CN101493430A - Hydrogen sulfide gas sensitive, preparation, and method for making hydrogen sulfide gas sensitive device - Google Patents
Hydrogen sulfide gas sensitive, preparation, and method for making hydrogen sulfide gas sensitive device Download PDFInfo
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- CN101493430A CN101493430A CNA2009100607723A CN200910060772A CN101493430A CN 101493430 A CN101493430 A CN 101493430A CN A2009100607723 A CNA2009100607723 A CN A2009100607723A CN 200910060772 A CN200910060772 A CN 200910060772A CN 101493430 A CN101493430 A CN 101493430A
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Abstract
The invention relates to a hydrogen sulfide gas-sensing material and preparation thereof as well as a method for manufacturing hydrogen sulfide gas-sensing devices, comprising: SnO2 powder and TiO2 powder are mixed according to the molar ratio of 6-10: 1 for obtaining SnO2-TiO2 nano-composite material; Pb(NO3)2 or AgNO3 is added and then fine grinded; the hydrogen sulfide gas-sensing material is regulated into a paste shape by using anhydrous ethanol and polyethylene glycol, and then evenly coated on the surface of an electrode tube; by annealing processing, a gas-sensing electrode tube is obtained; finally, the gas-sensing electrode tube is welded, electrically aged, and packaged according to a heater type structure traditional technology for manufacturing the hydrogen sulfide gas-sensing device. Compared with the prior art, the invention has the advantages that the hydrogen sulfide gas-sensing material has the quantum effect of the nano material, self-catalytic activity, surface effect, and the like, and also has high sensitivity to the hydrogen sulfide gas, high resolution, good choosing performance, short response time, and low operating temperature as a novel gas-sensing material.
Description
Technical field
The present invention relates to the method for making of a kind of sulfuretted hydrogen air-sensitive material and preparation thereof and stink damp sensing device, belong to Metal Oxide Semiconductor Gas Sensing Element Technology field.
Background technology
Sulfuretted hydrogen is one of major pollutants of atmosphere, and the sulfuretted hydrogen that the whole world enters atmosphere every year is about 100,000,000 tons.The people be cause at least more than 3,000,000 tons, main source is production runes such as steel-making, ironmaking, oil refining, pharmacy, process hides, papermaking, oil well, sewer, colliery, methane-generating pit also have hydrogen sulfide gas and produce.Sulfuretted hydrogen has severe toxicity, and being has strong nerve and choke damp, and 0.1%～0.15% sulfuretted hydrogen just can the causing death, and sulfuretted hydrogen can the heavy corrosion various device, has become one of typical public hazards.Therefore, the detection to hydrogen sulfide gas has crucial meaning.
The research of domestic and international now most metal-oxide semiconductor (MOS) stink damp dependent sensors and production are with SnO
2, ZnO, WO
3, Nb
2O
5-TiO
2Be the main matrix material, 95% is the gas sensor of traditional heater-type structure in the home market.And, be in exploration, conceptual phase at home for the stink damp dependent sensor, do not form commercialization as yet.Because the harmfulness of hydrogen sulfide gas is very big, therefore studying a kind of stink damp dependent sensor that can be easy, sensitive, quick, accurate, economic will have very big market outlook.
To the first-selected semiconductor gas sensor of the optimal method of the detection of hydrogen sulfide gas, because that it has is cheap, reaction is fast, highly sensitive, on-the-spotly detect, advantage such as easy to use.Wherein desirable gas sensor depends on the performance of gas sensitive, and the exploitation of gas sensitive is the most key part in the gas-sensitive sensor device research field.
Summary of the invention
Problem to be solved by this invention be propose at above-mentioned prior art a kind of highly sensitive, can Validity Test the gas sensitive and preparation method thereof of hydrogen sulfide gas.
Purpose in addition of the present invention is to propose a kind of method for making that adopts the stink damp sensing device of this sulfuretted hydrogen air-sensitive material.
The present invention is adopted solution to be by the problem of the above-mentioned proposition of solution: sulfuretted hydrogen air-sensitive material is characterized in that including
I) matrix SnO
2-TiO
2Nano composite material, wherein Sn: the Ti mol ratio is 6-10: 1,
Ii) Pb (NO
3)
2Or AgNO
3, its incorporation is matrix SnO
2-TiO
2The 1%-5% of nano composite material weight.
