CN110028097A - Sensitive material SnS-SnO for Hg (0) sensor2 - Google Patents
Sensitive material SnS-SnO for Hg (0) sensor2 Download PDFInfo
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- CN110028097A CN110028097A CN201910155264.7A CN201910155264A CN110028097A CN 110028097 A CN110028097 A CN 110028097A CN 201910155264 A CN201910155264 A CN 201910155264A CN 110028097 A CN110028097 A CN 110028097A
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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
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- 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
One kind being used for the sensitive material SnS-SnO of Hg (0) sensor2, belong to semiconductor transducer technical field.The purpose of the present invention is using sulfide semiconductor as the SnS-SnO of template2Resistance type sensor is used to detect the sensitive material SnS-SnO for Hg (0) sensor of Hg (0)2.Preparation method of the present invention is: weighing stannous chloride, is dissolved in deionized water under agitation；Then respectively by sodium hydroxide, thiocarbamide, ammonium fluoride, P123, successively under agitation to being dissolved completely in deionized water solution；10 min are stirred after being completely dissolved, are then moved into reaction kettle, 160 DEG C of hydro-thermal, keep 12h；By reaction kettle cooled to room temperature in a high voltage state, then black product is used to deionized water and ethyl alcohol centrifuge washing 3 times respectively；By the black product collected after washing, for 24 hours, vacuum oven temperature is set as 60 DEG C for drying in a vacuum drying oven.The present invention has good air-sensitive performance to Hg (0).The content of Hg (0) can finally be detected.
Description
Technical field
The invention belongs to semiconductor transducer technical fields.
Background technique
Mercury causes to seriously endanger as one of hypertoxic metallics to biology and environment.Since it has migration, biology
Cumulative bad and persistence, so that advanced bio is easier to accumulate than the low forms of life, the injury caused by advanced bio is more obvious.Its
It is coal fire discharged that ratio, which accounts for biggish, in middle anthropogenic discharge's amount, therefore the United Nations formulated coal fire discharged correlation in 2010 and arranges
It applies.Currently used detection method is based primarily upon cold atomic absorption spectrometry, cold-atomic fluorescence spectrometry principle.Based on this principle
Equipment it is more complicated and the disadvantages of human error is big, can not quickly and effectively detect elementary gas mercury content.
In recent years due to the rise of semiconductor material, there is good sensitivity, selection by the sensor of semiconductor fabrication
The features such as property, response recovery time is short, and stability is good.Therefore the mercury sensor for developing a long-range fast real-time monitoring has become
The trend of mercury detection.It interacts, has been researched and developed using golden material as the sensor of template currently based on amalgam.Such as develop gold
Thin-film electro resistance type sensor, golden material sound surface probe, gold nanorods fiber evanescent wave sensor, the wavelength detecting of golden material
Type surface plasma resonance sensor, gold nano grain composite carbon nanometer tube resistance type sensor.Golden sensor response restores
The features such as overlong time, detection range is narrow, and stability is poor.
Summary of the invention
The purpose of the present invention is using sulfide semiconductor as the SnS-SnO of template2Resistance type sensor is for detecting Hg (0)
The sensitive material SnS-SnO for Hg (0) sensor2。
Preparation method of the present invention is:
2mmol stannous chloride is accurately weighed, is dissolved in 50mL deionized water under agitation；Then respectively by 25mmol hydrogen
Sodium oxide molybdena, 4mmol thiocarbamide, 2mmol ammonium fluoride, 0.0787g P123, successively under agitation to being dissolved completely in deionization
In aqueous solution；10min is stirred after being completely dissolved, is then moved into 100mL reaction kettle, 160 DEG C of hydro-thermal, keeps 12h；It will reaction
Black product, is then used deionized water and ethyl alcohol centrifuge washing 3 times by kettle cooled to room temperature in a high voltage state respectively；It will
For 24 hours, vacuum oven temperature is set as 60 DEG C to the black product collected after washing for drying in a vacuum drying oven.
