CN107655942A - A kind of LaFeO based on core-shell particles structure3Acetone gas sensor of nano sensitive material and preparation method thereof - Google Patents
A kind of LaFeO based on core-shell particles structure3Acetone gas sensor of nano sensitive material and preparation method thereof Download PDFInfo
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- CN107655942A CN107655942A CN201710759576.XA CN201710759576A CN107655942A CN 107655942 A CN107655942 A CN 107655942A CN 201710759576 A CN201710759576 A CN 201710759576A CN 107655942 A CN107655942 A CN 107655942A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
A kind of LaFeO based on core-shell particles structure3Acetone gas sensor of nano sensitive material and preparation method thereof, belong to oxide semiconductor gas sensor technical field.Sensor is tubular structure, and the Al of two parallel and discrete ring-type Au electrodes is scribbled by outer surface2O3Earthenware, the Pt silks being welded on ring-type Au electrodes, through Al2O3Ni Cr alloys heating coils of earthenware tube core and coated in Al2O3The LaFeO of earthenware and the core-shell particles structure on ring-type Au electrodes3Nano sensitive material is formed.Sensor of the present invention has the advantages of high integrated level, simple in construction, cheap, small volume, durable and production in enormous quantities, and the test result of gas-sensitive property shows that the sensor can have faster response resume speed and splendid long-time stability to acetone gas, its acetone gas context of detection in indoor environment is had important application prospect.
Description
Technical field
The invention belongs to oxide semiconductor gas sensor technical field, and in particular to one kind is based on core-shell particles structure
LaFeO3Acetone gas sensor of nano sensitive material and preparation method thereof.
Background technology
With the development of modern science and technology, any discharge of vehicle exhaust, various toxic and harmful gas caused by industrial waste gas
And imflammable gas, destroy the living environment of the mankind.The gas such as benzene, formaldehyde, VOC gas etc., gas caused by house decoration
Exploded caused by leakage and all threaten the health and lives property safety of the mankind.So detection for toxic and harmful gas
It is particularly important.The research of gas sensitive for detecting these gases is also increasingly taken seriously.
In the gas detecting element of numerous kinds, resistance type semiconductor oxide gas detecting element occupies predominantly
Position, being primarily due to it has that detection sensitivity is high, response recovery time is fast, circuit is simple, it is simple to operate, component size is small,
The advantages that cheap.In recent years, with the development of nanoscale science and technology, people attempt to pass through such as exploitation new oxide matrix
Material, material is modified by the methods of doping, compound and surface modification and carried the methods of microscopic appearance structure optimization
The performance of high sensor.
LaFeO3It is that one kind typically has perovskite (ABO3) structure metal composite oxide, because of its stable crystal
Structure, unique electromagnetism, catalysis and air-sensitive performance, be always domestic and international association area study hotspot.However, as air-sensitive material
Material, although many synthesis preparation methods have been suggested and realized, because obtained material morphology is mainly that some are low
Structure is tieed up, so the sensitivity results of obtained detection gas are unsatisfactory.Therefore, using new synthetic route, height is prepared
The LaFeO of the microstructure of dimension3Nano sensitive material improves its identification function, translation function and sensitive body utilization rate, from
And more preferable sensing capabilities are obtained, become particularly significant.
The content of the invention
A kind of the present invention is intended to provide LaFeO based on core-shell particles structure3The acetone gas sensing of nano sensitive material
Device and preparation method thereof, so as to realize the detection to acetone gas low-power consumption.
The present invention is first with lanthanum nitrate hexahydrate, and Fe(NO3)39H2O is as lanthanum source and source of iron, the mixing of water and ethylene glycol
Solution, using the simple hydrothermal synthesis method without template, obtains LaFeO as solvent3The precursor liquid of nano sensitive material, it
Carry out high temperature sintering in atmosphere afterwards, remove physical absorption water and organic matter and other nitrate, finally carry out chemical attack
Undesired impurities are further removed, the LaFeO of final core-shell particles structure is obtained after drying3Nano sensitive material.It is this special
Structure, there is good porous and larger specific surface area, by increasing capacitance it is possible to increase the transmitance of object gas and adsorb more
Gas molecule, therefore improve the sensitivity of sensor.
