CN103149247B - Loose thin-wall gas sensor and preparation method thereof - Google Patents
Loose thin-wall gas sensor and preparation method thereof Download PDFInfo
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- CN103149247B CN103149247B CN201310068237.9A CN201310068237A CN103149247B CN 103149247 B CN103149247 B CN 103149247B CN 201310068237 A CN201310068237 A CN 201310068237A CN 103149247 B CN103149247 B CN 103149247B
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Abstract
The invention discloses gas sensor of a kind of loose thin-wall and preparation method thereof, this gas sensor comprises the metal oxide air-sensitive compound substance and substrate with loose thin-wall structure; Wherein, air-sensitive compound substance is precious metal doping, equally distributed nano particle.The method that the present invention prepares this gas sensor comprises: after carrying out pre-service to template, puts into precursor liquid and carries out three step dippings; Again successively through cleaning, dry, sintering processes, the metal oxide air-sensitive compound substance of obtained loose thin-wall structure; Finally be coated on substrate surface, and carried out burin-in process, the obtained study of metal oxide gas sensor with loose thin-wall structure.The invention also discloses a kind of method preparing the gas sensor of loose thin-wall, its technique is simple, by change compound kind, regulation and control nano particle size, select different templates to obtain the gas sensor with premium properties, obtained loose thin-wall gas sensor can reveal high sensitivity to gas meter to be measured.
Description
Technical field
The present invention relates to a kind of gas sensor and preparation method thereof, particularly relate to study of metal oxide gas sensor of a kind of loose thin-wall structure and preparation method thereof.
Background technology
Along with the high development of modern society, use in commercial production and the kind of poisonous, harmful gas that produces and quantity increasing.Meanwhile, liquefied petroleum gas (LPG), town gas and rock gas also use gas as family, are widely used.The accident quantity such as the blast that gassing and Leakage Gas cause, fire rise year by year.In recent decades, the problem of atmospheric pollution also result in the extensive concern of people.So being the guarantee to human society production and living safety to the monitoring of the timely high efficient and reliable of toxic and harmful, is also that the mankind urgently pay close attention to and one of urgent problem.
In numerous gas sensitive, to take tin oxide as the metal oxide of representative be studies one of gas sensitive the earliest, is also the gas sensitive applied the earliest.For the metal oxide gas sensitive of one-component, due to the deficiency of its granule surface activity, namely particle surface adsorb oxygen number is few, limits the further lifting of material to reducibility gas air-sensitive performance.Usually need to be optimized modification to it, to meet in actual application, to the requirement of material air-sensitive response, selectivity, long-time stability and working temperature etc.
At present, the optimization of metal oxide gas sensitive component, mainly concentrates on the compound of the compound between metal oxide, metal oxide and carbon nano-tube or polymkeric substance, and precious metal element finishing etc. (as Pd, Rh, Pt, Au, Ag etc.).Wherein, the surface modification of precious metal element is that current research is the most extensive, is also the most effective component modification mode.But the nano particle obtained by a lot of preparation method is uneven, limit the raising of material gas sensing property.
Therefore, those skilled in the art is devoted to develop a kind of metal oxide gas sensitive being evenly distributed, having excellent gas sensing property.
Summary of the invention
Because the above-mentioned defect of prior art, technical matters to be solved by this invention is to provide gas sensor of a kind of loose thin-wall and preparation method thereof.Loose thin-wall gas sensor provided by the invention has higher sensitivity to required detection gas; The reunion that its preparation method is simple, convenience of drawing materials, environmental protection, cost are low, effectively can prevent nano particle in material.The gas sensor that preparation method of the present invention obtains can keep the loose thin-wall structure of template, and can obtain and have premium properties.
For achieving the above object, on the one hand, the invention provides a kind of gas sensor of loose thin-wall, comprise the metal oxide air-sensitive compound substance and substrate with loose thin-wall structure; Wherein, the metal oxide air-sensitive compound substance of loose thin-wall structure is precious metal doping, equally distributed nano particle; Substrate is aluminium oxide ceramics.
In the present invention, described noble metal refer in palladium, platinum, gold one or more, but be not limited to this.
