CN104713915A - High-performance gas sensor based on laminated structure and preparation method for high-performance gas sensor - Google Patents
High-performance gas sensor based on laminated structure and preparation method for high-performance gas sensor Download PDFInfo
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Abstract
The invention discloses a high-performance gas sensor based on a laminated structure and a preparation method for the high-performance gas sensor. The preparation method comprises the following steps: adopting stannic oxide and zinc oxide as conducting layers, using tungsten trioxide, titanium dioxide, copper oxide and cobaltous oxide as sensitive layers, and meanwhile using palladium, platinum noble metal, cadmium sulfide and a cadmium stannide sensitizer to modify the prepared sensitive layers, so as to obtain the gas sensor. According to the method, the modified gas sensitive material is placed at the top layer by a lamination manner, and can be sufficiently reacted with atmosphere in the environment, so as to improve the responsibility of the gas sensor; the material with the better conductivity is placed at the bottom layer, so that the electron concentration change in the sensitive layers can be quickly transferred to an external circuit by the material, and the response and recovery time of the gas sensor can be shortened. Therefore, the method can be used for greatly improving the performances of the gas sensor.
Description
Technical field
The invention belongs to gas sensor field, be specifically related to gas sensor of a kind of rhythmo structure and preparation method thereof.Preparation method of the present invention is simple, and effectively can improve the performance of gas sensor.
Background technology
Gas sensor be a kind of can in perception environment certain gas and concentration thereof and by gaseous species and concentration convert electric signal to for information about thus carry out detecting, monitor, analyze, the device of reporting to the police or device.In recent years, gas sensor is widely used in, in a series of great demand fields such as food security, environmental monitoring, public safety, process control, being with a wide range of applications.
Along with the demand goed deep into and apply of gas sensor research, the focus that gas sensor field is studied at present reduces detection limit, improves susceptibility, improves and respond resume speed, reduction working temperature etc.Traditional material cannot reach requirement at present, and carry out to traditional material the emphasis that modification is research at present, concrete method of modifying comprises the methods such as nanometer, doping, modification and compound.In these methods, multiple material compound is adopted to be a kind of mode more efficiently improving air-sensitive performance, because compound can utilize the advantage of different materials.
In air-sensitive response process, the reaction between gas molecule and sensitive material makes gas sensitive resistance change.This process comprises two subprocess, and one is the reaction between gas sensitive and gas molecule, and two is changes of gas sensitive resistance.Reaction Shaoxing opera between gas sensitive and gas molecule is strong, and gas sensitive resistance variations Shaoxing opera is strong simultaneously, and overall air-sensitive performance just can be caused good.Adopt the mode of compound really can accelerate gas-sensitive reaction for the modification of gas sensitive, but recombination process makes the rambling arrangement of two-phase, this situation often reduces the change of gas sensitive resistance.Such as, when zinc paste and titanium dioxide compound tense, the compound substance of formation contributes to the gas-sensitive reaction accelerating PARA FORMALDEHYDE PRILLS(91,95) gas, namely achieves the object of acceleration " subprocess one ".But titanium dioxide and zinc paste is rambling arrangement in compound system, the potential barrier formed due to the interface contacted two again can stop the transmission of electric charge, comprehensively above-mentioned reason can make the resistance variations of gas sensitive entirety and not obvious, and the object of unrealized acceleration " subprocess two ".So, although this complex method improves overall air-sensitive response to a certain extent, the great advantage of two materials is not played.
Summary of the invention
Problem to be solved by this invention overcomes the technology drawback that can not play bi-material characteristic in existing complex method completely, and provide a kind of gas sensor, it possesses orderly rhythmo structure, significantly to provide its susceptibility and response recovery time; Present invention also offers the preparation method of this gas sensor.
Gas sensor provided by the invention, comprises substrate and electrode, it is characterized in that, substrate is stacked with conductive layer and sensitive layer successively, forms orderly rhythmo structure; Described electrode to be placed on substrate and to be positioned at described conductive layer two ends, described sensitive layer is as the place of air-sensitive response reaction, doped with the sensitization point formed by sensitizer in sensitive layer, sensitizer is modified sensitive layer, to improve susceptibility and the response recovery time of gas sensor.
