CN106501448A - A kind of carbonic acid gas lanthanum nano-particular film sensitive to carbon dioxide - Google Patents
A kind of carbonic acid gas lanthanum nano-particular film sensitive to carbon dioxide Download PDFInfo
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- CN106501448A CN106501448A CN201610901643.2A CN201610901643A CN106501448A CN 106501448 A CN106501448 A CN 106501448A CN 201610901643 A CN201610901643 A CN 201610901643A CN 106501448 A CN106501448 A CN 106501448A
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- carbonic acid
- certain amount
- acid gas
- air
- sensitivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—Specially adapted to detect a particular component
- G01N33/004—Specially adapted to detect a particular component for CO, CO2
Abstract
The invention provides one kind can be used to detect CO2Carbonic acid gas lanthanum (La2O2CO3) sensor film preparation method, belong to gas sensor technology field.We are dissolved in seventy flavors pearl pill in deionized water, and after adding polyethylene glycol, citric acid and NaOH to stir to clarify clear solution, carbonic acid gas lanthanum material is prepared for by using the method for Hydrothermal Synthesiss, film forming is prepared by silk screen print method again, the sample can detect the CO of certain limit concentration2, in air atmosphere to 2500ppm CO2Factor of merit be up to 56%.This preparation method is simple, and the cost of raw material is cheap, favorable repeatability, material membrane excellent performance, with good using value and prospect.
Description
Technical field
The invention belongs to gas sensor technology field, and in particular to a kind of carbonic acid gas lanthanum (La2O2CO3) nano-particular film
Preparation and its air-sensitive performance of carbon dioxide is studied.
Background technology
With the continuous development of human society, carbon dioxide (CO2) substantial amounts of discharge institute caused by greenhouse effects into
For the main cause of global warming, and natural calamity that this abnormal climate change is caused and disease etc. cause people
Highest attention.Therefore, design, new sensing material is utilized to CO in environment2Concentration fast and accurately detected with
Improving becomes particularly important to the security control of environment.Also, CO2Concentration is in biomedicine, chemical, agricultural production, energy
Source technology, etc. field also have important impact, therefore, design and prepare new CO2Gas sensor has caused the country
The extensive concern of outer scholars.
At present, CO is detected2The means of gas concentration mainly include optical type, solid electrolyte electrochemistry type, polymer-type
With methods such as metal oxides.Wherein, optical type is mainly based on infrared absorption type, with excellent selectivity, but its cost
High, volume is big, is unfavorable for realizing large-scale marketization application.The detection of electrochemistry type is relied primarily between gas molecule and electrode
Electrochemical reaction and realize, but its service life is general shorter and often need to demarcate, thus the need for being difficult to meet practical application
Ask.And metal oxide sensor relies primarily on electro transfer between gas molecule and oxide to realize the spy to gas
Survey, and which has the advantages that small volume, with low cost, sensitivity are high, responds and reply very fast, the preparation technology letter of its product
Single, easy to operate, have become one of current widely used in the world sensor.
It is well known that CO2It is a kind of highly stable non-polar gas of chemical property, using traditional metal oxide half
Conductor material tests CO2Sensitivity is very low.And Recent study personnel have found single-phase rare-earth oxide to titanium dioxide
Carbon has good sensitive property, and with low cost, preparation process is simple.For example, Igor Djerdj et al. are with organic solvent
And the simply sol-gel method without surfactant is prepared for neodymium hydroxide nano particle, and the side of heat treatment
Method obtains carbonic acid gas neodymium nano particle of knowing clearly, and have studied CO2Air-sensitive performance.The results show：Carbonic acid gas neodymium nano particle
Film is to CO2There is good sensitive property (Chem.Mater.2009,21,5375).
