CN105651814A - Nanometer tin-sulfide-based gas sensor and preparation method thereof - Google Patents
Nanometer tin-sulfide-based gas sensor and preparation method thereof Download PDFInfo
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- CN105651814A CN105651814A CN201410633570.4A CN201410633570A CN105651814A CN 105651814 A CN105651814 A CN 105651814A CN 201410633570 A CN201410633570 A CN 201410633570A CN 105651814 A CN105651814 A CN 105651814A
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Abstract
The present invention discloses a nanometer tin-sulfide-based gas sensor and a preparation method thereof. The sensor comprises an insulating ceramic pipe, a pair of metal electrodes arranged on the insulating ceramic pipe, a metal leading-out conducting wire arranged on the insulating ceramic pipe, and a gas sensitive material layer sprayed on the metal electrodes, wherein the gas sensitive material layer comprises nanometer tin-sulfide, and the preparation of the nanometer tin-sulfide comprises: adopting 30% hydrogen peroxide as an oxidizing agent, oxidizing a SnCl2 aqueous solution at a temperature of 90 DEG C to obtain a SnCl4 solution, and carrying out a reaction of the prepared SnCl4 aqueous solution and a thioacetamide or sodium sulfide aqueous solution in the presence of ultrasonic waves. According to the present invention, the sensor has characteristics of good ammonia gas selectivity, fast response, fast recovery and being free of sintering, can work at a room temperature, and can be used for determination of ammonia gas within a percentage concentration range and automatic control of the ammonia related production process.
Description
Technical field
The present invention relates to sensor field, in particular it relates to a kind of nanometer tin sulfide base ammonia gas sensor and preparation method thereof.
Background technology
The gas sensitive used in gas sensor can be divided into four classes: the first kind is metal-oxide and composite oxide semiconductor, and conventional oxide has SnO2��ZnO��TiO2����-Fe2O3��WO3, CuO-ZnO hetero-junctions etc.; Composite oxides have the material of perovskite-like structure, such as SrTiO3, spinel type ferrite, such as NiFe2O4; Equations of The Second Kind is formed by conductor and semiconductor combinations, such as metal and the Schottky diode of semiconductor contact composition, MOS field-effect transistor, MIS effect transistor; 3rd class is to have the solid electrolyte of ionic conductivity, if any divalent magnesium ion and the solid electrolyte of oxonium ion composition, silver ion glass; 4th class is organic polymer, such as polypyrrole, polyimides, metal phthalocyanine complex. Being most widely used at present, studying the most thorough is SnO2, metal sulfide base gas sensor is also little, is still in the development phase.
One of developing direction of sensor technology is the air-sensitive performance of exploitation known substance, and nanotechnology can make some known substances have new specific function, can provide excellent sensitive material for sensor. Gas nanosensor has the irreplaceable advantage of conventional sensors: one is that meter Sized Materials has huge interface, it is provided that a large amount of gas passages, thus substantially increasing sensitivity; Two is that operating temperature is greatly lowered; Three is the size reducing sensor.
Automation of Manufacturing Process is the developing direction of large chemical plant, to Chemical Manufacture implement automatically control it is crucial that develop and component a certain in raw material or product had gas sensor highly sensitive, that selectivity is good. Concentration of component change transitions a certain in raw material or product can be the signal of telecommunication by this gas sensor, flows to control equipment, thus realizing automatically controlling to Chemical Manufacture. Ammonia is important industrial chemicals, intermediate and product, relates to ammonia Chemical Manufacture and occupies very big ratio in chemical industry. Developing ammonia gas sensor highly sensitive, that selectivity is good is relate to ammonia Chemical Manufacture to realize the key of automatization. Owing to the ammonia concentration in Chemical Manufacture is higher, mostly at concentration range, accordingly, it would be desirable to this concentration range ammonia can be produced the gas sensor of response by some. At present, this class ammonia gas sensor awaits exploitation.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of nanometer tin sulfide material adopting ultrasonic technology to synthesize and the ammonia gas sensor and preparation method thereof based on nanometer tin sulfide.