The present invention uses sensitive material SnS-SnO2The method for manufacturing Hg (0) sensor is:
1. with Al2O3Ceramic tube is substrate, and two sections of ceramic tube respectively have a circular gold electrode, and each gold electrode has two
Platinum filament makees lead；
2. by SnS-SnO made from one2Nano material agate mortar is finely ground, instills a few drop deionized waters and is tuned into paste, then
The outer surface for being put on ceramic tube is brushed with fine, soft fur, coating layer thickness is uniform as far as possible, in addition to lead, the outer surface of ceramic tube and cyclic annular gold
Electrode is completely by SnS-SnO2The material of nano wire covers；
3. ceramic tube is natural or dries in the shade under infrared lamp, nichrome heater strip is penetrated from ceramic tube inside, finally by pin
It is welded on device tube socket, obtains Hg (0) gas sensor.
SnS-SnO of the present invention2Nano material, is made of and nano particle uniform nanometer sheet and nano particle
Uniformly it is embedded in nanometer sheet.Since nano particle and nanometer sheet form hetero-junctions, so that gas sensory air-sensitive
Performance increases.To have good air-sensitive performance to Hg (0).The content of Hg (0) can finally be detected.
Detailed description of the invention
Fig. 1 is the XRD spectra of photo (c) power spectrum spectrogram (d) material under photo (b) the SEM low power under (a) SEM high power；
Fig. 2 is (a) senser element schematic diagram, (b) sensor real image；
Fig. 3 is response curve of the sensor under different Hg (0) concentration in example 1；
Fig. 4 is that sensor is most preferably responding recovery curve in example 1；
Fig. 5 be in example 1 sensor to the selectivity of disturbance gas.
Specific embodiment
Resistance type sensor, response and recovery time are fast, respectively in 8-10min, 15-20min, and have good choosing
Selecting property, wider detection range is from 0.55-452.51mg/m3.Sulfide semiconductor is narrow before detection range ratio, the response time
Greater than 20min.It therefore is the SnS-SnO based on sulfide semiconductor for template prepared by the present invention2Resistance type sensor is used
In detection Hg (0).
SnS-SnO of the present invention2Nano material is made of uniform nanometer sheet and nano particle, and nano particle is equal
Even is embedded in nanometer sheet.
The present invention is first using stannous chloride, sodium hydroxide, thiocarbamide, ammonium fluoride and P123 as raw material, the hydro-thermal at 160 DEG C
12h is successfully prepared SnS-SnO2Nanocomposite；Material is finally built into Hg (0) sensor.It is of the present invention
SnS-SnO2Nano material specific the preparation method is as follows:
1.SnS-SnO2The preparation of nanocomposite
2mmol stannous chloride is accurately weighed, is dissolved in 50mL deionized water under agitation.Then respectively by 25mmol hydrogen
Sodium oxide molybdena, 4mmol thiocarbamide, 2mmol ammonium fluoride, 0.0787g P123, successively under agitation to being dissolved completely in deionization
In aqueous solution.10min is stirred after being completely dissolved, is then moved into 100mL reaction kettle, 160 DEG C of hydro-thermal, keeps 12h.It will reaction
Black product, is then used deionized water and ethyl alcohol centrifuge washing 3 times by kettle cooled to room temperature in a high voltage state respectively.It will
For 24 hours, vacuum oven temperature is set as 60 DEG C to the black product collected after washing for drying in a vacuum drying oven.
2. the production of gas sensor:
1. with Al2O3Ceramic tube is substrate, and two sections of ceramic tube respectively have a circular gold electrode, and each gold electrode has two
Platinum filament makees lead.
2. by SnS-SnO made from one2Nano material agate mortar is finely ground, instills a few drop deionized waters and is tuned into paste,
Then the outer surface for being put on ceramic tube is brushed with fine, soft fur, coating layer thickness is uniform as far as possible, in addition to lead, the outer surface of ceramic tube and ring
Shape gold electrode is completely by SnS-SnO2Nano material covering
3. ceramic tube is natural or dries in the shade under infrared lamp, nichrome heater strip is penetrated from ceramic tube inside, finally by pin
It is welded on device tube socket, obtains Hg (0) sensor.
Herein, the sensitivity definition of sensor is S=Rg/R0In formula: RgStablize electricity in tested gas for element
Resistance, R0For the aerial steady resistance of element；Response time is defined as the sensor output variation in tested gas and reaches
90% time of stationary value, recovery time are defined as sensor and reach incipient stability (in air) after gas is removed
Time needed for the 10% of value.SnS-SnO of the present invention2Nano material is when air-sensitive is tested using static distribution
Method.
