CN103487473B - Rare earth modified zinc oxide gas sensor and preparation method thereof - Google Patents
Rare earth modified zinc oxide gas sensor and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of rare earth modified zinc oxide gas sensor and preparation method thereof, belong to trace gas detection technical field. The present invention provides has high sensitivity, selectivity, stability the gas sensor with quick response recovery time and preparation method thereof to volatile organic matter. The present invention scribbles rare earth modified zinc oxide material on aluminium oxide ceramics tube outer surface. Rare earth modified zinc oxide gas sensitive is with different zinc sources for raw material, adopts hydro-thermal method original position to adulterate one or more rare earth elements to improve its sensitive property to different volatile organic matters. The invention have the advantage that production technology is simple, easy and simple to handle, production cost is low, it is little to pollute, adulterate or recombination process one step completes, organic volatile gas is had high sensitivity, strong selectivity, long-term stability and quick response recovery time by the sensor of preparation.
Description
Technical field
The present invention relates to a kind of rare earth modified zinc oxide gas sensor and preparation method thereof, belong to trace gas detection technical field.
Technical background
Along with the fast development of modern science and technology, commercial production scale sharply expands, and uses and the kind of inflammable and explosive and toxic and harmful and the quantity that produce also are continuously increased in production process. They once reveal will serious environment pollution, and have blast, fire and the danger that makes people poisoning. Along with extensive use and the bubble-tight raising of residential structure of organic decorative materials, household and the health problem that in working environment, the indoor polluted gas of release causes also are increasingly subject to pay attention to. In addition, the grade evaluation of agricultural products grain and vegetables and fruits etc. and safe storage, fresh-keeping and the storage of animal husbandry product meat milk product etc., the detection of fishery products Fish seafood freshness and preservation, airport customs explosive anti-terrorism safety check etc. aspect, is required for the kind to special gas and concentration is analyzed.
For guaranteeing safety, take preventive measures, in the urgent need to flammable, poisonous and dusty gas being carried out monitor in real time warning and qualitative and quantitative analysis detection. Predominant gas practical at present analyzes method to be had multiple, as: solution conductivity method, infrared absorption, gas chromatography etc. There is expensive equipment in these methods, complicated operation, error is big and analysis time the deficiency such as length. And semiconductor gas sensor due to have easy to use, cheap, respond rapid, highly sensitive, safeguard simple and gas concentration be directly changed into the feature such as voltage or current signal extraction, thus be accordingly used in that detection is inflammable and explosive and toxic and harmful obtains and develops rapidly. The core of sensor is sensitive material, and its size, pattern and structure directly affect device performance.
The advantages such as zinc oxide (ZnO) has abundant raw material, low price relative to other material, synthesis is simple, physicochemical property is stable and become gas sensor domain research the earliest with one of material of greatest concern.And the gas sensor scribbling zinc oxide at present to there is also sensitivity low, poor selectivity, the shortcoming such as response recovery time length and limit its further extensive use.
Summary of the invention
It is an object of the invention to provide a kind of highly sensitive, selectivity is strong, rare earth modified zinc oxide gas sensor that response recovery time is short and preparation method thereof.
Technical solution
Rare earth modified zinc oxide gas sensor, including: alumina ceramic tube, aluminium oxide ceramics tube outer surface scribbles rare earth modified zinc oxide material.