Press such scheme, described SnO
2-TiO
2Nano composite material is a nanometer fine powder, and its particle diameter is 20-100nm.
The technical scheme that the preparation of sulfuretted hydrogen air-sensitive material of the present invention is adopted is: the preparation of sulfuretted hydrogen air-sensitive material is characterized in that including following steps:
1) SnO
2-TiO
2The preparation of compound substance
With SnO
2Powder and TiO
2Powder is SnO in molar ratio
2: TiO
2=6-10: 1 ratio is mixed, and obtains SnO
2-TiO
2Nano composite material; Described TiO
2Powder is to adopt sol-gel process to make, and includes following steps:
(1) in volume parts, get 6-15 part tetrabutyl titanate under vigorous stirring, slowly add 20 parts of absolute ethyl alcohols and 6 parts of glacial acetic acid, continue stirring it is mixed fully, obtain clear solution A;
(2) with 3-6 part deionized water, 10 parts of absolute ethyl alcohols mixing obtain solution B;
(3) under stirring condition solution B dropwise is added drop-wise among the clear solution A, wherein clear solution A: solution B is 2.4-3 by volume: 1; Obtain mixed solution C, mixed solution C was obtained flaxen gel in water-bath 5-20 minute under 60 ℃ of conditions;
(4) will go up the light yellow gel that goes on foot gained, 80-120 ℃ of temperature range inner drying 4-8h obtains light yellow xerogel in vacuum drying chamber, grinds and obtains TiO
2Powder;
Described SnO
2Powder adopts coprecipitation to make, and includes following steps:
(1) with SnCl
45H
2O is configured to the aqueous solution of 0.05-0.2mol/L, and in molar ratio 1: 4-6 gets SnCl
4Solution mixes with citric acid fully;
(2) dropping ammonia is warming up to 80-100 ℃ to PH＞7, forms white emulsion.
(3) through suction filtration, washing, dry, grinding obtains SnO
2Powder.
2) with the SnO of step 1) gained
2-TiO
2Nano composite material is added Pb (NO by the 1%-5% of its weight ratio
3)
2Or AgNO
3, carry out fine gtinding then, promptly get sulfuretted hydrogen air-sensitive material.
Press such scheme, described drying is meant in 60-100 ℃ of scope carries out low temperature drying.
The technical scheme that the method for making of stink damp sensing device of the present invention adopts is: with sulfuretted hydrogen air-sensitive material with an amount of absolute ethyl alcohol and polyglycol furnishing pasty state, then it evenly is coated in the electrode tube surface, through 400-500 ℃ annealing in process 2-4 hour, promptly make the core of stink damp sensing device: the gas sensing electrode pipe, by heater-type structure traditional handicraft the gas sensing electrode pipe is welded at last, electricity is aging, and encapsulation makes the stink damp sensing device.
Beneficial effect compared with prior art of the present invention is:
The present invention proposes a kind of new sulfuretted hydrogen air-sensitive material, it possesses the quantum effect of nano material, the self-catalysis activity, characteristics such as surface effect, as a kind of gas sensitive of novelty, highly sensitive simultaneously to hydrogen sulfide gas, the resolution height, the selection performance is good, and the response time is short, working temperature is low, meets the requirement of the stink damp dependent sensor device of practical standard.
The stink damp sensing device the key technical indexes that is made by sulfuretted hydrogen air-sensitive material of the present invention is as follows:
1) device sensing range 10ppm-1000ppm (gas concentration);
2) device working temperature: 200 ℃-350 ℃;
3) detection sensitivity: 20-80;
4) Immunity Performance: to the interference gas hydrocarbon, acetone sensitivity≤5 (concentration 10-1000ppm, normal working temperature scope)
5) the device reaction time: less than 12s,
6) device release time: less than 35s.
Embodiment
Further introduce the present invention below by embodiment, but embodiment can not be construed as limiting the invention.