On the other hand, present invention also offers a kind of method preparing loose thin-wall gas sensor, comprise the following steps:
Step one, pre-service is carried out to loose thin-wall template;
Wherein, described loose thin-wall template is any one loose thin-wall biomaterial, is preferably plant pollen, but is not limited thereto;
Step 2, loose thin-wall template pretreated in the first step is put into precursor liquid carry out dip treating;
Step 3, by the loose thin-wall template after dipping successively through cleaning, dry, sintering processes, the metal oxide air-sensitive compound substance of obtained loose thin-wall structure;
Step 4, above-mentioned metal oxide air-sensitive compound substance is coated on substrate surface, and burin-in process is carried out to it, the obtained study of metal oxide gas sensor with loose thin-wall structure.
In better embodiment of the present invention, the pre-service described in the first step refers to; By the rinsing drying repeatedly in absolute ethyl alcohol of loose thin-wall template.
In the specific embodiment of the present invention, preferably, in second step pretreated loose thin-wall template put into as matrix the first precursor liquid and be used as the second precursor liquid of doped and compounded and carry out three step dippings.
Wherein, described first precursor liquid refers to that concentration is the metal salt solution of 0.0001 ~ 0.01mol/L; Described slaine is one or more in the chlorate of metal, sulfate, nitrate, but is not limited thereto; Described metal is one or more in tin, zinc, iron, but is not limited thereto.
Described second precursor liquid refers to that concentration is the precious metal salt solution of 0.0001 ~ 0.01mol/L; Described precious metal salt is one or more in the chlorate of noble metal, sulfate, nitrate, but is not limited thereto; Described noble metal is one or more in palladium, platinum, gold, but is not limited thereto.
In another better embodiment of the present invention, three step dippings described in second step comprise the following steps:
A) pretreated loose thin-wall template is scattered in the first precursor liquid, stirs 1 ~ 14h, after centrifuging, with washes of absolute alcohol, obtain the first macerate;
B) above-mentioned first macerate is scattered in the second precursor liquid, stirs 1 ~ 4h, after centrifuging, with washes of absolute alcohol, obtain the second macerate;
C) the second macerate is joined in distilled water, successively after surface hydrates process, centrifuging, washes of absolute alcohol, dry under the condition of 60 DEG C, be scattered in described first precursor liquid, electromagnetic agitation 1 ~ 4h, after centrifuging again, with washes of absolute alcohol, obtain the 3rd macerate.
In better embodiment of the present invention, the cleaning described in the 3rd step refers to: after the described loose thin-wall template ethanol-water solution process after dipping, in absolute ethyl alcohol, flood 30min, then centrifuging.
Preferably, the drying described in the 3rd step refers to: under 60 DEG C of conditions, keeps 3h.
Preferably, the sintering described in the 3rd step refers to: dried loose thin-wall template is placed in oxidation furnace, with ramp to 500 ~ 800 of 1 ~ 5 ° of C/min ° C, and keeps 90min under the condition of 500 ~ 800 ° of C, then naturally cools to room temperature.
In the preparation process in accordance with the present invention, preferably, the metal oxide air-sensitive compound substance described in the 4th step is coated on substrate surface and refers to: after being ground by metal oxide air-sensitive compound substance, with deionized water furnishing pasty state, and be evenly coated in substrate surface.
Further, the burin-in process described in the 4th step refers to: will be coated in the metal oxide air-sensitive compound substance of substrate surface under 400 ~ 600 DEG C of conditions, keeps 1 ~ 5h, and then logical direct current on agingtable, under 300 DEG C of conditions, keeps 1 ~ 10 day.
The present invention adopts plant pollen etc. to have the biomaterial of loose thin-wall, directly gas sensitive is synthesized with biological self-assembly system, not only simplify synthesis technique, the suction-operated of biomolecule can also be utilized simultaneously, solve the dispersed problem of doped chemical in matrix material.
In the present invention, not only using metal salt solution as precursor liquid, by precursor liquid infusion process, metal oxide is incorporated in gas sensitive; Also by using precious metal salt solution as precursor liquid, by precursor liquid infusion process, metal oxide containing precious metals is incorporated in gas sensitive, and its content controls by the mode changing Concentration of precursor solution.By precious metal element, finishing is carried out to loose thin-wall metal oxide, improve the adsorb oxygen number of material surface.Due to the catalytic action of noble metal of doping, improve the sensitivity of gas sensor to gas, thus the performance of gas sensor be greatly improved, can long-term working stability high, usable range is wide.
The present invention is by carrying out pre-service to loose thin-wall template, and put into precursor liquid after three step dippings, through the simple treatment step such as cleaning, drying, sintering, obtain the metal oxide composite of corresponding loose thin-wall structure, preparation method is simple, primary raw material is drawn materials conveniently, and environmental protection, cost is low.
