CN110028097B - Sensitive material SnS-SnO for Hg (0) sensor2 - Google Patents
Sensitive material SnS-SnO for Hg (0) sensor2 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 24
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 13
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 12
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 11
- 239000001119 stannous chloride Substances 0.000 claims abstract description 11
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 238000004090 dissolution Methods 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000000919 ceramic Substances 0.000 claims description 28
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 19
- 239000010931 gold Substances 0.000 claims description 19
- 229910052737 gold Inorganic materials 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 230000000149 penetrating effect Effects 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 238000003466 welding Methods 0.000 claims description 4
- 210000002268 wool Anatomy 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000002070 nanowire Substances 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims 2
- 239000004065 semiconductor Substances 0.000 abstract description 9
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 37
- 238000001514 detection method Methods 0.000 description 11
- 239000002114 nanocomposite Substances 0.000 description 9
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 8
- 229910052753 mercury Inorganic materials 0.000 description 8
- 239000002105 nanoparticle Substances 0.000 description 7
- 239000002086 nanomaterial Substances 0.000 description 6
- 239000002135 nanosheet Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 238000009826 distribution Methods 0.000 description 3
- 230000002452 interceptive effect Effects 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 241001411320 Eriogonum inflatum Species 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910000497 Amalgam Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000001391 atomic fluorescence spectroscopy Methods 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 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
- 239000013307 optical fiber Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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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
- 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
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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
- 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
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Abstract
A sensitive material SnS-SnO2 for Hg (0) sensor belongs to the technical field of semiconductor sensors. The invention aims to provide a SnS-SnO2 sensitive material for an Hg (0) sensor, wherein the SnS-SnO2 resistance type sensor takes a sulfide semiconductor as a template and is used for detecting Hg (0). The preparation method comprises the following steps: weighing stannous chloride, and dissolving the stannous chloride in deionized water under the stirring condition; then, sequentially dissolving sodium hydroxide, thiourea, ammonium fluoride and P123 in deionized water solution under the condition of stirring; stirring for 10min after complete dissolution, then transferring into a reaction kettle, performing hydrothermal treatment at 160 ℃, and keeping for 12 h; naturally cooling the reaction kettle to room temperature under a high-pressure state, and then centrifugally washing the black product for 3 times by using deionized water and ethanol respectively; the washed black product was dried in a vacuum oven set at 60 ℃ for 24 h. The invention has good gas-sensitive performance to Hg (0). Finally, the content of Hg (0) can be detected.
Description
Technical Field
The invention belongs to the technical field of semiconductor sensors.
Background
Mercury, as one of the highly toxic metal substances, poses serious hazards to living beings and the environment. Because of its mobility, bioaccumulation and persistence, higher organisms are more easily accumulated than lower organisms, and the damage to higher organisms is more obvious. The coal emission is the major part of the man-made emission, so the united nations set measures related to the coal emission in 2010. The detection method adopted at present is mainly based on the principles of cold atomic absorption spectrometry and cold atomic fluorescence spectrometry. The device based on the principle has the defects of complexity, large manual error and the like, and cannot rapidly and effectively detect the content of the gaseous element mercury.
In recent years, due to the rise of semiconductor materials, sensors made of semiconductors have the characteristics of good sensitivity, selectivity, short response recovery time, good stability and the like. Therefore, the development of a mercury sensor for remote, rapid and real-time monitoring has become a trend of mercury detection. At present, a sensor taking gold materials as a template is researched and developed based on the interaction of amalgam. For example, a gold film resistance type sensor, a gold material acoustic surface sensor, a gold nanorod optical fiber evanescent wave sensor, a gold material wavelength detection type surface plasma resonance sensor and a gold nanoparticle composite carbon nanotube resistance type sensor are developed. The gold sensor has the characteristics of overlong response recovery time, narrow detection range, poor stability and the like.
Disclosure of Invention
The invention aims to provide SnS-SnO with a sulfide semiconductor as a template2SnS-SnO sensitive material for Hg (0) sensor, used for detecting Hg (0) and provided with resistor type sensor2。
The preparation method comprises the following steps:
accurately weighing 2mmol of stannous chloride, and dissolving the stannous chloride in 50mL of deionized water under the stirring condition; then respectively dissolving 25mmol of sodium hydroxide, 4mmol of thiourea, 2mmol of ammonium fluoride and 0.0787g P123 in deionized water solution under stirring conditions; stirring for 10min after complete dissolution, then transferring into a 100mL reaction kettle, performing hydrothermal treatment at 160 ℃, and keeping for 12 h; naturally cooling the reaction kettle to room temperature under a high-pressure state, and then centrifugally washing the black product for 3 times by using deionized water and ethanol respectively; the washed black product was dried in a vacuum oven set at 60 ℃ for 24 h.