The preparation method of rare earth modified zinc oxide gas sensor, preparation method is as follows:
(1) with deionized water for solvent with being made into containing zinc aqueous solution containing zinc precursor, by mol ratio is 0.01-10%, one or more are molten to containing making rare earth-zinc saline solution in zinc aqueous solution containing rare earth nitrate simultaneously, another preparation molar concentration is the sodium hydroxide solution of 1-20mol/L or molar concentration is the carbamide of 0.01-2mol/L, it is added drop-wise in rare earth-zinc saline solution, or rare earth-zinc saline solution is added drop-wise in sodium hydroxide or urea liquid, make rare earth-zinc aqueous slkali, ethylenediamine or the cetyl trimethylammonium bromide auxiliary agent that molar concentration is 0.001-0.005mol/L is added at rare earth-zinc aqueous slkali, stirring or ultrasonic reaction 0.5-5h, or directly rare earth-zinc aqueous slkali is at room temperature stirred or ultrasonic reaction 0.5-5h, then stirring or ultrasonic solution are proceeded in water heating kettle and react 5-48h at 70-220 DEG C, reacted sample deionized water and washing with alcohol, dry, can be prepared by the zinc oxide of doping or compound rare-earth, for the test of air-sensitive performance directly or after heat treatment,
(2) zinc oxide material weighing rear-earth-doped or compound prepared by 1-20mg step (1) is put in agate mortar, adding volume ratio is 1-3:1 dehydrated alcohol and deionization mixed liquor, grind 10-30min, then it is evenly applied on the aluminium oxide ceramics tube core of acid, alcohol supersound process, stands and dry 6-15h;
(3) by step (2) coated ceramic die at 450-550 DEG C, heating rate is 1-5 DEG C/min, roasting 1-5h, install resistance wire additional and be welded on pedestal, make heater-type gas sensor, aging 5-10 days, between 80��440 DEG C, test its air-sensitive performance.
The described molar percentage making rare earth-zinc saline solution Rare Earth Ion and zinc ion is 0.01-10at%.
Described is the one in zinc nitrate, zinc acetate, zinc tartrate, zinc citrate, zinc sulfate or zinc chloride containing zinc precursor.
Described is one or more in lanthanum La, cerium Ce, praseodymium Pr, neodymium Nd, samarium Sm, europium Eu, gadolinium Gd, terbium Tb, dysprosium Dy, holmium Ho, erbium Er, thulium Tm, ytterbium Yb, lutecium Lu, yttrium Y containing rare earth nitrate rare earth elements.
The present invention adopts hydro-thermal method original position one or more rare earth elements that adulterate to prepare rare earth modified oxidation. On the one hand, rare earth element is widely used in catalyst, the field such as electrical and optical due to its special 4f electronic structure, and rare earth element is possible not only to promote to improve even to increase the activity of bulk catalyst, selectivity and stability as the adulterant of catalyst. On the other hand, the air-sensitive principle of gas sensor is namely based on redox reaction and makes the resistance of gas sensitive change thus causing the change of electric current, and then the kind of gas and concentration and its curent change is associated. And the oxygen species of gas sensitive surface adsorption are the oxidants of reaction, the process of its oxidability impact reaction, path and product, the material that oxidability is strong is conducive to improving air-sensitive performance under suitable operating temperature, and rare earth element is compared zinc element and had higher oxygen storage capacity, and then be conducive to improving its air-sensitive performance. The rare earth element with high oxygen storage power can be distributed in surface or the inside of zinc oxide by the present invention, for improve or improve pure zinc oxide to alcohols, aldehydes, ketone, amine, benzene class, halohydrocarbon volatile organic compounds (such as ethanol, toluene, acetone, formaldehyde, trimethylamine, dimethylamine, carbon tetrachloride) air-sensitive performance, volatile organic compounds is had high sensitivity, selectivity, stability to provide and there is the gas sensor of quick response recovery time.
The invention have the characteristics that
Production technology of the present invention is simple, easy and simple to handle, production cost is low, it is little to pollute, doping or recombination process one step complete, and organic volatile gas is had high sensitivity, selectivity, stability and quick response recovery time by the material of preparation.
Detailed description of the invention:
Embodiment 1:
0.25mol/LZn(NO3)2��6H2O is dissolved in the deionized water of 40mL and makes zinc solution, stirs 10min, takes 2mol/LNaOH solution 40ml and is added drop-wise to above-mentioned solution, stirs 30min, be transferred in 100mL autoclave, reacts 10h at 180 DEG C. Gained precipitate successively with distilled water, absolute ethanol washing repeatedly after, 80 DEG C to be dried into Zinc oxide powder standby.