The gas sensor of loose thin-wall structure of the present invention improves the rate of propagation of gas and the specific surface area of oxide, and overcomes the deficiency that nano particle easily assembles.Therefore, loose thin-wall gas sensor of the present invention will have very large market application foreground.
Be described further below with reference to the technique effect of accompanying drawing to design of the present invention, concrete structure and generation, to understand object of the present invention, characteristic sum effect fully.
Accompanying drawing explanation
Fig. 1 is template with rape pollen in the embodiment of the present invention 1, the FESEM figure of the tin oxide/palladium oxide air-sensitive compound substance of the loose thin-wall structure of preparation;
Fig. 2 is template with rape pollen in the embodiment of the present invention 1, the tin oxide/palladium oxide gas sensor of the loose thin-wall structure of preparation under the condition of 330 ° of C, to hydrogen periodic cycle test real-time response curve;
Fig. 3 is template with rape pollen in the embodiment of the present invention 2, the SEAD diffractogram of the transmission electron microscope of the tin oxide/palladium oxide air-sensitive compound substance of the loose thin-wall structure of preparation.
Embodiment
In the preferred embodiment, rape pollen is adopted to be loose thin-wall template, through simple treatment steps such as pre-service, three step dippings, cleaning, drying and sintering, prepare the metal oxide air-sensitive compound substance with loose thin-wall structure, and by the coating of this metal oxide air-sensitive compound substance and aluminium oxide ceramics substrate surface, burin-in process is carried out to it, the obtained study of metal oxide gas sensor with loose thin-wall structure.Gas sensor of the present invention has following characteristic:
1, may be used for detecting multiple gases, be preferably hydrogen, carbon monoxide, acetone.
2, the sensitivity detected is that, to the above-mentioned gas of 50 ~ 2000ppm, sensitivity is 10 ~ 131.
3, the corresponding release time detected is that show 50ppm hydrogen and respond fast and reply, the response time is only 1 ~ 3s, and turnaround time is also only 8 ~ 20s.
Wherein, sensitivity definition is R
a/ R
g, R
arepresent the resistance of gas sensor in dry pure air, R
grepresent the resistance of gas sensor in atmosphere to be measured.
4, there is certain selectivity, different to the detection sensitivity of often kind of gas.For in above-mentioned preferred detection gas, wherein, the highest to the detection sensitivity of 1000ppm hydrogen, be about 131.
Wherein, the pre-service of rape pollen is referred to rape pollen rinsing drying repeatedly in absolute ethyl alcohol.
Embodiment 1:
Selection rape pollen is template.Get the SnCl that pretreated rape pollen is scattered in the 0.0006mol/L of 50mL
4in precursor liquid, stir after 14h, centrifuging, through ethanol purge three times, obtain single-steeping thing, complete first step dip process.Again single-steeping thing is scattered in the PdCl of 0.0006mol/L
2in precursor liquid, stir after 4h, centrifuging, and through ethanol purge three times, obtain double-steeping thing.In order to improve the absorption/deposition of Sn at pollen, carry out third time dip treating, double-steeping thing is added in 50mL distilled water and carries out surface hydrates process, reclaimed by centrifuging again, again be scattered in 50mL ethanol, after 10min, at the dry 3h of 60 ° of C, be then scattered in the 0.0006mol/L SnCl of 50mL
4in precursor liquid, stir after 4h, centrifuging, and through ethanol purge three times, obtain three macerates.In 50mL ethanol, clean about 30min, centrifuging, be placed in dry 3h at 60 ° of C temperature.Dried three macerates are placed in oxidation furnace and carry out calcination processing, rise to 600 ° of C from room temperature, heating rate is 2 ° of C/min, and after 600 ° of C are incubated 90min, naturally cools to room temperature.Take out the product after calcination processing, namely obtain average grain size be 5nm, nanocrystal composition, the tin oxide/palladium oxide air-sensitive compound substance white powder of loose thin-wall structure.After obtained ground material, with appropriate deionized water furnishing pasty state, be coated on aluminium oxide ceramics substrate surface, and under 500 DEG C of conditions, keep 1h, then logical direct current on agingtable, under 300 DEG C of conditions, keep 7 days, obtained gas sensor after burin-in process.