Nanometer tin sulfide base ammonia gas sensor provided by the present invention is made up of insulating ceramics pipe, pair of metal electrodes, metal extraction wire and nanometer tin sulfide material layer successively, and wherein nanometer tin sulfide material layer includes polyvinyl alcohol adhesive.
Described insulating ceramics pipe is aluminum oxide ceramic pipe.
Described metal electrode is the interdigital electrode made by metal Au, and the distance between two electrodes is 1mm.
Described metal lead-outs is Pt metal silk.
The diameter of nano particles of described nanometer tin sulfide material layer is 40-120nm; The thickness of nanometer tin sulfide material layer is 50-200 ��m.
The detailed preparation method of described nanometer tin sulfide base gas sensor, including below step.
1) Tin disulfide nanoparticle is prepared, under the ultrasound wave of 80KHz, by SnCl4Aqueous solution reacts with precipitant, and described precipitant is Na2Any one of S and thioacetyl amine aqueous solution, reaction temperature is room temperature to 80 DEG C of scopes, SnCl4With Na2The mol ratio of S is 1:2, SnCl4It is 1:4 with the mol ratio of thioacetamide, after reaction terminates, sucking filtration, obtain yellow mercury oxide, with distilled water wash, dry at 120 DEG C and obtain Tin disulfide nanoparticle.
2) Tin disulfide nanoparticle step 1) prepared mixes with binding agent, grinds 3 hours, makes slurry after dilution.
3) Au slurry is coated on cleaned insulating ceramics pipe and makes interdigital electrode, after drying, weld metal lead-outs.
4) by step 2) slurry for rotary coating prepared prepares into nanometer tin sulfide material layer on metal electrode and insulating ceramics pipe, and then 120 DEG C of drying obtain sensor element.
Beneficial effect: it is good that nanometer tin sulfide base ammonia gas sensor provided by the invention has selectivity, response and recovery are fast, make simple, it is not necessary to sintering, work under room temperature, and consume energy the low advantage low with cost.
Accompanying drawing explanation
Fig. 1 is the structural representation of described nanometer tin sulfide base ammonia gas sensor. In Fig. 1,1 is aluminum oxide ceramic pipe, and 2 is Pt silk lead-out wire, and 3 is Au interdigital electrode, and 4 is nanometer tin sulfide material layer.
Fig. 2 is that the responsiveness of the nanometer tin sulfide base ammonia gas sensor of embodiment 1 preparation is with ammonia concentration change curve.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail, but the invention is not limited in this.
Embodiment 1.
1) 10.0 grams of SnCl are weighed2��2H2O(0.04 mole), put in 200 ml beakers, add 10 milliliters of concentrated hydrochloric acid and dissolve, now, solution shows slightly muddy. Under agitation by SnCl2Solution heats to 90 DEG C, treats SnCl2After solution clarification. Add the hydrogen peroxide 30 milliliters that concentration is 30%, and add water to 200 milliliters, stir 2h, stand one day in light protected environment, obtain SnCl4Solution. With vigorous stirring by the SnCl of preparation4Solution heats to boiling, and keeps boiling 20 minutes, subsequently by SnCl4Solution is placed in ultrasonic thermostatic water bath pot and heats to 80 DEG C, and constant temperature is also stirred vigorously 2 hours, so that the dioxygen water yield of remaining is decomposed completely. Open ultrasound wave, ultrasonic frequency is adjusted to 80kHz. Take the Na that concentration is 1.0 mol/L prepared2S solution 80 milliliters, is added dropwise to SnCl4In solution, SnCl4With Na2The mol ratio of S is 1:2, has a large amount of yellow mercury oxide to generate, treats that it reacts completely. It is cooled to room temperature, sucking filtration, precipitates three times with distilled water wash, the Tin disulfide solid obtained is put into baking oven, within two hours, obtains Tin disulfide nanoparticle 120 DEG C of drying.
2) Tin disulfide nanoparticle step 1) prepared and the polyvinyl alcohol of 0.1%, grind 3 hours, make slurry after dilution.
