CN105565382A - Preparation method for molybdenum trioxide nano-sheets and gas-sensitive detector manufactured from molybdenum trioxide nano-sheets - Google Patents
Preparation method for molybdenum trioxide nano-sheets and gas-sensitive detector manufactured from molybdenum trioxide nano-sheets Download PDFInfo
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- CN105565382A CN105565382A CN201610121080.5A CN201610121080A CN105565382A CN 105565382 A CN105565382 A CN 105565382A CN 201610121080 A CN201610121080 A CN 201610121080A CN 105565382 A CN105565382 A CN 105565382A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
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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
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
The invention discloses a preparation method for molybdenum trioxide nano-sheets and a gas-sensitive detector manufactured based on the molybdenum trioxide nano-sheets. The preparation method for the molybdenum trioxide nano-sheets uses a water bath method and mainly comprises the following steps of dissolving ammonium heptamolybdate tetrahydrate in deionized water, then, adding nitric acid into the aqueous solution, and then, carrying out a reaction in a water bath, thereby obtaining the molybdenum trioxide nano-sheets. The water vapor gas-sensitive detector is manufactured by taking the prepared molybdenum trioxide nano-sheets as a material. According to the preparation method for the molybdenum trioxide nano-sheets, the process is simple, the technology is mature, equipment is simple and readily available, and devices are stable and excellent in performance, so that commercial popularization is excellently facilitated. The molybdenum trioxide based water vapor gas-sensitive detector has very good response to water vapor atmosphere.
Description
Technical field
The present invention relates to novel energy resource material technology field, the preparation method particularly relating to a kind of molybdenum trioxide nanosheet and the water vapour gas-sensitive detector prepared by this nanometer sheet.
Background technology
The Application Areas of water vapor gas-sensitive detector is very wide, as fiber, paper, sensitive film, opticglass, hot pressing part, electronic component, Precision Machinery Elements and agriculturally as chamber crop cultivation, cereal and fruit store, poulty house and pig farm etc. also all need to control humidity.The significant parameter evaluating detector performance has switch when response speed, the performance that on-off ratio is larger, response speed illustrates gas-sensitive detector is sooner better, nowadays the water vapor gas-sensitive detector of multiple material base has been developed, as zno-based water vapor gas-sensitive detector, but the target that highly sensitive detector is every field to be pursued always.
Molybdic oxide is a kind of semiconductor material with laminate structure, and its band gap is 3.1eV, can be applied to electroluminescent/photochromic, ultracapacitor, lithium ion battery, the field such as photodetection and photovoltaic device; Nowadays there is multiple method to prepare molybdenum trioxide nanosheet, the preparation methods such as such as hydro-thermal-solvent-thermal method, sol-gel method and physical/chemical vapour deposition, but now lacked a kind of method succinctly preparing high quality molybdenum trioxide nanosheet efficiently; Based on this background, applicant's high-quality molybdenum trioxide nanosheet that utilized simple immersion method to prepare; And utilize the molybdenum trioxide nanosheet of preparation to prepare water vapor gas-sensitive detector, find that molybdic oxide base gas-sensitive detector has very high response sensitivity to water vapor through experiment, the industry that is very beneficial for is promoted.
Summary of the invention
The object of invention there are provided a kind of preparation method of molybdenum trioxide nanosheet and the gas-sensitive detector of preparation thereof.
To achieve these goals, technical scheme disclosed by the invention is as follows: a kind of preparation method of molybdenum trioxide nanosheet, comprises the following steps:
Step a, four hydration Ammonium Heptamolybdates to be dissolved in deionized water, and to utilize magnetic stirring apparatus vigorous stirring solution that four hydration Ammonium Heptamolybdates are dissolved completely;
Step b, in solution, drip nitric acid with glue head dropper, be divided into 10 droppings, a 40-50 μ L, magnetic stirring apparatus continuing vigorous stirs 10-15min afterwards;
Step c, solution is placed in water-bath under 55-75 DEG C of condition, heats 150-220min, obtain white powder; Dry 4-8h by the white powder deionized water eccentric cleaning that obtains and at 55-70 DEG C, sample preparation completes.
Preferably, when dripping nitric acid in described step b, magnetic stirring apparatus Keep agitation and often drip nitric acid interval 8-10s.