Of the present invention is a kind of LaFeO based on core-shell particles structure3The acetone gas sensing of nano sensitive material
Device is tubular structure, and the Al of two parallel and discrete ring-type Au electrodes is scribbled by outer surface2O3Earthenware, it is welded in ring-type Au electricity
Pt silks on extremely, through Al2O3The Ni-Cr alloy heating coil of earthenware tube core and coated in Al2O3Earthenware and ring-type Au electricity
Sensitive material on extremely is formed, it is characterised in that：Sensitive material is the LaFeO of core-shell particles structure3Nano sensitive material, and its
It is prepared by following steps：
(1) first by 0.3~0.4g La (NO3)3·6H2O and 0.2~0.4g Fe (NO3)3·9H2O is dissolved in 30~
In 50mL water and the mixed solution of ethylene glycol, water and ethylene glycol volume ratio 15~20：1,20~40min is stirred, is clarified
Transparent solution；
(2) 0.1~0.2g citric acids and 0.5~0.7g PVP are added in the solution obtained to step (1), continues stirring 20
~40min；
(3) solution for obtaining step (2) 10~15h of hydro-thermal reaction under the conditions of 120~160 DEG C；
(4) the obtained sediment of step (3) reaction is centrifuged repeatedly washing 5~8 times with ethanol and deionized water, after
10~20h is dried in air under the conditions of 70~90 DEG C；
(5) powder for obtaining step (4) sinters 1.5~3h under the conditions of 700~900 DEG C；
(6) powder that step (5) obtains is dissolved in 0.3~0.8mol/L hydrochloric acid solution, after stirring 5~15min,
10~20h is dried under the conditions of 70~90 DEG C and obtains the LaFeO of core-shell particles structure3Nano sensitive material.
A kind of LaFeO based on core-shell particles structure of the present invention3The acetone gas sensor of nano sensitive material
Preparation method, its step is as follows：
(1) LaFeO of 10~20mg core-shell particles structures is taken3Nano sensitive material powder mixes with 0.5~1mL deionized waters
Close, grinding form pasty slurry, then dip a small amount of slurry be uniformly coated on outer surface come with two parallel, ring-types and that
The Al of this discrete Au electrode2O3Ceramic tube outer surface, forms the sensitive material film of 10~30 μ m-thicks, and makes sensitive material complete
All standing annular Au electrodes；
(2) 30~45min is toasted at 50 DEG C~100 DEG C, after sensitive material drying, Al2O3Earthenware 400~
2~3h is sintered at 450 DEG C；Then the Ni-Cr alloy heating coil that resistance value is 30~40 Ω is passed through into Al2O3Ceramic tube inside
As heater strip, finally above-mentioned device is welded and encapsulated according to general heater-type gas sensor, so as to obtain being based on core
The LaFeO of shell micro-sphere structure3The acetone gas sensor of nano sensitive material.
Described Al2O3A length of 4~4.5mm of earthenware, external diameter are 1.2~1.5mm, and internal diameter is 0.8~1.0mm.
Tubular type acetone gas sensor of the present invention utilizes the LaFeO of core-shell particles structure3As sensitive material.Its
Mechanism is：The micro-sphere structure of nucleocapsid, loose porous, there is certain hollow structure inside, and specific surface area is big, so being more beneficial for gas
Body, which passes through, to be entered inside sensitive layer, while provides more avtive spots and surface occurs to adsorb more target gas molecules
Reaction, greatly increases the utilization rate of sensitive material.Present invention employs without hydrothermal template synthetic method, simple to operate, cost
Cheap, pollution is few, controllable appearance.Simple, the small volume using commercially available tubular type sensor process, produced in batches beneficial to industrial,
Therefore detected in medical treatment, industry security control etc. has broad application prospects.