So far, the CO of metal-oxide2Gas sensor mainly with traditional metal-oxide semiconductor (MOS) and
Based on its doping vario-property, reported using single-phase carbonic acid gas lanthanum nano particle as sensitive material also nobody.For example,
Andrea Haeusler et al. are prepared for barium titanate and the film of various metals semiconductors coupling is used for CO2Detection of gas, experiment
As a result show that different conductor oxidate doping have obtained spirit during the effect, wherein doping 3wt% lanthanas of different sensitivity
Sensitivity highest is 30% to the sensitivity of 7.5vol% (during the difference of the resistance in air in resistance and carbon dioxide is than upper air
Resistance) (Sens.Actuators B:1996,34,388).Chen et al. is prepared for carbonic acid gas neodymium using hydrothermal synthesis method
Nanometer rods, and have studied its CO under dry air and certain humidity2Sensitive property.Test result indicate that：At 325 DEG C,
CO in the air of 50% humidity, to 500-3000ppm2There is good sensitive property, wherein to 1000ppmCO2Sensitivity
About 2.3 (resistances on the resistance value ratio in air in carbon dioxide) are reached, but which is to 1000ppmCO2Response time and reply
Time is longer, respectively 15 and 30 minutes.Obviously, the performance of the sensor is unsatisfactory, and actual application value is relatively low.
Additionally, current CO2Test atmosphere mostly is in nitrogen or air, and few people were studied under different oxygen contents
Impact of the background gas atmosphere to sensitivity.Zhou et al. makees sensitive material with redox graphene, have studied nitrogen and
CO in air atmosphere2The change of sensitivity, test result indicate that：5000ppm CO2Under air, sensitivity is about 1.1, under a nitrogen
Sensitivity about 1.01 (Sens.Actuators B, 2014,203,135).As can be seen here, in background gas oxygen content
To CO2Sensitive property has important impact.
For solving CO2In sensitivity and response recovery time problem and system research background gas, oxygen content is to air-sensitive
The impact of performance, we are prepared for carbonic acid gas lanthanum nanometer with the inorganic salts of lanthanum as raw material using simply hydrothermal synthesis method
Grain, prepares film forming by silk screen print method, then carries out performance test.The method prepares simple, with low cost, repeatability
Good, to CO2Sensitivity is high, with good using value and prospect.
Content of the invention
It is an object of the invention to provide detecting CO under a kind of background gas atmosphere different in oxygen content2Sensor film
Preparation method.Carbonic acid gas lanthanum nano particle is prepared for using simply hydrothermal synthesis method, is prepared into by silk screen print method
Film.The features such as preparation method has with low cost, convenient and simple for operation quick.
Below with seventy flavors pearl pill (LaCl3.7H2O briefly explain the present invention as a example by) realizes process.Initially with hydro-thermal
Synthetic method prepares carbonic acid gas lanthanum nano particle, is coated in interdigital electricity after appropriate nano particle and organic ink are well mixed
Extremely go up, afterwards dry some minutes obtain one layer of uniform film.Above-mentioned sample is placed in tube furnace, 2 is processed at 400 DEG C little
When after take out, obtain testing substrate, test substrate be put in clean environment and preserved, the test of follow-up electrical properties is waited.The carbon
Sour oxygen lanthanum nano-particular film can be realized by step in detail below：
(1) a certain amount of seventy flavors pearl pill white powder is added in a certain amount of deionized water, in ceaselessly magnetic force
Under stirring so as to be completely dissolved；Add a certain amount of citric acid and cook nucleator, be subsequently adding a certain amount of polyethylene glycol
(PEG) dispersant is done, is persistently stirred 0.5 hour；
(2) a certain amount of NaOH is added in above-mentioned uniform dispersion, and persistently stirring becomes for 10 minutes
Even transparent precursor mixed solution；
(3) above-mentioned precursor solution is transferred to the polytetrafluoroethylene (PTFE) that volume is 100 milliliters of stainless autoclaves
In liner, and it is sealed against；Afterwards liner is loaded in stainless steel casing and is sealed；
(4) autoclave of good seal is put in air dry oven, suitable reaction time and reaction temperature is set
Degree, after reaction terminates, allows which to naturally cool to room temperature；
(5) be collected by centrifugation product, respectively deionized water and absolute ethanol washing several times, by centrifugation after product
60 DEG C of dryings 24 hours in drying box；
(6) above-mentioned desciccate is placed in tube furnace, in air atmosphere, 400 DEG C are processed 2 hours, are finally produced
Thing；
(7) it is screen printed onto in interdigital electrode after taking appropriate heat treatment gained sample and organic ink grinding uniformly, and will
Electrode is positioned in tube furnace under air background, calcines 2 hours, obtain final testing sample at 400 DEG C, and test substrate is put
Enter in clean environment and preserve, wait follow-up electrical properties test.