Embodiment 1
1. composite nanometre powder SnO
2-TiO
2Preparation
TiO
2Powder is to be made by sol-gel process, and basic process is as follows: get the 10ml tetrabutyl titanate under vigorous stirring, slowly add 20ml absolute ethyl alcohol and 6ml glacial acetic acid, continuation stirring a period of time is mixed it fully, obtains clear solution A; With the 3ml deionized water, the mixing of 10ml absolute ethyl alcohol obtains solution B; Under stirring condition, solution B is added drop-wise among the clear solution A gradually, obtains colourless transparent solution C, colourless transparent solution C water-bath under 60 ℃ of conditions was obtained the gel of faint yellow clear in 15 minutes; After resulting gel seal left standstill 24 hours, 100 ℃ of dry 6h obtained light yellow xerogel in drying box; Obtain TiO after the grinding
2Powder.
SnO
2Powder is to be made by coprecipitation, and basic process is as follows: with SnCl
45H
2O is configured to the solution of 0.1mol/L, gets the SnCl of 10ml 0.1mol/L
4Solution mixes with 10ml 0.4mol/L citric acid, is stirred to dissolving fully.Dropping ammonia is to PH＞7, is warming up to 80 ℃ and be incubated 30 minutes, forms white emulsion.Through suction filtration, after the washing precipitation (with AgNO
3Solution detects no remaining Cl
-), in drying box, obtain xerogel with 80 ℃ of low temperature dryings, grind and obtain SnO
2Powder.
By changing SnO
2And TiO
2The amount of powder obtains mol ratio Sn: Ti=6: 1 matrix SnO
2-TiO
2Nano composite material.
2. with the matrix SnO of step 1 gained
2-TiO
2Nano composite material is added Pb (NO by 1% of its weight ratio
3)
2, improving sensitivity and selectivity to hydrogen sulfide gas, behind the fine gtinding with an amount of absolute ethyl alcohol and polyglycol (SnO
2-TiO
2The compound substance gross mass 1%) the furnishing pasty state, evenly be coated in the electrode tube surface, through 400 ℃ of annealing in process 3 hours, promptly make the core of stink damp sensing device: the gas sensing electrode pipe.By heater-type structure traditional handicraft the gas sensing electrode pipe is welded at last, electricity is aging, and encapsulation makes the stink damp sensing device.
Embodiment 2
1. composite nanometre powder SnO
2-TiO
2Preparation
TiO
2Powder is to be made by sol-gel process, and basic process is as follows: get the 15ml tetrabutyl titanate under vigorous stirring, slowly add 20ml absolute ethyl alcohol and 6ml glacial acetic acid, continuation stirring a period of time is mixed it fully, obtains clear solution A; With the 5ml deionized water, the mixing of 10ml absolute ethyl alcohol obtains solution B; Under stirring condition, solution B is added drop-wise among the clear solution A gradually, obtains colourless transparent solution C, colourless transparent solution C water-bath under 60 ℃ of conditions was obtained the gel of faint yellow clear in 20 minutes; After resulting gel seal left standstill 24 hours, 120 ℃ of dry 4h obtained light yellow xerogel and grind and obtain TiO in drying box
2Powder;
SnO
2Powder is to be made by coprecipitation, and basic process is as follows: with SnCl
45H
2O is configured to the solution of 0.05mol/L, gets the SnCl of 20ml 0.05mol/L
4Solution mixes with 20ml 0.3mol/L citric acid, is stirred to dissolving fully.Dropping ammonia is to PH＞7, is warming up to 100 ℃ and be incubated 15 minutes, forms white emulsion.Through suction filtration, after the washing precipitation (with AgNO
3Solution detects no remaining Cl
-), in drying box, obtain xerogel with 100 ℃ of low temperature dryings, grind and obtain SnO
2Powder.
By changing SnO
2And TiO
2The amount of powder obtains mol ratio Sn: Ti=10: 1 matrix SnO
2-TiO
2Nano composite material.
