CN107219269A - With ammonia gas sensor at room temperature and preparation method thereof - Google Patents
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Abstract
The invention belongs to sensor technical field, and in particular to a kind of ammonia gas sensor used at room temperature and preparation method thereof, the ammonia gas sensor includes gas sensitive and substrate, and the gas sensitive is one-dimensional SrGe4O9Nanotube.Institute's gas sensitive is one-dimensional SrGe4O9Nanotube and noble metal, the load capacity of noble metal is 0.01 2%wt.Present invention has the advantages that：Due to using above-mentioned technical proposal, performance of the present invention in terms of normal temperature air-sensitive is excavated.Electrostatic spinning technique make use of to be prepared for SrGe4O9Nanotube；This dominance structure of nanotube is make use of, it is effective to improve its performance, in SrGe4O9Depositing noble metal Pt on the basis of nanotube, improves its air-sensitive performance.Due to Pt SrGe4O9Normal temperature air-sensitive performance, be that its application on flexible electronic device is provided convenience, the gas sensor of normal temperature be made in substrate.
Description
Technical field：
The invention belongs to sensor technical field, and in particular to a kind of with ammonia gas sensor at room temperature and preparation method thereof.
Background technology：
As modern industrial technology is developed rapidly, natural environment inevitably subjects serious burden, wherein atmosphere pollution
It is exactly an acid test.Poisonous, pernicious gas leakage pollution environment destruction life in industrial waste gas and life in production
State, not only causes huge property loss, goes back that entail dangers to is healthy and life security.Detection, prison to harmful poisonous gas
Control, the research of alarm increasingly cause the great attention of people.The appearance of gas sensor is solution detection toxic and harmful gas
Provide convenience, high-performance gas sensor turns into the emphasis and focus studied both at home and abroad in recent years.Gas sensor is a kind of
Gas componant and change in concentration can be converted into electric signal be used for detect electronic device, be with a wide range of applications with it is wide
Development prospect.Detection at present both at home and abroad for various gases is main or for harmful gas, such as ammonia, ethanol,
Hydrogen, hydrogen sulfide, toluene, piped gas etc. are gone back based on imflammable gas and toxic gas, widely used gas sensitive
Mainly SnO2、ZnO、In3O4、Fe2O3、WO3Deng metal oxide materials.But these materials when being applied to gas sensor all
Need under conditions of certain temperature, thus it is significant to the research of gas sensor at room temperature.
As nanosecond science and technology are in the sustained and rapid development in the whole world, size that nano material is reduced due to it, higher precision
And the concern of vast researcher is obtained, nano material has larger specific surface area, high surface-active, with conventional material
Compared to the advantage for having uniqueness.And application of the nanometer technology on gas sensitive, it can largely solve traditional gas sensitive
The poor selectivity of presence, the problems such as sensitivity is low, stability is poor.
The content of the invention：
It is simple it is an object of the invention to provide a kind of method in order to solve the above problems, and improve gas absorption effect and phase
The ammonia gas sensor of the use for the reaction speed answered at room temperature and preparation method thereof.
The technical scheme is that：A kind of ammonia gas sensor used at room temperature, the ammonia gas sensor includes air-sensitive material
Material and substrate, the gas sensitive are one-dimensional SrGe4O9Nanotube.
Further, the gas sensitive is the one-dimensional SrGe of S4O9Nanotube and noble metal, the load capacity of the noble metal is
0.01-2%wt。
Further, the noble metal is Pt or Pd.
Further, the substrate is flexible material or rigid material.
Further, the flexible material includes PET, PI or PC.
Further, the rigid material includes ceramics, glass or titanium dioxide silicon chip.
