CN105699440A - Method for preparing tungsten oxide nanoflower hydrogen sensor - Google Patents
Method for preparing tungsten oxide nanoflower hydrogen sensor Download PDFInfo
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- CN105699440A CN105699440A CN201610118627.6A CN201610118627A CN105699440A CN 105699440 A CN105699440 A CN 105699440A CN 201610118627 A CN201610118627 A CN 201610118627A CN 105699440 A CN105699440 A CN 105699440A
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- Prior art keywords
- tungsten oxide
- hydrogen gas
- gas sensor
- oxide nanometer
- flower
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- 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 60
- 229910001930 tungsten oxide Inorganic materials 0.000 title claims abstract description 60
- 239000001257 hydrogen Substances 0.000 title abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 title abstract description 18
- 239000002057 nanoflower Substances 0.000 title abstract description 9
- 238000000034 method Methods 0.000 title abstract description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title abstract 7
- 239000000758 substrate Substances 0.000 claims abstract description 29
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000010970 precious metal Substances 0.000 claims abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 53
- 238000002360 preparation method Methods 0.000 claims description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910000510 noble metal Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical group O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 11
- 239000002070 nanowire Substances 0.000 abstract description 5
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 238000000137 annealing Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 241000549556 Nanos Species 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- -1 piezoid or potsherd Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention provides a method for preparing a tungsten oxide nanoflower hydrogen sensor. The method comprises the following steps that firstly, tungsten oxide nanowires grow on a substrate, and tungsten powder is attached to the surfaces of the tungsten oxide nanowires; secondly, the tungsten powder on the substrate grows into a tungsten oxide nanoflower structural body; thirdly, after the substrate is heated and annealed, the tungsten oxide nanoflower structural body is doped with precious metal to obtain a hydrogen sensor sensitive material; fourthly, electrodes are prepared at the two ends of the hydrogen sensor sensitive material, and then wire leading packaging is conducted to obtain the tungsten oxide nanoflower hydrogen sensor. According to the method for preparing the tungsten oxide nanoflower hydrogen sensor, due to the fact that the tungsten oxide nanoflower structural body which is stable in structure and high in specific area grows on the substrate, the hydrogen sensor which is stable in electrical data and high in responding sensitivity at the room temperature is prepared; the preparing method is simple, and cost is low.
Description
Technical field
The invention belongs to sensor field, particularly to the preparation method of a kind of tungsten oxide nanometer flower hydrogen gas sensor。
Background technology
In the industrial production, hydrogen is of great interest as a kind of pollution-free green energy resource。But, hydrogen has the characteristics such as volatile, burning-point is low, colorless and odorless, and aerial concentration is very easily burnt or explodes when running into naked light when being 4-75%, is a kind of breakneck fuel gas。Therefore to the monitoring technology of hydrogen and research, in ensureing personal safety as well as the property safety, vital effect is played。
At present, resistive memory hydrogen gas sensor is mainly using metal-oxides such as SnO2, ZnO, TiO2, WO3 as sensitive material。Metal oxide semiconductor hydrogen gas sensor obtains the concentration of hydrogen by detecting the change of the resistance value of sensitive material, and it is with low cost, obtains socially and promotes widely。But the specific surface area of this hydrogen gas sensor sensitive material is generally relatively low, the response sensitivity of reducibility gas is relatively low, generally require higher operating temperature and can be only achieved higher response sensitivity, therefore there is also the hidden danger causing combustion of hydrogen or blast。Although part researcher is in order to improve the specific surface area of sensitive material, prepare the sensitive material with nanostructureds such as nano wire, nanometer sheet, nanotrees, but due to the reasons such as pattern is unstable, loosely organized produced, cause that its prepared sensor yield rate is low, bigger by the impact of external force of environment。