Under above-mentioned experiment condition, the Sm (NO of the 7at% that adulterates at zinc solution situ3)3��6H2O, stirs 10min, takes the NaOH solution that 40ml molar concentration is 2mol/L and is added drop-wise to above-mentioned solution, stirs 30min, be transferred in 100mL autoclave, reacts 10h at 180 DEG C. Gained precipitate dries the zinc oxide preparing compound samariums for 80 DEG C after using distilled water, absolute ethanol washing repeatedly successively.
The Zinc oxide powder taking 10mg zinc oxide or compound samarium is placed in agate mortar, add dehydrated alcohol and deionized water mixed liquor that volume ratio is 1:1, grind pulping, then it is evenly applied in the ceramic die of hydrochloric acid and Ethanol Treatment, after standing dries 10 hours, (2 DEG C/min of heating rate) roasting 4h at 500 DEG C, after installing resistance wire additional and being welded to pedestal on agingtable one week of aging, subsequently adopt WS-30A gas sensor tester carry out air-sensitive performance test and calculate contrast its sensitivity.
This sample improves significantly at 400 DEG C of pure ZnO tools of the remolding sensitivity to 50-1000ppm acetone. The sensitivity of acetone can be reached 639.89 when 1000ppm by the ZnO of the Sm of compound 7%, and its sensitivity meets good linear relationship with concentration, and fit equation is: Y=0.6658*X-11.9577, and coefficient R is 0.9974. The ZnO of the Sm of compound 7% to the acetone of 100ppm at 400 DEG C of response recovery time respectively 3s and 4s. Under the interference of some gases, 8-18 times that sensitivity is other gas sensitivities to acetone, is 4-6 times of methanol and ethanol. The ZnO of the Sm of compound 7% is only small to the sensitivity fluctuation of the acetone of 100ppm at 400 DEG C in 30 days, illustrates that it has good stability.
Embodiment 2:
0.17mol/LZn(NO3)2��6H2O is dissolved in the deionized water of 40mL and makes zinc solution, stirs 10min, is added drop-wise in the NaOH solution that 30mL molar concentration is 1.2mol/L, and adds the ethylenediamine of 0.0019mol/L, ultrasonic 30min, be transferred in 100mL autoclave, reacts 20h at 180 DEG C. Gained precipitate successively with distilled water, absolute ethanol washing repeatedly after, 80 DEG C to be dried into white oxide zinc powder standby.
Under above-mentioned experiment condition, the Er (NO of the 5at% that adulterates at zinc solution situ3)3��6H2O, stirs 10min, is added drop-wise in the NaOH solution that 30mL molar concentration is 1.2mol/L, and adds the ethylenediamine of 0.0019mol/L, ultrasonic 30min, be transferred in 100mL autoclave, reacts 20h at 180 DEG C. After gained precipitate uses distilled water, absolute ethanol washing repeatedly successively, 80 DEG C of Zinc oxide powders being dried into erbium doped are standby.
The Zinc oxide powder taking 15mg zinc oxide or erbium doped is placed in agate mortar, add dehydrated alcohol and deionized water mixed liquor that volume ratio is 1:2, grind pulping, then it is evenly applied in the ceramic die of hydrochloric acid and Ethanol Treatment, after standing dries 10 hours, (2 DEG C/min of heating rate) roasting 2h at 500 DEG C, after installing resistance wire additional and being welded to pedestal on agingtable one week of aging, subsequently adopt WS-30A gas sensor tester carry out air-sensitive performance test and calculate contrast its sensitivity.
The sensitivity of ethanol is improved about 5 times by the purer ZnO of ZnO of erbium doped, and response recovery time is also shorter, is 7s and 5s at 300 DEG C of response recovery times to the ethanol of 100ppm.Under the interference of some gases, 7-15 times that sensitivity is other gas sensitivities to ethanol. The ZnO of the erbium of doping 5% is only small to the sensitivity fluctuation of the ethanol of 100ppm at 300 DEG C in 30 days, illustrates that it has good stability.
