanol gas context of detection.
Description
Technical field
The present invention relates to a kind of preparation method of the nano indium oxide to n-butanol hypersensitivity, belong to advanced nano functional
Material preparation process technical field.
Background technology
In recent years, with the quickening of process of industrialization, it is discharged into the species sum of volatile organic matter in air (VOCs)
Amount substantial increase.Much there is the harm such as carcinogenic, teratogenesis, mutagenesis in these VOCs, the formation of photochemical fog is also resulted in
With increasing for haze weather, great threaten is produced to human health.Therefore, air trace VOCs is carried out in real time, quickly
Detection is a urgent task, while the demand to high performance gas sensor is also more urgent.Because semi-conductor gas is passed
Sensor has that detection sensitivity is high, response recovers fast, circuit is simple, simple to operate, component size is smaller, the spy such as cheap
Point, is widely used in various field of gas detection.
The air-sensitive performance of semi-conducting material is mainly influenceed by cell configuration and surface topography.According to gas sensing mechanism not
Together, semiconductor can be divided into n-type and p-type.Indium oxide is a kind of n-type transparent semiconductor functional material, wide with wider forbidden band
Degree, less resistivity and higher catalytic activity, extensively should have been obtained in terms of photoelectric field, gas sensor, catalyst
With.And indium oxide particles size reach Nano grade when in addition to function above, be also equipped with nano material skin effect, amount
Sub- dimensional effect, small-size effect and macro quanta tunnel effect etc..It can be controlled by methods such as solvent-thermal process synthesized
Nano oxidized phosphide material surface topography so that the material for possessing different-shape shows different air-sensitive performances.
The content of the invention
It is an object of the present invention to overcome existing gas sensor poor selectivity, sensitivity is not high, and stability difference is waited not
There is provided a kind of preparation method of the nano indium oxide to n-butanol hypersensitivity for foot.This method simple production process, raw material is easy
, yield is high, and production cost is low, composition and reaction temperature only by changing liquid phase, it is not necessary to any template and structure directing
Agent can be prepared by the nano oxidized phosphide material with different-shape and air-sensitive performance.
The present invention is for the technical scheme that is used of its technical problem of solution：A kind of nano oxygen to n-butanol hypersensitivity
Change the preparation method of indium, it is characterised in that：Using indium nitrate, ethanol, ethylene glycol and monoethanolamine as raw material, through solvent thermal reaction, forge
Burning processing, obtains the oxidation indium nanometer particle with special appearance, has good air-sensitive performance to n-butanol gas after testing,
Specific synthesis step is as follows：
(1) a certain amount of indium nitrate is weighed in reactor, ethanol, the ethylene glycol of certain volume is sequentially added, and mixing is equal
It is even, and indium nitrate is fully dissolved, the volume ratio of the ethylene glycol and ethanol is 1: 6, and indium nitrate accounts for ethanol, ethylene glycol mixture
The 0.80%~0.85% of gross weight；
(2) monoethanolamine of certain volume is added in the mixed liquor obtained into step (1), is well mixed, and at room temperature
Stirring 1 hour, the volume of the monoethanolamine is 1: 1 with the volume ratio of ethylene glycol in step (1)；
(3) mixed liquor obtained by step (2) is moved into polytetrafluoroethyllining lining, the liner is then loaded into stainless steel reaction
Kettle, seals kettle；
(4) reactor is heated to 120~180 DEG C, is incubated 6 hours；
(5) after hydro-thermal reaction terminates, reactor is naturally cooled into room temperature, then by liquid centrifugal filtration, reacted
Product；
(6) product obtained in step (5) is repeatedly washed with distilled water, ethanol successively, until during pH value of solution is in
Property, obtain the compound of indium；
(7) compound for the indium for obtaining step (6) is placed in 80 DEG C of air dry ovens, is dried 6 hours；
(8) compound of the indium of the drying obtained in step (7) is placed in Muffle furnace, be heat-treated at 300~500 DEG C
2 hours, room temperature is naturally cooled to, that is, obtains aligning the nano indium oxide of butanol hypersensitivity.
Brief description of the drawings
The invention will be further described below in conjunction with the accompanying drawings.
