CN105486721A - Method for preparing nitrogen oxide sensor element based on tungsten oxide nanometer blocks - Google Patents
Method for preparing nitrogen oxide sensor element based on tungsten oxide nanometer blocks Download PDFInfo
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- CN105486721A CN105486721A CN201610010996.3A CN201610010996A CN105486721A CN 105486721 A CN105486721 A CN 105486721A CN 201610010996 A CN201610010996 A CN 201610010996A CN 105486721 A CN105486721 A CN 105486721A
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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 37
- 229910001930 tungsten oxide Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 5
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims abstract 15
- 239000007789 gas Substances 0.000 claims abstract description 56
- 239000000758 substrate Substances 0.000 claims abstract description 31
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000000919 ceramic Substances 0.000 claims abstract 7
- 238000004729 solvothermal method Methods 0.000 claims abstract 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 21
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- 229910052697 platinum Inorganic materials 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 238000004544 sputter deposition Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- -1 polytetrafluoroethylene Polymers 0.000 claims 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims 1
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 239000013077 target material Substances 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 11
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 abstract description 8
- 239000011540 sensing material Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000010218 electron microscopic analysis Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
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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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
本发明公开了一种基于氧化钨纳米块的氮氧化物传感器元件的制备方法，具有以下步骤：(1)陶瓷片基底的清洗；(2)制备Pt的叉指电极；(3)制备反应溶液；(4)制备气敏传感器；(5)清洗反应后氧化铝基底；(6)气敏传感器元件的热处理。本发明采用溶剂热法在陶瓷片基底上制备了三氧化钨纳米块结构，其具有巨大的比表面积和较大的表面活性，并将该纳米块结构应用于气敏传感器领域，结果表明：该三氧化钨纳米块气敏材料能在低温(～100℃)条件下有效检测氮氧化物，并具有很高的气敏性、优良的重复性和很好的稳定性。
The invention discloses a method for preparing a nitrogen oxide sensor element based on tungsten oxide nanoblocks, which comprises the following steps: (1) cleaning the ceramic substrate; (2) preparing Pt interdigitated electrodes; (3) preparing a reaction solution ; (4) Prepare the gas sensor; (5) Clean the alumina substrate after the reaction; (6) Heat treatment of the gas sensor element. In the present invention, a tungsten trioxide nano-block structure is prepared on a ceramic sheet substrate by a solvothermal method, which has a huge specific surface area and a large surface activity, and the nano-block structure is applied to the field of gas sensor. The results show that: the The tungsten trioxide nanoblock gas-sensing material can effectively detect nitrogen oxides at low temperature (~100°C), and has high gas sensitivity, excellent repeatability and good stability.
Description
Technical field
The present invention relates to gas sensor technology field, particularly a kind of preparation method of the NOx sensor element based on tungsten oxide nanometer block.
Background technology
Oxides of nitrogen (NO
x) be a kind ofly cause the environmental problem such as acid rain and photo-chemical smog and the mankind formed to the toxic and harmful of grave danger.High performance gas sensitive and the device of studying the accurate examination and controlling being used for oxides of nitrogen are vital to human health.Tungsten oxide is a kind of N-type semiconductor material of broad stopband, and it has a wide range of applications in gas sensor field.As the high performance gas sensitive of one, tungsten oxide can be widely used in various toxic and harmful as NO
x, SO
2, NH
3deng detection.But, WO
3the shortcoming of gas sensitive working temperature high (about 250 DEG C) brings complicacy and instability to sensor-based system is integrated.For this reason, scientific and technical personnel are devoted to the research of the gas sensor for low-temperature working always.And tungsten oxide nanometer block has larger specific surface area and stronger gas sorption ability, thus effectively reduce working temperature while the sensitivity of gas sensor being improved further.
Summary of the invention
In order to solve problems of the prior art, the invention provides a kind of preparation method of the NOx sensor element based on tungsten oxide nanometer block, overcoming the problem that the working temperature of tungsten oxide gas sensor existence in prior art is higher.