Embodiment 3:
0.15mol/LZn(CH3COO)2��6H2O is dissolved in the deionized water of 40mL and makes zinc solution, stirs 10min, is added drop-wise in the NaOH solution that 40mL molar concentration is 3mol/L, and ultrasonic 30min is transferred in 100mL autoclave, reacts 15h at 100 DEG C. Gained precipitate successively with distilled water, absolute ethanol washing repeatedly after, it is standby that Zinc oxide powder is made in 80 DEG C of drying.
Under above-mentioned experiment condition, the Y (NO of the 4at% that adulterates at zinc solution situ3)3��6H2O, stirs 10min, is added drop-wise in the NaOH solution that 40mL molar concentration is 3mol/L, and ultrasonic 30min is transferred in 100mL autoclave, reacts 15h at 100 DEG C. Gained precipitate successively with distilled water, absolute ethanol washing repeatedly after, the Zinc oxide powder that doped with yttrium is made in 80 DEG C of drying is standby. .
The zinc oxide or the Zinc oxide powder that take 8mg doped with yttrium are placed in agate mortar, add dehydrated alcohol and deionized water mixed liquor that volume ratio is 1:3, grind pulping, then it is evenly applied in the ceramic die of hydrochloric acid and Ethanol Treatment, after standing dries 12 hours, (3 DEG C/min of heating rate) roasting 1h at 500 DEG C, after installing resistance wire additional and being welded to pedestal on agingtable one week of aging, subsequently adopt WS-30A gas sensor tester carry out air-sensitive performance test and calculate contrast its sensitivity.
The sensitivity of the purer ZnO PARA FORMALDEHYDE PRILLS(91,95) of ZnO of doped with yttrium improves about 6 times, and response recovery time is also shorter, is 10s and 15s at 290 DEG C of response recovery times to the formaldehyde of 100ppm. Under the interference of some gases, the sensitivity of PARA FORMALDEHYDE PRILLS(91,95) is 6-20 times of other gas sensitivities. The ZnO of the Y of compound 4% is only small to the sensitivity fluctuation of the formaldehyde of 100ppm at 290 DEG C in 30 days, illustrates that it has good stability.
Embodiment 4:
0.12mol/LZnCl2The deionized water being dissolved in 40mL makes zinc solution, stirs 10min, is added drop-wise in the urea liquid that 40mL molar concentration is 0.18mol/L, and magnetic agitation 10min is transferred in 100mL autoclave, reacts 24h at 80 DEG C. Gained precipitate successively with distilled water, absolute ethanol washing repeatedly after, 80 DEG C of drying, and 300 DEG C of roasting 1h in atmosphere, make Zinc oxide powder standby.
Under above-mentioned experiment condition, the Sm (NO of the 3at% that adulterates at zinc solution situ3)3��6H2Ce (the NO of O and 1at%3)3��6H2O, stirs 10min, is added drop-wise in the urea liquid that 40mL molar concentration is 0.18mol/L, and magnetic agitation 10min is transferred in 100mL autoclave, reacts 24h at 80 DEG C. Gained precipitate successively with distilled water, absolute ethanol washing repeatedly after, 80 DEG C of drying, and 300 DEG C of roasting 1h in atmosphere, the Zinc oxide powder making compound samarium cerium is standby.
The zinc oxide or the Zinc oxide powder that take 18mg compound samarium cerium are placed in agate mortar, add dehydrated alcohol and deionized water mixed liquor that volume ratio is 1:1.5, grind pulping, then it is evenly applied in the ceramic die of hydrochloric acid and Ethanol Treatment, after standing dries 12 hours, (1 DEG C/min of heating rate) roasting 1h at 520 DEG C, after installing resistance wire additional and being welded to pedestal on agingtable aging 5 days, WS-30A gas sensor tester is adopted to carry out air-sensitive performance test and calculate its sensitivity of contrast subsequently.