Brief description of the drawings
Fig. 1 is the LaFeO of the core-shell particles structure of the present invention3The SEM figures of nano sensitive material, wherein the amplification of (a) figure
Multiple is 5000 times, and the multiplication factor of (b) figure is 70000 times；
Fig. 2 is the LaFeO of the core-shell particles structure of the present invention3The XRD spectrum of nano sensitive material；
Fig. 3 is spirit of the sensor at a temperature of different operating to 20ppm acetone in comparative example 1 and embodiment 1 of the invention
Sensitivity comparison diagram；
Fig. 4 be the present invention comparative example 1 and embodiment 1 in sensor respectively when operating temperature is 250 DEG C and 225 DEG C,
To the selective comparison diagram of 100ppm gas with various；
Fig. 5 be the present invention comparative example 1 and embodiment 1 in sensor respectively when operating temperature is 250 DEG C and 225 DEG C,
Device sensitivity-acetone concentration characteristic curve.
As shown in figure 1, (a) it can be seen from the figure that of embodiment 1, the material of preparation is shaggy spherical structure, directly
Footpath is 1~1.5 μm；(b), it can be seen that material is a kind of nucleocapsid of the nested solid bead of hollow sphere enclosure in figure
Structure.
As shown in Fig. 2 the LaFeO of core-shell particles structure prepared by embodiment 13The XRD of nano sensitive material.From figure
It can be seen that the characteristic peak of prepared material complies fully with standard card, without the appearance at other unnecessary peaks, illustrate the material prepared
Expect for pure LaFeO3。
As shown in figure 3, the optimum working temperature of comparative example 1 is 250 DEG C, the optimum working temperature of embodiment 1 is 225 DEG C,
Now sensitivity of the device to 20ppm acetone is respectively 2.9 and and 6.7.
As shown in figure 4, sensor has higher sensitivity to acetone in comparative example 1 and embodiment 1.And and comparative example
Compare, the selectivity of sensor is greatly improved in embodiment.
As shown in figure 5, when device is in respective optimum working temperature, the sensitivity of all devices is with acetone concentration
Increase and increase, and growth trend gradually slows down.Wherein, sensor sheet reveals optimal gas-sensitive property in embodiment 1.
The electric current of Ni-Cr alloy heating coil is flowed through to regulate and control the operating temperature of sensor by changing, and is passed through to measure and is passed
The resistance value that sensor is in when in gas with various between two ring-type Au electrodes can obtain the sensitivity of sensor.Sensor pair
It is defined as in the sensitivity S of acetone gas：S=Rg/Ra, wherein RgAnd RaRespectively acetone gas of the sensor in given concentration
And resistance value when in air between two gold electrodes.Pass through sensitivity and gas concentration characteristic curve, it is possible to achieve to unknown acetone
The measurement of gas concentration.
Embodiment
Comparative example 1：
With the LaFeO of the solid microsphere structure prepared by shortening the hydro-thermal reaction time3Tubular type is made as sensitive material
Acetone gas sensor, its specific manufacturing process are as follows：
1) first by 0.32g La (NO3)3·6H2O and 0.3g Fe (NO3)3·9H2O is dissolved in 40mL water and ethylene glycol
Mixed solution (volume ratio 19:1) in, 30min is stirred, 0.16g citric acids is added, 0.6g PVP, continues to stir 30min.
2) solution for obtaining step 1 is put into 50mL polytetrafluoroethylkettle kettle lining, and stainless steel cauldron is put into after sealing
Lid is inside screwed, is transferred in baking oven and reacts 6h at 140 DEG C.After question response terminates, after naturally cooling to room temperature, by kettle substrate
The sediment in portion retains, and is centrifuged repeatedly washing 6 times with ethanol and deionized water, after 80 DEG C of drying 12h in air.
