CN106018480B - A kind of heater-type ammonia gas sensor and preparation method - Google Patents
A kind of heater-type ammonia gas sensor and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of heater-type ammonia gas sensors, including ceramic tube, gas sensor, electrode and heating wire；Gas sensor is set on ceramic tube, and gas sensor is provided at both ends with electrode, and heating wire, which is set in ceramic tube, is used for heating ceramic pipe；Gas sensor uses gas sensitive Ag WS2Nano-powder makes；Ammonium metatungstate (NH is chosen first4)6H2W12O40Ammonium metatungstate (NH has been prepared using method of electrostatic spinning with PVP (K90) for polymer precursor Polymer Solution for raw material4)6H2W12O40/ PVP composite fibrofelts；Composite fibrofelt is put into high temperature resistance furnace annealing calcining and has obtained WO from being taken off on aluminium-foil paper3Fiber；By WO in tube furnace3Fiber carries out the nanometer WS that vulcanization reaction has synthesized lamellar with sulphur powder under nitrogen protection2, while by Ag nanoparticle depositions to WS2The surface of nanometer sheet, this preparation method is compared to conventional method, and operating procedure is simple and energy consumption is less.There is higher sensitivity and selectivity to ammonia.
Description
Technical field
The present invention relates to setting for conductor oxidate gas sensitive field, especially a kind of heater-type ammonia gas sensor
Meter method.
Background technology
Gas sensor and daily life are closely bound up, and weight is occupied in terms of national science and technology field and national defense construction
Status is wanted, for detecting a variety of toxic and harmful gas, such as ammonia, hydrogen sulfide, sulfur dioxide.Based on metal oxide semiconductor
Gas sensor there is highly sensitive, response and many advantages, such as recovery time is fast, operate with method is simple, at low cost,
But there are still yet unresolved issues in the application of actual production and living.First, stability difference and presence signal drift, make
Obtain the less reliable stabilization of final measurement.Second, lack accurate gas-selectively, due to often being deposited in actually detected
In some interference gas, this can cause sensor to generate the response that should not have and send out wrong report, and greatly limit it uses model
It encloses.Third, the resistance fluctuation of conductor oxidate at the working temperature change greatly, mainly by the purity of material, at film thickness
The influence of the factors such as degree, sintering temperature so that element resistance is more discrete, cannot meet the highly sensitive survey under certain occasion
Examination demand.
The gas sensor haveing excellent performance is prepared, can quickly and accurately be detected poisonous and harmful, inflammable and explosive in air
Gas becomes current social development essential condition.Traditional gas sensitive, crystal grain or pore size are larger, lead
It causes that its specific surface area is smaller and film thickness is larger, is unfavorable for the design and fabrication of high-performance gas sensor.
High performance gas sensor is prepared using efficiently excellent gas sensitive material therefore, it is necessary to a kind of.
Invention content
The problem to be solved in the present invention is to provide a kind of for the required heater-type gas sensing of ammonia detection sensor
The design method of device has excellent response sensitivity using nanometer gas sensor prepared by the preparation method to ammonia.
The purpose of the present invention is achieved through the following technical solutions：
A kind of heater-type ammonia gas sensor provided by the invention, including ceramic tube, gas sensor, electrode and heating wire；Institute
It states gas sensor to be set on ceramic tube, the gas sensor is provided at both ends with electrode, and the heating wire is set in ceramic tube
For heating ceramic pipe；The gas sensor uses gas sensitive Ag-WS2Nano-powder makes.
