CN106525916A - Lanthanum-stannic oxide nanometer hollow porous membrane sensitive to oxygen at room temperature - Google Patents
Lanthanum-stannic oxide nanometer hollow porous membrane sensitive to oxygen at room temperature Download PDFInfo
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- CN106525916A CN106525916A CN201610974070.6A CN201610974070A CN106525916A CN 106525916 A CN106525916 A CN 106525916A CN 201610974070 A CN201610974070 A CN 201610974070A CN 106525916 A CN106525916 A CN 106525916A
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- room temperature
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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 invention provides a preparing method of a La-SnO2 sensor membrane capable of being used for detecting O2 at the room temperature, and belongs to the technical field of air-sensitive sensors. The preparing method includes the steps that stannous chloride dehydrate and lanthanum chloride are mixed, a La-SnO2 material is prepared with the carbon template method, and is prepared into the membrane with the silkscreen printing method, and under ultraviolet excitation, the 250-ppm-O2 response value of a sample at the room temperature is 2.25, and the response/recovery time are 161/1,003 seconds respectively. In addition, the La-SnO2 sensor membrane can also detect O2 (100 ppm-7,000 ppm) with the large-range concentration at the room temperature, and the La-SnO2 sensor membrane has the high O2 selectivity. The preparing method of the sensor membrane is simple in preparing method, low in raw material cost, excellent in material membrane performance and good in repeatability, and has the quite good application value and prospects.
Description
Technical field
The invention belongs to gas sensor technology field, and in particular to a kind of lanthanum-tin ash (La-SnO2) hollow nano
The preparation of perforated membrane and its air-sensitive performance to oxygen are studied.
Background technology
In recent years, sensitivity is high, respond rapid oxygen sensor suffers from great demand in all trades and professions.For example, exist
Industrial circle, oxygen sensor are widely used in heating furnace, oilfield exploitation, monitoring mining, to prevent gassing.Lead in traffic
Domain, oxygen sensor are commonly used for car engine, control air-fuel ratio to improve engine efficiency.In medical field, oxygen sensor is normal
Auxiliary medical breathing machine is using treating pneumonopathy and oxygen debt warning etc..In addition, oxygen sensor is also widely used for food
The industries such as process, refuse classification management.Therefore, the oxygen sensor for developing excellent performance is necessary.
Currently, detect O2Means mainly include electrochemical process, Fiber Optic Sensor.But, this kind of sensor construction is complicated, price
Costliness, and be difficult to reduce size.As the resistance (conductance) of metal-oxide semiconductor (MOS) (MOS) is strongly depend in air
Partial pressure of oxygen, therefore most of metal-oxide is suitable for the detection of oxygen in theory.Due to wide material sources, prepare simple, performance
It is excellent etc., tin ash (SnO2) it is the one kind for being usually used in gas detecting in numerous MOS, it is particularly common in the detection to oxygen.
Galatsis et al. is prepared for SnO using mechanochemistry and spin coating proceeding2Thin film sensor, at 400 DEG C, which is to 1000ppm O2's
Response value is 5.1(Sens.Actuators B,2001,77,491).Tiburcio-Silver et al. leads to
Cross spray pyrolysis and be prepared for Ga-SnO2Thin film sensor, factor of merit of the sensor at 350 DEG C to 133.3Pa partial pressure of oxygens
For 2.1(Mater.Sci.Eng.B,2004,110,268).Choi et al. electrostatic spinning and original
Sublayer sedimentation has synthesized SnO2- ZnO nuclear fibre structures, 300 DEG C of lower sensors are to 70-2000ppm O2Response value be
1.2-4.2 (Nanotechnology,2009,20,20135).But, these oxygen sensors are all
Need to use at high temperature, and high temperature detection meeting acceleration equipment is aging, sensor stability is declined and is increased energy consumption etc..And
And, in some fields such as food processing and destructor plant, it is sometimes desirable to monitor oxygen at low temperature.Unfortunately, for SnO2
For this conductance is strongly dependent on the material of temperature, low temperature detection inevitably reduces sensitivity, extends response extensive
The multiple time.Therefore, develop excellent performance and the oxygen sensor that can use in room temperature or under being close to room temperature is significant.Ahmed etc.