2. with the matrix SnO of step 1 gained
2-TiO
2Nano composite material is added Pb (NO by 4% of its weight ratio
3)
2,, (account for SnO with an amount of absolute ethyl alcohol and polyglycol behind the fine gtinding to improve sensitivity and selectivity to hydrogen sulfide gas
2-TiO
2The compound substance gross mass 5%) the furnishing pasty state, evenly be coated in the electrode tube surface, through 450 ℃ of annealing in process 2 hours, promptly make the core of stink damp sensing device: the gas sensing electrode pipe.By heater-type structure traditional handicraft the gas sensing electrode pipe is welded at last, electricity is aging, and encapsulation makes the stink damp sensing device.
Embodiment 3
1. composite nanometre powder SnO
2-TiO
2Preparation
TiO
2Powder is to be made by sol-gel process, and basic process is as follows: get the 6ml tetrabutyl titanate under vigorous stirring, slowly add 20ml absolute ethyl alcohol and 6ml glacial acetic acid, continuation stirring a period of time is mixed it fully, obtains clear solution A; With the 3ml deionized water, the mixing of 10ml absolute ethyl alcohol obtains solution B; Under stirring condition, solution B is added drop-wise among the clear solution A gradually, obtains colourless transparent solution C, colourless transparent solution C water-bath under 60 ℃ of conditions was obtained the gel of faint yellow clear in 8 minutes; After resulting gel seal left standstill 24 hours, 80 ℃ of dry 8h obtained light yellow xerogel in drying box, ground to obtain TiO
2Powder;
SnO
2Powder is to be made by coprecipitation, and basic process is as follows: with SnCl
45H
2O is configured to the solution of 0.2mol/L, gets the SnCl of 5ml 0.1mol/L
4Solution mixes with 5ml 0.5mol/L citric acid, is stirred to dissolving fully.Dropping ammonia is to PH＞7, is warming up to 90 ℃ and be incubated 20 minutes, forms white emulsion.Through suction filtration, after the washing precipitation (with AgNO
3Solution detects no remaining Cl
-), in drying box, obtain xerogel with 60 ℃ of low temperature dryings, grind and obtain SnO
2Powder.
By changing SnO
2And TiO
2The amount of powder obtains mol ratio Sn: Ti=8: 1 matrix SnO
2-TiO
2Nano composite material.
2. with the matrix SnO of step 1 gained
2-TiO
2Nano composite material is added AgNO by 5% of its weight ratio
3,, (account for SnO with an amount of absolute ethyl alcohol and polyglycol behind the fine gtinding to improve sensitivity and selectivity to hydrogen sulfide gas
2-TiO
2The compound substance gross mass 3%) the furnishing pasty state, evenly be coated in the electrode tube surface, through 500 ℃ of annealing in process 2 hours, promptly make the core of stink damp sensing device: the gas sensing electrode pipe.By heater-type structure traditional handicraft the gas sensing electrode pipe is welded at last, electricity is aging, and encapsulation makes the stink damp sensing device.
Each cited raw material of the present invention can both be realized the present invention, and the bound value of each raw material, interval value can both realize the present invention; Do not enumerate embodiment one by one at this.Bound value, the interval value of technological parameter of the present invention (as temperature, time etc.) can both be realized the present invention, do not enumerate embodiment one by one at this.
Claims (5)
1, sulfuretted hydrogen air-sensitive material is characterized in that including
I) matrix SnO
2-TiO
2Nano composite material, wherein Sn: the Ti mol ratio is 6-10: 1,
Ii) Pb (NO
3)
2Or AgNO
3, its incorporation is matrix SnO
2-TiO
2The 1%-5% of nano composite material weight.
2, by the described sulfuretted hydrogen air-sensitive of claim 1 material, it is characterized in that described SnO
2-TiO
2Nano composite material is a nanometer fine powder, and its particle diameter is 20-100nm.