It is a further object of the present invention to provide the method for above-mentioned ammonia gas sensor, following steps are specifically included：
The configuration of step 1. precursor solution：At room temperature, according to mol ratio 1:4 mix strontium salt powder and ethyoxyl germanium,
Add 2g-4g absolute ethyl alcohols, 16g-18g N,N-dimethylformamides（DMF）With it is molten in 0.5g-1g deionized water mixed solutions
Solution, adds 2.5g-3g polyvinylpyrrolidonepowder powders, finally, by mixed solution magnetic agitation 4-7 hour, until mixing
Close solution clear homogeneous, then, draw about solution with dropper and instill disposable syringe, prepare to start electrospinning；
The preparation of step 2. nanotube：The syringe needle of disposable syringe is connect to the positive pole of high-voltage DC power supply, and is fixed on from receipts
At the height 15-20cm for collecting plate, spinning voltage is set to 15-20KV, and clean aluminium foil is fixed into desktop is connected to high voltage power supply
Negative pole.High voltage power supply is opened, the syringe needle of disposable needle tubing taylor cone occurs and starts spinning, one is deposited on receiver aluminium foil and is sunk
Nanofiber, after spinning terminates, puts it into Muffle furnace and makes annealing treatment, heating rate is 4-6 DEG C/min, is warming up to 680-
720 DEG C, soaking time is 3.5-5 hours, is then freely cooled to room temperature, finally obtains one-dimensional SrGe4O9Nanotube；
The making of step 3. sensor：
Step 3.1：Substrate is cleaned successively using acetone, ethanol and distilled water, it is standby；
Step 3.2：Weigh appropriate one-dimensional SrGe4O9Nanotube is put into mortar, is added appropriate deionized water, is ground
Mill, is dipped with fine, soft fur pen and is coated on rigid electrode, that is, obtain ammonia gas sensor；Or photoresist is spin-coated on PET at 5000 turns
30s, 100 DEG C of 3 min of heating, then use ultraviolet photolithographic machine photoetching, and are developed with developer solution on flexible substrates, obtain and
The corresponding interdigital electrode of mask plate, then 50nm gold is plated on surface, unnecessary gold is washed away with acetone, step 2 prepares one
Tie up SrGe4O9Nanotube and Kynoar (PVDF) with mass ratio 9：1 ratio mixing, it is uniform to be coated in interdigital electrode；
Obtain ammonia gas sensor.
Further, the step 2 is further comprising the steps of：Then platinum acid chloride solution is prepared, the sample calcined in right amount is taken
Mortar is placed in, a small amount of platinum acid chloride solution is taken, mortar and SrGe are added dropwise to according to the ratio of load 0.01-2%wt noble metal4O9Receive
Mitron is sufficiently mixed.
Further, the technique made annealing treatment in the step 2 is：Heating rate is 4-6 DEG C/min, is warming up to 680-720
DEG C, soaking time is 3.5-5 hours.
Further, the strontium salt includes strontium nitrate or strontium acetate.
The present invention has the characteristics that and advantage compared with prior art：
（1）SrGe4O9This lithium electricity that is all used in mostly waits other aspects.Its performance in terms of normal temperature air-sensitive is dug
Pick.
（2）SrGe4O9This existing pattern of material is mainly nano wire, make use of electrostatic spinning technique to be prepared for
SrGe4O9Nanotube；This dominance structure of nanotube is make use of, it is effective to improve its performance.
（3）In SrGe4O9Depositing noble metal Pt on the basis of nanotube, improves its air-sensitive performance.
（4）Due to Pt-SrGe4O9Normal temperature air-sensitive performance, be that its application on flexible electronic device is provided convenience,
The gas sensor of normal temperature has been made on flexible substrates.（It please supplement experimental data）Experimental data will add to beneficial effect
In.
Brief description of the drawings：
Fig. 1 is a kind of structural representation with ammonia gas sensor at room temperature of the present invention.
Fig. 2 is SrGe of the present invention4O9The SEM figures of nanotube.
Fig. 3 is Pt-SrGe of the present invention4O9The SEM figures of nanotube.
Fig. 4 is SrGe of the present invention4O9The test chart of the ceramic base gas sensor of nanotube.
Fig. 5 is Pt-SrGe4O9The test chart of the ceramic base gas sensor of nanotube.
Fig. 6 is Pt-SrGe4O9The differently curved angle measurement figure of flexible gas sensor of nanotube.
In figure：
1. substrate, 2. gas sensitives, 3. electrodes.
Embodiment：
It is described further below by embodiment and with reference to accompanying drawing, but the present invention is not limited to following examples.
A kind of ammonia gas sensor used at room temperature of the present invention, the ammonia gas sensor includes gas sensitive and substrate, described
Gas sensitive is one-dimensional SrGe4O9Nanotube.
The gas sensitive is the one-dimensional SrGe of S4O9Nanotube and noble metal, the load capacity of the noble metal is 0.01-2%
wt。
The noble metal is Pt or Pd.
The substrate is flexible material or rigid material.
The flexible material includes PET, PI or PC.
The rigid material includes ceramics, glass or titanium dioxide silicon chip.