The sensitivity of toluene is improved about 8 times by the purer ZnO of ZnO of compound samarium cerium, and response recovery time is also shorter, is 9s and 13s at 300 DEG C of response recovery times to the toluene of 100ppm.Under the interference of some gases, 5-10 times that sensitivity is other gas sensitivities to toluene. The ZnO of compound samarium cerium is only small to the sensitivity fluctuation of the toluene of 100ppm at 300 DEG C in 30 days, illustrates that it has good stability.
Claims (4)
1. the preparation method of rare earth modified zinc oxide gas sensor, it is characterised in that adopting hydro-thermal method one step to complete, concrete preparation method is as follows:
1) 0.25mol/LZn (NO3)2��6H2O is dissolved in 40mL deionized water and makes zinc solution, stirring 10min, take 2mol/LNaOH solution 40ml and be added drop-wise to above-mentioned solution, stirring 30min, it is transferred in 100mL autoclave, react 10h at 180 DEG C, gained precipitate successively with distilled water, absolute ethanol washing repeatedly after, 80 DEG C to be dried into Zinc oxide powder standby;
2) at the Sm (NO of zinc solution situ doping 7at%3)3��6H2O, stirs 10min, takes the NaOH solution that 40ml molar concentration is 2mol/L and be added drop-wise to above-mentioned solution, stirring 30min, is transferred in 100mL autoclave, reacts 10h at 180 DEG C, gained precipitate is dried for 80 DEG C and is prepared composite S m (NO after using distilled water, absolute ethanol washing repeatedly successively3)36H2The zinc oxide of O;
3) 10mg zinc oxide or composite S m (NO are taken3)36H2The Zinc oxide powder of O is placed in agate mortar, add dehydrated alcohol and deionized water mixed liquor that volume ratio is 1:1, grind pulping, then it is evenly applied in the ceramic die of hydrochloric acid and Ethanol Treatment, after standing dries 10 hours, with 2 DEG C/min ramp to 500 DEG C, roasting 4h, after installing resistance wire additional and being welded to pedestal on agingtable one week of aging, subsequently adopt WS-30A gas sensor tester carry out air-sensitive performance test and calculate contrast zinc oxide, composite S m (NO3)36H2The sensitivity of the zinc oxide of O;
4) composite S m (NO3)36H2The zinc oxide sample of O improves significantly at 400 DEG C of pure ZnO tools of the remolding sensitivity to 50-1000ppm acetone, the Sm (NO of compound 7at%3)3��6H2The sensitivity of acetone can be reached 639.89 when 1000ppm by the ZnO of O, and its sensitivity Y and acetone concentration X meets good linear relationship, and fit equation is: Y=0.6658*X-11.9577; Sm (the NO of compound 7at%3)36H2The ZnO of O to the acetone of 100ppm 400 DEG C response, recovery time respectively 3s and 4s; Under the interference of toluene, acetone, formaldehyde, trimethylamine, dimethylamine, carbon tetrachloride or alcohol gas, 8-18 times that sensitivity is toluene, formaldehyde, dimethylamine, trimethylamine or carbon tetrachloride gas sensitivity to acetone, is 4-6 times of ethanol; Sm (the NO of compound 7at%3)36H2The ZnO of O 400 DEG C of sensitivity fluctuation to the acetone of 100ppm in 30 days are only small.
