CN106645308A - Making method of acetone gas sensors based on alloy tungsten molybdenum disulfide nano-sheets - Google Patents
Making method of acetone gas sensors based on alloy tungsten molybdenum disulfide nano-sheets Download PDFInfo
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- CN106645308A CN106645308A CN201610886894.8A CN201610886894A CN106645308A CN 106645308 A CN106645308 A CN 106645308A CN 201610886894 A CN201610886894 A CN 201610886894A CN 106645308 A CN106645308 A CN 106645308A
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- Prior art keywords
- acetone
- acetone gas
- resistance
- gas
- molybdenum bisuphide
- Prior art date
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 title claims abstract description 140
- 239000000956 alloy Substances 0.000 title claims abstract description 7
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title abstract description 8
- DOIKGWMZXKJLJV-UHFFFAOYSA-N [W].[Mo](=S)=S Chemical compound [W].[Mo](=S)=S DOIKGWMZXKJLJV-UHFFFAOYSA-N 0.000 title abstract 5
- 239000002135 nanosheet Substances 0.000 title abstract 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 34
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 5
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 4
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 78
- 229910052750 molybdenum Inorganic materials 0.000 claims description 30
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 29
- 239000011733 molybdenum Substances 0.000 claims description 29
- 229910052721 tungsten Inorganic materials 0.000 claims description 28
- 239000010937 tungsten Substances 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 abstract 1
- 239000012528 membrane Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 229910052723 transition metal Inorganic materials 0.000 description 15
- 150000003624 transition metals Chemical class 0.000 description 15
- 239000000463 material Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 238000000137 annealing Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 2
- 206010012601 diabetes mellitus Diseases 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- GRWZHXKQBITJKP-UHFFFAOYSA-L dithionite(2-) Chemical compound [O-]S(=O)S([O-])=O GRWZHXKQBITJKP-UHFFFAOYSA-L 0.000 description 1
- 238000001548 drop coating Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-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
Abstract
The invention discloses a making method of acetone gas sensors based on alloy tungsten molybdenum disulfide nano-sheets and an application of the acetone gas sensors. The making method includes the steps: mixing ammonium molybdate, ammonium tungstate and thiourea according to a certain proportion, taking water as solvents, and adding the mixture into a hydrothermal reactor taking 50mL polytetrafluoroethylene as a liner; heating for dozens of hours, and naturally cooling after reaction is finished; centrifugally separating products obtained in a reacted manner to obtain the tungsten molybdenum disulfide nano-sheets; dripping water solution of the tungsten molybdenum disulfide nano-sheets on a gold-cross electrode, drying the electrode at the temperature of 60 DEG C to form a membrane, enabling the surface of the gold-cross electrode to expose electrodes of two ends, and covering the rest portions with the tungsten molybdenum disulfide nano-sheets to prepare the acetone gas sensors capable of measuring acetone gas concentration.
Description
Technical field
The present invention relates to gas sensor technical field, and in particular to prepared using transition metal molybdenum bisuphide tungsten nanometer sheet
The method of acetone gas sensor.
Background technology
Two-dimensional material, such as Graphene and class grapheme material, because its unique property is received with ultra-thin thickness
Extensive concern.In numerous class grapheme two-dimension materials, stratiform transition metal dichalcogenide (such as tungsten disulfide, molybdenum bisuphide)
Show excellent structure, electricity, optics, chemistry and macroscopic property so that they electronics, catalyst, energy storage and
Conversion and sensor field have huge application prospect.
Research discovery, crystal structure, pattern, geometry arrangement, component of transition metal dichalcogenide etc., to device performance pole
For important.For example, to some electronic devices, such as gas sensor, the nearest attraction of heterogeneous section is formed by adjusting phase wide
General concern.The structure of the heterogeneous section of this phase, is generally mutually tied by chemical vapor deposition with lithium ion intercalation or laser emission
The method of conjunction is obtained, but this method is not suitable for a large amount of preparations.Additionally, the formation of heterogeneous section, such as metal-semiconductor section, right
Sensing capabilities can be effectively improved in gas sensor.Therefore, the transition metal dichalcogenide containing the heterogeneous section of a large amount of phases has
Hope for preparing gas sensor.
