CN103626233A - Tungsten trioxide nanosheet and tungsten trioxide nanosheet-doped gas sensor - Google Patents
Tungsten trioxide nanosheet and tungsten trioxide nanosheet-doped gas sensor Download PDFInfo
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- CN103626233A CN103626233A CN201310626670.XA CN201310626670A CN103626233A CN 103626233 A CN103626233 A CN 103626233A CN 201310626670 A CN201310626670 A CN 201310626670A CN 103626233 A CN103626233 A CN 103626233A
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- trioxide nano
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- tungstic
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- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000002135 nanosheet Substances 0.000 title abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 45
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 6
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- 230000002687 intercalation Effects 0.000 claims abstract description 4
- 238000009830 intercalation Methods 0.000 claims abstract description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 3
- 230000003647 oxidation Effects 0.000 claims abstract description 3
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 3
- 239000002253 acid Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 claims description 10
- 239000010931 gold Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 229910052763 palladium Inorganic materials 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 238000007669 thermal treatment Methods 0.000 claims description 4
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical group CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 230000004044 response Effects 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 7
- -1 alcohol amine Chemical class 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 abstract 5
- 239000002994 raw material Substances 0.000 abstract 2
- 229910009112 xH2O Inorganic materials 0.000 abstract 1
- 230000005059 dormancy Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000007704 wet chemistry method Methods 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention relates to a tungsten trioxide nanosheet and a tungsten trioxide nanosheet-doped gas sensor. The preparation method of the tungsten trioxide nanosheet comprises the following steps: with tungstic acid (WO)3·xH2O) is used as a raw material, tungstic acid and alcohol amine react to obtain a layered compound of alcohol amine intercalation tungstic acid, and tungsten trioxide nano-sheets can be obtained by removing alcohol amine through concentrated nitric acid oxidation and heat treatment. The preparation method is simple and easy to implement, has low requirement on equipment, and realizes the purposes of stable mass production and remarkable reduction of the preparation cost of the tungsten trioxide nano-sheets by taking the tungstic acid with the size of micron or millimeter as a raw material. According to the invention, trace noble metal is doped into the tungsten trioxide nanosheet, so that the gas sensor with the rapid response capability to gases such as hydrogen sulfide is obtained.
Description
Technical field
The present invention relates to the new gas sensor that a kind of novel method that can prepare in batches tungstic trioxide nano-slice and minute amount of noble metal doping tungstic trioxide nano-slice are gas sensitive material, belong to nanoscale science and technology and field of new.
Background technology
Nano material, because having unique physical and chemical performance such as high-specific surface area, quantum size effect, small-size effect and macro quanta tunnel effect, has become one of focus of current research, and has caused various countries scientists' greatly concern.The beginning of this century, western developed country has strengthened the research and development of micro-nano technology to drop in succession, the national sectors such as USDOE, Department of Defense, the Department of Health input in this field in 2012 reaches 1,800,000,000 dollars, China has also set up a plurality of research in nanotechnologys center, and in fields such as catalysis, gas sensings, has obtained some achievements significantly.The preparation method of nano material can be summarized as wet chemistry method, chemical Vapor deposition process, vapor transportation method etc.Wherein, wet chemistry method cost is low and be easy to a large amount of synthesizing, and is one of at present conventional important channel.It is reported, with H
2w
2o
7for presoma, adopt wet chemistry method can prepare tungstic oxide nano-sheets, but H
2w
2o
7cost is high, synthetic difficult, has seriously hindered the preparation of tungstic trioxide nano-slice.The present invention be take wolframic acid cheap and easy to get as starting material, can meet the requirement of in batches synthetic tungstic trioxide nano-slice, and the tungstic trioxide nano-slice of minute amount of noble metal doping simultaneously has capability of fast response to gases such as hydrogen sulfide, is good gas sensitive material.
Summary of the invention
The invention provides the new gas sensor that a kind of novel method that can prepare in batches two-dimentional tungstic trioxide nano-slice and minute amount of noble metal doping tungstic trioxide nano-slice are gas sensitive material.