Further, the gas sensitive Ag-WS2Nano-powder is through the following steps that make：
S1：Ammonium metatungstate is dissolved in deionized water, heating water bath stirring, so that it is fully dissolved formation and contain charged particle
Inorganic salts；
S2：Appropriate PVP, absolute ethyl alcohol and DMF are weighed, is equipped with PVP macromolecule precursor solutions, and ammonium metatungstate solution is equal
It is even to be added dropwise in PVP solution；It is put into experiment cabinet and stands after sealing；
S3：It takes out the composite solution after standing and is uniformly mixed；
S4：Extract appropriate precursor solution；
S5：Start electrospinning device and forms composite fibrofelt in metallic plate：
S6：Metallic plate is put into air dry oven to be dried；The composite fibrofelt removed after drying on metallic plate is placed
It is being sintered in resistance furnace, powder is taken out in furnace cooling to room temperature；By the powder mull of taking-up it is uniform after be laid in crucible；
S7：It takes appropriate S powder to be fitted into crucible and is put into progress vulcanization reaction generation tungsten disulphide powder in burner hearth；It is cooled to room
Temperature takes out tungsten disulphide powder；
S8：Tungsten disulphide powder is ground uniformly, places in vacuum drying chamber and is dried to obtain sample；
S9：Sample is subjected to envelope characterization；
S91：By AgNO3It is dissolved in deionized water, PVP solution is then added, is stirred evenly after to be dissolved；
S92：NaBH is added4Dissolving obtains reaction precursor solution；
S93：Tungsten disulphide powder is added in reaction precursor solution and stirs to get sediment；
S94：Respectively with absolute ethyl alcohol and deionized water by sediment carry out the impurity in centrifuge washing removal sediment from
Son obtains impurity elimination sediment；
S96：Impurity elimination sediment is placed in drying in air dry oven and obtains Ag-WS2。
Further, the cleaning of the ceramic tube uses chemical cleaning；The chemical cleaning refers to that ceramic tube is immersed in one
Determine a period of time in the dilute hydrochloric acid of concentration, ceramic tube is put into the beaker equipped with absolute ethyl alcohol again after having impregnated and carries out ultrasound clearly
It washes；Ceramic tube is taken out, is placed in vacuum drying chamber dry.
The present invention also provides a kind of preparation methods of heater-type ammonia gas sensor, include the following steps：
Suitable gas sensitive Ag-WS is weighed first2Nano-powder and organic binder, which pour into mortar, to be fully ground
It is even；Appropriate amount of deionized water is instilled in mortar, and powder is reconciled into air-sensitive slurry；It is cleaned and dried ceramic tube；
Then air-sensitive slurry is uniformly coated on dried ceramic tube, is put into drying box and is dried after coating；
And then it is sintered and obtains slug type heater-type gas sensor；Heating wire is penetrated into ceramic tube；
The fixing pin of gas sensor electrode is finally set on ceramic tube；Consolidating for heating wire electrode is set on ceramic tube
Fixed tube foot；And aging gas sensor obtains heater-type ammonia gas sensor.
Further, the gas sensitive Ag-WS2The making of nano-powder is as follows：
S1：Ammonium metatungstate is dissolved in deionized water, heating water bath stirring, so that it is fully dissolved formation and contain charged particle
Inorganic salts；
S2：Appropriate PVP, absolute ethyl alcohol and DMF are weighed, is equipped with PVP macromolecule precursor solutions, and ammonium metatungstate solution is equal
It is even to be added dropwise in PVP solution；It is put into experiment cabinet and stands after sealing；
S3：It takes out the composite solution after standing and is uniformly mixed；
S4：Extract appropriate precursor solution；
S5：Start electrospinning device and collects composite fibrofelt in metallic plate：
S6：Metallic plate is put into air dry oven to be dried；The composite fibrofelt removed after drying on metallic plate is placed
It is being sintered in resistance furnace, powder is taken out in furnace cooling to room temperature；By the powder mull of taking-up it is uniform after be laid in crucible；
S7：It takes appropriate S powder to be fitted into crucible and is put into progress vulcanization reaction generation tungsten disulphide powder in burner hearth；It is cooled to room
Temperature takes out tungsten disulphide powder；
S8：Tungsten disulphide powder is ground uniformly, places in vacuum drying chamber and is dried to obtain sample；
S9：Sample is subjected to envelope characterization.