The invention adopts sensitive material SnS-SnO2The method for manufacturing the Hg (0) sensor comprises the following steps:
al is used2O3The ceramic tube is a substrate, two sections of the ceramic tube are respectively provided with a circular gold electrode, and each gold electrode is provided with two platinum wires as leads;
② the prepared SnS-SnO2The nanometer material is porphyrized by an agate mortar, a few drops of deionized water are dripped into the mixture to be mixed into paste, then the paste is brushed and smeared on the outer surface of the ceramic tube by fine wool, the thickness of the coating is as uniform as possible, and the outer surface of the ceramic tube and the annular gold electrode except the lead are completely SnS-SnO2Material coverage of the nanowires;
and thirdly, naturally drying the ceramic tube or drying the ceramic tube in the shade under an infrared lamp, penetrating a nickel-chromium alloy heating wire into the ceramic tube, and finally welding pins on a tube seat of the device to obtain the Hg (0) gas sensor.
The SnS-SnO provided by the invention2The nano material consists of uniform nano sheets and nano particles, and the nano particles are uniformly embedded on the nano sheets. The gas-sensitive semiconductor has increased gas-sensitive performance because the nano particles and the nano sheets form a heterojunction. Thereby having good gas-sensitive performance to Hg (0). Finally, the content of Hg (0) can be detected.
Drawings
FIG. 1 is (a) a photograph at high SEM magnification (b) a photograph at low SEM magnification (c) an XRD spectrum of the material (d);
FIG. 2 is (a) a schematic diagram of a sensing device, (b) an actual image of the sensor;
FIG. 3 is a graph of the response of the sensor of example 1 at different Hg (0) concentrations;
FIG. 4 is a graph of the recovery of the sensor in example 1 at the optimum response;
fig. 5 is the selectivity of the sensor to different interfering gases in example 1.
Detailed Description
The resistance type sensor has fast response and recovery time of 8-10min and 15-20min, good selectivity and wide detection range of 0.55-452.51mg/m 3. The detection range is narrower than that of the prior sulfide semiconductor, and the response time is also longer than 20 min. Therefore, the SnS-SnO prepared by the invention based on the sulfide semiconductor as the template2The resistance type sensor is used for detecting Hg (0).
The SnS-SnO provided by the invention2The nano material consists of nano sheets and nano particles, and the nano particles are uniformly embedded on the nano sheets.
The invention firstly takes stannous chloride, sodium hydroxide, thiourea, ammonium fluoride and P123 as raw materials, and carries out hydrothermal reaction for 12h at 160 ℃, thereby successfully preparing SnS-SnO2A nanocomposite; finally, the material is constructed into an Hg (0) sensor. The SnS-SnO provided by the invention2The specific preparation method of the nano material comprises the following steps:
1.SnS-SnO2preparation of nanocomposites
Accurately weighing 2mmol of stannous chloride, and dissolving the stannous chloride in 50mL of deionized water under the stirring condition. Then 25mmol of sodium hydroxide, 4mmol of thiourea, 2mmol of ammonium fluoride and 0.0787g P123 are dissolved in deionized water solution under stirring. After complete dissolution, the mixture was stirred for 10min, and then transferred into a 100mL reaction kettle and kept at 160 ℃ for 12 h. The reaction kettle is naturally cooled to room temperature under a high pressure state, and then the black product is centrifugally washed for 3 times by deionized water and ethanol respectively. The washed black product was dried in a vacuum oven set at 60 ℃ for 24 h.
2. Manufacturing a gas sensor:
al is used2O3The ceramic tube is a substrate, two sections of the ceramic tube are respectively provided with a circular gold electrode, and each gold electrode is provided with two platinum wires as leads.
② the prepared SnS-SnO2The nanometer material is porphyrized by an agate mortar, a few drops of deionized water are dripped into the mixture to be mixed into paste, then the paste is brushed and smeared on the outer surface of the ceramic tube by fine wool, the thickness of the coating is as uniform as possible, and the outer surface of the ceramic tube and the annular gold electrode except the lead are completely SnS-SnO2Nanomaterial coating
And thirdly, naturally drying the ceramic tube or drying the ceramic tube in the shade under an infrared lamp, penetrating a nickel-chromium alloy heating wire into the ceramic tube, and finally welding pins on a tube seat of the device to obtain the Hg (0) sensor.
