CN106525916B - A kind of lanthanum-stannic oxide nanometer hollow porous membranes oxysensible at room temperature - Google Patents
A kind of lanthanum-stannic oxide nanometer hollow porous membranes oxysensible at room temperature Download PDFInfo
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- CN106525916B CN106525916B CN201610974070.6A CN201610974070A CN106525916B CN 106525916 B CN106525916 B CN 106525916B CN 201610974070 A CN201610974070 A CN 201610974070A CN 106525916 B CN106525916 B CN 106525916B
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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
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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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
Abstract
The present invention provides one kind can be used for room temperature detection O2La-SnO2The preparation method of sensor film belongs to gas sensor technology field.We mix stannous chloride dihydrate with lanthanum chloride, are prepared for La-SnO by carbon template2Material, then prepared and formed a film by silk screen print method, under ultraviolet excitation, the sample is at room temperature to 250ppm O2Response reach 2.25, response/recovery time is respectively 161/1003 second.In addition to this, the La-SnO2Sensor film can also room temperature detection concentration O2(100-7000ppm), and to O2Selectivity with higher.This sensor film preparation method is simple, and cost of material is low, and material membrane is had excellent performance, favorable repeatability, has good application value and prospect.
Description
Technical field
The invention belongs to gas sensor technology fields, and in particular to a kind of lanthanum-stannic oxide (La-SnO2) hollow nano
Perforated membrane preparing and its studying the air-sensitive performance of oxygen.
Background technique
In recent years, high sensitivity, the rapid lambda sensor of response suffer from great demand in all trades and professions.For example,
Industrial circle, lambda sensor are widely used in heating furnace, oilfield exploitation, monitoring mining, to prevent gassing.It is led in traffic
Domain, lambda sensor are commonly used for car engine, to control air-fuel ratio to improve engine efficiency.In medical field, lambda sensor is normal
Auxiliary medical breathing machine use treat tuberculosis and it is oxygen debt alarm etc..In addition to this, lambda sensor is also widely used for food
The industries such as processing, garbage classification management.Therefore, it is necessary to develop the lambda sensor haveing excellent performance.
Currently, O is detected2Means mainly include electrochemical process, Fiber Optic Sensor.But this kind of sensor structure is complicated, price
Valuableness, and be difficult to reduce size.Since the resistance (conductance) of metal-oxide semiconductor (MOS) (MOS) is strongly depend in atmosphere
Partial pressure of oxygen, therefore theoretically most of metal oxide is suitable for the detection of oxygen.Stannic oxide (SnO2) be it is a kind of it is non-often with
Representational MOS, since from a wealth of sources, preparation is simple, has excellent performance, SnO2It is usually used in gas detection, especially to oxygen
The detection of gas.Galatsis et al. is prepared for SnO using mechanochemistry and spin coating proceeding2Thin film sensor, its is right at 400 DEG C
1000ppm O2Response be 5.1(Sens.Actuators B,2001,77,491)。Tiburcio-
Silver et al. is prepared for Ga-SnO by spray pyrolysis2Thin film sensor, the sensor is at 350 DEG C to 133.3Pa oxygen
The factor of merit of partial pressure is 2.1(Mater.Sci.Eng.B,2004,110,268).Choi et al. is used
Electrostatic spinning and atomic layer deposition method have synthesized SnO2- ZnO nuclear fibre structure, 300 DEG C of lower sensors are to 70-2000ppm O2
Response be 1.2-4.2(Nanotechnology,2009,20,20135).But these
Lambda sensor requires to use at high temperature, and high temperature detection meeting acceleration equipment aging, and sensor stability is made to decline and increase
Energy consumption etc..Moreover, in some fields such as food processing and destructor plant, it is sometimes desirable to monitor oxygen at low temperature.Regrettably,
For SnO2This conductance is strongly dependent on for the material of temperature, and low temperature detection inevitably reduces sensitivity, is prolonged
Long response recovery time.Therefore, exploitation has excellent performance and can be significant in room temperature or the close lambda sensor used at room temperature.
Ahmed et al. is prepared for pure zinc oxide and manganese-zinc oxide (Mn-ZnO) nanometer rods by micro-wave oven hydro-thermal method, and compare this two
Kind material is at room temperature to low concentration O2Response, as a result, it has been found that Mn-ZnO sensor is to O2Response be substantially better than pure ZnO, it is former
Because being that Mn-ZnO nanometer rods specific surface is higher, so as to adsorb more oxygen (Curr.Appl.Phys., 2013,13, S64).It loses
Regret, to oxygen concentration be greater than 15ppm the case where, author does not give and reports.Hu et al. is prepared for using high-energy ball milling method
Strontium titanates (the SrTiO that can be used under nearly room temperature (40 DEG C)3) lambda sensor, still, the perovskite material electric conductivity is very poor, this
It is unfavorable for carrying out electrical signal acquisition (J.Phys.Chem.B, 2004,108,11214) with traditional test equipment.Neri et al.