Carbonic acid gas lanthanum nano-particular film can be obtained by said process.It is to test in background gas in air and nitrogen respectively
2500ppm CO at 300-400 DEG C2Sensitivity, test result shows, there is at 320 DEG C highest sensitivity and stable sound
Answer recovery curve.With nitrogen as background gas, different oxygen contents are adjusted, with the continuous increasing of oxygen content in background gas
Plus, the sensitivity of material increases.CO at 320 DEG C, to 300-10000ppm2Show good stable response characteristic.
The method for preparing carbonic acid gas lanthanum nano-particular film provided by the present invention, may be implemented under air and nitrogen background,
CO of the low concentration to high concentration2Detection.The preparation method is simple, low raw-material cost, favorable repeatability, and practicality is high, has
Good using value and prospect.
Description of the drawings
Fig. 1 prepares schematic diagram for test sample.
Fig. 2 be air and nitrogen be under background gas under different temperatures to 2500ppm CO2Sensitivity vary with temperature
Curve map.
Fig. 3 be air and nitrogen be under background gas under different temperatures to 2500ppm CO2Sensitivity response reply bent
Line chart.
Fig. 4 is different oxygen concentration background gas, at 320 DEG C, to 2500ppm CO2Change of sensitivity curve map and not
With the response return curve figure under oxygen content.
Fig. 5 is at 320 DEG C of air atmosphere, to 300-10000ppmCO2Change of sensitivity curve and response return curve
Figure.
Specific embodiment
With reference to the accompanying drawings and examples describing the present invention in detail.
Embodiment 1,1.11 grams of seventy flavors pearl pill white powder is added in 60 milliliters of deionized water, ceaselessly
Under magnetic agitation so as to be completely dissolved.The citric acid for adding 1.26 grams cooks nucleator, is subsequently adding 0.75 gram of polyethylene glycol
(PEG) dispersant is done, and 0.5 hour is persistently stirred to solution clear.2.16 grams of NaOH is added, 10 are persistently stirred
Minute becomes the precursor mixed solution of homogeneous transparent；Above-mentioned precursor solution is transferred to volume stainless for 100 milliliters
In the polytetrafluoroethyllining lining of the autoclave of steel, and it is sealed against, loads liner in stainless steel casing afterwards and seal.Will
The autoclave of good seal is put in air dry oven, reacts 24 hours, after reaction terminates, make which naturally cold at 180 DEG C
But to room temperature.Be collected by centrifugation product, respectively deionized water and absolute ethanol washing several times, by centrifugation after product in
60 DEG C of dryings 24 hours in drying box.Above-mentioned desciccate is placed in tube furnace, in air atmosphere, 400 DEG C are processed 2 hours,
The heating rate of tube furnace is 2 DEG C/min, obtains final product.Take 70 milligrams of above-mentioned samples and 30 milligrams of organic ink mixing
Be screen-printed to after uniform and be printed on the substrate of platinum electrode, obtain one layer of uniform film, and by electrode be positioned in tube furnace in
Under air background, process 2 hours at 400 DEG C, obtain final testing sample, its process is as shown in Figure 1.
Fig. 2 give air and nitrogen be background gas, under different temperatures to 2500ppm CO2Sensitivity with temperature become
Change curve map.It can be seen that in the range of measured temperature, at 320 DEG C, material membrane is to 1000CO2Sensitivity highest.
Fig. 3 give air and nitrogen be background gas, under different temperatures to 2500ppm CO2Sensitivity response reply
Curve map.It can be seen that air and nitrogen be background gas, under different temperatures to 2500ppm CO2It is respectively provided with good, stable
Response recovery cycles curve, that is, be passed through CO2Material resistance declines afterwards, stops being passed through CO2Material can return to initial electricity quickly afterwards
Resistance.