People is prepared for pure zinc oxide and manganese-Zinc Oxide (Mn-ZnO) nanometer rods by microwave oven hydro-thermal method, and compares both materials
At room temperature to low concentration O2Response, as a result find Mn-ZnO sensors to O2Response be substantially better than pure ZnO, reason is Mn-
ZnO nanorod specific surface is higher, so as to adsorb more oxygen (Curr.Appl.Phys., 2013,13, S64).Regrettably,
It is more than the situation of 15ppm to oxygen concentration, author gives and reports.Hu et al. is prepared for using high-energy ball milling method can be in nearly room
Strontium titanates (the SrTiO used under warm (40 DEG C)3) oxygen sensor, but, the perovskite material electric conductivity is very poor, and this causes to use
Traditional test equipment come read electrical signal become it is difficult (J.Phys.Chem.B, 2004,108,11214).Neri et al. is adopted
Platinum-Indium sesquioxide. (Pt-In is prepared for sol-gel process2O3) room temperature oxygen sensor, the sensor is to 20%O2Response value be
95 But its response/recovery time is up to 18/35 minute, and longer response recovery time is limited
Application of the sensor at aspects such as Rapid Alarm, long-time continuous detecting.
Therefore, how to develop the oxygen sensor that sensitivity is high, response recovery is fast and can use at room temperature？In recent years,
Surface light excitation technique enjoys various countries to pay close attention to as a kind of means for being effectively improved material surface or interface conductance.Li et al. grinds
Single zinc oxide nanowire field effect transistor has been studied carefully under room temperature, ultraviolet excitation to O2Sensitive features (App.Phys.Lett.,
2004,85,6389), Feng et al. have studied under room temperature, ultraviolet excitation beta-gallium oxide nano wire to O2Quick response
(App.Phys.Lett.,2006,89,112114).Ultraviolet light on the one hand alternative heat increasing the activation energy of material surface, separately
On the one hand the recovery time of material can significantly be shortened.
To realize under room temperature to O2Highly sensitive, quick detection, we are prepared for pure SnO using carbon template2With
10at.%La-SnO2Hollow nano porous ball.Film forming is prepared by silk screen print method, performance test is then carried out.Party's legal system
Standby simple, cost of material is low, favorable repeatability, to O2Sensitivity is high and response recovery time is shorter, selectivity is high, can be to big model
Enclose O2(100-7000ppm) detected, with good using value and prospect.
The content of the invention
It is an object of the invention to provide a kind of room temperature detects O2Sensor film preparation method.Prepared by carbon template
La-SnO2Hollow nano porous ball, then film forming is prepared by silk screen print method.The preparation method has with low cost, operation letter
Single, convenient and swift the features such as.
Below with stannous chloride dihydrate (SnCl2·2H2O as a example by), the brief description present invention's realizes process.Initially with carbon
Template prepares La-SnO2Hollow nano porous ball, by silk after appropriate hollow nano porous ball and organic ink mix homogeneously
Net is printed in interdigital electrode, and placement allows for 15 minutes, respectively at 350 DEG C and 550
Take out after processing 2 hours at DEG C, obtain testing substrate.The La-SnO2Hollow porous membranes can be realized by step in detail below：
(1) a certain amount of glucose is dissolved in into deionized water, forms colorless cleared solution, then pour this solution into stainless
Hydro-thermal reaction is carried out in steel reactor, hydrothermal condition is 180 DEG C, 12 hours；
(2) by the black product after hydro-thermal reaction, deionized water and dehydrated alcohol carry out 5 centrifuge washings respectively, then
80 DEG C of dryings in an oven, obtain carbon ball powder；
(3) by after a certain amount of stannous chloride dihydrate and lanthanum chloride (atomic ratio of lanthanum and stannum is respectively 0 and 10%) mixing
Appropriate dimethylformamide (DMF) is dissolved in, is persistently stirred 30 minutes；
(4) carbon ball powder prepared by appropriate step (2) is taken, dimethylformamide is dissolved in and is carried out ultrasound, then by step
(3) solution for preparing is instilled in the carbon ball solution with the speed that every five seconds for example 1 is dripped, and ultrasound adds 2 milliliters after 30 minutes toward solution
Deionized water, continues ultrasound after 1.5 hours, solution is stood 2 days at room temperature；
(5) deionized water and dehydrated alcohol carry out 5 centrifuge washings, Ran Hou to the solution for preparing step (4) respectively
Dried sample is finally placed in tube furnace 450 DEG C and is processed 2 hours, obtains pure SnO by 80 DEG C of vacuum drying in baking oven2With
10at.%La-SnO2Hollow nano porous ball powder；
(6) appropriate above-mentioned sample and organic ink mix homogeneously are taken, the potsherd for being printed on platinum electrode is then screen-printed to
On, obtained film is placed to allow within 15 minutes be placed in Muffle furnace after its uniform levelling, at 350 DEG C and 550 DEG C, process 2 is little respectively
When after take out, obtain test substrate.