Preferably, the concentration of nitric acid is 3.5-5.0mol/L.
The invention discloses a kind of molybdic oxide base gas-sensitive detector, described molybdic oxide base gas-sensitive detector is disperseed by molybdenum trioxide nanosheet alcohol, is spun on by dispersion liquid and has on the glass of ITO electrode, prepare after drying.
The invention has the beneficial effects as follows: the procedure that the present invention prepares molybdic oxide is simple, technology maturation, and equipment is simple and easy to get, and device performance is stable excellent, is very beneficial for commercialization and promotes.And utilize molybdenum trioxide nanosheet to be made into water vapor gas-sensitive detector part for material, test and show that the molybdic oxide base water vapor gas-sensitive detector prepared has well for the response of water vapour atmosphere.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the sample of preparation in embodiment 4;
Fig. 2 is the XRD figure of the sample of preparation in embodiment 4;
Fig. 3 be in embodiment 6 device for the response curve of water vapor.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
Please refer to accompanying drawing 1-3, the embodiment of the present invention comprises:
Embodiment 1: a kind of preparation method of molybdenum trioxide nanosheet, comprises the following steps:
Step a, four hydration Ammonium Heptamolybdates to be dissolved in deionized water, and to utilize magnetic stirring apparatus vigorous stirring solution that four hydration Ammonium Heptamolybdates are dissolved completely;
Step b, in solution, drip nitric acid with glue head dropper, be divided into 10 droppings, a 40-50 μ L, magnetic stirring apparatus continuing vigorous stirs 10-15min afterwards;
Step c, solution is placed in water-bath under 55-75 DEG C of condition, heats 150-220min, obtain white powder; Dry 4-8h by the white powder deionized water eccentric cleaning that obtains and at 55-70 DEG C, sample preparation completes.
Embodiment 2: the difference of the present embodiment and embodiment 1 is, in the present embodiment, when dripping nitric acid in step b, magnetic stirring apparatus Keep agitation and often drip nitric acid interval 8-10s.
Embodiment 3: the difference of the present embodiment and embodiment 1 is, in the present embodiment, the concentration of nitric acid is 3.5-5.0mol/L.
Embodiment 4: a kind of preparation of molybdenum trioxide nanosheet, is dissolved in 0.9g tetra-hydration Ammonium Heptamolybdate in 10mL deionized water, and utilizes magnetic stirring apparatus vigorous stirring solution that four hydration Ammonium Heptamolybdates are dissolved completely; Then in solution, drip the nitric acid of 4.5mol/L with glue head dropper, being divided into 10 droppings, is once 50 μ L, uses magnetic stirring apparatus continuing vigorous stirred solution 10min afterwards, afterwards solution is placed in water-bath and heats 180min under 65 DEG C of temperature condition; Dry 6h by the white powder deionized water eccentric cleaning that obtains and at 60 DEG C.
In the present embodiment, drip 10, nitric acid the most suitable, too much can increase the size of molybdenum trioxide nanosheet, thus affect test result.
In the present embodiment, use water-bath will continue the magnetic stirrer solution using water-bath to carry when heating.
Embodiment 5: a kind of preparation method of molybdic oxide base gas-sensitive detector, disperses molybdenum trioxide nanosheet alcohol, is spun on by dispersion liquid and has on the glass of ITO electrode, and after dry prepared by device.
Embodiment 6: the molybdenum trioxide nanosheet alcohol of the preparation in embodiment 4 is disperseed, being spun on by dispersion liquid has on the glass of ITO electrode, after dry prepared by device, tested by the device prepared: the instrument of employing is CHI660D electrochemical workstation, result shows that device has good water vapor air-sensitive sensitivity of detection.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize specification sheets of the present invention and accompanying drawing content to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (4)
1. a preparation method for molybdenum trioxide nanosheet, is characterized in that, comprises the following steps:
Step a, four hydration Ammonium Heptamolybdates to be dissolved in deionized water, and to utilize magnetic stirring apparatus vigorous stirring solution that four hydration Ammonium Heptamolybdates are dissolved completely;
Step b, in solution, drip nitric acid with glue head dropper, be divided into 10 droppings, a 40-50 μ L, magnetic stirring apparatus continuing vigorous stirs 10-15min afterwards;
Step c, solution is placed in water-bath under 55-75 DEG C of condition, heats 150-220min, obtain white powder; Dry 4-8h by the white powder deionized water eccentric cleaning that obtains and at 55-70 DEG C, sample preparation completes.