Acetone gas are the biomarkers of diabetes, detection performance of the sensor to acetone gas are improved, to realizing nothing
Wound detection diabetes are significant.
The present invention is by hydro-thermal method, and with ammonium tungstate, ammonium molybdate and thiocarbamide are raw material, such as warm under specific reaction condition
Degree, reaction time, material content etc., can be obtained the adjustable transition metal molybdenum bisuphide tungsten nanometer sheet of phase, by these nanometers
Piece is by drop coating or is sprayed on golden crossed electrode, is prepared into gas sensor, realizes under 1ppm concentration to acetone gas
Detection.
The content of the invention
Technical scheme discloses application of the transition metal dithionite molybdenum tungsten nanometer sheet in acetone gas sensor,
And the performance of sensor is further improved by phase adjustment.
Technical scheme is as follows：
Based on the preparation method of the acetone gas sensor of alloy molybdenum bisuphide tungsten nanometer sheet, its step is as follows：
(1) by ammonium molybdate, ammonium tungstate, thiocarbamide mixes by a certain percentage, with water as solvent, adds with 50mL polytetrafluoroethylene (PTFE)
For in the water heating kettle of inner bag；
(2) 24-48 hours are heated at 200-240 DEG C, reaction terminates rear natural cooling；
(3) the product centrifugation for obtaining reaction, washes with water respectively twice, and ethanol is washed twice, obtains molybdenum bisuphide tungsten
Nanometer sheet；
(4) molybdenum bisuphide tungsten nanometer sheet is put into a crucible, after crucible is put into tube furnace, lead to argon gas 30 minutes
Drain the air in tube furnace, be then heated to 300 DEG C by the speed of 10 DEG C/min, be incubated 1 hour, then natural cooling；
(5) the 100 μ L molybdenum bisuphide tungsten nanometer sheet aqueous solution are dropped on golden crossed electrode, is dried under temperature 60 C
Two end electrodes are only exposed on film, golden crossed electrode surface, and remaining position is covered by molybdenum bisuphide tungsten nanometer sheet, and being obtained can determine third
The acetone gas sensor of ketone gas concentration.
Applying step based on the acetone gas sensor of alloy molybdenum bisuphide tungsten nanometer sheet is as follows：
(1) two end electrodes of gas sensor are connected by wire with a data acquisition unit, and gas sensor is placed in one
In the box of individual two ends perforate, under test gas are entered by a stomidium, and another stomidium is discharged；
(2) during obstructed acetone gas, baseline electrical resistance R of gas sensor is determined0；
(3) determine resistance when being passed through acetone gas, it is ensured that the flow of acetone gas is 500sccm, concentration by 1ppm by
Cumulative to be added to 1000ppm, carrier gas is nitrogen；
(4) under each test concentrations, the resistance of sensor with the addition of acetone reach balance when, acetone gas are changed
It is used to purge into pure nitrogen gas so that sensor resistance returns to baseline electrical resistance；
(5) resistance for measuring is converted into Δ R/R0, wherein R0It is the baseline electrical resistance in obstructed acetone, and Δ R is logical acetone
When with respect to baseline electrical resistance resistance change；
(6) by Δ R/R0It is plotted against time, with the increase of acetone gas concentration, resistance variations accordingly increase；
The test concentrations of (7) acetone gas by resistance variations to reaching after equalization point, then be passed through one it is higher
Concentration, repeat step (3) to (6).
Beneficial effect：Transition metal molybdenum bisuphide tungsten nanometer sheet is applied to acetone gas sensor by the present invention first, and
And by regulating and controlling phase, further increase the performance of sensor.
Description of the drawings
Figure 1A is the Mo in embodiment 10.87W0.13S2The SEM figures of (30%1T, 70%2H).
Figure 1B is Mo in embodiment 10.87W0.13S2The EDX figures of (30%1T, 70%2H).
Fig. 1 C are Mo in embodiment 10.87W0.13S2The XRD of (30%1T, 70%2H).
Fig. 1 D are Mo in embodiment 10.87W0.13S2The XPS figures of the Mo 3d of (30%1T, 70%2H).
Fig. 1 E are Mo in embodiment 10.87W0.13S2The XPS figures of the S 2p of (30%1T, 70%2H).