A kind of method of ammonia gas sensor, specifically includes following steps：
The configuration of step 1. precursor solution：At room temperature, according to mol ratio 1:4 by strontium nitrate Sr (NO3)2Powder and ethyoxyl
Germanium is mixed, and adds 2g-4g absolute ethyl alcohols, 16g-18g DMFs（DMF）With the mixing of 0.5g-1g deionized waters
Dissolved in solution, add 2.5g-3g polyvinylpyrrolidonepowder powders, it is finally, mixed solution magnetic agitation 4-7 is small
When, until mixed solution clear is homogeneous, then, draws about solution with dropper and instill disposable syringe, prepare to start electricity
Spin；
The preparation of step 2. nanotube：The syringe needle of disposable syringe is connect to the positive pole of high-voltage DC power supply, and is fixed on from receipts
At the height 15-20cm for collecting plate, spinning voltage is set to 15-20KV, and clean aluminium foil is fixed into desktop is connected to high voltage power supply
Negative pole.High voltage power supply is opened, the syringe needle of disposable needle tubing taylor cone occurs and starts spinning, one is deposited on receiver aluminium foil and is sunk
Nanofiber, after spinning terminates, puts it into Muffle furnace and makes annealing treatment, heating rate is 4-6 DEG C/min, is warming up to 680-
720 DEG C, soaking time is 3.5-5 hours, is then freely cooled to room temperature, finally obtains one-dimensional SrGe4O9Nanotube；
The making of step 3. sensor：
Step 3.1：Substrate is cleaned successively using acetone, ethanol and distilled water, it is standby；
Step 3.2：Weigh appropriate one-dimensional SrGe4O9Nanotube is put into mortar, is added appropriate deionized water, is ground
Mill, is dipped with fine, soft fur pen and is coated on rigid electrode, that is, obtain ammonia gas sensor；Or photoresist is spin-coated on PET at 5000 turns
30s, 100 DEG C of 3 min of heating, then use ultraviolet photolithographic machine photoetching, and are developed with developer solution on flexible substrates, obtain and
The corresponding interdigital electrode of mask plate, then 50nm gold is plated on surface, unnecessary gold is washed away with acetone, step 2 prepares one
Tie up SrGe4O9Nanotube and Kynoar (PVDF) with mass ratio 9：1 ratio mixing, it is uniform to be coated in interdigital electrode；
Obtain ammonia gas sensor.
The step 2 is further comprising the steps of：Then platinum acid chloride solution is prepared, takes the sample calcined in right amount to be placed in and grinds
Alms bowl, takes a small amount of platinum acid chloride solution, and mortar and SrGe are added dropwise to according to the ratio of load 0.01-2%wt noble metal4O9Nanotube fills
Divide mixing.
The technique made annealing treatment in the step 2 is：Heating rate is 4-6 DEG C/min, is warming up to 680-720 DEG C, insulation
Time is 3.5-5 hours.
Embodiment 1：
With one-dimensional SrGe4O9Preparation process is discussed in detail exemplified by nanotube：
（1）The configuration of precursor solution：At room temperature, according to mol ratio 1:4 by 0.1046g strontium nitrate Sr (NO3)2Powder and
0.5g ethyoxyl germanium（[Ge(OEt)4]）Mix, be put into 3.5g absolute ethyl alcohols, 17.5g DMFs（DMF）With
Dissolved in 0.5g deionized water mixed solutions, add 2.99g polyvinylpyrrolidone（PVP, 1,300,000 molecular weight）Powder.
Finally, by mixed solution magnetic agitation 4 hours, until mixed solution clear is homogeneous.Then, drawn about with dropper
1ml solution instills disposable syringe, prepares to start electrospinning.
（2）The preparation of nanotube：The syringe needle of disposable syringe is connect to the positive pole of high-voltage DC power supply, and is fixed on from receipts
At the height 15cm for collecting plate.Spinning voltage is set to 15KV or so.Clean aluminium foil is fixed into desktop and is connected to the negative of high voltage power supply
Pole.High voltage power supply is opened, the syringe needle of disposable needle tubing taylor cone occurs and starts spinning.Deposition one is heavy on receiver aluminium foil receives
Rice fiber.After spinning terminates, put it into Muffle furnace and anneal, the technique of annealing is：Heating rate is 5 DEG C/min, is risen
Temperature is to 700 DEG C, and soaking time is 4 hours, is then freely cooled to room temperature, finally obtains pure metal oxide nanotubes,
As shown in Figure 2.Then platinum acid chloride solution is prepared, takes the sample calcined in right amount to be placed in mortar, a small amount of platinum acid chloride solution is taken, presses
Ratio according to load 0.5wt% Pt is added dropwise to mortar and SrGe4O9Nanotube is sufficiently mixed, and 500 DEG C of calcinings are carried out after drying, are protected
Warm 1 hour, obtain deposited Pt one-dimensional SrGe4O9Nanotube, such as accompanying drawing 3.