The preparation method of gas sensor provided by the invention, is characterized in that, the method comprises the following steps:
(1) preparation of substrate:
Substrate ultrasonic cleaning in acetone soln, as substrate, is removed surface blot, is then taken out substrate washed with de-ionized water and fall residual organic solution by selective oxidation aluminium, monox, glass or sapphire inert material;
Adopt serigraphy or the mode of mask lithography makes metal conducting electrodes on substrate, obtain sensor base plate;
(2) conductive layer preparation:
Choose tin oxide or zinc paste as raw material, adopt serigraphy, Hydrothermal Synthesis or pulsed laser deposition mode on sensor base plate, make one deck conductive;
(3) sensitive layer preparation:
Choose tungstic acid, titania, cupric oxide or cobalt oxide as raw material, adopt serigraphy, Hydrothermal Synthesis or pulsed laser deposition mode to make one deck sensitive layer on described conductive layer;
(4) sensitive layer is modified:
Choose the chloride of palladium, platinum, the nitrate of palladium, platinum, cadmium sulfide, or tin cadmium is as sensitizer, adopts the mode instiled or soak to modify sensitive layer, and obtain the gas sensor of orderly rhythmo structure at 300 ~ 600 DEG C through calcining in 2 ~ 4 hours.
The gas sensor prepared according to this method has orderly rhythmo structure, and its conductive layer can as the conductive channel of electronics, and sensitive layer is as the place of air-sensitive response reaction.Compare traditional complex method, lamination compound can utilize the feature of tin oxide, zinc paste good conductivity, the change of the electron concentration produced after sensitive layer generation gas-sensitive reaction is passed to external circuit rapidly by conductive layer, effectively improves gas sensor response resume speed.In addition, adopt sensitizer to carry out sensitive layer modifying the responsiveness that can improve gas sensor further, reduce detection limit.The present invention adopts the mode of working along both lines to improve gas sensor performance.
Accompanying drawing explanation
Fig. 1 is the high-performance gas sensor schematic diagram based on rhythmo structure;
In figure, 1 is substrate, and 2 is electrode, and 3 is conductive layer, and 4 is sensitive layer, and 5 is sensitization point.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described further.It should be noted that at this, the explanation for these embodiments understands the present invention for helping, but does not form limitation of the invention.In addition, if below in described each embodiment of the present invention involved technical characteristic do not form conflict each other and just can mutually combine.
As shown in Figure 1, the structure of the ordered composite gas sensor based on heterojunction structure provided by the invention is: be stacked with conductive layer 3 and sensitive layer 4 on substrate 1 successively, substrate is also provided with electrode 2, and the material of conductive layer 3 is zinc paste or tin oxide.Sensitive layer 4 material is tungstic acid, titania, cupric oxide or cobalt oxide, doped with chloride, the nitrate by palladium, platinum in sensitive layer 4, and the sensitization point 5 that cadmium sulfide or tin cadmium are formed as sensitizer.This structure is different from traditional composite mode, and the structure of compound is the pattern adopting stacked in layers, and every one deck has its specific purposes.
Sensitive layer is the main place that gas-sensitive reaction occurs, and when in sensitive layer material and environment, gas molecule reacts, the process of receiving and losing electrons can cause the change of sensitive layer electrical property, and this changes is exactly the air-sensitive performance of sensitive layer material.What therefore sensitive layer was selected is the sensitive material with good air-sensitive performance, and adopts sensitizer to improve the activity of sensitive layer further.Conductive layer is the passage of conduct charges, compared to sensitive layer, the conductivity of conductive is higher than sensitive layer, and the change of the electron concentration produced after making sensitive layer generation gas-sensitive reaction passes to external circuit fast by conductive layer, improves the gas-sensitive reaction speed of sensitive layer.The heterojunction simultaneously formed between sensitive layer and conductive layer different materials can improve the effect of charge separation, is conducive to promoting gas-sensitive reaction.Therefore, relative to conventional composite mode, adopt the mode of orderly lamination compound to remain the effect of the hetero-junction electric-charge separation that conventional composite mode is brought on the one hand, the maximum performance bi-material of energy characteristic separately on the other hand, promotes susceptibility and the response recovery time of sensor further.