Technical scheme of the present invention is: a kind of preparation method of the NOx sensor element based on tungsten oxide nanometer block, has following steps:
(1) cleaning of potsherd substrate
Adopt potsherd as substrate, potsherd substrate is put into successively acetone solvent, absolute ethyl alcohol sonic oscillation 15-20min, removing surface organic matter impurity.Subsequently deionized water is put in potsherd substrate to clean, after having rinsed, put into absolute ethyl alcohol, and be placed in IR bake and dry;
(2) interdigital electrode of Pt is prepared
Potsherd substrate is placed in the vacuum chamber of DPS-III type high vacuum facing-target magnetron sputtering system equipment, adopt the metal platinum of quality purity 99.99% as target, using the argon gas of quality purity 99.999% as working gas, sputtering operating pressure is 2.0Pa, sputtering power 80-90W, sputtering time 8-10min, base reservoir temperature is room temperature, forms interdigital platinum electrode at alumina base basal surface;
(3) preparation feedback solution
First configure the tungsten hexachloride solution of 0.025M-0.1M, be dissolved in by tungsten hexachloride in 65ml deionized water, magnetic agitation, to all dissolving, forms the tungsten hexachloride solution of white;
(4) gas sensor is prepared
The alumina substrate being coated with platinum electrode in step (2) is placed in the stainless steel hydrothermal reaction kettle that liner is teflon, tungsten hexachloride solution prepared by step (3) is also transferred in reactor simultaneously, sealing, then reactor is placed in thermostatic drying chamber, at alumina base basal surface synthesis tungsten oxide nanometer block structure at temperature of reaction 200 DEG C, reaction time is 6-9h, after completion of the reaction, reactor is naturally cooled to room temperature;
(5) cleaning reaction rear oxidation aluminium substrate
By the alumina substrate after solvent thermal reaction in step (4), repeatedly through deionized water and soaked in absolute ethyl alcohol cleaning, then dry 8-10h in the vacuum drying chamber of 60-80 DEG C;
(6) thermal treatment of gas sensor element
Tungsten oxide nanometer block structure gas sensor element prepared by step (5) is placed in muffle furnace heat-treat, heat treatment temperature is 300-400 DEG C, temperature retention time is 2h, and heating rate is 2-5 DEG C/min, in order to increase the crystallinity of tungsten oxide nanometer block.
Beneficial effect of the present invention is: the present invention adopts solvent-thermal method to prepare tungsten trioxide nano block structure in potsherd substrate, it has huge specific surface area and larger surfactivity, and this nanometer blocks structure is applied to gas sensor field, result shows: this tungsten trioxide nano block gas sensitive effectively can detect oxides of nitrogen under low temperature (~ 100 DEG C) condition, to oxides of nitrogen gas extremely low concentration detection (0.1ppm can be reached), and there is very high gas sensing property, excellent repeatability and good stability.And emphasis have studied the impact of solvent thermal reaction time on gas sensor element air-sensitive performance.The method has that equipment is simple, easy to operate, favorable repeatability, the advantage such as with low cost, has important practice and Research Significance.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the tungsten oxide nanometer block prepared by embodiment 1, and scale is 100nm;
Fig. 2 is the XRD collection of illustrative plates of the tungsten oxide nanometer block prepared by embodiment 1;
Fig. 3 be tungsten oxide nanometer block structure gas sensor element prepared by embodiment 1 at different operating temperature to 1ppmNO
2the corresponding relation figure of gas;
Fig. 4 be tungsten oxide nanometer block structure gas sensor element prepared by embodiment 1 under 100 DEG C of conditions to 1ppmNO
2the dynamic response curve of gas;
Fig. 5 is the sensitivity under 100 DEG C of conditions of tungsten oxide nanometer block structure gas sensor element prepared by embodiment 1 and NO
2the corresponding relation figure of gas concentration;
Fig. 6 is that tungsten oxide nanometer block structure gas sensor element prepared by embodiment 1 is to the selectivity schematic diagram of multiple gases.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is elaborated.
The present invention is raw materials used all adopts commercially available chemically pure reagent.
Embodiment 1
(1) cleaning of potsherd substrate:
Adopt potsherd (1cm × 2cm) as substrate, potsherd substrate is put into successively acetone solvent, absolute ethyl alcohol sonic oscillation 15min, removing surface organic matter impurity.And be placed in IR bake and dry stand-by.
(2) interdigital electrode of Pt is prepared:
Potsherd substrate is placed in the vacuum chamber of DPS-III type high vacuum facing-target magnetron sputtering system equipment, adopt the metal platinum of quality purity 99.99% as target, using the argon gas of quality purity 99.999% as working gas, sputtering operating pressure is 2.0Pa, sputtering power 85W, sputtering time 10min, base reservoir temperature is room temperature, forms interdigital platinum electrode at alumina base basal surface.
(3) preparation feedback solution:
First configure the tungsten hexachloride solution of 0.05M, take 1.19g tungsten hexachloride and be dissolved in 65ml deionized water, magnetic agitation, to all dissolving, forms the tungsten hexachloride solution of white.
(4) gas sensor is prepared:
The alumina substrate being coated with platinum electrode in step (2) is placed in the polytetrafluoroethyllining lining of 100ml hydrothermal reaction kettle, tungsten hexachloride solution prepared by step (3) is also transferred in reactor simultaneously, sealing, then reactor is placed in thermostatic drying chamber, at alumina base basal surface synthesis tungsten oxide nanometer block structure at temperature of reaction 200 DEG C, reaction time is 7h, after completion of the reaction, reactor is naturally cooled to room temperature;
(5) cleaning reaction rear oxidation aluminium substrate:
By the alumina substrate after solvent thermal reaction in step (4), repeatedly through deionized water and soaked in absolute ethyl alcohol cleaning, then dry 9h in the vacuum drying chamber of 80 DEG C.