Further, further comprising the steps of：
S91：By AgNO3It is dissolved in deionized water, PVP solution is then added, is stirred evenly after to be dissolved；
S92：NaBH is added4Dissolving obtains reaction precursor solution；
S93：Tungsten disulphide powder is added in reaction precursor solution and stirs to get sediment；
S94：Respectively with absolute ethyl alcohol and deionized water by sediment carry out the impurity in centrifuge washing removal sediment from
Son obtains impurity elimination sediment；
S96：Impurity elimination sediment is placed in drying in air dry oven and obtains Ag-WS2。
Further, the temperature of the heating water bath in the step S1 is 50-70 DEG C；The heating stirring time is 1-2 hours；
Sealing in the step S2 is sealed using sealed membrane；Time of repose is 24-48 hours；
The stirring of composite solution in the step S3 uses magnetic stirrer 2-3h；
Metallic plate drying in the step S5, which uses, is integrally put into aluminum metal sheets in air dry oven, drying temperature
It is 60-80 DEG C；Drying time is 6-8h；
The temperature of resistance furnace in the step S7 is 700-800 degree；Sintering time is 3-5h；
Placing powder in vacuum drying chamber in the step 10, drying time 6-8h.
Further, the startup electrospinning device forms composite fibrofelt in metallic plate, and detailed process is as follows：It will polish
Syringe needle point be connected with high-voltage positive electrode, stick aluminium-foil paper aluminum metal sheets be grounded as cathode；Regulate spinning voltage,
Fltting speed starts spinning after receiving distance.
By adopting the above-described technical solution, the present invention has the advantage that：
The present invention is prepared using the method that electrostatic spinning combines annealing；Choose ammonium metatungstate (NH4)6H2W12O40For original
Ammonium metatungstate (NH has been prepared using method of electrostatic spinning with PVP (K90) for polymer precursor Polymer Solution in material4)6H2W12O40/ PVP composite fibrofelts；Composite fibrofelt is put into high temperature resistance furnace annealing calcining and obtained from being taken off on aluminium-foil paper
WO3Fiber；By WO in tube furnace3Fiber carries out the nanometer that vulcanization reaction has synthesized lamellar with sulphur powder under nitrogen protection
WS2, while using polyalcohol chemical method by Ag nanoparticle depositions to WS2The surface of nanometer sheet, in WS2The surface of nanometer sheet is equal
It deposited a large amount of Ag nano particles evenly, and sample does not occur too with undoped sample in structure and pattern after doping
It is change more.
Method provided by the invention can prepare the WS of high quality2Nano material, due to the doping of noble metal nano particles
Adsorption capacity of the gas sensitive surface to target gas molecules can be promoted, by being received with stratiform that is being doped with noble metal to undoped
Rice WS2Carry out gas sensitization performance contrast test, the results showed that：Under 220 DEG C of optimum working temperature, nanometer WS2Gas sensor
There are excellent response sensitivity, excellent selectivity, quickly response and recovery characteristics to ammonia, and the doping of Ag particles carries
The high sensitivity of gas sensor and do not influence selection characteristic and response recovery characteristics.
Other advantages, target and the feature of the present invention will be illustrated in the following description to a certain extent, and
And to a certain extent, based on will be apparent to those skilled in the art to investigating hereafter, Huo Zheke
To be instructed from the practice of the present invention.The target and other advantages of the present invention can by following specification realizing and
It obtains.
Description of the drawings
The description of the drawings of the present invention is as follows.
Fig. 1 is the lamellar WS of the present invention2Nanometer sheet preparation process schematic diagram.
Fig. 2 is the Ag-WS of the present invention2Preparation process schematic diagram.
Fig. 3 is the heater-type gas-sensitive element structure schematic diagram of the present invention.
Fig. 4 is the gas sensor fabrication processing of the present invention.
In figure：1. ceramic tube；2. gas sensor；3. electrode；4. heating wire.
Specific implementation mode
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1
The present embodiment introduces the main process about method of electrostatic spinning first：
1. presoma Polymer Solution charges under electrostatic field and generate deformation, pendency taper drop is formed in injection
Tip end；2. when adjusting DC high-voltage power supply makes electrostatic field intensity be more than critical value, tip end droplet surface charge
Repulsion is more than its surface tension, and polymer solution is ejected with pattern from tip end high speed；3. in the jet stream short time
By the high-speed stretch of electric field force, the natural volatilization of organic solvent, it is finally deposited on receiver board, forms polymer fiber.