2. the preparation method of rare earth modified zinc oxide gas sensor, it is characterised in that adopting hydro-thermal method one step to complete, concrete preparation method is as follows:
1) 0.17mol/LZn (NO3)2��6H2O is dissolved in the deionized water of 40mL and makes zinc solution, stirring 10min, it is added drop-wise in the NaOH solution that 30mL molar concentration is 1.2mol/L, and add the ethylenediamine of 0.0019mol/L, ultrasonic 30min, is transferred in 100mL autoclave, reacts 20h at 180 DEG C, gained precipitate successively with distilled water, absolute ethanol washing repeatedly after, 80 DEG C to be dried into white oxide zinc powder standby;
2) 0.17mol/LZn (NO3)2��6H2O is dissolved in the deionized water of 40mL and makes zinc solution, the Er (NO of the 5at% that adulterates at zinc solution situ3)3��6H2O, stirring 10min, it is added drop-wise in the NaOH solution that 30mL molar concentration is 1.2mol/L, and add the ethylenediamine of 0.0019mol/L, ultrasonic 30min, is transferred in 100mL autoclave, reacts 20h at 180 DEG C, after gained precipitate uses distilled water, absolute ethanol washing repeatedly successively, 80 DEG C are dried into doping Er (NO3)36H2The Zinc oxide powder of O is standby;
3) 15mg zinc oxide or doping Er (NO are taken3)36H2The Zinc oxide powder of O is placed in agate mortar, add dehydrated alcohol and deionized water mixed liquor that volume ratio is 1:2, grind pulping, then it is evenly applied in the ceramic die of hydrochloric acid and Ethanol Treatment, after standing dries 10 hours, with 2 DEG C/min ramp to 500 DEG C, roasting 2h, after installing resistance wire additional and being welded to pedestal on agingtable one week of aging, subsequently adopt WS-30A gas sensor tester carry out air-sensitive performance test and calculate contrast zinc oxide, doping Er (NO3)36H2The zinc oxide sensitivity of O;
4) doping Er (NO3)36H2The sensitivity of ethanol is improved about 5 times by the purer ZnO of ZnO of O, and response recovery time is also shorter, is 7s and 5s at 300 DEG C to the response of the ethanol of 100ppm, recovery time; Under the interference of toluene, acetone, formaldehyde, trimethylamine, dimethylamine, carbon tetrachloride or alcohol gas,To the sensitivity of ethanol it isToluene, acetone, formaldehyde, trimethylamine, dimethylamine, 7-15 times of carbon tetrachloride gas sensitivity; Er (the NO of doping 5at%3)36H2The ZnO of O 300 DEG C of sensitivity fluctuation to the ethanol of 100ppm in 30 days are only small.
3. the preparation method of rare earth modified zinc oxide gas sensor, it is characterised in that adopting hydro-thermal method one step to complete, concrete preparation method is as follows:
1) 0.15mol/LZn (CH3COO)2��6H2O is dissolved in the deionized water of 40mL and makes zinc solution, stirring 10min, it is added drop-wise in the NaOH solution that 40mL molar concentration is 3mol/L, ultrasonic 30min, it is transferred in 100mL autoclave, react 15h at 100 DEG C, gained precipitate successively with distilled water, absolute ethanol washing repeatedly after, it is standby that Zinc oxide powder is made in 80 DEG C of drying;
2) 0.15mol/LZn (CH3COO)2��6H2O is dissolved in the deionized water of 40mL and makes zinc solution, the Y (NO of the 4at% that adulterates at zinc solution situ3)3��6H2O, stirs 10min, is added drop-wise in the NaOH solution that 40mL molar concentration is 3mol/L, ultrasonic 30min, is transferred in 100mL autoclave, reacts 15h at 100 DEG C, after gained precipitate uses distilled water, absolute ethanol washing repeatedly successively, doping Y (NO is made in 80 DEG C of drying3)36H2The Zinc oxide powder of O is standby;
3) 8mg doping Y (NO is taken3)36H2The zinc oxide of O or Zinc oxide powder are placed in agate mortar, add dehydrated alcohol and deionized water mixed liquor that volume ratio is 1:3, grind pulping, then it is evenly applied in the ceramic die of hydrochloric acid and Ethanol Treatment, after standing dries 12 hours, with 3 DEG C/min ramp to 500 DEG C, roasting 1h, after installing resistance wire additional and being welded to pedestal on agingtable one week of aging, subsequently adopt WS-30A gas sensor tester carry out air-sensitive performance test and calculate contrast doping Y (NO3)36H2The zinc oxide of O, zinc oxide sensitivity;
4) sensitivity of the purer ZnO PARA FORMALDEHYDE PRILLS(91,95) of ZnO of doping Y (NO3) 36H2O improves about 6 times, and response recovery time is also shorter, is 10s and 15s at 290 DEG C of response recovery times to the formaldehyde of 100ppm; Under the interference of toluene, acetone, formaldehyde, trimethylamine, dimethylamine, carbon tetrachloride or alcohol gas, the sensitivity of PARA FORMALDEHYDE PRILLS(91,95) is 6-20 times of toluene, ethanol, acetone, dimethylamine, trimethylamine or carbon tetrachloride gas sensitivity; ZnO 290 DEG C of sensitivity fluctuation to the formaldehyde of 100ppm in 30 days of Y (NO3) 3 6H2O of compound 4at% are only small.