It addition, namely some metal film types resistance-type hydrogen gas sensors have higher response sensitivity under relatively low operating temperature, but because of its high cost and complicated preparation technology, the hydrogen gas sensor of low-temperature high-sensitivity is made to be difficult to promote。
Summary of the invention
The present invention solves the deficiencies in the prior art, the preparation method providing a kind of tungsten oxide nanometer flower hydrogen gas sensor, its sensitive material of hydrogen gas sensor prepared has nanostructured that pattern determines, specific surface area is bigger, with low cost, hydrogen can have higher response sensitivity at a lower temperature。
The purpose of the present invention is achieved through the following technical solutions:
The preparation method of a kind of tungsten oxide nanometer flower hydrogen gas sensor, comprises the following steps:
(1) go out tungsten oxide nano at Grown, and tungsten powder attaches in its surface；
(2) tungsten powder on substrate is grown to tungsten oxide nanometer floral structure body；
(3) after silicon being annealed, doped precious metal on tungsten oxide nanometer floral structure body, obtain hydrogen gas sensor sensitive material；
(4) prepare electrode then lead packages at hydrogen gas sensor sensitive material two ends, obtain tungsten oxide nanometer flower hydrogen gas sensor。
Further, step (1) comprises the following steps:
(1a) tungsten powder is layered on heating unit surface；
(1b) substrate is tipped upside down on tungsten powder surface；
(1c) heat in aerobic environment and be incubated, making Grown go out tungsten oxide nano, and tungsten powder attaches in its surface。
Preferably, further comprising the steps of before step (1a): first by the substrate cleanout fluid ultrasonic waves for cleaning of well cutting and dry。
Further, step (2) comprises the following steps:
(2a) by substrate face upward, it is placed in the environment of aerobic；
(2b) by silicon and be incubated, tungsten powder is made to be grown to tungsten oxide nanometer floral structure body。
Preferably, step (2b) is that 2.5sccm, argon flow amount heat when being 200sccm and be incubated substrate at the vacuum of 5Pa, oxygen flow。
Preferably, the noble metal described in step (3) is any one in platinum, gold, palladium, nickel, silver。
Compared to prior art, the preparation method of the tungsten oxide nanometer provided by the invention flower hydrogen gas sensor tungsten oxide nanometer floral structure body by going out Stability Analysis of Structures at Grown, specific surface area is higher, prepare that electrical data is stable, response sensitivity is high under room temperature hydrogen gas sensor, and its preparation method is simple, with low cost。
The present invention also provides for a kind of tungsten oxide nanometer flower hydrogen gas sensor prepared according to above-mentioned preparation method。Compared to prior art, tungsten oxide nanometer of the present invention flower hydrogen gas sensor electrical data is stable, response sensitivity is high under room temperature, and its preparation method is simple, with low cost。
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the preparation method of oxidate nano of the present invention flower hydrogen gas sensor；
Fig. 2 is the SEM figure that grown tungsten oxide nano back substrate cross section；
Fig. 3 is the SEM figure that grown the substrate cross-section after tungsten oxide nanometer is spent；
Fig. 4 is the TEM figure of tungsten oxide nanometer flower before annealing；
Fig. 5 is the XRD spectra of tungsten oxide nanometer flower before annealing；
Fig. 6 is the Raman spectrogram of annealing rear oxidation tungsten nano flower；
The characteristic curve that when Fig. 7 is 25 DEG C, the resistance change rate of hydrogen gas sensor changes with density of hydrogen。
Detailed description of the invention
Referring to Fig. 1, it is the schematic flow sheet that oxidate nano of the present invention spends the preparation method of hydrogen gas sensor；The preparation method of the tungsten oxide nanometer flower hydrogen gas sensor of the present invention, comprises the following steps:
(1) grow tungsten oxide nano 21 over the substrate 10, and tungsten powder 20 attaches in its surface；Specifically, this step includes three below step:
(1a) tungsten powder 20 is layered on heating unit surface；