3) powder for obtaining step 2 is placed in Muffle furnace, is warming up to 800 DEG C of sintering 2h.Obtained powder is dissolved in
In 0.5mol/L hydrochloric acid solution, after stirring 10min, it is put into 80 DEG C of baking ovens and dries 10h, obtain final solid microsphere structure
LaFeO3Nano sensitive material.
4) by the LaFeO of solid microsphere structure3Nano sensitive material is dissolved in deionized water and slurry is made, and is dipped with brush few
Amount slurry is uniformly coated on the Al that commercially available outer surface comes with two parallel, ring-types and Au electrodes separate2O3Ceramics
Pipe surface, the sensitive material film of 30 μ m-thicks, a length of 4mm, external diameter 1.2mm, the internal diameter 0.8mm of earthenware are formed, and made
Annular Au electrodes are completely covered in sensitive material；
5) toasted 30 minutes under infrared lamp, after sensitive material drying, make Al2O3It is small that earthenware sinters 2 at 400 DEG C
When；Then the Ni-Cr alloy heating coil that resistance value is 40 Ω is passed through into Al2O3Earthenware, finally by above-mentioned device according to general
Heater-type gas sensor is welded and encapsulated, so as to obtain the LaFeO based on solid microsphere structure3Gas sensor.
Embodiment 1：
With the LaFeO of the core-shell particles structure prepared by the hydro-thermal reaction of long period3For the acetone gas of sensitive material
Body sensor, its specific manufacturing process are as follows：
1) first by 0.32g La (NO3)3·6H2O and 0.3g Fe (NO3)3·9H2O is dissolved in 40mL water and ethylene glycol
Mixed solution (volume ratio 19:1) in, 30min is stirred, 0.16g citric acids is added, 0.6g PVP, continues to stir 30min.
2) solution for obtaining step 1 is put into 50mL polytetrafluoroethylkettle kettle lining, and stainless steel cauldron is put into after sealing
Lid is inside screwed, is transferred in baking oven and reacts 12h at 140 DEG C.After question response terminates, after naturally cooling to room temperature, kettle is served as a contrast
The sediment of bottom retains, and is centrifuged repeatedly washing 6 times with ethanol and deionized water, after 80 DEG C of drying 12h in air.
3) powder for obtaining step 2 is placed in Muffle furnace, is warming up to 800 DEG C of sintering 2h.Obtained powder is dissolved in
In 0.5mol/L hydrochloric acid solution, after stirring 10min, it is put into 80 DEG C of baking ovens and dries 10h, obtain final core-shell particles structure
LaFeO3Nano sensitive material.
4) by the LaFeO of core-shell particles structure3Nano sensitive material is dissolved in deionized water and slurry is made, and is dipped with brush few
Amount slurry is uniformly coated on the Al that commercially available outer surface comes with two parallel, ring-types and Au electrodes separate2O3Ceramics
Pipe surface, the sensitive material film of 30 μ m-thicks, a length of 4mm, external diameter 1.2mm, the internal diameter 0.8mm of earthenware are formed, and made
Annular Au electrodes are completely covered in sensitive material；
5) toasted 30 minutes under infrared lamp, after sensitive material drying, make Al2O3It is small that earthenware sinters 2 at 400 DEG C
When；Then the Ni-Cr alloy heating coil that resistance value is 40 Ω is passed through into Al2O3Earthenware, finally by above-mentioned device according to general
Heater-type gas sensor is welded and encapsulated, so as to obtain the LaFeO based on core-shell particles structure3Gas sensor.