Can be prepared in batches a tungstic trioxide nano-slice, it is characterized in that: with wolframic acid WO
3xH
2o is that starting material are prepared tungstic trioxide nano-slice, described WO
3xH
2x=1 in O or 2, by the alcohol mixeding liquid reaction of wolframic acid and hydramine, obtain the lamellar compound of hydramine intercalation wolframic acid, the mol ratio of described wolframic acid, hydramine, ethanol is 1:(10-40): (20-80), the nitric acid oxidation that is 1-10 M through volumetric molar concentration is removed hydramine and is obtained wolframic acid nanometer sheet, and gained nanometer sheet is warming up to 250-600 ° of C with 1-5 ° of C/min heating rate, after constant temperature 1-5 h, be cooled to room temperature, can obtain tungstic trioxide nano-slice.
The technical scheme that the present invention prepares Au doping tungstic trioxide nano-slice gas sensitive material is: the HAuCl that 120 mg tungstic trioxide nano-slices is placed in to 1 mL 20 mM
43H
2in the O aqueous solution, polyvinylpyrrolidone (the Polyvinylpyrrolidone that adds 2 mg, molecular-weight average 40000), after dispersed, solution is added drop-wise to the gas sensor substrate with having heaters, 80 ° of C thermal treatment 10 min, subsequently temperature is risen to 400-500 ° of C, constant temperature 0.5-2 h, takes out and is cooled to room temperature, is gas sensor.
Described tungstic trioxide nano-slice is monoclinic phase (JCPDS#43-1035).
Described tungstic trioxide nano-slice area is the nm of (80-800) nm * (80-800), and thickness is 5-50 nm.
Described hydramine is α-amino isopropyl alcohol.
Described gold also can be replaced by platinum or palladium.
Described hotchpotch is gold, and gold is 1 %-10 % with the weight ratio of tungstic oxide.
Described hotchpotch is platinum, and the weight ratio of platinum and tungstic oxide is 1 %-10 %.
Described hotchpotch is palladium, and the weight ratio of palladium and tungstic oxide is 1 %-10 %.
Described gas sensitive material is used for surveying hydrogen sulfide, surveys hydrogen or surveys methane.
Preparation process of the present invention is simple, low for equipment requirements, and to take the wolframic acid of micron or mm size be starting material, has realized stable mass production and has significantly reduced the object of tungstic trioxide nano-slice preparation cost.The present invention also mixes tungstic trioxide nano-slice by minute amount of noble metal, obtains the gases such as hydrogen sulfide to have the gas sensor of capability of fast response.
Accompanying drawing explanation
Fig. 1: WO
3h
2o structural representation;
Fig. 2: wolframic acid/organic stratiform structural representation;
Fig. 3: WO
3the stereoscan photograph of nanometer sheet;
Fig. 4: show the 50 ppm gas response curves of " dormancy " phenomenon, dotted line is gas response curve for the first time, solid line is gas response curve for the second time;
Fig. 5: without the 50 ppm gas response curves of " dormancy " phenomenon, dotted line is gas response curve for the first time, solid line is gas response curve for the second time.
Embodiment
Example 1:
After 20 mL α-amino isopropyl alcohols and 40 mL ethanol are fully mixed, add 4 g wolframic acid (H
2wO
4or WO
3h
2o), the laminate structure schematic diagram that Fig. 1 is wolframic acid.At room temperature, after magnetic agitation 120 h, wolframic acid color, by the light yellow creamy white that becomes gradually, through centrifugation, can obtain white solid.Gained sample cleans after twice with ethanol, and the dry gained white powder of room temperature low pressure is wolframic acid/organic intercalation compound, the structural representation that Fig. 2 is this compound.White powder is added in the salpeter solution of 50 mL 5 M, magnetic agitation 12h, after centrifugation ethanol cleans, obtains light yellow wolframic acid (WO
32H
2o) nanometer sheet, inserts this nanometer sheet in alumina crucible subsequently, with 5 ° of C/min speed, is heated to 500 ° of C, constant temperature 2 h in air, and cool to room temperature, can obtain tungstic trioxide nano-slice.The stereoscan photograph of tungstic trioxide nano-slice as shown in Figure 3.
Example 2:
120 mg tungstic trioxide nano-slices are scattered in to the HAuCl of 1 mL 20mM
43H
2in the O aqueous solution, solution is added drop-wise to the gas sensor substrate with having heaters, 80 ° of C thermal treatment 10 min, rise to temperature 400-500 ° of C subsequently, and constant temperature 0.5-2 h takes out cool to room temperature, is gas sensor.