Fig. 1 F are Mo in embodiment 10.87W0.13S2The XPS figures of the W 3f of (30%1T, 70%2H).
Fig. 2A is Mo in embodiment 20.87W0.13S2The SEM figures of (10%1T, 90%2H).
Fig. 2 B are Mo in embodiment 20.87W0.13S2The EDX figures of (10%1T, 90%2H).
Fig. 2 C are Mo in embodiment 20.87W0.13S2The XRD of (10%1T, 90%2H).
Fig. 2 D are Mo in embodiment 20.87W0.13S2The XPS figures of Mo 3d in (10%1T, 90%2H).
Fig. 2 E are Mo in embodiment 20.87W0.13S2The XPS figures of S 2p in (10%1T, 90%2H).
Fig. 2 F are Mo in embodiment 20.87W0.13S2The XPS figures of W 4f in (10%1T, 90%2H).
Fig. 3 A are Mo in embodiment 30.87W0.13S2The resistance of (10%1T, 90%2H) changes over figure.
Fig. 3 B are Mo in embodiment 30.87W0.13S2(annealed) resistance changes over figure.
Fig. 3 C are Mo in embodiment 30.87W0.13S2The resistance of (30%1T, 70%2H) changes over figure.
Fig. 3 D are Mo in embodiment 30.87W0.13S2(10%1T, 90%2H) resistance variations under different acetone gas concentration
Amount and time chart.
Fig. 3 E are Mo in embodiment 30.87W0.13S2(10%1T, 90%2H) and Mo0.87W0.13S2(annealed) identical
Resistance change and time chart under acetone gas concentration.
Fig. 3 F are Mo in embodiment 30.87W0.13S2(10%1T, 90%2H), Mo0.87W0.13S2(30%1T, 70%2H),
Mo0.87W0.13S2(annealed) resistance change and acetone concentration graph of a relation.
Specific embodiment
For a better understanding of the present invention, the skill of the present invention is illustrated by specific embodiment below in conjunction with the accompanying drawings
Art scheme.
In transition metal molybdenum bisuphide tungsten nanometer sheet phase, 1T phases are octahedral structure, and 2H phases are triangular prism structure, above-mentioned
The heterogeneous energy-conservation of phase enough effectively improves the sensing capabilities of gas sensor, therefore, the transition metal containing the heterogeneous section of a large amount of phases
Disulphide can be used for preparing gas sensor.
Embodiment 1：With Mo0.87W0.13S2(30%1T, 70%2H) and Mo0.87W0.13S2(annealed) acetone gas are prepared
The method of sensor
(1) 0.25mmol, 0.3120g ammonium molybdates, 0.25mmol, 0.8743g ammonium tungstate, 30mmol, 2.3067g thiocarbamide are taken
And 35mL water, while adding in the water heating kettle with 50mL polytetrafluoroethylene (PTFE) as inner bag；
(2) baking oven for being warming up to 240 DEG C in advance is put into, is heated 48 hours at 240 DEG C；
(3) after reaction terminates, it is placed on room temperature environment natural cooling；
(4) black solid for obtaining reaction by centrifugation, twice, wash again twice, finally gives mesh for washing by ethanol
Mark product Mo0.87W0.13S2(30%1T, 70%2H).
(5) molybdenum bisuphide tungsten nanometer sheet is put into a crucible, after crucible is put into tube furnace, lead to argon gas 30 minutes
Drain the air in tube furnace so as to avoid sample from being oxidized, be then heated to 300 DEG C by the speed of 10 DEG C/min, insulation 1 is little
When, then natural cooling, the product Mo after being annealed0.87W0.13S2(annealed)；
(6) the 100 μ L molybdenum bisuphide tungsten nanometer sheet aqueous solution are dropped on golden crossed electrode, is dried under temperature 60 C
Two end electrodes are only exposed on film, golden crossed electrode surface, and remaining position is all covered by molybdenum bisuphide tungsten nanometer sheet, and being obtained to survey
Determine the gas sensor of acetone gas concentration.
To the product Mo in embodiment 10.87W0.13S2(30%1T, 70%2H) is analyzed, as shown in Figure 1A,
Mo0.87W0.13S2The SEM figures of (30%1T, 70%2H), the Mo that can illustrate to finally give by SEM figures0.87W0.13S2For nanometer
It is flower-shaped.