Platinum-indium oxide (Pt-In is prepared for using sol-gel method2O3) room temperature lambda sensor, the sensor is to 20%O2Response
It is 95But its response/recovery time is up to 18/35 minute, and longer response recovery time limits
Application of sensor in terms of Rapid Alarm, continuous for a long time.
Therefore, high sensitivity how is developed, response restores lambda sensor that is fast and can using at room temperature? in recent years,
Surface light excitation technique is paid close attention to as a kind of means for being effectively improved material surface or interface conductance by various countries.Li et al. people grinds
Single zinc oxide nanowire field-effect tube has been studied carefully under room temperature, ultraviolet excitation to O2Sensitive features (App.Phys.Lett.,
2004,85,6389), Feng et al. has studied under room temperature, ultraviolet excitation beta-gallium oxide nano wire to O2Quick response
(App.Phys.Lett.,2006,89,112114).On the one hand alternative heat increases the activation energy of material surface to ultraviolet light, separately
On the one hand the recovery time of material can significantly be shortened.
To realize at room temperature to O2Highly sensitive, quick detection, we are prepared for pure SnO using carbon template2With
10at.%La-SnO2Hollow nano porous ball.It is prepared and is formed a film by silk screen print method, is then tested for the property.Party's legal system
Standby simple, cost of material is low, favorable repeatability, to O2High sensitivity and response recovery time is shorter, selectivity is high, can be to big model
Enclose O2(100-7000ppm) is detected, and has good application value and prospect.
Summary of the invention
The object of the present invention is to provide a kind of room temperatures to detect O2Sensor film preparation method.It is prepared by carbon template
La-SnO2Hollow nano porous ball, then prepared and formed a film by silk screen print method.The preparation method has low in cost, operation letter
The features such as single, convenient and efficient.
Below with stannous chloride dihydrate (SnCl2·2H2O realization process of the invention is briefly explained for).Carbon is used first
Template prepares La-SnO2Hollow nano porous ball, by suitable hollow nano porous ball and organic ink silk after mixing
Net is printed in interdigital electrode, is placed and is placed it in Muffle furnace after allowing within 15 minutes the uniform levelling of film, respectively at 350 DEG C and 550
It is taken out after being handled 2 hours at DEG C, obtains test substrate.The La-SnO2Hollow porous membranes can be realized by step in detail below:
(1) a certain amount of glucose is dissolved in deionized water, forms colorless cleared solution, then pours this solution into stainless
Hydro-thermal reaction is carried out in steel reaction kettle, hydrothermal condition is 180 DEG C, 12 hours；
(2) black product after hydro-thermal reaction is subjected to 5 centrifuge washings with deionized water and dehydrated alcohol respectively, then
80 DEG C of dryings in an oven obtain carbon ball powder；
(3) a certain amount of stannous chloride dihydrate and lanthanum chloride are mixed, prepares two samples, chlorination is not added in one of sample
Lanthanum, the atomic ratio of lanthanum and tin is 1:10 in another sample, is then dissolved in appropriate dimethylformamide (DMF), persistently stirs 30 points
Clock；
(4) the carbon ball powder for taking appropriate step (2) to prepare, is dissolved in dimethylformamide and carries out ultrasound, then by step
(3) solution prepared is instilled in the carbon ball solution with the rate that every five seconds 1 is dripped, and ultrasound is added after 30 minutes into the carbon ball solution
2 ml deionized waters continue ultrasound after 1.5 hours, stand 2 days at room temperature；
(5) solution prepared by step (4) is subjected to 5 centrifuge washings with deionized water and dehydrated alcohol respectively, then existed
Sample after drying is finally placed in tube furnace and handles 2 hours for 450 DEG C, obtains pure SnO by 80 DEG C of vacuum drying in baking oven2With
10at.%La-SnO2Hollow nano porous ball powder；
(6) appropriate above-mentioned pure SnO is taken2Or 10at.%La-SnO2Hollow nano porous ball powder sample and organic ink are mixed
It closes uniformly, the mass ratio of sample and slurry is 7:3, is then screen-printed on the potsherd for being printed on platinum electrode, by film obtained
Placing 15 minutes allows its uniform levelling to be placed in Muffle furnace, takes out, obtains after handling 2 hours at 350 DEG C and 550 DEG C respectively
Test substrate.