3) take aluminum oxide ceramic pipe 1, put into the sodium hydroxide solution that concentration is 8 mol/L and boil 30 minutes, take out after cooling, with distilled water flushing three times, be placed in baking oven and dry. Au slurry is coated on cleaned Al 2 O earthenware and makes Au interdigital electrode 2, dries, then the Pt wire bond of diameter 0.1mm is received on electrode as lead-out wire 3.
4) by step 2) slurry for rotary coating prepared prepares into, on Au electrode and aluminum oxide ceramic pipe, the nanometer tin sulfide material layer 4 that thickness is 50 ��m, then obtains sensor element 120 DEG C of drying.
Embodiment 2.
1) 10.0 grams of SnCl are weighed2��2H2O(0.04 mole), put in 200 ml beakers, add 10 milliliters of concentrated hydrochloric acid and dissolve, now, solution shows slightly muddy. Under agitation by SnCl2Solution heats to 90 DEG C, treats SnCl2After solution clarification. Add the hydrogen peroxide 30 milliliters that concentration is 30%, and add water to 200 milliliters, stir 2h, stand one day in light protected environment, obtain SnCl4Solution. With vigorous stirring by the SnCl of preparation4Solution heats to boiling, and keeps boiling 20 minutes, subsequently by SnCl4Solution is placed in ultrasonic thermostatic water bath pot and heats to 80 DEG C, and constant temperature is also stirred vigorously 2 hours, so that the dioxygen water yield of remaining is decomposed completely. It is then turned on ultrasound wave after being cooled to room temperature, ultrasonic frequency is adjusted to 80kHz. Take the Na that concentration is 1.0 mol/L prepared2S solution 80 milliliters, is at room temperature added dropwise to SnCl4In solution, SnCl4With Na2The mol ratio of S is 1:2, has a large amount of yellow mercury oxide to generate. Treat that it reacts completely, sucking filtration, precipitates three times with distilled water wash, the Tin disulfide solid obtained is put into baking oven, within two hours, obtains Tin disulfide nanoparticle 120 DEG C of drying.
2) Tin disulfide nanoparticle step 1) prepared and the polyvinyl alcohol of 0.1%, grind 2.5 hours, make slurry after dilution.
3) take aluminum oxide ceramic pipe 1, put into the sodium hydroxide solution that concentration is 8 mol/L and boil 30 minutes, take out after cooling, with distilled water flushing three times, be placed in baking oven and dry. Au slurry is coated on cleaned Al 2 O earthenware and makes interdigital electrode 2, dries, then the Pt wire bond of diameter 0.1mm is received on electrode as lead-out wire 3.
4) by step 2) slurry for rotary coating prepared prepares into, on Au electrode and aluminum oxide ceramic pipe, the nanometer tin sulfide material layer 4 that thickness is 120 ��m, then obtains sensor element 120 DEG C of drying.
Embodiment 3.
1) 10.0 grams of SnCl are weighed2��2H2O(0.04 mole), put in 200 ml beakers, add 10 milliliters of concentrated hydrochloric acid and dissolve, now, solution shows slightly muddy. Under agitation by SnCl2Solution heats to 90 DEG C, treats SnCl2After solution clarification. Add the hydrogen peroxide 30 milliliters that concentration is 30%, and add water to 200 milliliters, stir 2h, stand one day in light protected environment, obtain SnCl4Solution. With vigorous stirring by the SnCl of preparation4Solution heats to boiling, and keeps boiling 20 minutes, subsequently by SnCl4Solution is placed in ultrasonic thermostatic water bath pot and heats to 80 DEG C, and constant temperature is also stirred vigorously 2 hours, so that the dioxygen water yield of remaining is decomposed completely. Open ultrasound wave, ultrasonic frequency is adjusted to 80kHz. Take the thioacetyl amine aqueous solution 160 milliliters that concentration is 1.0 mol/L prepared, be added dropwise to SnCl4In solution, SnCl4It is 1:4 with the mol ratio of thioacetamide, has yellow mercury oxide slowly generate and progressively increase, treat that it reacts completely.It is cooled to room temperature, sucking filtration, precipitates three times with distilled water wash, the Tin disulfide solid obtained is put into baking oven, within two hours, obtains Tin disulfide nanoparticle 120 DEG C of drying.