The electron microscopic analysis result of the surface topography of the tungsten oxide nanometer block prepared by embodiment 1 as shown in Figure 1.The nanometer blocks of square and rectangular parallelepiped can be formed on alumina substrates.
(6) thermal treatment of gas sensor element:
Tungsten oxide nanometer block structure gas sensor element prepared by step (5) is placed in muffle furnace heat-treat, heat treatment temperature is 350 DEG C, and temperature retention time is 2h, and heating rate is 2.5 DEG C/min.
The X-ray diffraction analysis result of the tungsten oxide nanometer block prepared by embodiment 1 as shown in Figure 2.The crystalline phase of XRD spectra display tungsten oxide nanometer block is the WO that monoclinic phase mixes mutually with six sides
3, and there is good crystallinity.
The obtained tungsten oxide nanometer block structure gas sensor element of embodiment 1 at different operating temperature to 1ppmNO
2the corresponding relation figure of gas as shown in Figure 3, can find out that the optimum working temperature of tungsten oxide nanometer block structure sensor is 100 DEG C.Its sensitivity at 100 DEG C and 1ppmNO
2the dynamic response figure of gas concentration as shown in Figure 4.
The sensitivity of the obtained tungsten oxide nanometer block structure gas sensor element of embodiment 1 at 100 DEG C and NO
2the corresponding relation schematic diagram of gas concentration as shown in Figure 5, wherein to 0.1,0.5,1,2,3ppmNO
2the sensitivity of gas is respectively 3.24,11.78,33.84,41.11 and 49.39.
Tungsten oxide nanometer block structure gas sensor element obtained by embodiment 1 is respectively 2.22,1.85,1.55,1.33,1.19,1.15 to the sensitivity of 100ppm ammonia, ethanol, isopropyl alcohol, methyl alcohol, acetone steam at 100 DEG C, and to 1ppmNO
2the sensitivity of gas is 33.84, as shown in Figure 6.This shows that this tungsten oxide nanometer block structure gas sensor element is to NO
2gas has excellent selectivity.
Embodiment 2
The difference of the present embodiment and embodiment 1 is: in the solvent thermal reaction liquid configured in step (3), the concentration of tungsten hexachloride is 0.025M, obtained tungsten oxide nanometer block structure gas sensor element at 100 DEG C to lppmNO
2the sensitivity of gas is 9.72.
Embodiment 3
The difference of the present embodiment and embodiment 1 is: in the solvent thermal reaction liquid configured in step (3), the concentration of tungsten hexachloride is 0.075M, obtained tungsten oxide nanometer block structure gas sensor element at 100 DEG C to lppmNO
2the sensitivity of gas is 18.34.
Embodiment 4
The difference of the present embodiment and embodiment 1 is: in the solvent thermal reaction liquid configured in step (3), the concentration of tungsten hexachloride is 0.1M, obtained tungsten oxide nanometer block structure gas sensor element at 100 DEG C to lppmNO
2the sensitivity of gas is 14.87.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (2)
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757095A (en) * | 2011-04-29 | 2012-10-31 | 北京化工大学 | Tungsten oxide nanoflake self-assembly nanosphere and application method and application of tungsten oxide nanoflake self-assembly nanosphere |
| CN103245699A (en) * | 2013-05-11 | 2013-08-14 | 天津大学 | Preparation method of gas sensitive element capable of detecting nitric oxides at room temperature |
| CN103267779A (en) * | 2013-05-08 | 2013-08-28 | 天津大学 | Preparation method of ethanol gas sensor element based on vanadium pentoxide multilevel nano-network structure |
| CN103852496A (en) * | 2014-03-07 | 2014-06-11 | 天津大学 | Preparation method of gas sensor element based on quasi-directed tungsten oxide nanowires |
-
2016
- 2016-01-05 CN CN201610010996.3A patent/CN105486721A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757095A (en) * | 2011-04-29 | 2012-10-31 | 北京化工大学 | Tungsten oxide nanoflake self-assembly nanosphere and application method and application of tungsten oxide nanoflake self-assembly nanosphere |
| CN103267779A (en) * | 2013-05-08 | 2013-08-28 | 天津大学 | Preparation method of ethanol gas sensor element based on vanadium pentoxide multilevel nano-network structure |
| CN103245699A (en) * | 2013-05-11 | 2013-08-14 | 天津大学 | Preparation method of gas sensitive element capable of detecting nitric oxides at room temperature |
| CN103852496A (en) * | 2014-03-07 | 2014-06-11 | 天津大学 | Preparation method of gas sensor element based on quasi-directed tungsten oxide nanowires |
Non-Patent Citations (1)
| Title |
|---|
| HONG GOO CHOI 等: "Solvothermal Synthesis of Tungsten Oxide Nanorod/Nanowire/Nanosheet", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
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Application publication date: 20160413 |