CN108152337A - A kind of LaFeO of high air-sensitive property energy3Base alcohol gas sensor and preparation method thereof - Google Patents
A kind of LaFeO of high air-sensitive property energy3Base alcohol gas sensor and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the preparing technical fields of gas sensor, provide a kind of LaFeO of high air-sensitive property energy3Base alcohol gas sensor and preparation method thereof, the La that sol-gal process is prepared2/3Ba1/3Fe2/3Ti1/3O3Nano-powder is prepared into heater-type ceramic tube construction gas sensor element as operation material.In LaFeO3La and Fe introducing equivalent Ba and Ti element in lattice increases nano powder surface absorption oxygen ability, does not add under heavy metal and rare earth noble metal, and alcohol gas sensor element is made to have relatively low operating temperature, higher gas response and selectivity.Optimum working temperature to ethyl alcohol is 128 DEG C, is 48.1 to the response of the gas of 100ppm ethyl alcohol under optimum working temperature；It is less than 22.4 to 100ppm acetone, DMF, dichloromethane, n-hexane, carbon dioxide, hydrogen gas response；The gas of 20ppm ethyl alcohol is responded up to 15.1.
Description
Technical field
The invention belongs to the preparing technical fields of gas sensor, and in particular to a kind of LaFeO of high air-sensitive property energy3Base second
Alcohol gas sensor and preparation method thereof, with LaFeO3Nano particle is the sensor element of groundwork substance, improves its second
Alcohol air-sensitive performance.
Background technology
With the development of modern society, people increasingly focus on health and safety problem, ethyl alcohol be various wine it is main into
Point, while be with imflammable gas again, the leakage part of excessive drinking, drunk driving and ethyl alcohol has very big health and safety hidden danger,
Therefore with highly sensitive, highly selective, reliable and stable alcohol gas sensor to health and life security with weighing
Want meaning.At present, doped semiconductor oxide S nO2、ZnO、TiO2、Fe2O3、V2O5It is detected etc. alcohol gas is widely used in,
Its principle is to be reacted using oxygen of the absorption on conductor oxidate surface with detected alcohol gas, is partly led so as to change
The resistance of body material realizes the detection of alcohol gas by the variation for measuring resistance.But this kind of alcohol gas sensor is generally deposited
Operating temperature is higher, gas response is relatively low, response recovery time is longer, selectivity is poor the problems such as, it is unfavorable for gas sensing
The development of technology.
Perofskite type oxide LaFeO3It is a kind of p-type semiconductor, is exposed to resistance in reducibility gas as ethyl alcohol
It can increase.In recent years, with LaFeO3Based on alcohol gas sensor element research receive significant attention, because of this kind of sensing
Device stability is very high.However, based on the previous research work of researcher we have found that：LaFeO3Resistance itself is very big, no
Conducive to practical application, and LaFeO3The optimum working temperature of base alcohol gas sensor element is still higher, usually at 200 DEG C
More than, it is unfavorable for the research of low energy-consumption electronic device；It is high not enough to the response of the gas of alcohol gas under optimum working temperature, especially
It is that the alcohol gas response of low concentration is need to be improved.Current method is exactly mainly by the divalent such as Ca, Sr, Ba, Pb member
Element doping substitutes the position of trivalent La or the position of trivalent Fe is substituted with element dopings such as Co, Mg, Ni, provides more skies
Cave carrier so as to reduce the resistance of material, and improves its air-sensitive performance, but gas responds higher LaFeO at present3Base ethyl alcohol
Gas sensor element, LaFeO of the optimum working temperature below 200 DEG C3Base alcohol gas sensor element or contain
Heavy metal element as Pb, is unfavorable for environmental protection or containing rare earth noble metal as Sm, and cost is higher.
