CN106745273A - A kind of multilist planar defect tungsten oxide nanometer gas sensitive and preparation and application - Google Patents
A kind of multilist planar defect tungsten oxide nanometer gas sensitive and preparation and application Download PDFInfo
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- CN106745273A CN106745273A CN201611064816.6A CN201611064816A CN106745273A CN 106745273 A CN106745273 A CN 106745273A CN 201611064816 A CN201611064816 A CN 201611064816A CN 106745273 A CN106745273 A CN 106745273A
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- tungsten oxide
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- 230000007547 defect Effects 0.000 title claims abstract description 23
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910001930 tungsten oxide Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000013019 agitation Methods 0.000 claims abstract description 8
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical class Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 claims abstract description 8
- 238000005119 centrifugation Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000003643 water by type Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 241000257465 Echinoidea Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
-
- 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
-
- 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
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0047—Organic compounds
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Medicinal Chemistry (AREA)
- Materials Engineering (AREA)
- Combustion & Propulsion (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Food Science & Technology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of multilist planar defect tungsten oxide nanometer gas sensitive and preparation and application, 2g tungsten hexachlorides are dissolved in the low-temperature anhydrous ethanol of 100ml, magnetic agitation is to whole dissolvings, 10ml deionized waters are slow added into afterwards, stir 30 minutes at low ambient temperatures, then 50 DEG C of stirred in water bath 24 hours again；Solution cools down low temperature；1g tungsten hexachlorides are dissolved in the low-temperature anhydrous ethanol of 10ml, magnetic agitation is subsequently poured into above-mentioned solution to whole dissolvings；The solution of preparation is transferred in reactor, is sealed, be then placed in reactor, reacted at 180 DEG C, 6 12 hours, be subsequently cooled to room temperature;By prepared powder, centrifugation, washing, drying.Tungsten oxide surface defect prepared by the present invention is enriched, high to acetone gas detection sensitivity, and selectivity is good.
Description
Technical field
The invention belongs to material chemistry technical field, it is related to a kind of multilist planar defect tungsten oxide nanometer gas sensitive and preparation
And application, the material surface microstructure is coarse, and surface super oxygen vacancy defect is more, high to acetone gas detection sensitivity, choosing
Selecting property is good.
Background technology
In Semiconductor gas sensors investigation of materials field, tungsten oxide（WO3）Because it is easy to regulation and control, selective strong, good stability, spirit
Sensitivity is high, the low advantage of air-sensitive operating temperature, as research emphasis in recent years.The gas sensing mechanism of WO3 gas-sensitive nano materials can
Explained with exhausting layer model.WO3The oxygen vacancies on surface can turn into the electron donor of conduction band, so that the material turns into
N-type semiconductor.Therefore, in actual applications, by increasing the specific surface area and surface defect of tungsten oxide nanometer material, Ke Yiti
Its air-sensitive performance high.
Having various methods at present can for example prepare nano-hollow ball, sea urchin shape with increasing specific surface area or surface defect
The methods such as nano particle, nano wire, meso-porous nano material, the above method to be mainly by the adjustment of nanostructured and compare table being lifted
Area and surface defect, and then lift air-sensitive performance.
The content of the invention
To overcome the deficiencies in the prior art, the present invention to provide a kind of multilist planar defect tungsten oxide nanometer gas sensitive and preparation
And application,
A kind of preparation method of multilist planar defect tungsten oxide nanometer gas sensitive, it is characterised in that comprise the following steps：
（1）2g tungsten hexachlorides are dissolved in the low-temperature anhydrous ethanol of 100ml, magnetic agitation is slow added into afterwards to whole dissolvings
10ml deionized waters, stir 30 minutes at low ambient temperatures, then 50 DEG C of stirred in water bath 24 hours again；
（2）By step（1）The solution cools down low temperature；
（3）1g tungsten hexachlorides are dissolved in the low-temperature anhydrous ethanol of 10ml, magnetic agitation is subsequently poured into step to whole dissolvings（2）
In the solution；
（4）By step（3）The solution of middle preparation is transferred in reactor, sealing, is then placed in reactor, anti-at 180 DEG C
Should, 6-12 hours, it is subsequently cooled to room temperature;
（5）By step（4）Prepared powder, centrifugation, washing, drying.
Step（1）Described in low-temperature anhydrous ethanol, its temperature be 0-20 DEG C.