Here, the sensitivity of the sensor is defined as S ═ Rg/R0In the formula: rgFor stable resistance of the element in the gas to be measured, R0Is the stable resistance of the element in the air; the response time is defined as the time for the sensor output to change to 90% of the steady value in the measured gas, and the recovery time is defined as the time required for the sensor to reach 10% of the initial steady value (in air) after the gas is removed. The SnS-SnO provided by the invention2The nano material adopts a static gas distribution method in the gas-sensitive test.
As shown in fig. 1: the product obtained from scheme (d) in example 1 is SnS-SnO2The product has no other impurity phase. SnS-SnO can be seen from (a) low magnification SEM2The nano composite material is formed by clustering small flakes and small particles together into flower-like morphology. FIG. b is a high-power SEM showing that SnS-SnO is present2The nano composite material is formed by uniformly inlaying diamond-shaped nano particles on a nano sheet. The existence of Sn, S and O elements is further verified by (c), and SnS-SnO can be further determined by combining the graph (d)2And (4) forming the nano material.
As shown in fig. 2: the Hg (0) gas sensor of example 1 was composed of two parts, a gas sensor made of Al and a base2O3Substrate, SnS-SnO2The nano composite material, the annular Au electrode, the Pt wire and the nickel-chromium alloy resistance wire 5.
As can be seen from fig. 3: the response sensitivity curve of the Hg (0) gas sensor in example 1 to different Hg (0) concentrations shows that the response to Hg (0) is optimal when the concentration is 0.3mg/m3, and the lower limit of response detection can reach 0.1mg/m 3.
As can be seen from fig. 4: the Hg (0) gas sensor in example 1 gave the best response curve. It can be seen that both response and recovery times are around 1 min.
As can be seen from fig. 5: selectivity of Hg (0) gas sensor to different interfering gases in example 1. To H2S、SO2、 NH3And the interfering gas has good selectivity.
Example 1:
based on SnS-SnO2The preparation method of the Hg (0) gas sensor made of the nano composite material comprises the following steps:
weighing 2mmol of stannous chloride accurately, and dissolving the stannous chloride in 50mL of deionized water under the stirring condition. Then 25mmol of sodium hydroxide, 4mmol of thiourea, 2mmol of ammonium fluoride and 0.0787g P123 are dissolved in deionized water solution under stirring. After complete dissolution, the mixture was stirred for 10min, and then transferred into a 100mL reaction kettle and kept at 160 ℃ for 12 h. The reaction kettle is naturally cooled to room temperature under a high pressure state, and then the black product is centrifugally washed for 3 times by deionized water and ethanol respectively. The washed black product was dried in a vacuum oven set at 60 ℃ for 24 h.
② with Al2O3The ceramic tube is a substrate, two sections of the ceramic tube are respectively provided with a circular gold electrode, and each gold electrode is provided with two platinum wires as leads.
Fifthly, the prepared SnS-SnO2The nanometer composite material is porphyrized by an agate mortar, a few drops of deionized water are dripped into the mixture to be mixed into paste, then fine wool is used for brushing and coating the mixture on the outer surface of the ceramic tube, the thickness of the coating is as uniform as possible, and the outer surface of the ceramic tube and the annular gold electrode except a lead are completely SnS-SnO2Nanocomposite coating
Naturally drying the ceramic tube or drying the ceramic tube in the shade under an infrared lamp, naturally cooling, penetrating a nickel-chromium alloy heating wire into the ceramic tube, and finally welding pins on a tube seat of a device to obtain the Hg (0) gas sensor.
Example 2
Based on SnS-SnO2A gas sensor of Hg (0) of a nanocomposite, detecting Hg (0) at different concentrations:
firstly, opening a precision digital multimeter, programming a direct current power supply and a computer. And (3) opening a software 'FLUCK' on a computer, and setting 5s for detection once. The manufactured sensitive element is inserted into the test socket, so that the instant resistance of the sensitive element can be immediately seen on a display screen of the precise digital multimeter, and a change curve of the resistance can also be seen on a software window. The output current value of the programmable DC power supply is adjusted, the temperature of the sensitive element is changed, and the resistance is stabilized. Record the resistance R at this time0Heating current and voltage.
② 100ml Hg (0) gas is filled into a 1L static gas distribution bottle by a syringe (the oil bath pot is used for heating the mercury too, the heating temperature is 30 ℃, the concentration of the Hg (0) distributed at the time is 3mg/m3), and the bottle stopper is tightly plugged. The stopper was opened, and the Hg (0) gas sensor was inserted into the gas cylinder so that the Hg (0) gas sensor was in the Hg (0) gas atmosphere. After the resistance is stable, recording the resistance Rg at the moment; the Hg (0) gas sensor was removed and placed in situ to restore the resistance to stability. The one-time detection is completed, and the response of the sensor to Hg (0) is measured under the condition that the mercury concentration is changed and the mercury concentration is measured sequentially.