Invention content
The present invention provides a kind of LaFeO of high air-sensitive property energy3Base alcohol gas sensor and preparation method thereof, selection are closed
Suitable preparation parameter, the La that will be prepared using sol-gal process2/3Ba1/3Fe2/3Ti1/3O3Nano-powder is as operation material
It is prepared into heater-type ceramic tube construction gas sensor element.By in LaFeO3 La and Fe introduces equivalent simultaneously in lattice
Ba and Ti elements, increase LaFeO3Nano powder surface adsorbs the ability of oxygen, is not adding heavy metal and rare earth noble metal item
Under part, so as to get LaFeO3Base alcohol gas sensor element has relatively low operating temperature, the response of higher gas and choosing
The ratio of selecting property, wherein gas response definition for sensor element resistance and the resistance in dry air under under test gas environment
Value.
The present invention is achieved by following technical solution：
A kind of LaFeO of high air-sensitive property energy3Base alcohol gas sensor prepares La using sol-gal process2/3Ba1/3Fe2/3Ti1/ 3O3Then nano-powder is prepared into heater-type ceramic tube formation gases sensor element.
Specifically preparation method is：
（1）La2/3Ba1/3Fe2/3Ti1/3O3The preparation of nano-powder：It is stoichiometrically 2:2:1:1 precise La
(NO3)3·6H2O、Fe(NO3)3·9H2O、Ba(NO3)2[CH3(CH2)3O]4Ti is dissolved in deionized water；By cationic summation
Molar ratio with citric acid is 1:2 add in citric acid, according to preparation 1mol La2/3Ba1/3Fe2/3Ti1/3O3Nano-powder adds
The ratio of 10g polyethylene glycol PEG-6000 adds in polyethylene glycol PEG-6000, be placed in stirring in 70-80 DEG C of water-bath formed it is molten
Glue continues stirring to xerogel state；Xerogel is put into 380-420 DEG C of heating in crucible, until xerogel burning becomes completely
Powdered form, until no longer burning, organics removal, gained powder is put into Muffle furnace after being fully ground, and is burnt at 990-1010 DEG C
2h is tied, obtains nanoscale La2/3Ba1/3Fe2/3Ti1/3O3Powder；
（2）Heater-type ceramic tube constructs the preparation of gas sensor element：Take 0.1 ± 0.05g La2/3Ba1/3Fe2/3Ti1/3O3It receives
Rice flour body is placed in agate mortar, is added in 0.025 ± 0.005g glass fibres, is added in the terpinol of 0.2-0.3ml, grind together
To paste；In band there are two the ceramic die outer surface of cyclic annular gold electrode and four Pt conducting wires one layer of paste of uniform smearing, put
Enter Muffle furnace, anneal 10min at 90-110 DEG C；Then second layer paste is uniformly smeared, Muffle furnace is put into, at 90-110 DEG C
Lower annealing 10min；Third layer paste is uniformly smeared again, is put into Muffle furnace, anneal 2h at 190-210 DEG C；It is by resistance
The Ni-Cr heater strips of 35 ± 2 Ω pass through ceramic tube and four electrode cables to be welded in sensor base together, install the outer enclosure
Ring, using agingtable, for 24 hours, heater-type gas sensor element is made in aging under 120 mA electric currents.
Step（2）3 layers of paste of middle smearing are 35-45um per layer thickness.The nanoscale La obtained2/3Ba1/3Fe2/ 3Ti1/3O3Powder is single-phase LaFeO3Orthohormbic structure nano-scale particle, granular size are 46.1 to 83.9nm.
It is prepared with La2/3Ba1/3Fe2/3Ti1/3O3Nano-powder is the gas sensor element of operation material to ethyl alcohol
Optimum working temperature be 128 DEG C.
La (NO of the present invention3)3·6H2O、Fe(NO3)3·9H2O、Ba(NO3)2[CH3(CH2)3O]4The molar ratio of Ti
It is 2:2:1:1, the selection of the molar ratio ensures that obtained powder keeps LaFeO3Orthohormbic structure.Ba(NO3)2[CH3(CH2)3O]4Ti equivalent introduces can increase the ability for preparing powder surface absorption oxygen.Powder is sintered 2 h at 990-1010 DEG C, temperature
The combination of degree and time ensures obtained La2/3Ba1/3Fe2/3Ti1/3O3Powder is orthohormbic structure single phase nano grade particles.