Electrostatic spinning prepares the nanofiber that draw ratio is more than 1000, and mild condition, yield is huge, applied widely
And production process is simple.The structure of the 1-dimention nano fiber prepared by electrostatic spinning technique is conducive to the transfer mesh of rapid, high volume
Mark molecule reaches or leaves conversion zone, since it is with continuous length, can easily be incited somebody to action between working electrode
Sensing electric signal shifts back and forth, to strengthen sensing capabilities, reduces consumption of the electrical signal in transmittance process, and then improve
Response-recovery time and raising sensitivity, can prepare high efficiency gas sensor.
As shown in Figure 1, the preparation method provided in this embodiment for making the gas sensitive of heater-type ammonia gas sensor,
Specifically include following steps：
S1：Ammonium metatungstate is dissolved in deionized water, heating water bath stirring, so that it is fully dissolved formation and contain charged particle
Inorganic salts；
S2：Appropriate PVP, absolute ethyl alcohol and DMF are weighed, is equipped with PVP macromolecule precursor solutions, and ammonium metatungstate solution is equal
It is even to be added dropwise in PVP solution；It is put into experiment cabinet and stands after sealing；
S3：It takes out the composite solution after standing and is uniformly mixed；
S4：Extract appropriate precursor solution；
S5：Start electrospinning device and forms composite fibrofelt in metallic plate：
S6：Metallic plate is put into air dry oven to be dried；The composite fibrofelt removed after drying on metallic plate is placed
It is being sintered in resistance furnace, powder is taken out in furnace cooling to room temperature；By the powder mull of taking-up it is uniform after be laid in crucible；
S7：It takes appropriate S powder to be fitted into crucible and is put into progress vulcanization reaction generation tungsten disulphide powder in burner hearth；It is cooled to room
Temperature takes out tungsten disulphide powder；
S8：Tungsten disulphide powder is ground uniformly, places in vacuum drying chamber and is dried to obtain sample；
S9：Sample is subjected to envelope characterization.
S91：By AgNO3It is dissolved in deionized water, PVP solution is then added, is stirred evenly after to be dissolved；
S92：NaBH is added4Dissolving obtains reaction precursor solution；
S93：Tungsten disulphide powder is added in reaction precursor solution and stirs to get sediment；
S94：Respectively with absolute ethyl alcohol and deionized water by sediment carry out the impurity in centrifuge washing removal sediment from
Son obtains impurity elimination sediment；
S96：Impurity elimination sediment is placed in drying in air dry oven and obtains Ag-WS2。
The temperature of heating water bath in the step S1 is 50-70 DEG C；The heating stirring time is 1-2 hours；
Sealing in the step S2 is sealed using sealed membrane；Time of repose is 24-48 hours；
The stirring of composite solution in the step S3 uses magnetic stirrer 2-3h；
Metallic plate drying in the step S5, which uses, is integrally put into aluminum metal sheets in air dry oven, drying temperature
It is 60-80 DEG C；Drying time is 6-8h；
The temperature of resistance furnace in the step S7 is 700-800 degree；Sintering time is 3-5h；
Placing powder in vacuum drying chamber in the step 10, drying time 6-8h.
The startup electrospinning device forms composite fibrofelt in metallic plate, and detailed process is as follows：The injection that will be polished
Device needle point is connected with high-voltage positive electrode, and the aluminum metal sheets for sticking aluminium-foil paper is grounded as cathode；It regulates spinning voltage, promote speed
Degree starts spinning after receiving distance.
Embodiment 2
As shown in Fig. 2, gas sensor preparation method provided in this embodiment, includes the following steps：
S51：Weigh suitable gas sensitive Ag-WS2Nano-powder and organic binder, which pour into mortar, to be fully ground
It is even；
S52：Appropriate amount of deionized water is instilled in mortar, and powder is reconciled into air-sensitive slurry；
S53：It is cleaned and dried ceramic tube；
S54：Air-sensitive slurry is uniformly coated on dried ceramic tube, is put into drying box and is dried after coating；
S55：Sintering obtains slug type heater-type gas sensor；
S56：Heating wire is penetrated into ceramic tube；
S57：The fixing pin of gas sensor electrode is set on ceramic tube；Consolidating for heating wire electrode is set on ceramic tube
Fixed tube foot；
S58：Aging gas sensor.