A kind of ordered composite gas sensor preparation method based on heterojunction structure provided by the invention, specifically comprises the following steps:
(1) preparation of substrate:
Substrate ultrasonic cleaning in acetone soln, as substrate, is removed surface blot, is then taken out substrate washed with de-ionized water and fall residual organic solution by selective oxidation aluminium, monox, glass or sapphire inert material.
Adopt serigraphy or the mode of mask lithography makes metal conducting electrodes on substrate, as gold, silver, platinum, obtain sensor base plate.
(2) conductive layer preparation:
Choose tin oxide or zinc paste as raw material, adopt serigraphy, Hydrothermal Synthesis, pulsed laser deposition mode on sensor base plate, make one deck conductive.
(3) sensitive layer preparation:
Choose tungstic acid, titania, cupric oxide or cobalt oxide as raw material, adopt serigraphy, Hydrothermal Synthesis or pulsed laser deposition mode to make one deck sensitive layer material on the electrically conductive.
(4) sensitive layer is modified:
Choose palladium, the chloride of platinum, nitrate, cadmium sulfide or tin cadmium as sensitizer, adopt instil or soak mode sensitive layer is modified, and put into muffle furnace 300 ~ 600 DEG C through 2 ~ 4 hours calcining obtain gas sensor finished product.
Example:
Example 1:
Selective oxidation aluminium is as substrate.By aluminum oxide substrate ultrasonic cleaning 10 minutes in acetone soln, remove surface blot, then take out substrate washed with de-ionized water and fall residual organic solution.Adopt screen printing mode on substrate, make platinum conductive electrode platinum, obtain sensor base plate.
Choose tin oxide powder as raw material, according to mass ratio 6: 3: 1 by terpinol, butyl carbitol acetate, dibutyl phthalate is thoroughly mixed to form organic solvent, again tin oxide material powder is mixed according to mass ratio 6: 4 with organic solvent, with the rotating speed ball milling 3 hours of 400 revs/min, obtain slurry, adopt screen printing mode on sensor base plate, print one deck fin oxide condutire layer material.Put into 120 DEG C of baking oven insulations 2 hours again, conductive is solidified.
Choose tungstic acid powder as raw material, tungstic acid material powder is mixed according to mass ratio 6: 4 with the organic solvent of above-mentioned configuration, with the rotating speed ball milling 3 hours of 400 revs/min, obtain slurry, adopt screen printing mode on above-mentioned conductive layer, print one deck tungstic acid sensitive layer material.Put into 120 DEG C of baking oven insulations 2 hours again, make sensitive layer material cured.
Choose 1mM/L palladium chloride solution as sensitizer, adopt dropper to extract palladium chloride solution, the 30 μ L palladium chloride solutions that instil on sensitive layer, then will be put into muffle furnace and within 2 hours, obtain gas sensor finished product 600 DEG C of calcinings.
Example 2:
Select glass material as substrate.By glass substrate ultrasonic cleaning 10 minutes in acetone soln, remove surface blot, then take out substrate washed with de-ionized water and fall residual organic solution.Adopt the mode of mask lithography on substrate, make silver-colored conductive electrode, obtain sensor base plate.
Choosing zinc nitrate as solute, take deionized water as solvent, preparation 0.05mol/L zinc unit solution, add with the hexamethylenetetramine of zinc nitrate mol ratio 1: 1 as releasing ammonia agent, obtain zinc oxide growth solution, substrate is put into growth solution, at 90 DEG C, carry out hydrothermal growth 4 hours.Repeatedly rinse with deionized water after taking-up, finally dry in 80 DEG C of baking ovens, obtain one deck zinc oxide conductive layer.
After concentrated hydrochloric acid is mixed with volume ratio 1: 1 with deionized water, 1: 0.0125 instillation butyl titanate also fully stirs by volume, obtain titania growth solution, the above-mentioned substrate containing conductive layer is put into growth solution, at 150 DEG C, carries out hydrothermal growth 8 hours.Repeatedly rinse with deionized water after taking-up, finally dry in 80 DEG C of baking ovens, obtain layer of titanium dioxide sensitive layer.