Fig. 4 gives different oxygen concentration background gas, at 320 DEG C, to 2500ppm CO2Change of sensitivity curve map with
And the response return curve figure under different oxygen contents.It can be seen that being continuously increased with oxygen content, sensitivity is gradually
Increase, when the content of oxygen reach 80% and above when, the resistance of material is excessive, close to state of insulation, so sensitivity is again
Can decline.And as can be seen that to 2500ppm under different oxygen contents in the response return curve figure under different oxygen contents
CO2All there is well stable cyclic curve.
Fig. 5 is given at 320 DEG C of air atmosphere, to 300-10000ppmCO2Change of sensitivity curve and response are replied
Curve map.It can be seen that when at 320 DEG C, background gas are air, CO of the material to variable concentrations2Have well stable
Circulation, with CO2The increase of concentration, sensitivity increase.The CO of low concentration is passed through2Material resistance declines afterwards, stops being passed through CO2
Material can return to initial resistance quickly afterwards；The CO of high concentration is passed through again2When the resistance fall of material is higher than low concentration afterwards
The fall of material resistance, stops being passed through CO2Afterwards, material resistance can finally return to initial resistance.
Claims (1)
1. a kind of carbonic acid gas lanthanum nano-particular film sensitive to carbon dioxide and preparation method thereof, its preparation process includes：
(1) a certain amount of seventy flavors pearl pill white powder is added in a certain amount of deionized water, in ceaselessly magnetic agitation
Under so as to it is completely dissolved；Add a certain amount of citric acid and cook nucleator, be subsequently adding a certain amount of polyethylene glycol (PEG) and do
Dispersant, persistently stirs 0.5 hour；
(2) a certain amount of NaOH is added in above-mentioned uniform dispersion, and persistently stirring becomes uniform saturating for 10 minutes
Bright precursor mixed solution；
(3) above-mentioned precursor solution is transferred to the polytetrafluoroethyllining lining that volume is 100 milliliters of stainless autoclaves
In, and be sealed against；Afterwards liner is loaded in stainless steel casing and is sealed；
(4) autoclave of good seal is put in air dry oven, suitable reaction time and reaction temperature is set, when
After reaction terminates, which is allowed to naturally cool to room temperature；
(5) be collected by centrifugation product, respectively deionized water and absolute ethanol washing several times, by centrifugation after product in dry
60 DEG C of dryings 24 hours in dry case；
(6) above-mentioned desciccate is placed in tube furnace, in air atmosphere, 400 DEG C are processed 2 hours, obtain final product；
(7) take appropriate heat treatment gained sample and organic ink grinding uniform after be screen printed onto in interdigital electrode, and by electrode
It is positioned in tube furnace under air background, calcines 2 hours at 400 DEG C, obtain final test substrate, test substrate is put into clean
Preserve in net environment, wait follow-up electrical properties test.
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Cited By (3)
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| CN106970116A (en) * | 2017-03-20 | 2017-07-21 | 中国石油大学(华东) | A kind of polyhedral cobaltosic oxide three-dimensional porous Graphene gel composite material film sensitive to acetone |
| WO2020012870A1 (en) * | 2018-07-13 | 2020-01-16 | 富士電機株式会社 | Carbon dioxide gas sensor |
| CN115463678A (en) * | 2021-06-11 | 2022-12-13 | 中国石油化工股份有限公司 | Lanthanum oxycarbonate catalyst, preparation method and application thereof |
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Cited By (7)
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|---|---|---|---|---|
| CN106970116A (en) * | 2017-03-20 | 2017-07-21 | 中国石油大学(华东) | A kind of polyhedral cobaltosic oxide three-dimensional porous Graphene gel composite material film sensitive to acetone |
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| CN115463678A (en) * | 2021-06-11 | 2022-12-13 | 中国石油化工股份有限公司 | Lanthanum oxycarbonate catalyst, preparation method and application thereof |
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Application publication date: 20170315 |