Example 3:
120 mg tungstic trioxide nano-slices are placed in to the HAuCl of 1 mL 20 mM
43H
2in the O aqueous solution, polyvinylpyrrolidone (the Polyvinylpyrrolidone that adds 2 mg, molecular-weight average 40000), after dispersed, solution is added drop-wise to the gas sensor substrate with having heaters, 80 ° of C thermal treatment 10 min, subsequently temperature is risen to 300-500 ° of C, constant temperature 0.5-2 h, takes out cool to room temperature, is gas sensor.In to the sensing testing of 50 ppm hydrogen sulfide, find: traditional solid gas sensor sheet reveals " dormancy " phenomenon, be exposed in clean environment when sensor, after for some time (several hours to some months not etc.), the T to gas for the first time
90(reaching the required time of gas 90% concentration) is obviously longer than for the second time, differs approximately 20 s, as shown in Figure 4, adopts gold doping tungstic trioxide nano-slice gas sensor to show stable response speed, twice T
90be 25 s, do not show " dormancy " phenomenon, as shown in Figure 5.
Claims (10)
1. the tungstic trioxide nano-slice that can prepare in batches, is characterized in that: with wolframic acid WO
3xH
2o is that starting material are prepared tungstic trioxide nano-slice, described WO
3xH
2x=1 in O or 2, by the alcohol mixeding liquid reaction of wolframic acid and hydramine, obtain the lamellar compound of hydramine intercalation wolframic acid, the mol ratio of described wolframic acid, hydramine, ethanol is 1:(10-40): (20-80), the nitric acid oxidation that is 1-10 M through volumetric molar concentration is removed hydramine and is obtained wolframic acid nanometer sheet, and gained nanometer sheet is warming up to 250-600 ° of C with 1-5 ° of C/min heating rate, after constant temperature 1-5 h, be cooled to room temperature, can obtain tungstic trioxide nano-slice.
2. the new gas sensor that minute amount of noble metal doping tungstic trioxide nano-slice claimed in claim 1 is gas sensitive material, is characterized in that: the technical scheme that the present invention prepares Au doping tungstic trioxide nano-slice gas sensitive material is: the HAuCl that 120 mg tungstic trioxide nano-slices is placed in to 1 mL 20 mM
43H
2in the O aqueous solution, polyvinylpyrrolidone (the Polyvinylpyrrolidone that adds 2 mg, molecular-weight average 40000), after dispersed, solution is added drop-wise to the gas sensor substrate with having heaters, 80 ° of C thermal treatment 10 min, subsequently temperature is risen to 400-500 ° of C, constant temperature 0.5-2 h, takes out and is cooled to room temperature, is gas sensor.
3. doping tungstic trioxide nano-slice gas sensor according to claim 1, is characterized in that: described tungstic trioxide nano-slice is monoclinic phase (JCPDS#43-1035).
4. doping tungstic trioxide nano-slice gas sensor according to claim 1, is characterized in that: described tungstic trioxide nano-slice area is the nm of (80-800) nm * (80-800), and thickness is 5-50 nm.
5. doping tungstic trioxide nano-slice gas sensor according to claim 1, is characterized in that: described hydramine is α-amino isopropyl alcohol.
6. doping tungstic trioxide nano-slice gas sensor according to claim 2, is characterized in that: described gold also can be replaced by platinum or palladium.
7. doping tungstic trioxide nano-slice gas sensor according to claim 2, is characterized in that: described hotchpotch is gold, and gold is 1 %-10 % with the weight ratio of tungstic oxide.
8. according to the doping tungstic trioxide nano-slice gas sensor described in claim 2,6, it is characterized in that: described hotchpotch is platinum, the weight ratio of platinum and tungstic oxide is 1 %-10 %.
9. according to the doping tungstic trioxide nano-slice gas sensor described in claim 2,6, it is characterized in that: described hotchpotch is palladium, the weight ratio of palladium and tungstic oxide is 1 %-10 %.
10. doping tungstic trioxide nano-slice gas sensor according to claim 1, is characterized in that: described gas sensitive material is used for surveying hydrogen sulfide, surveys hydrogen or surveys methane.