Choose 1mM/L platinum chloride as sensitizer, the sensitive layer of above-mentioned preparation to be dipped in platinum chloride solution 2 hours, to put into muffle furnace after taking-up and within 3 hours, obtain gas sensor finished product 300 DEG C of calcinings
Example 3:
Selective oxidation silicon materials are as substrate.By the ultrasonic cleaning 10 minutes in acetone soln of monox substrate, remove surface blot, then take out substrate washed with de-ionized water and fall residual organic solution.Adopt the mode of mask lithography on substrate, make golden conductive electrode, obtain sensor base plate.
Choose tin oxide as target, adopt pulsed laser deposition mode on sensor base plate, make one deck conductive, parameters is: laser power 2J/cm
2, laser pulse frequency is 5Hz, and substrate pitch is 8cm, and substrate temperature is 400 DEG C, and vacuum tightness is less than 10
-4mbar.
Choose cobalt oxide as target, adopt pulsed laser deposition mode to make one deck sensitive layer material on the electrically conductive, parameters is: laser power 2J/cm
2, laser pulse frequency is 5Hz, and substrate pitch is 8cm, and substrate temperature is 400 DEG C, and vacuum tightness is less than 10
-4mbar.。
The sensitive layer of above-mentioned preparation, as sensitizer, to be dipped in cadmium sulfide solution 2 hours, to put into muffle furnace and within 4 hours, obtain gas sensor finished product 200 DEG C of calcinings after taking-up by cadmium sulfide.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the content disclosed in this embodiment and accompanying drawing.The equivalence completed under not departing from spirit disclosed in this invention so every or amendment, all fall into the scope of protection of the invention.
Claims (5)
1. a gas sensor, comprises substrate and electrode, it is characterized in that, substrate is stacked with conductive layer and sensitive layer successively, forms orderly rhythmo structure; Described electrode to be placed on substrate and to be positioned at described conductive layer two ends, described sensitive layer is as the place of air-sensitive response reaction, doped with the sensitization point formed by sensitizer in sensitive layer, sensitizer is modified sensitive layer, to improve susceptibility and the response recovery time of gas sensor.
2. gas sensor according to claim 1, is characterized in that, the material of described conductive layer is zinc paste or tin oxide.
3. gas sensor according to claim 1, is characterized in that, described sensitive layer material is tungstic acid, titania, cupric oxide or cobalt oxide.
4. the gas sensor according to claim 1,2 or 3, is characterized in that, described sensitizer is the nitrate of the chloride of palladium, platinum, palladium, platinum, cadmium sulfide, or tin cadmium.
5. a preparation method for gas sensor, is characterized in that, the method comprises the following steps:
(1) preparation of substrate:
Substrate ultrasonic cleaning in acetone soln, as substrate, is removed surface blot, is then taken out substrate washed with de-ionized water and fall residual organic solution by selective oxidation aluminium, monox, glass or sapphire inert material;
Adopt serigraphy or the mode of mask lithography makes metal conducting electrodes on substrate, obtain sensor base plate;
(2) conductive layer preparation:
Choose tin oxide or zinc paste as raw material, adopt serigraphy, Hydrothermal Synthesis or pulsed laser deposition mode on sensor base plate, make one deck conductive;
(3) sensitive layer preparation:
Choose tungstic acid, titania, cupric oxide or cobalt oxide as raw material, adopt serigraphy, Hydrothermal Synthesis or pulsed laser deposition mode to make one deck sensitive layer on described conductive layer;
(4) sensitive layer is modified:
Choose the chloride of palladium, platinum, the nitrate of palladium, platinum, cadmium sulfide, or tin cadmium is as sensitizer, adopts the mode instiled or soak to modify sensitive layer, and obtain the gas sensor with rhythmo structure at 300 ~ 600 DEG C through calcining in 2 ~ 4 hours.
