CN103487473A - 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 invention relates to a rare earth modified zinc oxide gas sensor and a preparation method thereof and belongs to the technical field of trace gas detection. The invention provides the gas sensor which has high sensitivity, selectivity and stability to volatile organic materials and has short response recovery time and further provides the preparation method of the gas sensor. According to the invention, a rare earth modified zinc oxide material is applied on the outer surface of an aluminium oxide ceramic pipe; a rare earth modified zinc oxide gas-sensing material uses different zinc sources as raw materials, a hydrothermal method is adopted, and one or multiple rare earth elements are doped in situ to improve the sensitivity of the material to different volatile organic materials. The invention has the advantages that the production technology is simple, the operation is simple and convenient, the manufacturing cost is low, the pollution is low, the doping or compounding process is accomplished at one step, and a prepared sensor has high sensitivity, strong selectivity and long-term stability to organic volatile gas and short response recovery time.
Description
Technical field
The present invention relates to a kind of rare earth modified zinc paste gas sensor and preparation method thereof, belong to the trace gas detection technical field.
Technical background
Along with the fast development of modern science and technology, commercial production scale sharply enlarges, and in production run, uses and kind and the quantity of the inflammable and explosive and toxic and harmful that produces also constantly increase.Once their are revealed will serious environment pollution, and have blast, fire and make the poisoning danger of people.Along with widespread use and the bubble-tight raising of residential structure of organic ornament materials, the health problem that the indoor polluted gas discharged in household and working environment causes also comes into one's own day by day.In addition, grade evaluation and the safe storage of agricultural products grain and vegetables and fruits etc., fresh-keeping and the storage of animal husbandry product meat dairy produce etc., fishery products fish seafood freshness detects and preserves, airport customs explosive anti-terrorism safety check etc. aspect, all need kind and the concentration of special gas are analyzed.
For guaranteeing safety, take preventive measures, in the urgent need to flammable, poisonous and dusty gas being carried out to real-time monitoring alarm and qualitative and quantitative analysis, detect.Current practical main analysis method for gases has multiple, as: solution conductivity method, infrared absorption, vapor-phase chromatography etc.There is the instrument costliness in these methods, complicated operation, the deficiency such as error is large and grow analysis time.And semiconductor gas sensor easy to use owing to having, cheap, respond rapid, highly sensitive, safeguard simple and gas concentration be directly changed into to the characteristics such as voltage or current signal extraction, therefore for detection of inflammable and explosive and toxic and harmful, obtained developing rapidly.The core of sensor is sensitive material, and its size, pattern and structure directly affect device performance.
Zinc paste (ZnO) there is abundant raw material, low price, synthetic simple, the advantage such as physicochemical property is stable with respect to other material and become the gas sensor area research the earliest with one of material of greatest concern.And the gas sensor that scribbles at present zinc paste also exists sensitivity low, poor selectivity, the shortcoming such as response recovery time is long and limit its further widespread use.
Summary of the invention
The object of the present invention is to provide a kind of highly sensitively, selectivity is strong, rare earth modified zinc paste gas sensor that response recovery time is short and preparation method thereof.
Technical solution
Rare earth modified zinc paste gas sensor comprises: alumina ceramic tube scribbles rare earth modified zinc oxide material on the aluminium oxide ceramics tube outer surface.
The preparation method of rare earth modified zinc paste gas sensor, the preparation method is as follows:
(1) take deionized water as solvent with being made into containing the zinc aqueous solution containing the zinc precursor body, one or more that are simultaneously 0.01-10% by mol ratio are molten to containing in the zinc aqueous solution, making rare earth-zinc solution containing rare earth nitrades, the urea that the sodium hydroxide solution that another preparation volumetric molar concentration is 1-20mol/L or volumetric molar concentration are 0.01-2mol/L, be added drop-wise in rare earth-zinc solution, perhaps rare earth-zinc solution is added drop-wise in NaOH or urea liquid, make rare earth-zinc aqueous slkali, add at rare earth-zinc aqueous slkali ethylenediamine or the cetyl trimethyl ammonium bromide auxiliary agent that volumetric molar concentration is 0.001-0.005mol/L, stir 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 will stir or ultrasonic solution proceeds in water heating kettle at 70-220 ℃ of reaction 5-48h, deionized water and ethanol washing for reacted sample, drying, can make the zinc paste of doping or compound rare-earth, directly or after thermal treatment for the test of air-sensitive performance,
(2) take rear-earth-doped or compound zinc oxide material prepared by 1-20mg step (1) and put into agate mortar, adding volume ratio is 1-3:1 absolute ethyl alcohol and deionization mixed liquor again, grind 10-30min, then it evenly is coated on the aluminium oxide ceramics tube core of acid, pure ultrasonic processing to the standing 6-15h that dries;
(3) by the coated ceramic die of step (2) under 450-550 ℃, heating rate is 1-5 ℃/min, roasting 1-5h, install resistance wire additional and it is welded on pedestal, make the heater-type gas sensor, aging 5-10 days, its air-sensitive performance of test between 80～440 ℃.