Fig. 1 is the XRD of products therefrom；
Abscissa is 2 θ angles, and ordinate is diffraction peak intensity, and temperature when data label refers to solvent-thermal process is：120 DEG C,
150 DEG C, 180 DEG C；
Fig. 2 schemes for the SEM of products therefrom；
A, b, c refer to the SEM figures of the sample synthesized under 120 DEG C, 150 DEG C, 180 DEG C of solvent heats respectively；
Fig. 3 is concentration-sensitivity curve of the gas sensor that is made of products therefrom to n-butanol；
Abscissa is n-butanol gas concentration, and unit ppm, ordinate is sensitivity；
Fig. 4 is response-recovery curve of the gas sensor that is made of products therefrom to various concentrations n-butanol gas；
Fig. 5 is response-recovery curve of the gas sensor that is made of products therefrom to 5ppm n-butanol gases；
Fig. 6 is sensitivity curve of the gas sensor that is made of products therefrom at a temperature of different operating；
Fig. 7 is sensitivity curve of the gas sensor that is made of products therefrom to gas with various；
Embodiment
(1) 0.6g indium nitrate is weighed in 250ml conical flasks, 60ml ethanol, 10ml ethylene glycol is sequentially added, and mixing is equal
It is even；
(2) conical flask is placed on magnetic stirring apparatus, magnetic agitation makes indium nitrate fully dissolve；
(3) 10ml monoethanolamine is added in the mixed liquor obtained into step (2), is well mixed, continues magnetic at room temperature
Power is stirred 1 hour；；
(4) mixed liquor obtained by step (3) is moved into polytetrafluoroethyllining lining, the liner is then loaded into stainless steel reaction
Kettle, seals kettle；
(5) reactor is heated to 180 DEG C, is incubated 6 hours；
(6) after hydro-thermal reaction terminates, reactor is naturally cooled into room temperature, then by liquid centrifugal filtration, reacted
Product；
(7) product obtained in step (6) is repeatedly washed with distilled water, ethanol successively, until during pH value of solution is in
Property, obtain the compound of indium；
(8) compound for the indium for obtaining step (7) is placed in 80 DEG C of air dry ovens, is dried 6 hours；
(9) compound of the indium of the drying obtained in step (8) is placed in Muffle furnace, 2 is heat-treated at 300 DEG C small
When, room temperature is naturally cooled to, that is, obtains aligning the nano indium oxide of butanol hypersensitivity.
Claims (1)
1. the preparation method of a kind of nano indium oxide to n-butanol hypersensitivity, it is characterised in that described to n-butanol Gao Xuan
The nano indium oxide of selecting property is prepared by raw material indium nitrate, ethanol, ethylene glycol and monoethanolamine through following steps：
(1) a certain amount of indium nitrate is weighed in reactor, ethanol, the ethylene glycol of certain volume is sequentially added, and is well mixed, and
Indium nitrate is set fully to dissolve, the volume ratio of the ethylene glycol and ethanol is 1: 6, and indium nitrate accounts for ethanol, ethylene glycol mixture gross weight
0.80%~0.85%；
(2) monoethanolamine of certain volume is added in the mixed liquor obtained into step (1), is well mixed, and be stirred at room temperature 1
Hour, the volume of the monoethanolamine is 1: 1 with the volume ratio of ethylene glycol in step (1)；
(3) mixed liquor obtained by step (2) is moved into polytetrafluoroethyllining lining, the liner is then loaded into stainless steel cauldron, envelope
Kettle；
(4) reactor is heated to 120~180 DEG C, is incubated 6 hours；
(5) after hydro-thermal reaction terminates, reactor is naturally cooled into room temperature, then by liquid centrifugal filtration, reaction product is obtained；
(6) product obtained in step (5) is repeatedly washed with distilled water, ethanol successively, until pH value of solution is obtained in neutrality
To the compound of indium；
(7) compound for the indium for obtaining step (6) is placed in 80 DEG C of air dry ovens, is dried 6 hours；
(8) compound of the drying indium obtained in step (7) is placed in Muffle furnace, is heat-treated 2 hours at 300~500 DEG C,
Room temperature is naturally cooled to, that is, obtains aligning the nano indium oxide of butanol hypersensitivity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710300240.7A CN106986375A (en) | 2017-04-28 | 2017-04-28 | A kind of preparation method of nano indium oxide to n-butanol hypersensitivity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710300240.7A CN106986375A (en) | 2017-04-28 | 2017-04-28 | A kind of preparation method of nano indium oxide to n-butanol hypersensitivity |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106986375A true CN106986375A (en) | 2017-07-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710300240.7A Pending CN106986375A (en) | 2017-04-28 | 2017-04-28 | A kind of preparation method of nano indium oxide to n-butanol hypersensitivity |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760831A (en) * | 2018-03-29 | 2018-11-06 | 宁波大学 | A kind of preparation method of indium oxide gas sensor |
| CN110550653A (en) * | 2019-09-30 | 2019-12-10 | 郑州大学 | In 2 O 3/Li 0.5 La 0.5 TiO 3 hydrogen sulfide gas-sensitive composite material and preparation method and application thereof |
-
2017
- 2017-04-28 CN CN201710300240.7A patent/CN106986375A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760831A (en) * | 2018-03-29 | 2018-11-06 | 宁波大学 | A kind of preparation method of indium oxide gas sensor |
| CN110550653A (en) * | 2019-09-30 | 2019-12-10 | 郑州大学 | In 2 O 3/Li 0.5 La 0.5 TiO 3 hydrogen sulfide gas-sensitive composite material and preparation method and application thereof |
| CN110550653B (en) * | 2019-09-30 | 2022-04-01 | 郑州大学 | In2O3/Li0.5La0.5TiO3Hydrogen sulfide gas-sensitive composite material and preparation method and application thereof |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170728 |
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| WD01 | Invention patent application deemed withdrawn after publication |