It is as shown in Figure 1: SnS-SnO by scheming the product that (d) is obtained in example 12, product is without the presence of other miscellaneous phases.By (a)
Low power figure SEM can see SnS-SnO2Nanocomposite is that flower-shaped shape is formed together with little particle cluster by flakelet
Looks.That schemes (b) high power SEM can see SnS-SnO2Nanocomposite is uniformly inlayed by uniform diamond shape nanometer little particle
In nanometer sheet.The presence that Sn, S, O element are further demonstrated by (c) may further determine that SnS- in conjunction with figure (d)
SnO2The formation of nano material.
It is as shown in Figure 2: being constituted by Hg (0) gas sensor by gas sensor and pedestal two parts in example 1, wherein gas
Quick element is by Al2O3Substrate, SnS-SnO2Nanocomposite, 5 part structure of ring-type Au electrode, Pt line and nichrome resistance wire
At.
As shown in Figure 3: Hg (0) gas sensor is to the response sensitivity curve of different Hg (0) concentration in example 1, therefrom
It can be seen that concentration is optimal to the response of Hg (0) in 0.3mg/m3, Monitoring lower-cut is responded up to 0.1mg/m3.
As shown in Figure 4: the best response curve of Hg (0) gas sensor in example 1.Therefrom it can be seen that when responding and restoring
Between in 1min or so.
As shown in Figure 5: selectivity of Hg (0) gas sensor to disturbance gas in example 1.To H2S、SO2、 NH3
Equal interference gas have good selectivity.
Example 1:
Based on SnS-SnO2Hg (0) gas sensor of nanocomposite, preparation method are as follows:
1. accurately weighing 2mmol stannous chloride, it is dissolved in 50mL deionized water under agitation.Then respectively by 25mmol
Sodium hydroxide, 4mmol thiocarbamide, 2mmol ammonium fluoride, 0.0787g P123, successively under agitation to be dissolved completely in from
In sub- aqueous solution.10min is stirred after being completely dissolved, is then moved into 100mL reaction kettle, 160 DEG C of hydro-thermal, keeps 12h.It will be anti-
Kettle cooled to room temperature in a high voltage state is answered, then black product is used to deionized water and ethyl alcohol centrifuge washing 3 times respectively.
By the black product collected after washing, for 24 hours, vacuum oven temperature is set as 60 DEG C for drying in a vacuum drying oven.
2. with Al2O3Ceramic tube is substrate, and two sections of ceramic tube respectively have a circular gold electrode, and each gold electrode has two
Platinum filament makees lead.
5. by SnS-SnO made from one2Nanocomposite agate mortar is finely ground, instills a few drop deionized waters and is tuned into paste,
Then the outer surface for being put on ceramic tube is brushed with fine, soft fur, coating layer thickness is uniform as far as possible, in addition to lead, the outer surface of ceramic tube and ring
Shape gold electrode is completely by SnS-SnO2Nanocomposite covering
6. ceramic tube is natural or dries in the shade under infrared lamp, after natural cooling, nichrome heater strip is penetrated from ceramic tube inside,
Finally pin is welded on device tube socket, obtains Hg (0) gas sensor.
Example 2
Based on SnS-SnO2Hg (0) gas sensor of nanocomposite, detects Hg (0) under various concentration:
1. opening precision digital multimeter, programmable DC power supply and computer.Software " FLUCK " is opened on computers, setting
5s detection is primary.The sensing element of production is inserted on testing jack, it can be immediately in the display screen of precision digital multimeter
On see the instant resistance of sensing element, and it is also seen that the change curve of resistance on software window.It adjusts programmable
The output current value of DC power supply changes the temperature of sensing element, makes resistance stabilization.Record resistance R at this time0, heating electricity
Stream and voltage.
2. (being heated, being added to too mercury with oil bath pan with being filled with 100ml Hg (0) gas with syringe in gas cylinder in 1L static state
Hot temperature is 30 DEG C, and the concentration of matched Hg (0) is 3mg/m3 at this time), stopper bottle stopper.Bottle stopper is opened, by Hg (0) gas sensor
It is inserted into gas cylinder, is in Hg (0) gas sensor in the atmosphere of Hg (0) gas.After resistance stabilization, record at this time
Resistance Rg；Hg (0) gas sensor is taken out, Yu Yuanwei placement location makes resistance be restored to stabilization.3. one-time detection completion changes
Mercury concentration successively measures under various concentration, response of the sensor to (0) Hg.