As shown in Figure 1B, Mo0.87W0.13S2The EDX figures of (30%1T, 70%2H), by EDX figures W can be illustrated:Mo≈1:
6, the content of correspondence W is about 13%.
As shown in Figure 1 C, Mo0.87W0.13S2The XRD of (30%1T, 70%2H), 9 ° in figure, 14 °, 33 ° correspond to respectively
(002)1T,(002)2H(100) face.
As shown in figure ip, Mo0.87W0.13S2In (30%1T, 70%2H) Mo 3d XPS figure, in figure 228.6eV and
Peak correspondence 1T Mo at 231.7eV4+, 229.2eV 2H Mos corresponding with the peak at 232.4eV4+, 233.12 eV and 235.91eV
The peak correspondence Mo at place6+, 226.2eV correspondence S 2s tracks.By the peak area for comparing 1T and 2H, can calculate 1T contents are about
30%.
As referring to figure 1e, Mo0.87W0.13S2The XPS figures of S 2p in (30%1T, 70%2H).In figure 161.2eV and
Peak correspondence 1T S at 162.3eV2-, 162.1eV 2H Ss corresponding with the peak at 163.3eV2-.By the peak face for comparing 1T and 2H
Product, can calculate 1T contents are about 30%.
As shown in fig. 1f, Mo0.87W0.13S2The XPS figures of W 4f in (30%1T, 70%2H).31.7eV and 33.9eV in figure
The peak correspondence 1T W at place4+, 32.6eV 2H Ws corresponding with the peak at 34.5eV4+, 35.7eV Ws corresponding with the peak at 37.8eV6+, this
Outward, the peak at 39.3eV and 36.6eV corresponds to respectively W 5p tracks and Mo 4p tracks.By the peak area for comparing 1T and 2H, can
With calculate 1T contents are about 30%.
Embodiment 2：With Mo0.87W0.13S2The method that (10%1T, 90%2H) prepares acetone gas sensor
(1) by 0.25mmol, 0.3120g ammonium molybdates, 0.25mmol, 0.8743g ammonium tungstate, 30mmol, 2.3067g thiocarbamide
And 35mL water, while adding in the water heating kettle with 50mL polytetrafluoroethylene (PTFE) as inner bag；
(2) baking oven for being warming up to 200 DEG C in advance is put into, is heated 24 hours at 200 DEG C, then heated to 240 DEG C and protect
Hold 24 hours；
(3) after reaction terminates, it is placed on room temperature environment natural cooling；
(4) black solid for obtaining reaction by centrifugation, twice, wash again twice for washing by ethanol, finally give mesh
Mark product；
(5) the 100 μ L molybdenum bisuphide tungsten nanometer sheet aqueous solution are dropped on golden crossed electrode, is dried under temperature 60 C
Two end electrodes are only exposed on film, golden crossed electrode surface, and remaining position is all covered by molybdenum bisuphide tungsten nanometer sheet, and being obtained to survey
Determine the gas sensor of acetone gas concentration.
To the product Mo in embodiment 20.87W0.13S2(10%1T, 90%2H) is analyzed, as shown in Figure 2 A,
Mo0.87W0.13S2The SEM figures of (10%1T, 90%2H), the Mo that can illustrate to finally give by SEM figures0.87W0.13S2For nanometer
It is flower-shaped.
As shown in Figure 2 B, Mo0.87W0.13S2The EDX figures of (10%1T, 90%2H), by EDX figures W can be illustrated:Mo≈1:
6.8, the content of correspondence W is about 13%.
As shown in Figure 2 C, Mo0.87W0.13S2The XRD of (10%1T, 90%2H), 9 ° in figure, 14 °, 33 ° correspond to respectively
(002)1T,(002)2H(100) face.
As shown in Figure 2 D, Mo0.87W0.13S2In (10%1T, 90%2H) Mo 3d XPS figure, in figure 228.6eV and
Peak correspondence 1T Mo at 231.7eV4+, 229.2eV 2H Mos corresponding with the peak at 232.4eV4+, 233.12eV and 235.91eV
The peak correspondence Mo at place6+, 226.2eV correspondence S 2s tracks.By the peak area for comparing 1T and 2H, can calculate 1T contents are about
10%.