Gas sensitive Ag-WS in the step S512Nano-powder is through the following steps that make：
S1：Ammonium metatungstate is dissolved in deionized water, heating water bath stirring, so that it is fully dissolved formation and contain charged particle
Inorganic salts；
S2：Appropriate PVP, absolute ethyl alcohol and DMF are weighed, is equipped with PVP macromolecule precursor solutions, and ammonium metatungstate solution is equal
It is even to be added dropwise in PVP solution；It is put into experiment cabinet and stands after sealing；
S3：It takes out the composite solution after standing and is uniformly mixed；
S4：Extract appropriate precursor solution；
S5：Start electrospinning device and forms composite fibrofelt in metallic plate：
S6：Metallic plate is put into air dry oven to be dried；The composite fibrofelt removed after drying on metallic plate is placed
It is being sintered in resistance furnace, powder is taken out in furnace cooling to room temperature；By the powder mull of taking-up it is uniform after be laid in crucible；
S7：It takes appropriate S powder to be fitted into crucible and is put into progress vulcanization reaction generation tungsten disulphide powder in burner hearth；It is cooled to room
Temperature takes out tungsten disulphide powder；
S8：Tungsten disulphide powder is ground uniformly, places in vacuum drying chamber and is dried to obtain sample；
S9：Sample is subjected to envelope characterization.
S91：By AgNO3It is dissolved in deionized water, PVP solution is then added, is stirred evenly after to be dissolved；
S92：NaBH is added4Dissolving obtains reaction precursor solution；
S93：Tungsten disulphide powder is added in reaction precursor solution and stirs to get sediment；
S94：Respectively with absolute ethyl alcohol and deionized water by sediment carry out the impurity in centrifuge washing removal sediment from
Son obtains impurity elimination sediment；
S96：Impurity elimination sediment is placed in drying in air dry oven and obtains Ag-WS2。
The cleaning of the ceramic tube uses chemical cleaning；The chemical cleaning refer to ceramic tube is immersed in it is certain density
Ceramic tube, is put into the beaker equipped with absolute ethyl alcohol after having impregnated and is cleaned by ultrasonic by a period of time again in dilute hydrochloric acid；It takes out
Ceramic tube is placed in vacuum drying chamber dry.
Embodiment 3
As shown in Figure 3 and Figure 4, heater-type gas sensor provided in this embodiment, including ceramic tube, gas sensor, electricity
Pole and heating wire；The gas sensor is set on ceramic tube, and the gas sensor is provided at both ends with electrode, and the heating wire is set
It is placed in ceramic tube and is used for heating ceramic pipe.
The gas sensor uses gas sensitive Ag-WS2Nano-powder makes, the gas sensitive Ag-WS2Nano-powder
Through the following steps that make：
S1：Ammonium metatungstate is dissolved in deionized water, heating water bath stirring, so that it is fully dissolved formation and contain charged particle
Inorganic salts；
S2：Appropriate PVP, absolute ethyl alcohol and DMF are weighed, is equipped with PVP macromolecule precursor solutions, and ammonium metatungstate solution is equal
It is even to be added dropwise in PVP solution；It is put into experiment cabinet and stands after sealing；
S3：It takes out the composite solution after standing and is uniformly mixed；
S4：Extract appropriate precursor solution；
S5：Start electrospinning device and forms composite fibrofelt in metallic plate：
S6：Metallic plate is put into air dry oven to be dried；The composite fibrofelt removed after drying on metallic plate is placed
It is being sintered in resistance furnace, powder is taken out in furnace cooling to room temperature；By the powder mull of taking-up it is uniform after be laid in crucible；
S7：It takes appropriate S powder to be fitted into crucible and is put into progress vulcanization reaction generation tungsten disulphide powder in burner hearth；It is cooled to room
Temperature takes out tungsten disulphide powder；
S8：Tungsten disulphide powder is ground uniformly, places in vacuum drying chamber and is dried to obtain sample；
S9：Sample is subjected to envelope characterization.