3, the preparation of the described sulfuretted hydrogen air-sensitive of claim 1 material is characterized in that including following steps:
1) SnO
2-TiO
2The preparation of compound substance
With SnO
2Powder and TiO
2Powder is SnO in molar ratio
2: TiO
2=6-10: 1 ratio is mixed, and obtains SnO
2-TiO
2Nano composite material; Described TiO
2Powder is to adopt sol-gel process to make, and includes following steps:
(1) in volume parts, get 6-15 part tetrabutyl titanate under vigorous stirring, slowly add 20 parts of absolute ethyl alcohols and 6 parts of glacial acetic acid, continue stirring it is mixed fully, obtain clear solution A;
(2) with 3-6 part deionized water, 10 parts of absolute ethyl alcohols mixing obtain solution B;
(3) under stirring condition solution B dropwise is added drop-wise among the clear solution A, wherein clear solution A: solution B is 2.4-3 by volume: 1; Obtain mixed solution C, mixed solution C was obtained flaxen gel in water-bath 5-20 minute under 60 ℃ of conditions;
(4) will go up the light yellow gel that goes on foot gained, 80-120 ℃ of temperature range inner drying 4-8h obtains light yellow xerogel in vacuum drying chamber, grinds and obtains TiO
2Powder;
Described SnO
2Powder adopts coprecipitation to make, and includes following steps:
(1) with SnCl
45H
2O is configured to the aqueous solution of 0.05-0.2mol/L, and in molar ratio 1: 4-6 gets SnCl
4Solution mixes with citric acid fully;
(2) dropping ammonia is warming up to 80-100 ℃ to PH＞7, forms white emulsion;
(3) through suction filtration, washing, dry, grinding obtains SnO
2Powder;
2) with the SnO of step 1) gained
2-TiO
2Nano composite material is added Pb (NO by the 1%-5% of its weight ratio
3)
2Or AgNO
3, carry out fine gtinding then, promptly get sulfuretted hydrogen air-sensitive material.
4, by the preparation of the described sulfuretted hydrogen air-sensitive of claim 3 material, it is characterized in that SnO
2Drying described in the preparation of powder is meant in 60-100 ℃ of scope carries out low temperature drying.
5, the method for making of stink damp sensing device is characterized in that including following steps:
1) SnO
2-TiO
2The preparation of compound substance
With SnO
2Powder and TiO
2Powder is SnO in molar ratio
2: TiO
2=6-10: 1 ratio is mixed, and obtains SnO
2-TiO
2Nano composite material; Described TiO
2Powder is to adopt sol-gel process to make, and includes following steps:
(1) in volume parts, get 6-15 part tetrabutyl titanate under vigorous stirring, slowly add 20 parts of absolute ethyl alcohols and 6 parts of glacial acetic acid, continue stirring it is mixed fully, obtain clear solution A;
(2) with 3-6 part deionized water, 10 parts of absolute ethyl alcohols mixing obtain solution B;
(3) under stirring condition solution B dropwise is added drop-wise among the clear solution A, wherein clear solution A: solution B is 2.4-3 by volume: 1; Obtain mixed solution C, mixed solution C was obtained flaxen gel in water-bath 5-20 minute under 60 ℃ of conditions;
(4) will go up the light yellow gel that goes on foot gained, 80-120 ℃ of temperature range inner drying 4-8h obtains light yellow xerogel in vacuum drying chamber, grinds and obtains TiO
2Powder;
Described SnO
2Powder adopts coprecipitation to make, and includes following steps:
(1) with SnCl
45H
2O is configured to the aqueous solution of 0.05-0.2mol/L, and in molar ratio 1: 4-6 gets SnCl
4Solution mixes with citric acid fully;
(2) dropping ammonia is warming up to 80-100 ℃ to PH＞7, forms white emulsion;
(3) through suction filtration, washing, dry, grinding obtains SnO
2Powder;
2) with the SnO of step 1) gained
2-TiO
2Nano composite material is added Pb (NO by the 1%-5% of its weight ratio
3)
2Or AgNO
3, carry out fine gtinding then, promptly get sulfuretted hydrogen air-sensitive material;
3) with sulfuretted hydrogen air-sensitive material with an amount of absolute ethyl alcohol and polyglycol furnishing pasty state, then it evenly is coated in the electrode tube surface, through 400-500 ℃ annealing in process 2-4 hour, promptly make the core of stink damp sensing device: the gas sensing electrode pipe, by heater-type structure traditional handicraft the gas sensing electrode pipe is welded at last, electricity is aging, and encapsulation makes the stink damp sensing device.
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|---|---|---|---|
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|---|---|---|---|
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