Fig. 1 gives the FESEM figure of loose thin-wall structure tin oxide/palladium oxide air-sensitive compound substance that the present embodiment obtains.As can be seen from Figure 1, on overall pattern, tin oxide/palladium oxide air-sensitive compound substance remains the elliposoidal structure of original pollen.Compared to original pollen, dimensional contraction more than 50%, the three-dimensional open classifying porous skeleton on surface is well retained.
Fig. 2 be the tin oxide/palladium oxide gas sensor of the present embodiment gained loose thin-wall structure under 330 DEG C of conditions, to the sensitivity curve of hydrogen.As shown in Figure 2, under 330 DEG C of conditions, the tin oxide/palladium oxide gas sensor of the loose thin-wall structure that the present embodiment obtains can reach 97 to hydrogen sensitivity, is better than the tin dioxide composite material of other structures generally.
Embodiment 2:
Selection rape pollen is template.Get the SnCl that pretreated rape pollen is scattered in the 0.0006mol/L of 50mL
4in precursor liquid, stir 14h, centrifuging, after ethanol purge three times, obtains single-steeping thing, completes first step dip process.Again single-steeping thing is scattered in the PdCl of 0.006mol/L
2in precursor liquid, stir 4h, centrifuging, and after ethanol purge three times, obtain double-steeping thing.In order to improve the absorption/deposition of Sn in rape pollen, carry out third time dip treating, double-steeping thing is joined in 50mL distilled water, carry out surface hydrates process, reclaimed by centrifuging again, be again scattered in 50mL ethanol, after 10min, at the dry 3h of 60 ° of C, be then scattered in the 0.0006mol/L SnCl of 50mL
4in precursor liquid, stir 4h, centrifuging, and after ethanol purge three times, obtain three macerates.In 50mL ethanol, clean about 30min, centrifuging, be placed in dry 3h under 60 ° of C conditions.Dried three macerates are placed in oxidation furnace and carry out calcination processing, be warming up to 600 ° of C, heating rate is 2 ° of C/min.After 600 ° of C are incubated 90min, naturally cool to room temperature.Take out the product after calcining, namely obtain average grain size be 3.5nm, nanocrystal composition, the tin oxide/palladium oxide air-sensitive compound substance white powder of loose thin-wall structure.After obtained ground material, with appropriate deionized water furnishing pasty state, be coated on aluminium oxide ceramics substrate surface, and under 500 DEG C of conditions, keep 1h, then logical direct current on agingtable, under 300 DEG C of conditions, keep 7 days, obtained gas sensor after burin-in process.
Fig. 3 be the loose thin-wall structure tin oxide/palladium oxide air-sensitive compound substance of this example gained the SEAD diffractogram of transmission electron microscope.As can be seen from Figure 3, pattern is a series of donut.Show that tin oxide/palladium oxide air-sensitive compound substance is the polycrystalline particle of irregular orientation.Polycrystalline diffraction annulus from inside to outside successively with Rutile Type SnO
2(110), (101), (200), (211), (310) crystal face corresponding.
Embodiment 3:
Selection rape pollen is template.Get the SnCl that pretreated rape pollen is scattered in the 0.0006mol/L of 50mL
4in precursor liquid, stir 14h, centrifuging, after ethanol purge three times, obtains single-steeping thing, completes first step dip process.Again single-steeping thing is scattered in the PdCl of 0.004mol/L
2in precursor liquid, stir 4h, centrifuging, and after ethanol purge three times, obtain double-steeping thing.In order to improve the absorption/deposition of Sn in rape pollen, carry out third time dip treating, double-steeping thing is added in 50mL distilled water and carries out surface hydrates process, reclaimed by centrifuging again, again be scattered in 50mL ethanol, after 10min, at the dry 3h of 60 ° of C, be then scattered in the 0.0006mol/L SnCl of 50mL
4in precursor liquid, stir 4h, centrifuging, and after ethanol purge three times, obtain three macerates.In 50mL ethanol, clean about 30min, centrifuging, be placed in dry 3h at 60 ° of C temperature.Dried three macerates are placed in oxidation furnace and carry out calcination processing, be warming up to 600 ° of C, heating rate is 2 ° of C/min, and after 600 ° of C are incubated 90min, naturally cools to room temperature.Take out the product after calcination processing, namely obtain average grain size be 4nm, nanocrystal composition, the tin oxide/palladium oxide air-sensitive compound substance white powder of loose thin-wall structure.After obtained ground material, with appropriate deionized water furnishing pasty state, be coated on aluminium oxide ceramics substrate surface, and under 500 DEG C of conditions, keep 1h, then logical direct current on agingtable, under 300 DEG C of conditions, keep 7 days, obtained gas sensor after burin-in process.