Pure SnO can be obtained by the above process2And 10at.%La-SnO2Hollow nano perforated membrane.Comparison room temperature+be not added
Light, 100 DEG C+light, room temperature+blue light, room temperature+ultraviolet light test condition is not added, find the material under room temperature+ultraviolet light test condition
Material is to O2Sensitivity highest, and La doped can significantly improve material to O2Response.By comparing 10at.%La-SnO2Nanometer
The hollow porous membranes test to oxygen, hydrogen, methane, ammonia, carbon dioxide respectively, it can be found that material is to O2There is higher choosing
Selecting property.The 10at.%La-SnO prepared with traditional precipitation method2Nano particle comparison, hollow porous structure is to O2Response it is more aobvious
It writes.
La-SnO provided by the present invention2The preparation method of hollow nano perforated membrane is, it can be achieved that at room temperature to a wide range of O2It is dense
The detection of degree.This method preparation is simple, and cost of material is low, favorable repeatability, has good application value and prospect.
Detailed description of the invention
Fig. 1 is that test substrate prepares schematic diagram.
Fig. 2 is+light, 100 DEG C to be not added+respectively in room temperature to be not added under light, room temperature+blue light, room temperature+ultraviolet light test condition,
10at.%La-SnO2The resistance of hollow nano perforated membrane is with 1000ppm O2On-off gas change curve.
Fig. 3 is pure SnO under room temperature+ultraviolet light conditions2And 10at.%La-SnO2The resistance of hollow nano perforated membrane with
250ppm O2On-off gas change curve.
Fig. 4 (a) is pure SnO2And 10at.%La-SnO2The resistance of hollow nano perforated membrane is with various concentration O2On-off gas becomes
Change curve graph, Fig. 4 (b) is pure SnO2And 10at.%La-SnO2Hollow nano perforated membrane is to O2Sensitivity with O2Concentration variation
(illustration is the resistance of two kinds of materials with 100ppm O to curve graph2On-off gas change curve).
Fig. 5 is 10at.%La-SnO2Hollow nano perforated membrane and 10at.%La-SnO2The resistance of nano-particular film with
250ppm O2On-off gas change curve.
Specific embodiment
Carry out the present invention is described in detail with reference to the accompanying drawings and examples.
8 grams of glucose are dissolved in 40 ml deionized waters, form colorless cleared solution, then fall the solution by embodiment 1
Enter and carry out hydro-thermal reaction in 100 milliliters of stainless steel cauldrons, hydrothermal condition is 180 DEG C, 12 hours.By the black after hydro-thermal reaction
Product carries out 5 centrifuge washings with deionized water and dehydrated alcohol respectively, and then 80 DEG C of dryings in an oven, obtain carbon ball powder
End.1.2 grams of stannous chloride dihydrates and lanthanum chloride are mixed, prepare two samples, lanthanum chloride is not added in one of sample, in another sample
The atomic ratio of lanthanum and tin is 1:10, is then dissolved in 20 milliliters of dimethylformamides (DMF), is persistently stirred 30 minutes.Take above-mentioned system
1.5 grams of standby carbon ball powder is dissolved in 40 milliliters of dimethylformamides and carries out ultrasound, then that the stannous chloride of above-mentioned preparation is molten
Liquid is instilled in the carbon ball solution with the rate that every five seconds 1 is dripped.2 milliliters of deionizations are added into the carbon ball solution after 30 minutes for ultrasound
Water continues ultrasound after 1.5 hours, stands 2 days at room temperature.Solution after standing is carried out with deionized water and dehydrated alcohol respectively
5 centrifuge washings, then 80 DEG C of vacuum drying in an oven, are finally placed in 450 DEG C of processing 2 in tube furnace for the sample after drying
Hour, obtain powdered pure SnO2And 10at.%La-SnO2Hollow nano porous ball；Take appropriate above-mentioned pure SnO2Or
10at.%La-SnO2Hollow nano porous ball powder sample and organic ink are uniformly mixed, and the mass ratio of sample and slurry is 7:
3, it is then screen-printed on the potsherd for being printed on platinum electrode, obtains one layer of uniform film；Muffle is placed it in after equal films levelling
It in furnace, is taken out after being handled 2 hours at 350 DEG C and 550 DEG C respectively, obtains test substrate, process is as shown in Figure 1.