(1b) substrate 10 is tipped upside down on tungsten powder 20 surface, as shown in Fig. 1 (a)；Described substrate 10 can be selected for the high-temperature insulation material such as piezoid or potsherd, and substrate first cuts into before preparation certain size (such as 3mm × 15mm), then with the cleanout fluid such as ethanol and deionized water successively ultrasonic cleaning each 10 minutes, then dry；
(1c) heat in aerobic environment and be incubated, making substrate 10 grows tungsten oxide nano 21, and tungsten powder 20 attaches in its surface, as shown in Fig. 1 (b)；
(2) tungsten powder 20 on substrate 10 is grown to tungsten oxide nanometer floral structure body 22, as shown in Fig. 1 (c)；Specifically, this step has included two steps following:
(2a) substrate 10 is faced up, be placed in the environment of aerobic；
(2b) it is that 2.5sccm, argon flow amount heat when being 200sccm and be incubated by substrate 10 at the vacuum of 5Pa, oxygen flow, makes tungsten powder be grown to tungsten oxide nanometer floral structure body 22；
(3) silicon is annealed, as shown in Fig. 1 (d)；Then doped precious metal 30 on tungsten oxide nanometer floral structure body 22, as shown in Fig. 1 (e), obtains hydrogen gas sensor sensitive material；Described noble metal is any one in platinum, gold, palladium, nickel, silver；
(4) prepare electrode 40 then lead packages at hydrogen gas sensor sensitive material two ends, as shown in Fig. 1 (f), obtain tungsten oxide nanometer flower hydrogen gas sensor。
Referring to Fig. 2, it is the SEM figure that grown tungsten oxide nano back substrate cross section；It can be seen that define the nano wire layer of densification between substrate and tungsten powder, become the adhesive band between substrate and tungsten powder, solve lattice between tungsten powder and substrate and do not mate the problem that the gas sensitive layer adhesion caused is poor。
Referring to Fig. 3, it is the SEM figure that grown the substrate cross-section after tungsten oxide nanometer is spent；It can be seen that spending for tungsten oxide nanometer on nano wire upper strata, described tungsten oxide nanometer flower refers to the radial structure grown by many tungsten oxide nanos round tungsten powder, and its structure has bigger specific surface area。
Referring to Fig. 4, it is the TEM figure of tungsten oxide nanometer flower before annealing；It can be seen that the structure of tungsten oxide nanometer flower is radial structure, its diameter is about 2 μm。
Referring to Fig. 5, it is the XRD spectra of tungsten oxide nanometer flower before annealing；It can be seen that the diffraction maximum of 23.5 ° is corresponding to the W18O49 structure of monocline γ phase, it does not have other dephasign peaks, there is higher degree of crystallinity。
Measure the component of the sample after annealing with Raman spectrometer, the exciting light of test adopts wavelength to be the laser of 488nm。Referring to Fig. 6, it is the Raman spectrogram of annealing rear oxidation tungsten nano flower；Four peaks in spectrogram are positioned at 135cm-1、275cm-1、724cm-1、813cm-1, it is WO3Characteristic peak, further illustrating the sample after annealing is WO3, it does not have other dephasigns。
The tungsten oxide nanometer flower hydrogen gas sensor adopting above-mentioned preparation method to be prepared from is carried out performance test, obtains the characteristic curve that during 25 DEG C as shown in Figure 7, the resistance change rate of hydrogen gas sensor changes with density of hydrogen。It can be seen that when 25 DEG C, along with the increase of density of hydrogen, the resistance change rate of device is gradually increased, its density of hydrogen and resistance change rate are linear, and its hydrogen measurement sensitivity can reach 50ppm, and still do not have common sensor saturation limit when 10000ppm。
Compared to prior art, the preparation method of the tungsten oxide nanometer provided by the invention flower hydrogen gas sensor tungsten oxide nanometer floral structure body by going out Stability Analysis of Structures at Grown, specific surface area is higher, prepare that electrical data is stable, response sensitivity is high under room temperature hydrogen gas sensor, and its preparation method is simple, with low cost。The method can be easily applicable in industrialized production and the related industry of the hydrogen gas sensor of low cost high technology。
The present invention also provides for a kind of tungsten oxide nanometer flower hydrogen gas sensor prepared according to above-mentioned preparation method。Compared to prior art, the sensitive material of tungsten oxide nanometer of the present invention flower hydrogen gas sensor has the nanostructured that pattern is determined, its specific surface area is big, degree of crystallinity is high, sensitivity is higher；Described tungsten oxide nanometer flower hydrogen gas sensor electrical data is stable, response sensitivity is high under room temperature, and its preparation method is simple, with low cost。