The described molar percentage of making rare earth-zinc solution Rare Earth Ion and zinc ion is 0.01-10at%.
Described is a kind of in zinc nitrate, zinc acetate, zinc tartrate, zinc citrate, zinc sulfate or zinc chloride containing the zinc precursor body.
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, lutetium Lu, yttrium Y containing the rare earth nitrades rare earth elements.
The present invention adopts in-situ doped one or more rare earth element of hydro-thermal method to make rare earth modified oxidation.On the one hand, rare earth element is because its special 4f electronic structure is widely used in the fields such as catalyzer, electricity and optics, and rare earth element not only can promote to improve activity, selectivity and the stability that even can increase the main body catalyzer as the adulterant of catalyzer.On the other hand, thereby the air-sensitive principle of gas sensor makes the resistance of gas sensitive change with regard to being based on redox reaction, cause the variation of electric current, and then carry out associated by the kind of gas and concentration with its curent change.And the oxygen species of gas sensitive adsorption are the oxygenants of reaction, process, path and the product of its oxidability impact reaction, the material that oxidability is strong is conducive to improve air-sensitive performance under suitable working temperature, and rare earth element compares the zinc element and have stronger oxygen storage capacity, and then be conducive to improve its air-sensitive performance.The present invention can be distributed in the rare earth element with high oxygen storage power the surperficial or inner of zinc paste, for improving or improving the air-sensitive performance of pure zinc oxide to alcohols, aldehydes, ketone, amine, benzene class, halohydrocarbon volatile organic compounds (as: ethanol, toluene, acetone, formaldehyde, trimethylamine, dimethylamine, phenixin), to provide, volatile organic compounds is had high sensitivity, selectivity, stability and has the gas sensor of response recovery time fast.
Characteristics of the present invention are:
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 the material of preparation has high sensitivity, selectivity, stability and response recovery time fast to organic volatile gas.
Embodiment:
Embodiment 1:
0.25mol/L Zn (NO
3)
26H
2o is dissolved in the deionized water of 40mL and makes zinc solution, stirs 10min, gets 2mol/LNaOH solution 40ml and is added drop-wise to above-mentioned solution, stirs 30min, is transferred in the 100mL autoclave, reacts 10h under 180 ℃.After the gained sediment uses distilled water, absolute ethanol washing repeatedly successively, 80 ℃ to be dried into Zinc oxide powder standby.
Under above-mentioned experiment condition, at the Sm (NO of zinc solution situ doping 7at%
3)
36H
2o, stir 10min, and the NaOH solution that to get the 40ml volumetric molar concentration be 2mol/L is added drop-wise to above-mentioned solution, stirs 30min, is transferred in the 100mL autoclave, reacts 10h under 180 ℃.After the gained sediment uses distilled water, absolute ethanol washing repeatedly successively, 80 ℃ of oven dry make the zinc paste of compound samarium.
The Zinc oxide powder of getting 10mg zinc paste or compound samarium is placed in agate mortar, add absolute ethyl alcohol and deionized water mixed liquor that volume ratio is 1:1, grind pulping, then it evenly is coated on the ceramic die of hydrochloric acid and Ethanol Treatment, standing dry 10 hours after, (2 ℃/min of heating rate) roasting 4h under 500 ℃, install resistance wire additional and it is welded to after pedestal on agingtable to aging one week, adopt subsequently WS-30A gas sensor tester to carry out the air-sensitive performance test and calculate its sensitivity of contrast.
This sample has obvious improvement at 400 ℃ of pure ZnO of the remolding sensitivity to 50-1000ppm acetone.The ZnO of compound 7% Sm sensitivity to acetone when 1000ppm can reach 639.89, and its sensitivity and concentration meets good linear relationship, and fit equation is: Y=0.6658*X-11.9577, coefficient R is 0.9974.The ZnO of compound 7% Sm to the acetone of 100ppm 400
should be respectively 3s and 4s release time.Under the interference of some gases, the 8-18 that is other gas sensitivities to the sensitivity of acetone doubly, be the 4-6 of methyl alcohol and ethanol doubly.The ZnO of compound 7% Sm is in 30 days 400
sensitivity fluctuation to the acetone of 100ppm is very little, illustrates that it has good stability.