4. the preparation method of rare earth modified zinc oxide gas sensor, it is characterised in that adopting hydro-thermal method one step to complete, concrete preparation method is as follows:
1) 0.12mol/LZnCl2The deionized water being dissolved in 40mL makes zinc solution, stirring 10min, it is added drop-wise in the urea liquid that 40mL molar concentration is 0.18mol/L, magnetic agitation 10min, is transferred in 100mL autoclave, reacts 24h at 80 DEG C, after gained precipitate uses distilled water, absolute ethanol washing repeatedly successively, 80 DEG C of drying, and 300 DEG C of roasting 1h in atmosphere, make Zinc oxide powder standby;
2) 0.12mol/LZnCl2 is dissolved in the deionized water of 40mL and makes zinc solution, Ce (NO3) 3 6H2O at Sm (NO3) 3 6H2O and the 1at% of zinc solution situ doping 3at%, stirring 10min, it is added drop-wise in the urea liquid that 40mL molar concentration is 0.18mol/L, magnetic agitation 10min, it is transferred in 100mL autoclave, 24h is reacted at 80 DEG C, gained precipitate is successively with distilled water, absolute ethanol washing repeatedly after, 80 DEG C of drying, and 300 DEG C of roasting 1h in atmosphere, the Zinc oxide powder making composite S m (NO3) 36H2O and Ce (NO3) 36H2O is standby,
3) zinc oxide or the Zinc oxide powder that take 18mg composite S m (NO3) 36H2O and Ce (NO3) 36H2O are placed in agate mortar, add dehydrated alcohol and deionized water mixed liquor that volume ratio is 1:1.5, grind pulping, then it is evenly applied in the ceramic die of hydrochloric acid and Ethanol Treatment, after standing dries 12 hours, with 1 DEG C/min ramp to 520 DEG C, roasting 1h, after installing resistance wire additional and being welded to pedestal on agingtable aging 5 days, WS-30A gas sensor tester is adopted to carry out air-sensitive performance test and calculate the zinc oxide of contrast composite S m (NO3) 36H2O and Ce (NO3) 36H2O subsequently, zinc oxide sensitivity,
4) composite S m (NO3)36H2O and Ce (NO3)36H2The sensitivity of toluene is improved about 8 times by the purer ZnO of ZnO of O, and response recovery time is also shorter, is 9s and 13s at 300 DEG C of response recovery times to the toluene of 100ppm; Under the interference of toluene, acetone, formaldehyde, trimethylamine, dimethylamine, carbon tetrachloride or alcohol gas, 5-10 times that sensitivity is ethanol, acetone, carbon tetrachloride, dimethylamine or trimethylamine gas sensitivity to toluene; Compound 3at%Sm (NO3)36H2O and 1at%Ce (NO3)36H2The ZnO of O 300 DEG C of sensitivity fluctuation to the toluene of 100ppm in 30 days are only small.
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| CN113447535A (en) * | 2021-08-02 | 2021-09-28 | 上海海洋大学 | Gas sensitive material, preparation method and application thereof, and gas sensor element |
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