2) Tin disulfide nanoparticle step 1) prepared and the polyvinyl alcohol of 0.1%, grind 2 hours, make slurry after dilution.
3) take aluminum oxide ceramic pipe 1, put into the sodium hydroxide solution that concentration is 8 mol/L and boil 30 minutes, take out after cooling, with distilled water flushing three times, be placed in baking oven and dry. Au slurry is coated on cleaned Al 2 O earthenware and makes interdigital electrode 2, dries, then the Pt wire bond of diameter 0.1mm is received on electrode as lead-out wire 3.
4) by step 2) slurry for rotary coating prepared prepares into the nanometer tin sulfide material layer 4 of thickness 200 ��m on Au electrode and aluminum oxide ceramic pipe, then obtains sensor element 120 DEG C of drying.
Claims (6)
1. a gas sensor, it is characterised in that: being made up of insulating ceramics pipe, pair of metal electrodes, metal extraction wire and nanometer tin sulfide material layer successively, wherein nanometer tin sulfide material layer includes a kind of polyvinyl alcohol adhesive.
2. the gas sensor described in claim 1 is a kind of ammonia gas sensor, it is characterised in that: described insulating ceramics pipe is aluminum oxide ceramic pipe.
3. the gas sensor described in claim 1, it is characterised in that: the interdigital electrode that described metal electrode is made up of metal Au, the distance between two electrodes is 1mm.
4. the gas sensor described in claim 1, it is characterised in that: described metal lead-outs is Pt metal silk.
5. the gas sensor described in claim 1, it is characterised in that: the diameter of nano particles of described nanometer tin sulfide material layer is 40-120nm; The thickness of described nanometer tin sulfide material layer is 50-200 ��m.
6. the method for gas sensor according to any one of preparation claim 1-5, including below step:
1) Tin disulfide nanoparticle is prepared, the hydrogen peroxide as oxidant being 30% with concentration, aoxidize SnCl at 90 DEG C2Solution obtains SnCl4Solution, under the ultrasound wave of 80KHz, by the SnCl of preparation4Aqueous solution reacts with precipitant, and described precipitant is Na2Any one of S and thioacetyl amine aqueous solution, reaction temperature is room temperature to 80 DEG C of scopes, SnCl4With Na2The mol ratio of S is 1:2, SnCl4Being 1:4 with the mol ratio of thioacetamide, reaction terminates, and sucking filtration obtains yellow mercury oxide, and with distilled water wash, 120 DEG C dry obtains Tin disulfide nanoparticle;
2) Tin disulfide nanoparticle step 1) prepared mixes with binding agent, grinds 2-3 hour, makes slurry after dilution;
3) Au slurry is coated on the insulating ceramics pipe after cleaning, after drying, welds metal lead-outs;
4) by step 2) slurry for rotary coating prepared prepares into nanometer tin sulfide material layer on metal electrode with insulating ceramics pipe, and then 120 DEG C of drying obtain sensor element.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106706719A (en) * | 2017-01-16 | 2017-05-24 | 中国石油大学(华东) | Tin sulfide nano flower film sensitive to ammonia gas at low temperature |
| CN109959681A (en) * | 2017-12-22 | 2019-07-02 | 中国科学院物理研究所 | A kind of gas-sensitive sensor device and its preparation method and application |
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| CN2700876Y (en) * | 2003-12-23 | 2005-05-18 | 西安交通大学 | Carbon nano tube thin film gas transducer |
| CN1885025A (en) * | 2006-07-11 | 2006-12-27 | 电子科技大学 | Organic nitrogen oxide sensitive composite material and nitrogen oxide gas sensor |
| CN203011891U (en) * | 2013-01-01 | 2013-06-19 | 淮南联合大学 | Surface acoustic wave NO2 gas sensor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106706719A (en) * | 2017-01-16 | 2017-05-24 | 中国石油大学(华东) | Tin sulfide nano flower film sensitive to ammonia gas at low temperature |
| CN109959681A (en) * | 2017-12-22 | 2019-07-02 | 中国科学院物理研究所 | A kind of gas-sensitive sensor device and its preparation method and application |
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