Embodiment 2:
0.17mol/L Zn (NO
3)
26H
2o is dissolved in the deionized water of 40mL and makes zinc solution, stirs 10min, in the NaOH solution that to be added drop-wise to the 30mL volumetric molar concentration be 1.2mol/L, and adds the ethylenediamine of 0.0019mol/L, and ultrasonic 30min, be transferred in the 100mL autoclave, reacts 20h under 180 ℃.After the gained sediment uses distilled water, absolute ethanol washing repeatedly successively, 80 ℃ to be dried into the white zinc oxide powder standby.
Under above-mentioned experiment condition, at the Er (NO of zinc solution situ doping 5at%
3)
36H
2o, stir 10min, in the NaOH solution that to be added drop-wise to the 30mL volumetric molar concentration be 1.2mol/L, and adds the ethylenediamine of 0.0019mol/L, and ultrasonic 30min, be transferred in the 100mL autoclave, reacts 20h under 180 ℃.After the gained sediment uses distilled water, absolute ethanol washing repeatedly successively, 80 ℃ of Zinc oxide powders that are dried into the doping erbium are standby.
The Zinc oxide powder of getting 15mg zinc paste or doping erbium is placed in agate mortar, add absolute ethyl alcohol and deionized water mixed liquor that volume ratio is 1:2, grind pulping, then it evenly is coated on the ceramic die of hydrochloric acid and Ethanol Treatment, standing dry 10 hours after, (2 ℃/min of heating rate) roasting 2h under 500 ℃, install resistance wire additional and it is welded to after pedestal on agingtable to aging one week, adopt subsequently WS-30A gas sensor tester to carry out the air-sensitive performance test and calculate its sensitivity of contrast.
The purer ZnO of ZnO of doping erbium improves 5 times of left and right to the sensitivity of ethanol, and response recovery time is also shorter, 300
the response recovery time of the ethanol of 100ppm is 7s and 5s.Under the interference of some gases, the 7-15 that is other gas sensitivities to the sensitivity of ethanol doubly.The ZnO of doping 5% erbium is in 30 days 300
sensitivity fluctuation to the ethanol of 100ppm is very little, illustrates that it has good stability.
Embodiment 3:
0.15mol/L Zn (CH
3cOO)
26H
2o is dissolved in the deionized water of 40mL and makes zinc solution, stirs 10min, and in the NaOH solution that to be added drop-wise to the 40mL volumetric molar concentration be 3mol/L, ultrasonic 30min, be transferred in the 100mL autoclave, reacts 15h under 100 ℃.After the gained sediment uses distilled water, absolute ethanol washing repeatedly successively, it is standby that Zinc oxide powder is made in 80 ℃ of oven dry.
Under above-mentioned experiment condition, at the Y (NO of zinc solution situ doping 4at%
3)
36H
2o, stir 10min, and in the NaOH solution that to be added drop-wise to the 40mL volumetric molar concentration be 3mol/L, ultrasonic 30min, be transferred in the 100mL autoclave, reacts 15h under 100 ℃.After the gained sediment uses distilled water, absolute ethanol washing repeatedly successively, the Zinc oxide powder that doped with yttrium is made in 80 ℃ of oven dry is standby.。
Zinc paste or the Zinc oxide powder of getting the 8mg doped with yttrium are placed in agate mortar, add absolute ethyl alcohol and deionized water mixed liquor that volume ratio is 1:3, grind pulping, then it evenly is coated on the ceramic die of hydrochloric acid and Ethanol Treatment, standing dry 12 hours after, (3 ℃/min of heating rate) roasting 1h under 500 ℃, install resistance wire additional and it is welded to after pedestal on agingtable to aging one week, adopt subsequently WS-30A gas sensor tester to carry out the air-sensitive performance test and calculate its sensitivity of contrast.
The sensitivity of the purer ZnO PARA FORMALDEHYDE PRILLS(91,95) of the ZnO of doped with yttrium improves 6 times of left and right, and response recovery time is also shorter, 290
the response recovery time of the formaldehyde of 100ppm is 10s and 15s.Under the interference of some gases, the 6-20 that the sensitivity of PARA FORMALDEHYDE PRILLS(91,95) is other gas sensitivities doubly.The ZnO of compound 4% Y is in 30 days 290
sensitivity fluctuation to the formaldehyde of 100ppm is very little, illustrates that it has good stability.
Embodiment 4:
0.12mol/L ZnCl
2the deionized water that is dissolved in 40mL is made zinc solution, stirs 10min, and in the urea liquid that to be added drop-wise to the 40mL volumetric molar concentration be 0.18mol/L, magnetic agitation 10min, be transferred in the 100mL autoclave, reacts 24h under 80 ℃.After the gained sediment uses distilled water, absolute ethanol washing repeatedly successively, 80 ℃ of oven dry, and in air 300 ℃ of roasting 1h, make Zinc oxide powder standby.