（3）Flexible gas sensor production：
In order to assemble flexible gas sensor, PET matrix is cleaned successively using acetone, ethanol and distilled water.Photoresist
PET is spin-coated in 5000 turns of 30s, 100 DEG C of 3 min of heating, then use ultraviolet photolithographic machine photoetching, and entered with developer solution on substrate
Row development.Interdigital electrode corresponding with mask plate is obtained, then 50nm gold is plated on surface, unnecessary gold is washed away with acetone.Institute
The Pt- SrGe of system4O9With Kynoar (PVDF) with mass ratio 9：1 ratio mixing, it is uniform to be coated in interdigital electrode；
To flexible gas sensor, such as accompanying drawing 4.
Embodiment 2：
With one-dimensional SrGe4O9Preparation process is discussed in detail exemplified by nanotube：
（1）The configuration of precursor solution：At room temperature, according to mol ratio 1:4 by 0.1046g strontium acetate Sr (NO3)2Powder and
0.5g ethyoxyl germanium（[Ge(OEt)4]）Mix, be put into 3.5g absolute ethyl alcohols, 17.5g DMFs（DMF）With
Dissolved in 0.5g deionized water mixed solutions, add 2.99g polyvinylpyrrolidone（PVP, 1,300,000 molecular weight）Powder.
Finally, by mixed solution magnetic agitation 4 hours, until mixed solution clear is homogeneous.Then, drawn about with dropper
1ml solution instills disposable syringe, prepares to start electrospinning.
（2）The preparation of nanotube：The syringe needle of disposable syringe is connect to the positive pole of high-voltage DC power supply, and is fixed on from receipts
At the height 20cm for collecting plate.Spinning voltage is set to 15KV or so.Clean aluminium foil is fixed into desktop and is connected to the negative of high voltage power supply
Pole.High voltage power supply is opened, the syringe needle of disposable needle tubing taylor cone occurs and starts spinning.Deposition one is heavy on receiver aluminium foil receives
Rice fiber.After spinning terminates, put it into Muffle furnace and anneal, the technique of annealing is：Heating rate is 6 DEG C/min, is risen
Temperature is to 680 DEG C, and soaking time is 5 hours, is then freely cooled to room temperature, finally obtains pure metal oxide nanotubes.
（4）Ceramic base gas sensor makes：
Weigh appropriate SrGe4O9Nanotube is put into mortar, is added appropriate deionized water, is ground, and is dipped in fine, soft fur pen
Take and be coated on ceramic electrode, that is, obtain ceramic base gas sensor.
Embodiment 3：
Step 1 is identical with embodiment 1 and embodiment 2；
Step 2：Platinum acid chloride solution is prepared and then prepared, takes the sample calcined in right amount to be placed in mortar, takes a small amount of platinum acid chloride solution,
Ratio according to load 1.5wt% Pt is added dropwise to mortar and SrGe4O9Nanotube is sufficiently mixed, and 500 DEG C of calcinings are carried out after drying,
1 hour is incubated, obtains deposited Pt one-dimensional SrGe4O9Nanotube, as shown in Figure 3.
Step 3：Weigh the appropriate one-dimensional SrGe that deposited Pt4O9Nanotube is put into mortar, adds appropriate deionization
Water, grinding is dipped with fine, soft fur pen and is coated on ceramic electrode, is designated as ceramics 2.
The air-sensitive performance test of device：
Using air-sensitive tester, ceramic 1 sensor is placed on test platform, probe on bundle, according to 1ppm-500ppm ammonia
Gas concentration, successively toward certain ammoniacal liquor is injected in the heating tank in chamber, makes its evaporation turn into ammonia and is full of whole chamber, pass through
Experimental data, the data such as accompanying drawing 5 of ceramic 1 gas sensor are tested and collected to analysis of test system.Then ceramics 2 are placed on survey
Try on platform, tested according to upper process, the data such as accompanying drawing 6 of ceramic 2 gas sensor.Last test flexibility gas sensor
Performance under device normal temperature, the response curve of differently curved angle is as shown in Figure 6 under 100ppm ammonia atmosphere.