S91：By AgNO3It is dissolved in deionized water, PVP solution is then added, is stirred evenly after to be dissolved；
S92：NaBH is added4Dissolving obtains reaction precursor solution；
S93：Tungsten disulphide powder is added in reaction precursor solution and stirs to get sediment；
S94：Respectively with absolute ethyl alcohol and deionized water by sediment carry out the impurity in centrifuge washing removal sediment from
Son obtains impurity elimination sediment；
S96：Impurity elimination sediment is placed in drying in air dry oven and obtains Ag-WS2。
Finally illustrate, the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although with reference to compared with
Good embodiment describes the invention in detail, it will be understood by those of ordinary skill in the art that, it can be to the skill of the present invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of the technical program, should all be covered in the present invention
Right in.
Claims (6)
1. a kind of heater-type ammonia gas sensor, it is characterised in that：Including ceramic tube, gas sensor, electrode and heating wire；The gas
Quick element is set on ceramic tube, and the gas sensor is provided at both ends with electrode, and the heating wire, which is set in ceramic tube, to be used for
Heating ceramic pipe；The gas sensor uses gas sensitive Ag-WS2Nano-powder makes；
The gas sensitive Ag-WS2Nano-powder is through the following steps that make：
S1：Ammonium metatungstate is dissolved in deionized water, heating water bath stirring makes it fully dissolve and forms the nothing containing charged particle
Machine salt；
S2：Appropriate PVP, absolute ethyl alcohol and DMF are weighed, is equipped with PVP macromolecule precursor solutions, and ammonium metatungstate solution is uniformly dripped
Enter into PVP solution；It is put into experiment cabinet and stands after sealing；
S3：It takes out the composite solution after standing and is uniformly mixed；
S4：Extract appropriate precursor solution；
S5：Start electrospinning device and forms composite fibrofelt in metallic plate：
S6：Metallic plate is put into air dry oven to be dried；The composite fibrofelt removed after drying on metallic plate is positioned over electricity
It is being sintered in resistance stove, powder is taken out in furnace cooling to room temperature；By the powder mull of taking-up it is uniform after be laid in crucible；
S7：It takes appropriate S powder to be fitted into crucible and is put into progress vulcanization reaction generation tungsten disulphide powder in burner hearth；Room temperature is cooled to take
Go out tungsten disulphide powder；
S8：Tungsten disulphide powder is ground uniformly, places in vacuum drying chamber and is dried to obtain sample；
S9：Sample is subjected to envelope characterization；
S91：By AgNO3It is dissolved in deionized water, PVP solution is then added, is stirred evenly after to be dissolved；
S92：NaBH is added4Dissolving obtains reaction precursor solution；
S93：Tungsten disulphide powder is added in reaction precursor solution and stirs to get sediment；
S94：Sediment the foreign ion in centrifuge washing removal sediment is carried out with absolute ethyl alcohol and deionized water respectively to obtain
To impurity elimination sediment；
S95 ：Impurity elimination sediment is placed in drying in air dry oven and obtains Ag-WS2。
2. heater-type ammonia gas sensor as described in claim 1, it is characterised in that：The cleaning of the ceramic tube is clear using chemistry
It washes；The chemical cleaning refers to that ceramic tube is immersed in a period of time in certain density dilute hydrochloric acid, again will be ceramic after having impregnated
Pipe, which is put into the beaker equipped with absolute ethyl alcohol, to be cleaned by ultrasonic；Ceramic tube is taken out, is placed in vacuum drying chamber dry.