Example 3
Based on SnS-SnO2Hg (0) gas sensor of nanocomposite, the response under different Hg (0) concentration:
1. opening precision digital multimeter, programmable DC power supply and computer.Software " FLUCK " is opened on computers, setting
1s detection is primary.The sensing element of production is inserted on testing jack, it can be immediately in the display screen of precision digital multimeter
On see the instant resistance of sensing element, and it is also seen that the change curve of resistance on software window.It records at this time
Resistance R0。
2. (being heated, being added to too mercury with oil bath pan with being filled with 100ml Hg (0) gas with syringe in gas cylinder in 1L static state
Hot temperature is 30 DEG C, and the concentration of matched Hg (0) is 3mg/m3 at this time), stopper bottle stopper.Bottle stopper is opened, by Hg (0) gas sensor
It is inserted into gas cylinder, is in Hg (0) gas sensor in the atmosphere of Hg (0) gas.After resistance stabilization, record at this time
Resistance Rg；Hg (0) gas sensor is taken out, Yu Yuanwei placement location makes resistance be restored to stabilization.3. one-time detection is completed successively
Change injection Hg (0) gas volume so that Hg (0) concentration be 0.1mg/3,0.15mg/m3,0.3mg/m3,3 mg/m3,
8mg/m3,30mg/m3,126mg/m3 test sensor.
Claims (2)
1. the sensitive material SnS-SnO that one kind is used for Hg (0) sensor2, it is characterised in that: preparation method is:
2mmol stannous chloride is accurately weighed, is dissolved in 50mL deionized water under agitation；Then respectively by 25mmol hydrogen-oxygen
Change sodium, 4mmol thiocarbamide, 2mmol ammonium fluoride, 0.0787g P123, successively under agitation to being dissolved completely in deionized water
In solution；10min is stirred after being completely dissolved, is then moved into 100mL reaction kettle, 160 DEG C of hydro-thermal, keeps 12h；Reaction kettle is existed
Then black product is used deionized water and ethyl alcohol centrifuge washing 3 times by cooled to room temperature under high pressure conditions respectively；It will washing
For 24 hours, vacuum oven temperature is set as 60 DEG C to the black product collected afterwards for drying in a vacuum drying oven.
2. the sensitive material SnS-SnO according to claim 1 for Hg (0) sensor2, it is characterised in that: using sensitive
Material SnS-SnO2The method for manufacturing Hg (0) sensor is:
1. with Al2O3Ceramic tube is substrate, and two sections of ceramic tube respectively have a circular gold electrode, and each gold electrode has two
Platinum filament makees lead；
2. by SnS-SnO made from one2Nano material agate mortar is finely ground, instills a few drop deionized waters and is tuned into paste, then uses
Fine, soft fur brushes the outer surface for being put on ceramic tube, and coating layer thickness is uniform as far as possible, in addition to lead, the outer surface of ceramic tube and cyclic annular gold electricity
Extremely completely by SnS-SnO2The material of nano wire covers；
3. ceramic tube is natural or dries in the shade under infrared lamp, nichrome heater strip is penetrated from ceramic tube inside, finally by pin
It is welded on device tube socket, obtains Hg (0) gas sensor.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112067666A (en) * | 2020-08-13 | 2020-12-11 | 东北电力大学 | Preparation method of silver phosphate doped tin dioxide gas sensor gas sensitive material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2019
- 2019-03-01 CN CN201910155264.7A patent/CN110028097B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| 姚龙: "SnS2/SnO2纳米复合材料的合成与光催化性质", 《中国优秀硕士学位论文全文数据库》 * |
| 胡蝶等: "SnS2纳米片负载SnO2纳米颗粒改性氨气气敏响应", 《科技创新与应用》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112067666A (en) * | 2020-08-13 | 2020-12-11 | 东北电力大学 | Preparation method of silver phosphate doped tin dioxide gas sensor gas sensitive material |
| CN112067666B (en) * | 2020-08-13 | 2024-03-29 | 东北电力大学 | Preparation method of silver phosphate doped tin dioxide gas sensor gas-sensitive material |
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