2. the preparation method of molybdenum trioxide nanosheet according to claim 1, is characterized in that, when dripping nitric acid in described step b, and magnetic stirring apparatus Keep agitation and often drip nitric acid interval 8-10s.
3. the preparation method of molybdenum trioxide nanosheet according to claim 1, is characterized in that, the concentration of nitric acid is 3.5-5.0mol/L.
4. a molybdic oxide base gas-sensitive detector, is characterized in that, described molybdic oxide base gas-sensitive detector is disperseed by molybdenum trioxide nanosheet alcohol, is spun on by dispersion liquid and has on the glass of ITO electrode, prepare after drying.
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| CN201610121080.5A CN105565382A (en) | 2016-03-03 | 2016-03-03 | Preparation method for molybdenum trioxide nano-sheets and gas-sensitive detector manufactured from molybdenum trioxide nano-sheets |
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| CN201610121080.5A CN105565382A (en) | 2016-03-03 | 2016-03-03 | Preparation method for molybdenum trioxide nano-sheets and gas-sensitive detector manufactured from molybdenum trioxide nano-sheets |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052475A (en) * | 2018-09-27 | 2018-12-21 | 济南大学 | A kind of rodlike MoO of area load particle3/ZnMoO4The synthetic method of structure |
| CN109884087A (en) * | 2019-04-22 | 2019-06-14 | 哈尔滨工业大学 | Based on the band-like MoO of two dimension3The highly sensitive microwave humidity sensor of nano material |
| CN110940708A (en) * | 2019-12-16 | 2020-03-31 | 中国科学院半导体研究所 | Humidity sensor, preparation method thereof, wearable humidity sensing system and application |
| CN110954578A (en) * | 2019-12-16 | 2020-04-03 | 中国科学院半导体研究所 | Humidity sensor and preparation method thereof, non-contact control screen and application |
Citations (3)
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| CN102139923A (en) * | 2011-04-29 | 2011-08-03 | 西安工程大学 | Method for preparing molybdenum trioxide material with orthorhombic phase single crystal nano belt structure |
| CN103332747A (en) * | 2013-06-19 | 2013-10-02 | 陕西科技大学 | Method for synthetizing h-MoO3 at low temperature |
| CN103342388A (en) * | 2013-07-18 | 2013-10-09 | 北京化工大学 | Alpha molybdenum oxide nanorod gas sensitive material and preparation method and application thereof |
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2016
- 2016-03-03 CN CN201610121080.5A patent/CN105565382A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139923A (en) * | 2011-04-29 | 2011-08-03 | 西安工程大学 | Method for preparing molybdenum trioxide material with orthorhombic phase single crystal nano belt structure |
| CN103332747A (en) * | 2013-06-19 | 2013-10-02 | 陕西科技大学 | Method for synthetizing h-MoO3 at low temperature |
| CN103342388A (en) * | 2013-07-18 | 2013-10-09 | 北京化工大学 | Alpha molybdenum oxide nanorod gas sensitive material and preparation method and application thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052475A (en) * | 2018-09-27 | 2018-12-21 | 济南大学 | A kind of rodlike MoO of area load particle3/ZnMoO4The synthetic method of structure |
| CN109884087A (en) * | 2019-04-22 | 2019-06-14 | 哈尔滨工业大学 | Based on the band-like MoO of two dimension3The highly sensitive microwave humidity sensor of nano material |
| CN109884087B (en) * | 2019-04-22 | 2021-07-13 | 哈尔滨工业大学 | Based on two-dimensional banded MoO3High-sensitivity microwave humidity sensor made of nano material |
| CN110940708A (en) * | 2019-12-16 | 2020-03-31 | 中国科学院半导体研究所 | Humidity sensor, preparation method thereof, wearable humidity sensing system and application |
| CN110954578A (en) * | 2019-12-16 | 2020-04-03 | 中国科学院半导体研究所 | Humidity sensor and preparation method thereof, non-contact control screen and application |
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Application publication date: 20160511 |
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