At present, the method preparing high-performance gas sensitive is in the art comparatively complicated.And gas sensitive involved in the present invention is metal oxide composite, its preparation method is simple, achieves detection to multiple gases, and show higher sensitivity by constructing loose thin-wall structure in lower temperature is to the detection of various gas.Compared to other structures, loose thin-wall gas sensor of the present invention shows more excellent air-sensitive performance.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that the ordinary skill of this area just design according to the present invention can make many modifications and variations without the need to creative work.Therefore, all technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (9)
1. a preparation method for the gas sensor of loose thin-wall, is characterized in that,
The gas sensor of described loose thin-wall comprises the metal oxide air-sensitive compound substance and substrate with loose thin-wall structure; The metal oxide air-sensitive compound substance of described loose thin-wall structure is precious metal doping, equally distributed nano particle, and described substrate is aluminium oxide ceramics; One or more in stanniferous in described metal oxide, zinc, iron;
Described noble metal is one or more in palladium, platinum, gold;
The preparation method of the gas sensor of described loose thin-wall comprises the following steps:
Step one, pre-service is carried out to loose thin-wall template;
Step 2, pretreated loose thin-wall template put into and carries out three step dippings as the first precursor liquid of matrix and the second precursor liquid of being used as doped and compounded;
Step 3, by the loose thin-wall template after dipping in step 2 successively through cleaning, dry, sintering processes, the metal oxide air-sensitive compound substance of obtained loose thin-wall structure;
Step 4, above-mentioned metal oxide air-sensitive compound substance is coated on substrate surface, and burin-in process is carried out to it, the obtained study of metal oxide gas sensor with loose thin-wall structure;
Wherein, described loose thin-wall template is plant pollen; Described first precursor liquid refers to that concentration is the metal salt solution of 0.0001 ~ 0.01mol/L; Described second precursor liquid refers to that concentration is the precious metal salt solution of 0.0001 ~ 0.01mol/L.
2. preparation method as claimed in claim 1, wherein, the pre-service described in described step one refers to; By the rinsing drying repeatedly in absolute ethyl alcohol of described loose thin-wall template.
3. preparation method as claimed in claim 1, described slaine is one or more in the chlorate of metal, sulfate, nitrate; Described metal is one or more in tin, zinc, iron;
Described precious metal salt is one or more in the chlorate of noble metal, sulfate, nitrate; Described noble metal is one or more in palladium, platinum, gold.
4. preparation method as claimed in claim 3, wherein, three described step dippings comprise the following steps:
A) described pretreated described loose thin-wall template is scattered in described first precursor liquid, stirs 1 ~ 14h, after centrifuging, with washes of absolute alcohol, obtain the first macerate;
B) described first macerate is scattered in described second precursor liquid, stirs 1 ~ 4h, after centrifuging, with washes of absolute alcohol, obtain the second macerate;
C) described second macerate joins in distilled water, successively after surface hydrates process, centrifuging, washes of absolute alcohol, dry, be scattered in electromagnetic agitation 1 ~ 4h in described first precursor liquid again, after centrifuging, with washes of absolute alcohol, obtain the 3rd macerate.
5. preparation method as claimed in claim 1, wherein, the cleaning described in described step 3 refers to: after the described loose thin-wall template ethanol-water solution process after dipping, in absolute ethyl alcohol, flood 30min, then centrifuging.
6. preparation method as claimed in claim 1, wherein, the drying described in described step 3 refers to: under 60 DEG C of conditions, keeps 3h.
7. preparation method as claimed in claim 1, wherein, the sintering described in described step 3 refers to: dried described loose thin-wall template is placed in oxidation furnace, with ramp to 500 ~ 800 DEG C of 1 ~ 5 DEG C/min, after keeping 90min, naturally cool to room temperature.
8. preparation method as claimed in claim 1, wherein, metal oxide air-sensitive compound substance described in described step 4 is coated on substrate surface and refers to: after being ground by described metal oxide air-sensitive compound substance, with deionized water furnishing pasty state, and be evenly coated in substrate surface.
9. preparation method as claimed in claim 1, wherein, burin-in process described in described step 4 refers to: described in be coated in the metal oxide air-sensitive compound substance of substrate surface under 400 ~ 600 DEG C of conditions, keep 1 ~ 5h, then logical direct current on agingtable, under 300 DEG C of conditions, keep 1 ~ 10 day.
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