Transducer sensitivity calculation method:Wherein,For electricity of the sensor under specific oxygen concentration
Resistance,It is sensor in N2Resistance under atmosphere.To study response of the different test condition lower sensors to oxygen, by 10at.%
La-SnO2+ light, 100 DEG C being not added+in room temperature and be not added light, room temperature+blue light (wavelength is 460 nanometers), room temperature+ultraviolet light, (wavelength is
380 nanometers) under test condition to 1000ppm O2Response compared, as shown in Fig. 2, it is found that sensor is in ultraviolet light
It is maximum according to lower response, it is 3.68.
The response time of sensor is defined as: since when contacting with certain density tested gas, reach this to resistance value
Under concentration the time required to the 90% of stable state resistance value；Recovery time is defined as: since when being detached from certain density tested gas,
The time required to restored variation resistance value to resistance value 90%.Influence for research La doped to sensor performance, by pure SnO2With
10at.%La-SnO2To 250ppm O2Response compared, as shown in figure 3, La doped not only increases the sound of sensor
It should be worth, and improve response/resume speed of sensor.Pure SnO2To 250ppm O2Response be only 1.14, response/recovery
Time is 182/1315 second, and 10at.%La-SnO2To 250ppm O2Response be up to 2.25, response/recovery time shortens
It is 161/1003 second.
Fig. 4 (a) is 10at.%La-SnO2Resistance with various concentration O2On-off gas change curve, is known, i.e., by Fig. 4 (a)
Make in 100ppm low concentration O2Under, sensor also shows that preferable response recovery curve.Fig. 4 (b) is it to O2Sensitivity with
O2Concentration curve figure, is known by Fig. 4 (b), within the scope of 100-7000ppm, 10at.%La-SnO2Sensitivity with O2Concentration
Change curve shows preferable linear relationship.
Finally we compared 10at.%La-SnO2Hollow nano porous structure and nanoparticle structure are to 250ppm O2
Response, as shown in Figure 5, it is known that compare grain structure (1.12), hollow porous structure can significantly improve sensor to 250ppm
O2Response (2.25).
Claims (1)
1. a kind of preparation method of lanthanum-stannic oxide nanometer hollow porous membranes oxysensible at room temperature, preparation step include:
(1) 8 grams of glucose are dissolved in 40 ml deionized waters, form colorless cleared solution, then pours this solution into stainless steel
Hydro-thermal reaction is carried out in reaction kettle, hydrothermal condition is 180 DEG C, 12 hours；
(2) black product after hydro-thermal reaction is subjected to 5 centrifuge washings with deionized water and dehydrated alcohol respectively, then dried
80 DEG C of dryings in case, obtain carbon ball powder；
(3) 1.2 grams of stannous chloride dihydrates and lanthanum chloride being mixed, prepares two samples, lanthanum chloride is not added in one of sample, another
The atomic ratio of lanthanum and tin is 1:10 in sample, is then dissolved in 20 milliliters of dimethylformamides (DMF), is persistently stirred 30 minutes；
(4) the carbon ball powder for taking 1.5 grams of steps (2) to prepare, is dissolved in 40 milliliters of dimethylformamides and carries out ultrasound, then will step
Suddenly the solution of (3) preparation is instilled in the carbon ball solution with the rate that every five seconds 1 is dripped, and ultrasound adds after 30 minutes into the carbon ball solution
Enter 2 ml deionized waters, continues ultrasound after 1.5 hours, stand 2 days at room temperature；
(5) solution prepared by step (4) is subjected to 5 centrifuge washings with deionized water and dehydrated alcohol respectively, then in baking oven
In 80 DEG C of vacuum drying, the sample after drying is finally placed in tube furnace 450 DEG C and is handled 2 hours, pure SnO is obtained2With
10at.%La-SnO2Hollow nano porous ball powder；
(6) appropriate above-mentioned pure SnO is taken2Or 10at.%La-SnO2Hollow nano porous ball powder sample and organic ink mixing are equal
Even, the mass ratio of sample and slurry is 7:3, is then screen-printed on the potsherd for being printed on platinum electrode, film obtained is placed
It allows within 15 minutes its uniform levelling to be placed in Muffle furnace, takes out, tested after being handled 2 hours at 350 DEG C and 550 DEG C respectively
Substrate.
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| CN108398464A (en) * | 2018-03-10 | 2018-08-14 | 吉林大学 | A kind of H2S sensors and preparation method thereof based on hollow spherical structure La doped indium oxide nano sensitive materials |
| CN113968591A (en) * | 2021-11-17 | 2022-01-25 | 青岛科技大学 | Method for preparing porous hollow single-crystal strontium titanate |
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| CN101746812A (en) * | 2009-12-11 | 2010-06-23 | 四川大学 | Preparation method of room-temperature ball-milling solid phase chemical reaction of rare earth mixing with nano stannic oxide |
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