Three layers of gas sensitive are successively uniformly smeared in ceramic die outer surface, the selection of the gas sensitive number of plies ensures gas sensitive element
The reduction of part resistance and the raising of air-sensitive performance.After uniformly smearing one and two layer of gas sensitive in ceramic die outer surface, in 90-
Anneal 10 min at 110 DEG C, and the combination of temperature and time ensures the curing on gas sensor surface, facilitates the painting of follow-up gas sensitive
It smears.After third layer gas sensitive is smeared, gas sensor is put into Muffle furnace, anneal 2 h at 190-210 DEG C, then 120
For 24 hours, the combination of annealing conditions and aging condition ensures that the air-sensitive performance of gas sensor has and stablizes well for aging under mA electric currents
Property.
The present invention passes through in LaFeO3 The La and Fe Ba and Ti element for appropriately introducing equivalent simultaneously, increases in lattice
LaFeO3Nano powder surface adsorbs the ability of oxygen, under the conditions of heavy metal and rare earth noble metal is not added, makes the LaFeO of preparation3
Base alcohol gas sensor element has relatively low operating temperature, the response of higher gas and selectivity.The La of preparation2/3Ba1/ 3Fe2/3Ti1/3O3Nano-powder crystal structure is single-phase LaFeO3Orthohormbic structure, granular size ranging from 46.1 to 83.9nm；With
La2/3Ba1/3Fe2/3Ti1/3O3Nano-powder is that the gas sensor element of operation material is 128 to the optimum working temperature of ethyl alcohol
DEG C, it is 48.1 to the response of the gas of 100ppm ethyl alcohol under optimum working temperature；Under optimum working temperature to 100ppm acetone,
The gases such as DMF, dichloromethane, n-hexane, carbon dioxide, hydrogen response 22.4 and hereinafter, with well selectivity；
15.1 can reach to the response of the gas of 20ppm ethyl alcohol under optimum working temperature, still there is very high gas to low-concentration ethanol gas
Body responds.
The beneficial effects of the invention are as follows：It is put forward for the first time the La prepared with sol-gal process2/3Ba1/3Fe2/3Ti1/3O3Nano powder
Body is operation material.By in LaFeO3 The La and Fe Ba and Ti element for appropriately introducing equivalent simultaneously, increases in lattice
LaFeO3Nano powder surface adsorbs the ability of oxygen, under the conditions of heavy metal and rare earth noble metal is not added, makes the LaFeO of preparation3
Base alcohol gas sensor element has relatively low operating temperature, the response of higher gas and selectivity.Using sol-gal process,
Using nitrate as raw material, heavy metal and rare earth noble metal are not added, and there is of low cost, environmental-friendly, simple for process, operation side
Just the advantages that.
Description of the drawings
Fig. 1 is the La prepared by embodiment 12/3Ba1/3Fe2/3Ti1/3O3The X-ray diffracting spectrum of nano-powder；Fig. 2 is to implement
La prepared by example 12/3Ba1/3Fe2/3Ti1/3O3The transmission electron microscope collection of illustrative plates of nano-powder；Fig. 3 is the La prepared by embodiment 12/ 3Ba1/3Fe2/3Ti1/3O3Nano-powder is operation material gas sensor element at different temperatures to 100ppm alcohol gas
Gas responds；Fig. 4 is the La prepared by embodiment 12/3Ba1/3Fe2/3Ti1/3O3Nano-powder is operation material gas sensor member
Part responds the gas of different concentration ethanol gas at 128 DEG C；Fig. 5 is the La prepared by embodiment 12/3Ba1/3Fe2/3Ti1/ 3O3Nano-powder for operation material gas sensor element at 128 DEG C to the dynamic response curve of 100ppm alcohol gas；Fig. 6
It is the La prepared by embodiment 12/3Ba1/3Fe2/3Ti1/3O3Nano-powder is operation material gas sensor element at 128 DEG C
The gas of 100ppm gas with various is responded.
Specific embodiment
All raw materials of the present invention do further the present invention with reference to specific embodiment using commercially available chemically pure reagent
Detailed description.