Example 3
Based on SnS-SnO2Hg (0) gas sensor of nanocomposite material, response at different Hg (0) concentrations:
firstly, opening a precision digital multimeter, programming a direct current power supply and a computer. And (3) opening a software 'FLUCK' on a computer, and setting 1s for detection once. The manufactured sensitive element is inserted into the test socket, so that the instant resistance of the sensitive element can be immediately seen on a display screen of the precise digital multimeter, and a change curve of the resistance can also be seen on a software window. Record the resistance R at this time0。
② 100ml Hg (0) gas is filled into a 1L static gas distribution bottle by a syringe (the oil bath pot is used for heating the mercury too, the heating temperature is 30 ℃, the concentration of the Hg (0) distributed at the time is 3mg/m3), and the bottle stopper is tightly plugged. The stopper was opened, and the Hg (0) gas sensor was inserted into the gas cylinder so that the Hg (0) gas sensor was in the Hg (0) gas atmosphere. After the resistance is stable, recording the resistance Rg at the moment; the Hg (0) gas sensor was removed and placed in situ to restore the resistance to stability. The detection is completed once, and the volume of the injected Hg (0) gas is changed in sequence, so that the Hg (0) concentration is 0.1mg/3, 0.15mg/m3, 0.3mg/m3, 3mg/m3, 8mg/m3, 30mg/m3 and 126mg/m3, and the sensor is tested.
Claims (1)
1. Sensitive material SnS-SnO for Hg (0) sensor2The method is characterized in that: the preparation method comprises the following steps:
accurately weighing 2mmol of stannous chloride, and dissolving the stannous chloride in 50mL of deionized water under the stirring condition; then respectively dissolving 25mmol of sodium hydroxide, 4mmol of thiourea, 2mmol of ammonium fluoride and 0.0787g P123 in deionized water solution under stirring conditions; stirring for 10min after complete dissolution, then transferring into a 100mL reaction kettle, performing hydrothermal treatment at 160 ℃, and keeping for 12 h; naturally cooling the reaction kettle to room temperature under a high-pressure state, and then centrifugally washing the black product for 3 times by using deionized water and ethanol respectively; drying the washed black product in a vacuum drying oven for 24 hours, wherein the temperature of the vacuum drying oven is set to be 60 ℃;
adopting sensitive material SnS-SnO2The method for manufacturing the Hg (0) sensor comprises the following steps:
al is used2O3The ceramic tube is a substrate, two sections of the ceramic tube are respectively provided with a circular gold electrode, and each gold electrode is provided with two platinum wires as leads;
② the prepared SnS-SnO2The nanometer material is porphyrized by an agate mortar, a few drops of deionized water are dripped into the mixture to be mixed into paste, then the paste is brushed and smeared on the outer surface of the ceramic tube by fine wool, the thickness of the coating is as uniform as possible, and the outer surface of the ceramic tube and the annular gold electrode except the lead are completely SnS-SnO2Material coverage of the nanowires;
and thirdly, naturally drying the ceramic tube or drying the ceramic tube in the shade under an infrared lamp, penetrating a nickel-chromium alloy heating wire into the ceramic tube, and finally welding pins on a tube seat of the device to obtain the Hg (0) gas sensor.
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| US3642464A (en) * | 1968-12-09 | 1972-02-15 | Univ Minnesota | Tin ore treating process |
| CN105080573A (en) * | 2015-08-13 | 2015-11-25 | 陕西科技大学 | Method for preparing SnS/SnO2 nano-photocatalysis composite material through microwave hydrothermal method |
| CN109107358A (en) * | 2018-09-20 | 2019-01-01 | 国网河北省电力有限公司电力科学研究院 | A kind of cerium oxide/copper oxide hetero-junctions composite oxides and its preparation method and application |
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2019
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| US3642464A (en) * | 1968-12-09 | 1972-02-15 | Univ Minnesota | Tin ore treating process |
| CN105080573A (en) * | 2015-08-13 | 2015-11-25 | 陕西科技大学 | Method for preparing SnS/SnO2 nano-photocatalysis composite material through microwave hydrothermal method |
| CN109107358A (en) * | 2018-09-20 | 2019-01-01 | 国网河北省电力有限公司电力科学研究院 | A kind of cerium oxide/copper oxide hetero-junctions composite oxides and its preparation method and application |
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