Step（1）Described in low temperature environment, its temperature be 0-20 DEG C.
Step（2）Described in low temperature, its temperature be 0-20 DEG C.
Step（3）Described in low-temperature anhydrous ethanol, its temperature be 0-20 DEG C.
A kind of multilist planar defect tungsten oxide nanometer gas sensitive, it is characterised in that prepared according to any of the above-described methods described
Obtain.
The application that a kind of multilist planar defect tungsten oxide nanometer gas sensitive is detected in acetone gas.
The present invention, proposes a kind of nanometer WO3Preparation method, by Heat of Hydrolysis mechanics in course of reaction, dynamic (dynamical)
Control, introduces a kind of new surface defect, the WO prepared by this method3Surface carries substantial amounts of superoxide radical, this to lack
Falling into being capable of its air-sensitive performance of lifting more significantly more efficient than general oxygen vacancies.
Beneficial effects of the present invention：
WO prepared by the present invention3Particle is ellipticity nano particle, and there is abundant defect sturcture on surface；Meanwhile, by reaction
Process thermodynamics, dynamic (dynamical) control so that surface has substantial amounts of superoxide radical, greatly improve its air-sensitive performance,
At relatively low temperature（180℃）, there is good sensitivity and selectivity to acetone.
Brief description of the drawings
Fig. 1 is the WO prepared by embodiment 13The SEM pictures of nano particle；
Fig. 2 is the WO prepared by embodiment 13The air-sensitive performance figure of nano particle.
Specific embodiment
Embodiment 1
1. 2g tungsten hexachlorides are dissolved in 0 DEG C of absolute ethyl alcohol of 100ml, magnetic agitation is slow added into afterwards to whole dissolvings
10ml deionized waters, stir 30 minutes under 0 DEG C of environment, then 50 DEG C of stirred in water bath 24 hours again；
2. solution described in step 1 is cooled down 0 DEG C；
3. 1g tungsten hexachlorides are dissolved in 0 DEG C of absolute ethyl alcohol of 10ml, magnetic agitation is subsequently poured into step 2 institute to whole dissolvings
In stating solution；
4. the solution prepared in step 3 is transferred in reactor, sealed, be then placed in reactor, reacted at 180 DEG C
12 hours, it is subsequently cooled to room temperature.
5. by the powder prepared by step 4, centrifugation, washing, drying.
Nanometer WO obtained by embodiment 13SEM pictures as shown in figure 1, nano particle is ellipsoidal structure, and surface
There are abundant fine defects.
Nanometer WO obtained by embodiment 13Dispersion is applied on six pin earthenware air-sensitive testing elements, is surveyed using gas sensor
Test system tests the response to acetone gas, and test temperature is 180 DEG C, and its dynamic response curve is as shown in Figure 2.As can be seen that
There is obvious response to below 1ppm.
Embodiment 2
The present embodiment is with the difference of embodiment 1：Absolute ethyl alcohol temperature is 10 DEG C in step 1- steps 3.
Embodiment 3
The present embodiment is with the difference of embodiment 1：Absolute ethyl alcohol temperature is 10 DEG C in step 1- steps 3, in step 4,
Reaction time is 6 hours.
The above-mentioned description to embodiment is to be understood that and apply this hair for ease of those skilled in the art
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiments without by performing creative labour.Therefore, the invention is not restricted to implementation here
Example, those skilled in the art's announcement of the invention, the improvement made for the present invention and modification all should be of the invention
Within protection domain.
Claims (7)
1. a kind of preparation method of multilist planar defect tungsten oxide nanometer gas sensitive, it is characterised in that comprise the following steps：
（1）2g tungsten hexachlorides are dissolved in the low-temperature anhydrous ethanol of 100ml, magnetic agitation is slow added into afterwards to whole dissolvings
10ml deionized waters, stir 30 minutes at low ambient temperatures, then 50 DEG C of stirred in water bath 24 hours again；
（2）By step（1）The solution cools down low temperature；
（3）1g tungsten hexachlorides are dissolved in the low-temperature anhydrous ethanol of 10ml, magnetic agitation is subsequently poured into step to whole dissolvings（2）
In the solution；
（4）By step（3）The solution of middle preparation is transferred in reactor, sealing, is then placed in reactor, anti-at 180 DEG C
Should, 6-12 hours, it is subsequently cooled to room temperature;
（5）By step（4）Prepared powder, centrifugation, washing, drying.