As shown in Figure 2 E, Mo0.87W0.13S2In (10%1T, 90%2H) S 2p XPS figure, in figure 161.2eV and
Peak correspondence 1T S at 162.3eV2-, 162.1eV 2H Ss corresponding with the peak at 163.3eV2-.By the peak face for comparing 1T and 2H
Product, can calculate 1T contents are about 10%.
As shown in Figure 2 F, Mo0.87W0.13S2The XPS figures of W 4f, 31.7eV and 33.9eV in figure in (10%1T, 90%2H)
The peak correspondence 1T W at place4+, 32.6eV 2H Ws corresponding with the peak at 34.5eV4+, 35.7eV Ws corresponding with the peak at 37.8eV6+, this
Outward, the peak at 39.3eV and 36.6eV corresponds to respectively W 5p tracks and Mo 4p tracks.By the peak area for comparing 1T and 2H, can
With calculate 1T contents are about 10%.
Embodiment 3：The application of acetone gas sensor -- the concentration of test acetone
(1) two end electrodes of gas sensor are then connected by wire with a data acquisition unit (Agilent 34971A),
At normal temperatures, the test to acetone gas sensing capabilities is carried out by the data acquisition unit；Gas sensor is placed in a two ends
In the box of perforate, under test gas are entered by one end nose end, are discharged by another stomidium；
(2) during obstructed acetone gas, baseline electrical resistance R of gas sensor is determined0；
(3) determine resistance when being passed through acetone gas, it is ensured that the flow of acetone gas is 500sccm, concentration by 1ppm by
Cumulative to be added to 1000ppm, carrier gas is nitrogen；
(4) under each test concentrations, the resistance of sensor with the addition of acetone reach balance when, acetone gas are changed
It is used to purge into pure nitrogen gas, makes sensor resistance return to baseline electrical resistance；
(5) resistance for measuring is converted into Δ R/R0, wherein R0It is the baseline electrical resistance in obstructed acetone, and Δ R is logical acetone
When with respect to baseline electrical resistance resistance change；
(6) by Δ R/R0It is plotted against time, with the increase of acetone concentration, resistance variations accordingly increase.
The test concentrations of (7) acetone gas by resistance variations to reaching after equalization point, then be passed through one it is higher
Concentration, repeat step (3) to (6).
Above-mentioned test result is analyzed, as shown in Figure 3A, Mo0.87W0.13S2The resistance of (10%1T, 90%2H) is at any time
Between variation diagram, resistance change becomes big with the increase of acetone gas concentration in figure.
As shown in Figure 3 B, Mo after annealing0.87W0.13S2Resistance change over figure, resistance change is with acetone in figure
The increase of gas concentration and become big.
As shown in Figure 3 C, Mo0.87W0.13S2The resistance of (30%1T, 70%2H) changes over figure, resistance change in figure
Become big with the increase of acetone gas concentration.
As shown in Figure 3 D, Mo0.87W0.13S2The resistance change and time chart of (10%1T, 90%2H), resistance in figure
Variable quantity becomes big with the increase of acetone gas concentration.
As shown in FIGURE 3 E, resistance change and time chart, identical acetone gas in figure under identical acetone gas concentration
Under concentration (50ppm), the Mo of 10%1T phases0.87W0.13S2Than the Mo after annealing0.87W0.13S2Resistance change is bigger.
As illustrated in Figure 3 F, resistance change and concentration relationship figure, the Mo of 10%1T phases in figure0.87W0.13S2With highest
Resistance change, and the minimum 1ppm of its test limit；The Mo of 30%1T phases0.87W0.13S2With highest resistance change, and its
The minimum 50ppm of test limit；And the Mo after annealing0.87W0.13S2The minimum 50ppm of test limit.
As shown in table 1, the phase of different phase transition metal molybdenum bisuphide tungsten nanometer sheet and baseline electrical resistance R0, it is different not
There are different baseline electrical resistances, the wherein Mo of 30%1T phases with phase transition metal molybdenum bisuphide tungsten nanometer sheet0.87W0.13S2Base
Line resistance is minimum, the Mo after annealing0.87W0.13S2Baseline electrical resistance is maximum.