Claims (2)
- A kind of 1. LaFeO based on core-shell particles structure3The acetone gas sensor of nano sensitive material, it is tubular structure, by outer Surface scribbles the Al of two parallel and discrete ring-type Au electrodes2O3Earthenware, the Pt silks being welded on ring-type Au electrodes, pass through Al2O3The Ni-Cr alloy heating coil of earthenware tube core and coated in Al2O3Sensitive material on earthenware and ring-type Au electrodes Form, it is characterised in that：Sensitive material is the LaFeO of core-shell particles structure3Nano sensitive material, and it is prepared by following steps Obtain,(1) first by 0.3~0.4g La (NO3)3·6H2O and 0.2~0.4g Fe (NO3)3·9H2O is dissolved in 30~50mL's In the mixed solution of water and ethylene glycol, water and ethylene glycol volume ratio 15~20：1,20~40min is stirred, obtains clear Solution；(2) 0.1~0.2g citric acids and 0.5~0.7g PVP are added in the solution obtained to step (1), continue stirring 20~ 40min；(3) solution for obtaining step (2) 10~15h of hydro-thermal reaction under the conditions of 120~160 DEG C；(4) the obtained sediment of step (3) reaction is centrifuged repeatedly washing 5~8 times with ethanol and deionized water, after air In 10~20h is dried under the conditions of 70~90 DEG C；(5) powder for obtaining step (4) sinters 1.5~3h under the conditions of 700~900 DEG C；(6) powder that step (5) obtains is dissolved in 0.3~0.8mol/L hydrochloric acid solution, after stirring 5~15min, 70~ 10~20h is dried under the conditions of 90 DEG C and obtains the LaFeO of core-shell particles structure3Nano sensitive material.
- A kind of 2. LaFeO based on core-shell particles structure described in claim 13The acetone gas sensor of nano sensitive material Preparation method, its step is as follows：(1) LaFeO of 10~20mg core-shell particles structures is taken3Nano sensitive material powder mixes with 0.5~1mL deionized waters, grinds Mill forms pasty slurry, then dips a small amount of slurry and is uniformly coated on outer surface and comes with two parallel, ring-types and divide each other The Al of vertical Au electrodes2O3Ceramic tube outer surface, forms the sensitive material film of 10~30 μ m-thicks, and sensitive material is covered completely Bezel ring, shape Au electrodes；(2) 30~45min is toasted at 50 DEG C~100 DEG C, after sensitive material drying, Al2O3Earthenware is at 400~450 DEG C 2~3h of lower sintering；Then the Ni-Cr alloy heating coil that resistance value is 30~40 Ω is passed through into Al2O3Ceramic tube inside, which is used as, to be added Heated filament, finally above-mentioned device is welded and encapsulated, so as to obtain the LaFeO based on core-shell particles structure3The sensitive material of nanometer The acetone gas sensor of material.
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| CN108387628A (en) * | 2018-03-07 | 2018-08-10 | 吉林大学 | With SmMO3Electric potential type triethylamine sensor and preparation method thereof is blended together for sensitive electrode material |
| CN109001264A (en) * | 2018-06-22 | 2018-12-14 | 吉林大学 | One kind being based on porous C uFe2O4The acetone gas sensor and preparation method thereof of microballoon sensitive material |
| CN110646480A (en) * | 2019-10-15 | 2020-01-03 | 常州大学 | Three-dimensional nano spherical LaFeO3Preparation method of enzyme-free sulfite electrochemical sensor |
| CN113219011A (en) * | 2021-05-19 | 2021-08-06 | 吉林大学 | Co-doped SnO2Formaldehyde-acetone gas sensor and preparation method thereof |
| CN113514506A (en) * | 2021-07-13 | 2021-10-19 | 吉林大学 | Based on porous LaFeO3Acetone gas sensor of microsphere nano sensitive material and preparation method thereof |
| CN114324499A (en) * | 2022-01-13 | 2022-04-12 | 吉林大学 | ZnCr based on core-shell structure2O4Xylene gas sensor of microsphere sensitive material and preparation method thereof |
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| CN114324499B (en) * | 2022-01-13 | 2023-01-31 | 吉林大学 | Core-shell structure based ZnCr 2 O 4 Xylene gas sensor of microsphere sensitive material and preparation method thereof |
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Application publication date: 20180202 |