2. a kind of preparation method of multilist planar defect tungsten oxide nanometer gas sensitive according to claim 1, it is characterised in that
Step（1）Described in low-temperature anhydrous ethanol, its temperature be 0-20 DEG C.
3. a kind of preparation method of multilist planar defect tungsten oxide nanometer gas sensitive according to claim 1, it is characterised in that
Step（1）Described in low temperature environment, its temperature be 0-20 DEG C.
4. a kind of preparation method of multilist planar defect tungsten oxide nanometer gas sensitive according to claim 1, it is characterised in that
Step（2）Described in low temperature, its temperature be 0-20 DEG C.
5. a kind of preparation method of multilist planar defect tungsten oxide nanometer gas sensitive according to claim 1, it is characterised in that
Step（3）Described in low-temperature anhydrous ethanol, its temperature be 0-20 DEG C.
6. a kind of multilist planar defect tungsten oxide nanometer gas sensitive, it is characterised in that according to any methods describeds of claim 1-5
Prepare.
7. the application that multilist planar defect tungsten oxide nanometer gas sensitive is detected in acetone gas according to claim 6.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611064816.6A CN106745273B (en) | 2016-11-22 | 2016-11-22 | A kind of multilist planar defect tungsten oxide nanometer gas sensitive and preparation and application |
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| CN201611064816.6A CN106745273B (en) | 2016-11-22 | 2016-11-22 | A kind of multilist planar defect tungsten oxide nanometer gas sensitive and preparation and application |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046328A (en) * | 2017-11-20 | 2018-05-18 | 湖北大学 | A kind of defect state tungsten oxide nanoparticles photothermal conversion materiat and its preparation method and application |
| CN108760833A (en) * | 2018-05-23 | 2018-11-06 | 上海理工大学 | It is a kind of to be used to detect sensitive material of acetone gas and preparation method thereof |
| CN112812375A (en) * | 2020-12-31 | 2021-05-18 | 宁波能之光新材料科技股份有限公司 | Preparation method of high-dispersion-stability photo-thermal conversion functional nano material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539205A (en) * | 2013-11-15 | 2014-01-29 | 哈尔滨工业大学 | Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles |
| CN105668637A (en) * | 2016-01-05 | 2016-06-15 | 天津大学 | Preparation method of tungsten oxide nanorod bundle structure gas-sensitive material |
-
2016
- 2016-11-22 CN CN201611064816.6A patent/CN106745273B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539205A (en) * | 2013-11-15 | 2014-01-29 | 哈尔滨工业大学 | Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles |
| CN105668637A (en) * | 2016-01-05 | 2016-06-15 | 天津大学 | Preparation method of tungsten oxide nanorod bundle structure gas-sensitive material |
Non-Patent Citations (3)
| Title |
|---|
| HONG GOO CHOI ET AL.: "Solvothermal Synthesis of Tungsten Oxide Nanorod/Nanowire/Nanosheet", 《HONG GOO CHOI ET AL.》 * |
| SHIBIN SUN ET AL.: "Solvothermal synthesis of tungsten oxide mesocrystals and their electrochromic performance", 《MATERIALSLETTERS》 * |
| SIAN-JHANG HONG ET AL.: "Synthesis of Tungsten Trioxide Nanowires by a Solvothermal Process", 《JOURNAL OF ENGINEERING TECHNOLOGY AND EDUCATION》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046328A (en) * | 2017-11-20 | 2018-05-18 | 湖北大学 | A kind of defect state tungsten oxide nanoparticles photothermal conversion materiat and its preparation method and application |
| CN108760833A (en) * | 2018-05-23 | 2018-11-06 | 上海理工大学 | It is a kind of to be used to detect sensitive material of acetone gas and preparation method thereof |
| CN108760833B (en) * | 2018-05-23 | 2020-10-09 | 上海理工大学 | Sensitive material for detecting acetone gas and preparation method thereof |
| CN112812375A (en) * | 2020-12-31 | 2021-05-18 | 宁波能之光新材料科技股份有限公司 | Preparation method of high-dispersion-stability photo-thermal conversion functional nano material |
| CN112812375B (en) * | 2020-12-31 | 2022-03-25 | 宁波能之光新材料科技股份有限公司 | Preparation method of high-dispersion-stability photo-thermal conversion functional nano material |
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