3. a kind of preparation method of heater-type ammonia gas sensor, it is characterised in that：Include the following steps：
Suitable gas sensitive Ag-WS is weighed first2Nano-powder and organic binder, which pour into mortar, to be fully ground uniformly；
Appropriate amount of deionized water is instilled in mortar, and powder is reconciled into air-sensitive slurry；It is cleaned and dried ceramic tube；
Then air-sensitive slurry is uniformly coated on dried ceramic tube, is put into drying box and is dried after coating；In turn
Sintering obtains slug type heater-type gas sensor；Heating wire is penetrated into ceramic tube；
The fixing pin of gas sensor electrode is finally set on ceramic tube；The fixing pipe of heating wire electrode is set on ceramic tube
Foot；And aging gas sensor obtains heater-type ammonia gas sensor；
The gas sensitive Ag-WS2The making of nano-powder is as follows：
S1：Ammonium metatungstate is dissolved in deionized water, heating water bath stirring makes it fully dissolve and forms the nothing containing charged particle
Machine salt；
S2：Appropriate PVP, absolute ethyl alcohol and DMF are weighed, is equipped with PVP macromolecule precursor solutions, and ammonium metatungstate solution is uniformly dripped
Enter into PVP solution；It is put into experiment cabinet and stands after sealing；
S3：It takes out the composite solution after standing and is uniformly mixed；
S4：Extract appropriate precursor solution；
S5：Start electrospinning device and collects composite fibrofelt in metallic plate：
S6：Metallic plate is put into air dry oven to be dried；The composite fibrofelt removed after drying on metallic plate is positioned over electricity
It is being sintered in resistance stove, powder is taken out in furnace cooling to room temperature；By the powder mull of taking-up it is uniform after be laid in crucible；
S7：It takes appropriate S powder to be fitted into crucible and is put into progress vulcanization reaction generation tungsten disulphide powder in burner hearth；Room temperature is cooled to take
Go out tungsten disulphide powder；
S8：Tungsten disulphide powder is ground uniformly, places in vacuum drying chamber and is dried to obtain sample；
S9：Sample is subjected to envelope characterization.
4. the preparation method of heater-type ammonia gas sensor as claimed in claim 3, it is characterised in that：It is further comprising the steps of：
S91：By AgNO3It is dissolved in deionized water, PVP solution is then added, is stirred evenly after to be dissolved；
S92：NaBH is added4Dissolving obtains reaction precursor solution；
S93：Tungsten disulphide powder is added in reaction precursor solution and stirs to get sediment；
S94：Sediment the foreign ion in centrifuge washing removal sediment is carried out with absolute ethyl alcohol and deionized water respectively to obtain
To impurity elimination sediment；
S95 ：Impurity elimination sediment is placed in drying in air dry oven and obtains Ag-WS2。
5. the preparation method of heater-type ammonia gas sensor as claimed in claim 3, it is characterised in that：Water in the step S1
The temperature of bath heating is 50-70 DEG C；The heating stirring time is 1-2 hours；
Sealing in the step S2 is sealed using sealed membrane；Time of repose is 24-48 hours；
The stirring of composite solution in the step S3 uses magnetic stirrer 2-3h；
Using aluminum metal sheets to be integrally put into air dry oven, drying temperature is for metallic plate drying in the step S6
60-80℃；Drying time is 6-8h；
The temperature of resistance furnace in the step S6 is 700-800 degree；Sintering time is 3-5h；
Placing powder in vacuum drying chamber in the step S8, drying time 6-8h.
6. the preparation method of heater-type ammonia gas sensor as claimed in claim 3, it is characterised in that：The startup electrostatic spinning
Equipment forms composite fibrofelt in metallic plate, and detailed process is as follows：The syringe needle point polished is connected with high-voltage positive electrode, is sticked
The aluminum metal sheets ground connection of aluminium-foil paper is used as cathode；Start spinning after regulating spinning voltage, fltting speed, reception distance.
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| CN106018480B true CN106018480B (en) | 2018-08-24 |
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| CN106596452B (en) * | 2016-12-30 | 2019-03-22 | 重庆理工大学 | The detection method of these hydrogen sulfide gas sensor and preparation method thereof and concentration of hydrogen sulfide |
| CN107219269B (en) * | 2017-04-26 | 2019-04-19 | 北京科技大学 | With ammonia gas sensor and preparation method thereof at room temperature |
| CN108240967B (en) * | 2018-01-11 | 2023-05-12 | 重庆理工大学 | Gas-sensitive characteristic response curve testing device with cover |
| CN112357944B (en) * | 2020-11-04 | 2023-04-07 | 广西大学 | Preparation method of lanthanum oxide composite material sensitive to low-concentration ammonia gas |
| CN114014367B (en) * | 2021-12-03 | 2023-12-01 | 四川恒瑞天成科技有限公司 | WO (WO) 3-x -WS 2 One-dimensional-two-dimensional heterojunction, preparation method and application |
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