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| CN105891126A (en) * | 2015-06-30 | 2016-08-24 | 四川智立方博导科技有限责任公司 | Low-cost portable hydrogen optical sensor |
| CN106365204A (en) * | 2016-11-03 | 2017-02-01 | 河北工业大学 | Preparation method of tungsten trioxide sensitive material for ammonia gas sensitive sensor |
| CN107324391A (en) * | 2017-08-16 | 2017-11-07 | 广东工业大学 | A kind of individual layer hydration tungstic trioxide nano-slice and preparation method thereof |
| WO2018091293A1 (en) * | 2016-11-21 | 2018-05-24 | Unilever N.V. | A gas sensor for detecting a gas component |
| CN108195891A (en) * | 2017-11-10 | 2018-06-22 | 中国人民解放军陆军防化学院 | The quantitative detecting method of semiconductor transducer and mustard gas or mustard gas simulant gas |
| CN109368703A (en) * | 2018-11-15 | 2019-02-22 | 厦门大学 | A kind of tungstic acid preparation of sections method |
| CN111111658A (en) * | 2020-01-20 | 2020-05-08 | 山东大学 | Single-atom Pt-loaded tungsten oxide single-layer nanosheet catalyst with ultrahigh catalytic activity and preparation method and application thereof |
| CN113088703A (en) * | 2015-03-31 | 2021-07-09 | 捷客斯金属株式会社 | Method for producing tungsten carbide |
| CN113511684A (en) * | 2020-04-10 | 2021-10-19 | 中国石油化工股份有限公司 | WO3Nanosheet and preparation method thereof and gas sensor |
| CN116002758A (en) * | 2023-02-09 | 2023-04-25 | 北京信息科技大学 | Preparation method of two-dimensional ammonium-doped hexagonal phase tungsten oxide |
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| CN113088703A (en) * | 2015-03-31 | 2021-07-09 | 捷客斯金属株式会社 | Method for producing tungsten carbide |
| CN105891126A (en) * | 2015-06-30 | 2016-08-24 | 四川智立方博导科技有限责任公司 | Low-cost portable hydrogen optical sensor |
| CN106365204A (en) * | 2016-11-03 | 2017-02-01 | 河北工业大学 | Preparation method of tungsten trioxide sensitive material for ammonia gas sensitive sensor |
| CN106365204B (en) * | 2016-11-03 | 2017-09-12 | 河北工业大学 | Preparation method for the tungstic acid sensitive material of ammonia gas sensor |
| WO2018091293A1 (en) * | 2016-11-21 | 2018-05-24 | Unilever N.V. | A gas sensor for detecting a gas component |
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| CN107324391B (en) * | 2017-08-16 | 2019-01-22 | 广东工业大学 | A kind of single layer hydration tungstic trioxide nano-slice and preparation method thereof |
| CN107324391A (en) * | 2017-08-16 | 2017-11-07 | 广东工业大学 | A kind of individual layer hydration tungstic trioxide nano-slice and preparation method thereof |
| CN108195891A (en) * | 2017-11-10 | 2018-06-22 | 中国人民解放军陆军防化学院 | The quantitative detecting method of semiconductor transducer and mustard gas or mustard gas simulant gas |
| CN109368703A (en) * | 2018-11-15 | 2019-02-22 | 厦门大学 | A kind of tungstic acid preparation of sections method |
| CN109368703B (en) * | 2018-11-15 | 2020-01-07 | 厦门大学 | Preparation method of tungsten trioxide thin sheet |
| CN111111658A (en) * | 2020-01-20 | 2020-05-08 | 山东大学 | Single-atom Pt-loaded tungsten oxide single-layer nanosheet catalyst with ultrahigh catalytic activity and preparation method and application thereof |
| CN113511684A (en) * | 2020-04-10 | 2021-10-19 | 中国石油化工股份有限公司 | WO3Nanosheet and preparation method thereof and gas sensor |
| CN113511684B (en) * | 2020-04-10 | 2024-03-22 | 中国石油化工股份有限公司 | WO 3 Nanosheets, preparation method thereof and gas sensor |
| CN116002758A (en) * | 2023-02-09 | 2023-04-25 | 北京信息科技大学 | Preparation method of two-dimensional ammonium-doped hexagonal phase tungsten oxide |
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