Pure SnO can be obtained by said process2And 10at.%La-SnO2Hollow nano perforated membrane.Contrast room temperature+be not added with
Light, 100 DEG C+be not added with light, room temperature+blue light, room temperature+ultraviolet light test condition, find under room temperature+ultraviolet light test condition, material
Material is to O2Sensitivity highest, and La doped can significantly improve material to O2Response.By comparing 10at.%La-SnO2Nanometer
Hollow porous membranes respectively to oxygen, hydrogen, methane, ammonia, carbon dioxide test, it can be found that material is to O2There is higher choosing
Selecting property.The 10at.%La-SnO prepared with traditional sedimentation method2Nano-particle is contrasted, and hollow loose structure is to O2Response it is more aobvious
Write.
La-SnO provided by the present invention2The preparation method of hollow nano perforated membrane, is capable of achieving under room temperature to O on a large scale2It is dense
The detection of degree.The method is prepared simply, and cost of material is low, favorable repeatability, with good using value and prospect.
Description of the drawings
Fig. 1 prepares schematic diagram for test substrate.
Fig. 2 for respectively room temperature+be not added with light, 100 DEG C+be not added with light, room temperature+blue light, room temperature+ultraviolet light test condition,
10at.%La-SnO2The resistance of hollow nano perforated membrane is with 1000ppm O2Break-make 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 O2Break-make gas change curve.
Fig. 4 (a) is pure SnO2And 10at.%La-SnO2The resistance of hollow nano perforated membrane is with variable concentrations O2Break-make gas becomes
Change curve chart, Fig. 4 (b) is pure SnO2And 10at.%La-SnO2Hollow nano perforated membrane is to O2Sensitivity with O2Concentration change
(illustration is the resistance of bi-material with 100ppm O to curve chart2Break-make gas change curve).
Fig. 5 is 10at.%La-SnO2Hollow nano perforated membrane and 10at.%La-SnO2The resistance of nano-particular film with
250ppm O2Break-make gas change curve.
Specific embodiment
With reference to the accompanying drawings and examples describing the present invention in detail.
8 grams of glucoses are dissolved in 40 ml deionized waters by embodiment 1, are formed colorless cleared solution, are then fallen the solution
Hydro-thermal reaction is carried out in entering 100 milliliters of stainless steel cauldrons, hydrothermal condition is 180 DEG C, 12 hours.By the black after hydro-thermal reaction
Deionized water and dehydrated alcohol carry out 5 centrifuge washings to product respectively, and then 80 DEG C of dryings in an oven, obtain carbon ball powder
End.20 milliliter two will be dissolved in after 1.2 grams of stannous chloride dihydrates and lanthanum chloride (atomic ratio of lanthanum and stannum is respectively 0 and 10%) mixing
Methylformamide (DMF), persistently stirs 30 minutes.1.5 grams of the carbon ball powder of above-mentioned preparation is taken, 40 milliliters of dimethyl formyls are dissolved in
Amine simultaneously carries out ultrasound, and then the stannous chloride solution of above-mentioned preparation is instilled in the carbon ball solution with the speed that every five seconds for example 1 is dripped.It is super
After sound 30 minutes, 2 ml deionized waters are added toward solution, continue ultrasound after 1.5 hours, solution is put and stand at room temperature 2
My god.By the solution after standing, deionized water and dehydrated alcohol carry out 5 centrifuge washings respectively, then 80 DEG C of vacuum in an oven
It is dried, dried sample is placed in in tube furnace 450 DEG C finally and is processed 2 hours, obtain the pure SnO of powder2And 10at.%
La-SnO2Hollow nano porous ball；(mass ratio of sample and slurry is 7 to take appropriate above-mentioned sample and organic ink mix homogeneously:
3), then it is screen-printed to and is printed on the potsherd of platinum electrode, obtains one layer of uniform film；Deng being placed on Muffle after film levelling
In stove, take out after processing 2 hours at 350 DEG C and 550 DEG C respectively, obtain testing substrate, its process is as shown in Figure 1.