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Cited By (11)
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| CN105181756A (en) * | 2015-09-24 | 2015-12-23 | 天津大学 | Mesomorphic copper oxide gas-sensitive material having high response sensitivity to ethyl alcohol |
| CN106770485A (en) * | 2017-01-25 | 2017-05-31 | 吉林大学 | A kind of conductive kernel sensitive layer and molecular sieve are except the exhalation sensor and preparation method of wet layer |
| CN108267488A (en) * | 2017-12-21 | 2018-07-10 | 南京邮电大学 | A kind of transparent gas sensor based on copper oxide/zinc oxide heterogeneous structure and preparation method thereof |
| CN108574019A (en) * | 2018-02-28 | 2018-09-25 | 广东工业大学 | A kind of tungstic acid semiconductive thin film and its preparation method and application |
| CN109580724A (en) * | 2017-09-29 | 2019-04-05 | 萧育仁 | Mini type gas sensor and its manufacturing method |
| CN110174442A (en) * | 2019-07-11 | 2019-08-27 | 苏州大学 | Titania-based gas sensor and preparation method thereof |
| CN110243872A (en) * | 2019-06-13 | 2019-09-17 | 华中科技大学 | A kind of excited by visible light gas sensor and preparation method thereof |
| CN110361426A (en) * | 2019-07-30 | 2019-10-22 | 电子科技大学 | A kind of film-type alcohol gas sensor and preparation method thereof |
| CN111693578A (en) * | 2020-06-11 | 2020-09-22 | 中国农业科学院农业信息研究所 | Crop growth information monitoring method and device and manufacturing method thereof |
| CN112553575A (en) * | 2020-12-02 | 2021-03-26 | 有研工程技术研究院有限公司 | Multilayer composite nitrogen dioxide gas-sensitive film and preparation method thereof |
| CN112666230A (en) * | 2020-12-29 | 2021-04-16 | 西安电子科技大学 | Acetone sensor, preparation method and acetone detection method |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105181756A (en) * | 2015-09-24 | 2015-12-23 | 天津大学 | Mesomorphic copper oxide gas-sensitive material having high response sensitivity to ethyl alcohol |
| CN106770485A (en) * | 2017-01-25 | 2017-05-31 | 吉林大学 | A kind of conductive kernel sensitive layer and molecular sieve are except the exhalation sensor and preparation method of wet layer |
| CN106770485B (en) * | 2017-01-25 | 2019-06-21 | 吉林大学 | It is a kind of conduction kernel sensitive layer and molecular sieve remove wet layer sensor and preparation method |
| CN109580724A (en) * | 2017-09-29 | 2019-04-05 | 萧育仁 | Mini type gas sensor and its manufacturing method |
| CN108267488B (en) * | 2017-12-21 | 2020-08-11 | 南京邮电大学 | Gas sensor based on copper oxide/zinc oxide heterostructure and preparation method thereof |
| CN108267488A (en) * | 2017-12-21 | 2018-07-10 | 南京邮电大学 | A kind of transparent gas sensor based on copper oxide/zinc oxide heterogeneous structure and preparation method thereof |
| CN108574019A (en) * | 2018-02-28 | 2018-09-25 | 广东工业大学 | A kind of tungstic acid semiconductive thin film and its preparation method and application |
| CN110243872A (en) * | 2019-06-13 | 2019-09-17 | 华中科技大学 | A kind of excited by visible light gas sensor and preparation method thereof |
| CN110174442A (en) * | 2019-07-11 | 2019-08-27 | 苏州大学 | Titania-based gas sensor and preparation method thereof |
| CN110361426A (en) * | 2019-07-30 | 2019-10-22 | 电子科技大学 | A kind of film-type alcohol gas sensor and preparation method thereof |
| CN111693578A (en) * | 2020-06-11 | 2020-09-22 | 中国农业科学院农业信息研究所 | Crop growth information monitoring method and device and manufacturing method thereof |
| CN112553575A (en) * | 2020-12-02 | 2021-03-26 | 有研工程技术研究院有限公司 | Multilayer composite nitrogen dioxide gas-sensitive film and preparation method thereof |
| CN112666230A (en) * | 2020-12-29 | 2021-04-16 | 西安电子科技大学 | Acetone sensor, preparation method and acetone detection method |
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