Under above-mentioned experiment condition, at the Sm (NO of zinc solution situ doping 3at%
3)
36H
2ce (the NO of O and 1at%
3)
36H
2o, stir 10min, and in the urea liquid that to be added drop-wise to the 40mL volumetric molar concentration be 0.18mol/L, magnetic agitation 10min, be transferred in the 100mL autoclave, reacts 24h under 80 ℃.After the gained sediment uses distilled water, absolute ethanol washing repeatedly successively, 80 ℃ of oven dry, and in air 300 ℃ of roasting 1h, the Zinc oxide powder of making compound samarium cerium is standby.
Zinc paste or the Zinc oxide powder of getting the compound samarium cerium of 18mg are placed in agate mortar, add absolute ethyl alcohol and deionized water mixed liquor that volume ratio is 1:1.5, grind pulping, then it evenly is coated on the ceramic die of hydrochloric acid and Ethanol Treatment, standing dry 12 hours after, (1 ℃/min of heating rate) roasting 1h under 520 ℃, install resistance wire additional and it is welded to after pedestal on agingtable to aging 5 days, adopt subsequently WS-30A gas sensor tester to carry out the air-sensitive performance test and calculate its sensitivity of contrast.
The purer ZnO of the ZnO of compound samarium cerium improves 8 times of left and right to the sensitivity of toluene, and response recovery time is also shorter, at 300 ℃ of response recovery times to the toluene of 100ppm, is 9s and 13s.Under the interference of some gases, the 5-10 that is other gas sensitivities to the sensitivity of toluene doubly.The ZnO of compound samarium cerium is in 30 days 300
sensitivity fluctuation to the toluene of 100ppm is very little, illustrates that it has good stability.
Claims (5)
1. rare earth modified zinc paste gas sensor comprises: alumina ceramic tube, it is characterized in that, and scribble rare earth modified zinc oxide material on the aluminium oxide ceramics tube outer surface.
2. the preparation method of rare earth modified zinc paste gas sensor, is characterized in that, adopts hydro-thermal method one step to complete, and concrete preparation method is as follows:
(1) take deionized water as solvent with being made into containing the zinc aqueous solution containing the zinc precursor body, one or more that are simultaneously 0.01-10% by mol ratio are molten to containing in the zinc aqueous solution containing rare earth nitrades, make rare earth-zinc solution, the urea liquid that the sodium hydroxide solution that another preparation volumetric molar concentration is 1-20mol/L or volumetric molar concentration are 0.01-2mol/L, be added drop-wise in rare earth-zinc solution, perhaps rare earth-zinc solution is added drop-wise in NaOH or urea liquid, make rare earth-zinc aqueous slkali, add at rare earth-zinc aqueous slkali ethylenediamine or the cetyl trimethyl ammonium bromide auxiliary agent that volumetric molar concentration is 0.001-0.005mol/L, stir 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 will stir or ultrasonic solution proceeds in water heating kettle at 70-220 ℃ of reaction 5-48h, deionized water and ethanol washing for reacted sample, drying, can make the zinc paste of doping or compound rare-earth, directly or after thermal treatment for gas sensitive,
(2) take rear-earth-doped or compound zinc oxide material prepared by 1-20mg step (1) and put into agate mortar, adding volume ratio is 1-3:1 absolute ethyl alcohol and deionization mixed liquor again, grind 10-30min, then it evenly is coated on the aluminium oxide ceramics tube core of acid, pure ultrasonic processing to the standing 6-15h that dries;
(3) by the coated ceramic die of step (2) under 450-550 ℃, heating rate is 1-5 ℃/min, roasting 1-5h, install resistance wire additional and it is welded on pedestal, make the heater-type gas sensor, aging 5-10 days, its air-sensitive performance of test between 80～440 ℃.
3. the preparation method of rare earth modified zinc paste gas sensor according to claim 2, is characterized in that, the molar percentage of making rare earth-zinc solution Rare Earth Ion and zinc ion is 0.01-10at%.
4. the preparation method of rare earth modified zinc paste gas sensor according to claim 2, is characterized in that, containing the zinc precursor body, is a kind of in zinc nitrate, zinc acetate, zinc tartrate, zinc citrate, zinc sulfate or zinc chloride.
5. the preparation method of rare earth modified zinc paste gas sensor according to claim 2, it is characterized in that, be 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, lutetium Lu, yttrium Y containing the rare earth nitrades rare earth elements.
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| CN113564812A (en) * | 2021-07-20 | 2021-10-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of alkalescent indium oxide for detecting ultralow-concentration formaldehyde, product and application thereof |
| 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 |
| CN113758976A (en) * | 2021-09-14 | 2021-12-07 | 北京化工大学 | Preparation and application of hydrotalcite-based ammonia gas-sensitive material |
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| CN117571793B (en) * | 2024-01-17 | 2024-04-26 | 乌镇实验室 | Composite metal oxide-based gas sensor and preparation method and application thereof |
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