Transducer sensitivity computational methods：Wherein,For electricity of the sensor under specific oxygen concentration
Resistance,It is sensor in N2Resistance under atmosphere.To study different responses of the test condition lower sensor to oxygen, by 10at.%
La-SnO2Room temperature+be not added with light, 100 DEG C+(wavelength is to be not added with light, room temperature+blue light (wavelength is 460 nanometers), room temperature+ultraviolet light
380 nanometers) under test condition to 1000ppm O2Response contrasted, as shown in Figure 2, it is known that, sensor is in ultraviolet light
It is maximum according to lower response value, it is 3.68.
The response time of sensor is defined as：From when contacting with certain density tested gas, this is reached to resistance
Under concentration the time required to the 90% of stable state resistance；Recovery time is defined as：During from certain density tested gas disengaging,
The time required to having recovered the 90% of change resistance to resistance.To study impact of the La doped to sensor performance, by pure SnO2With
10at.%La-SnO2To 250ppm O2Response contrasted, as shown in figure 3, La doped not only increases the sound of sensor
Should be worth, and improve the response/resume speed of sensor.Pure SnO2To 250ppm O2Response value be only 1.14, response/recover
Time is 182/1315 second, and 10at.%La-SnO2To 250ppm O2Response value be up to 2.25, response/recovery time shortens
For 161/1003 second.
Fig. 4 (a) is 10at.%La-SnO2Resistance with variable concentrations O2Break-make gas change curve, is known by Fig. 4 (a), i.e.,
Make in 100ppm low concentration O2Under, sensor also shows that preferably response recovery curve.Fig. 4 (b) is which to O2Sensitivity with
O2Concentration curve figure, is known by Fig. 4 (b), in the range of 100-7000ppm, 10at.%La-SnO2Sensitivity with O2Concentration
Change curve presents preferable linear relationship.
Finally we compared for 10at.%La-SnO2Hollow nano loose structure and nanoparticle structure are to 250ppm O2
Response, as shown in Figure 5, it is known that compare grain structure (1.12), hollow loose structure can significantly improve sensor to 250ppm
O2Response (2.25).
Claims (1)
1. oxysensible lanthanum-stannic oxide nanometer hollow porous membranes and preparation method thereof under a kind of room temperature, its preparation process bag
Include：
(1) a certain amount of glucose is dissolved in into deionized water, forms colorless cleared solution, then pour this solution into rustless steel anti-
Hydro-thermal reaction is carried out in answering kettle, hydrothermal condition is 180 DEG C, 12 hours；
(2) by the black product after hydro-thermal reaction, deionized water and dehydrated alcohol carry out 5 centrifuge washings respectively, are then drying
80 DEG C of dryings in case, obtain carbon ball powder；
(3) will be dissolved in after a certain amount of stannous chloride dihydrate and lanthanum chloride (atomic ratio of lanthanum and stannum is respectively 0 and 10%) mixing
Appropriate dimethylformamide (DMF), persistently stirs 30 minutes；
(4) carbon ball powder prepared by appropriate step (2) is taken, dimethylformamide is dissolved in and is carried out ultrasound, then step (3) is made
Standby solution is instilled in the carbon ball solution with the speed that every five seconds for example 1 is dripped, and ultrasound adds 2 milliliters of deionizations after 30 minutes, toward solution
Water, continues ultrasound after 1.5 hours, solution is stood 2 days at room temperature；
(5) deionized water and dehydrated alcohol carry out 5 centrifuge washings to the solution for preparing step (4) respectively, then in baking oven
In 80 DEG C of vacuum drying, dried sample is placed in in tube furnace 450 DEG C finally and is processed 2 hours, obtain pure SnO2With
10at.%La-SnO2Hollow nano porous ball powder；
(6) appropriate above-mentioned sample and organic ink mix homogeneously are taken, is then screen-printed to and is printed on the potsherd of platinum electrode, will
Obtained film is placed to be allowed for 15 minutes and be placed in Muffle furnace after its uniform levelling, respectively at 350 DEG C and 550 DEG C after process 2 hours
Take out, obtain testing substrate.
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Cited By (3)
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| CN107449805A (en) * | 2017-07-21 | 2017-12-08 | 中国石油大学(华东) | A kind of cobalt acid zinc nanometer more shell yolk shell films sensitive to acetone |
| 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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| CN107449805A (en) * | 2017-07-21 | 2017-12-08 | 中国石油大学(华东) | A kind of cobalt acid zinc nanometer more shell yolk shell films sensitive to acetone |
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| 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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