Embodiment 1：A kind of LaFeO of high air-sensitive property energy3Base alcohol gas sensor prepares La using sol-gal process2/ 3Ba1/3Fe2/3Ti1/3O3Then nano-powder is prepared into heater-type ceramic tube formation gases sensor element.
Specifically preparation method is：
（1）La2/3Ba1/3Fe2/3Ti1/3O3The preparation of nano-powder：Precise 0.02mol La (NO3)3· 6H2O and Fe
(NO3)3·9H2O, 0.01mol Ba (NO3)2[CH3(CH2)3O]4Ti is dissolved in deionized water；Add in 0.12mol lemons
Acid and 2g polyethylene glycol PEG-6000 are placed in stirring in 70-80 DEG C of water-bath and form colloidal sol, continue stirring to xerogel state；
Xerogel is put into 380-420 DEG C of heating in crucible, until xerogel burning becomes powdered form completely, until no longer burning, removal
Organic matter, gained powder are put into Muffle furnace after being fully ground, and 2 h are sintered at 990-1010 DEG C, obtain nanoscale La2/3Ba1/ 3Fe2/3Ti1/3O3Powder；
（2）Heater-type ceramic tube constructs the preparation of gas sensor element：Take 0.1 ± 0.05g La2/3Ba1/3Fe2/3Ti1/3O3It receives
Rice flour body is placed in agate mortar, adds in 0.025 ± 0.005g glass fibres, and the pine tar of 0.2-0.3ml is added in rubber head dropper
Alcohol is ground to paste together.Using coating pen, in band, there are two the ceramic die outer surfaces of cyclic annular gold electrode and four Pt conducting wires
One layer of gas sensitive is uniformly smeared, is put into Muffle furnace, anneal 10 min at 90-110 DEG C；Coating pen is reused uniformly to smear
Second layer gas sensitive, is put into Muffle furnace, and anneal 10 min at 90-110 DEG C；It reuses coating pen and uniformly smears third layer
Gas sensitive is put into Muffle furnace, and anneal 2 h at 190-210 DEG C；It is 35-45um per layer thickness；Resistance is left for 35 ± 2 Ω
Right Ni-Cr heater strips pass through ceramic tube and four electrode cables to be welded in sensor base together, install outer cover lantern ring, profit
With agingtable, for 24 hours, heater-type gas sensor element is made in aging under 120 mA electric currents.
Obtained La2/3Ba1/3Fe2/3Ti1/3O3Nano-powder X-ray diffracting spectrum, transmission electron microscope collection of illustrative plates can obtain：Crystal
Structure is single-phase LaFeO3Orthohormbic structure, granular size ranging from 46.1 to 83.9nm.
The prepared La of detection2/3Ba1/3Fe2/3Ti1/3O3Nano-powder is operation material gas sensor element in difference
At a temperature of the gas of 100ppm alcohol gas is responded, testing result is shown in Fig. 3, as a result shows：With La2/3Ba1/3Fe2/3Ti1/3O3
Nano-powder is that the gas sensor element of operation material is 128 DEG C to the optimum working temperature of ethyl alcohol.
Detection responds the gas of different concentration ethanol gas under optimum working temperature, as a result sees Fig. 4, as a result shows：
15.1 can reach to the response of the gas of 20ppm ethyl alcohol under optimum working temperature, still have to low-concentration ethanol gas very high
Gas responds.
Detection, to the dynamic response curve of 100ppm alcohol gas, is as a result shown in Fig. 5 under optimum working temperature, can by Fig. 5
Know：It is 48.1 to the response of the gas of 100ppm ethyl alcohol under optimum working temperature.
Detection responds the gas of 100ppm gas with various under optimum working temperature, and testing result is shown in Fig. 6, can by Fig. 6
Know：The gases such as 100ppm acetone, DMF, dichloromethane, n-hexane, carbon dioxide, hydrogen are responded under optimum working temperature equal
22.4 and hereinafter, with well selectivity.
The present invention measures La using static volumetric method2/3Ba1/3Fe2/3Ti1/3O3Nano-powder is passed for the gas of operation material
For sensor component to the gas-sensitive property of alcohol gas, the gas response definition of gas sensor element is that element is electric under test gas
Hinder the ratio of resistance Ra in Rg and dry air.