The invention is not limited in above-mentioned embodiment, if to the various changes of the present invention or deformation without departing from the spirit and scope of the present invention, if these are changed and deform within the claim and the equivalent technologies scope that belong to the present invention, then the present invention is also intended to comprise these changes and deformation。
Claims (7)
1. the preparation method of a tungsten oxide nanometer flower hydrogen gas sensor, it is characterised in that comprise the following steps:
(1) go out tungsten oxide nano at Grown, and tungsten powder attaches in its surface；
(2) tungsten powder on substrate is grown to tungsten oxide nanometer floral structure body；
(3) after silicon being annealed, doped precious metal on tungsten oxide nanometer floral structure body, obtain hydrogen gas sensor sensitive material；
(4) prepare electrode then lead packages at hydrogen gas sensor sensitive material two ends, obtain tungsten oxide nanometer flower hydrogen gas sensor。
2. the preparation method of tungsten oxide nanometer according to claim 1 flower hydrogen gas sensor, it is characterised in that: step (1) comprises the following steps:
(1a) tungsten powder is layered on heating unit surface；
(1b) substrate is tipped upside down on tungsten powder surface；
(1c) heat in aerobic environment and be incubated, making Grown go out tungsten oxide nano, and tungsten powder attaches in its surface。
3. the preparation method of tungsten oxide nanometer according to claim 2 flower hydrogen gas sensor, it is characterised in that: further comprising the steps of before step (1a): first by the substrate cleanout fluid ultrasonic waves for cleaning of well cutting and dry。
4. the preparation method of tungsten oxide nanometer according to claim 1 flower hydrogen gas sensor, it is characterised in that: step (2) comprises the following steps:
(2a) by substrate face upward, it is placed in the environment of aerobic；
(2b) by silicon and be incubated, tungsten powder is made to be grown to tungsten oxide nanometer floral structure body。
5. the preparation method of tungsten oxide nanometer according to claim 4 flower hydrogen gas sensor, it is characterised in that: step (2b) is that 2.5sccm, argon flow amount heat when being 200sccm and be incubated substrate at the vacuum of 5Pa, oxygen flow。
6. the preparation method of tungsten oxide nanometer according to any one of claim 1 to 5 flower hydrogen gas sensor, it is characterised in that: the noble metal described in step (3) is any one in platinum, gold, palladium, nickel, silver。
7. a tungsten oxide nanometer flower hydrogen gas sensor, it is characterised in that: the preparation method of the tungsten oxide nanometer flower hydrogen gas sensor according to any one of claim 1-6 is prepared from。
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Cited By (5)
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| CN106430087A (en) * | 2016-11-03 | 2017-02-22 | 中国检验检疫科学研究院 | Synthesis method of precious metal loaded tungsten oxide nanowires for gas sensor |
| CN107626300A (en) * | 2017-09-30 | 2018-01-26 | 五邑大学 | A kind of thermal drivers catalyst and its application |
| CN108333227A (en) * | 2018-01-12 | 2018-07-27 | 五邑大学 | A kind of flexible gas sensor and preparation method thereof |
| WO2019061584A1 (en) * | 2017-09-30 | 2019-04-04 | 五邑大学 | Metal tungsten quantum dot preparation method |
| CN111474214A (en) * | 2020-04-29 | 2020-07-31 | 青岛菲灿新材料科技服务有限责任公司 | Graphene-based high-sensitivity hydrogen sensor and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106430087A (en) * | 2016-11-03 | 2017-02-22 | 中国检验检疫科学研究院 | Synthesis method of precious metal loaded tungsten oxide nanowires for gas sensor |
| CN107626300A (en) * | 2017-09-30 | 2018-01-26 | 五邑大学 | A kind of thermal drivers catalyst and its application |
| WO2019061584A1 (en) * | 2017-09-30 | 2019-04-04 | 五邑大学 | Metal tungsten quantum dot preparation method |
| CN107626300B (en) * | 2017-09-30 | 2021-01-26 | 五邑大学 | Thermally driven catalyst and application thereof |
| CN108333227A (en) * | 2018-01-12 | 2018-07-27 | 五邑大学 | A kind of flexible gas sensor and preparation method thereof |
| CN111474214A (en) * | 2020-04-29 | 2020-07-31 | 青岛菲灿新材料科技服务有限责任公司 | Graphene-based high-sensitivity hydrogen sensor and preparation method thereof |
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| CN105699440B (en) | 2018-08-07 |
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