Table 1 is the phase and baseline electrical resistance of different phase transition metal molybdenum bisuphide tungsten nanometer sheet
It can be found that the resistance of sensor can significantly change, and minimum inspection with the addition of acetone gas by Fig. 3 A to 3F
Survey limit and reach 1ppm.The resistance of transition metal molybdenum bisuphide tungsten nanometer sheet has sensitiveness for acetone gas, can be used for inspection
The change of acetone gas is surveyed, and in above-mentioned several sensor materials, the Mo of 10%1T phases0.87W0.13S2With best sensing
Device performance, this is due to caused by the heterogeneous section of its phase.When acetone gas are detected, the nanometer sheet conduct of pure semiconductor phase itself
N-type semiconductor, resistance can be reduced due to the addition of the acetone gas of electron.When increasing by 10% metal phase, nanometer sheet
Heterogeneous section is formed between upper metal phase and semiconductor phase, potential barrier is produced, and the addition of the acetone gas of electron can then reduce gesture
Height is built, so as to reduce resistance.But when 30% metal phase is increased to, nanometer sheet is no longer using semiconductor mutually as definitely master
Lead, now add acetone gas, resistance increase but can be caused because of physical absorption.Appropriate increase metal phase, can strengthen biography
Sensor performance；But excessive metal phase, but reduces the performance of sensor.
Accordingly, it can be said that transition metal molybdenum bisuphide tungsten nanometer sheet can be used for acetone gas sensor, and pass through into
The phase of one successive step transition metal molybdenum bisuphide tungsten nanometer sheet can improve sensor performance.
Claims (2)
1. the preparation method of the acetone gas sensor of alloy molybdenum bisuphide tungsten nanometer sheet is based on, it is characterised in that its step is such as
Under：
(1) by ammonium molybdate, ammonium tungstate, thiocarbamide mixes by a certain percentage, with water as solvent, adds with 50mL polytetrafluoroethylene (PTFE) as interior
In the water heating kettle of courage；
(2) 24-48 hours are heated at 200-240 DEG C, reaction terminates rear natural cooling；
(3) the product centrifugation for obtaining reaction, washes with water respectively twice, and ethanol is washed twice, obtains molybdenum bisuphide tungsten nanometer
Piece；
(4) molybdenum bisuphide tungsten nanometer sheet is put into a crucible, after crucible is put into tube furnace, logical argon gas is drained for 30 minutes
Air in tube furnace, is then heated to 300 DEG C by the speed of 10 DEG C/min, is incubated 1 hour, then natural cooling；
(5) the 100 μ L molybdenum bisuphide tungsten nanometer sheet aqueous solution are dropped on golden crossed electrode, the drying and forming-film under temperature 60 C, gold
Two end electrodes are only exposed on crossed electrode surface, and remaining position is covered by molybdenum bisuphide tungsten nanometer sheet, and being obtained can determine acetone gas
The acetone gas sensor of bulk concentration.
2. the application of the acetone gas sensor of alloy molybdenum bisuphide tungsten nanometer sheet is based on, it is characterised in that its step is as follows：
(1) two end electrodes of gas sensor are connected by wire with a data acquisition unit, and gas sensor is placed in one two
In the box of end perforate, under test gas are entered by a stomidium, and another stomidium is discharged；
(2) during obstructed acetone gas, baseline electrical resistance R of gas sensor is determined0；
(3) resistance when being passed through acetone gas is determined, it is ensured that the flow of acetone gas is 500sccm, concentration is gradually increased by 1ppm
1000ppm is added to, carrier gas is nitrogen；
(4) under each test concentrations, the resistance of sensor with the addition of acetone reach balance when, acetone gas are made into pure
Nitrogen is used to purge so that sensor resistance returns to baseline electrical resistance；
(5) resistance for measuring is converted into Δ R/R0, wherein R0It is the baseline electrical resistance in obstructed acetone, and Δ R is logical acetone phase
Resistance change to baseline electrical resistance；
(6) by Δ R/R0It is plotted against time, with the increase of acetone gas concentration, resistance variations accordingly increase；
The test concentrations of (7) acetone gas to reaching after equalization point, then are passed through a higher concentration by resistance variations,
Repeat step (3) to (6).
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