Claims (5)
1. a kind of LaFeO of high air-sensitive property energy3Base alcohol gas sensor, it is characterised in that：La is prepared using sol-gal process2/ 3Ba1/3Fe2/3Ti1/3O3Then nano-powder is prepared into heater-type ceramic tube formation gases sensor element.
2. a kind of LaFeO of high air-sensitive property energy according to claim 13Base alcohol gas sensor, it is characterised in that：Tool
Preparation is：
（1）La2/3Ba1/3Fe2/3Ti1/3O3The preparation of nano-powder：It is stoichiometrically 2:2:1:1 precise La
(NO3)3·6H2O、Fe(NO3)3·9H2O、Ba(NO3)2[CH3(CH2)3O]4Ti is dissolved in deionized water；By cationic summation
Molar ratio with citric acid is 1:2 add in citric acid, according to preparation 1mol La2/3Ba1/3Fe2/3Ti1/3O3Nano-powder adds
The ratio of 10g polyethylene glycol PEG-6000 adds in polyethylene glycol PEG-6000, be placed in stirring in 70-80 DEG C of water-bath formed it is molten
Glue continues stirring to xerogel state；Xerogel is put into 380-420 DEG C of heating in crucible, until xerogel burning becomes completely
Powdered form, until no longer burning, organics removal, gained powder is put into Muffle furnace after being fully ground, and is burnt at 990-1010 DEG C
2h is tied, obtains nanoscale La2/3Ba1/3Fe2/3Ti1/3O3Powder；
（2）Heater-type ceramic tube constructs the preparation of gas sensor element：Take 0.1 ± 0.05g La2/3Ba1/3Fe2/3Ti1/3O3It receives
Rice flour body is placed in agate mortar, is added in 0.025 ± 0.005g glass fibres, is added in the terpinol of 0.2-0.3ml, grind together
To paste；In band there are two the ceramic die outer surface of cyclic annular gold electrode and four Pt conducting wires one layer of paste of uniform smearing, put
Enter Muffle furnace, anneal 10min at 90-110 DEG C；Then second layer paste is uniformly smeared, Muffle furnace is put into, at 90-110 DEG C
Lower annealing 10min；Third layer paste is uniformly smeared again, is put into Muffle furnace, anneal 2h at 190-210 DEG C；It is by resistance
The Ni-Cr heater strips of 35 ± 2 Ω pass through ceramic tube and four electrode cables to be welded in sensor base together, install the outer enclosure
Ring, using agingtable, for 24 hours, heater-type gas sensor element is made in aging under 120 mA electric currents.
3. a kind of LaFeO of high air-sensitive property energy according to claim 23Base alcohol gas sensor, it is characterised in that：Step
Suddenly（2）3 layers of paste of middle smearing are 35-45um per layer thickness.
4. a kind of LaFeO of high air-sensitive property energy according to claim 23Base alcohol gas sensor, it is characterised in that：Institute
The nanoscale La of acquisition2/3Ba1/3Fe2/3Ti1/3O3Powder is single-phase LaFeO3Orthohormbic structure nano-scale particle, granular size are
46.1 to 83.9nm.
5. a kind of LaFeO of high air-sensitive property energy according to claim 23Base alcohol gas sensor, it is characterised in that：Institute
Prepare with La2/3Ba1/3Fe2/3Ti1/3O3Nano-powder is best effort of the gas sensor element to ethyl alcohol of operation material
Temperature is 128 DEG C.
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| CN109799270A (en) * | 2019-02-18 | 2019-05-24 | 蔡涛 | Sensitive membrane capable of effectively improving response performance to ethanol gas |
| CN109799270B (en) * | 2019-02-18 | 2022-05-13 | 江门市润宇传感器科技有限公司 | Sensitive membrane capable of effectively improving response performance to ethanol gas |
| CN110031591A (en) * | 2019-04-19 | 2019-07-19 | 东北大学 | A kind of micro-nano gas sensor array dynamic testing method |
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