Claims (10)
1. a kind of ammonia gas sensor used at room temperature, the ammonia gas sensor includes gas sensitive and substrate, it is characterised in that institute
Gas sensitive is stated for one-dimensional SrGe4O9Nanotube.
2. the ammonia gas sensor according to right 1, it is characterised in that the gas sensitive also includes noble metal, your gold
The load capacity of category is one-dimensional SrGe4O9The 0.01-2%wt of Nanotube quality.
3. the ammonia gas sensor according to right 2, it is characterised in that the noble metal is Pt or Pd.
4. the ammonia gas sensor according to right 1, it is characterised in that the substrate is flexible material or rigid material.
5. the ammonia gas sensor according to right 1, it is characterised in that the flexible material includes PET, PI or PC.
6. the ammonia gas sensor according to right 1, it is characterised in that the rigid material includes ceramics, glass or titanium dioxide
Silicon chip.
7. a kind of method for preparing ammonia gas sensor as claimed in any one of claims 1 to 6, it is characterised in that specifically include
Following steps：
The configuration of step 1. precursor solution：At room temperature, according to mol ratio 1:4 mix strontium salt powder and ethyoxyl germanium,
Add 2g-4g absolute ethyl alcohols, 16g-18g N,N-dimethylformamides（DMF）With it is molten in 0.5g-1g deionized water mixed solutions
Solution, adds 2.5g-3g polyvinylpyrrolidonepowder powders, finally, by mixed solution magnetic agitation 4-7 hour, until mixing
Close solution clear homogeneous, then, draw about solution with dropper and instill disposable syringe, prepare to start electrospinning；
The preparation of step 2. nanotube：The syringe needle of disposable syringe is connect to the positive pole of high-voltage DC power supply, and is fixed on from receipts
At the height 15-20cm for collecting plate, spinning voltage is set to 15-20KV, and clean aluminium foil is fixed into desktop is connected to high voltage power supply
Negative pole, opens high voltage power supply, and the syringe needle of disposable needle tubing taylor cone occurs and starts spinning, and one is deposited on receiver aluminium foil and is sunk
Nanofiber, after spinning terminates, puts it into Muffle furnace and makes annealing treatment, heating rate is 4-6 DEG C/min, is warming up to 680-
720 DEG C, soaking time is 3.5-5 hours, is then freely cooled to room temperature, finally obtains one-dimensional SrGe4O9Nanotube；
The making of step 3. sensor：
3.1：Substrate is cleaned successively using acetone, ethanol and distilled water, it is standby；
Step 3.2：Weigh appropriate one-dimensional SrGe4O9Nanotube is put into mortar, is added appropriate deionized water, is ground,
Dipped and be coated on rigid electrode with fine, soft fur pen, that is, obtain ammonia gas sensor；Or photoresist is spin-coated on PET in 5000 turns of 30s,
100 DEG C of 3 min of heating, then use ultraviolet photolithographic machine photoetching on flexible base board, and are developed with developer solution, obtain and mask plate
Corresponding interdigital electrode, then 50nm gold is plated on surface, unnecessary gold is washed away with acetone, step 2 prepares one-dimensional
SrGe4O9Nanotube and Kynoar (PVDF) with mass ratio 9：1 ratio mixing, it is uniform to be coated in interdigital electrode；
To ammonia gas sensor.
8. method according to claim 7, it is characterised in that the step 2 is further comprising the steps of：Then chlorine platinum is prepared
Acid solution, takes the sample calcined in right amount to be placed in mortar, takes a small amount of platinum acid chloride solution, according to load 0.01-2%wt noble metal
Ratio be added dropwise to mortar and SrGe4O9Nanotube is sufficiently mixed.
9. method according to claim 7, it is characterised in that the technique made annealing treatment in the step 2 is：Heating rate
For 4-6 DEG C/min, 680-720 DEG C is warming up to, soaking time is 3.5-5 hours.
10. method according to claim 7, it is characterised in that the strontium salt includes strontium nitrate or strontium acetate.
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| CN111089882A (en) * | 2020-01-02 | 2020-05-01 | 宁波大学 | Hydrogen sensor structure and preparation method thereof |
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| Publication number | Publication date |
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| CN107219269B (en) | 2019-04-19 |
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