CN108572199A - Based on SnO2The method that base gas sensor realizes congeniality gas concentration simultaneous quantitative - Google Patents

Based on SnO2The method that base gas sensor realizes congeniality gas concentration simultaneous quantitative Download PDF

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CN108572199A
CN108572199A CN201810523581.5A CN201810523581A CN108572199A CN 108572199 A CN108572199 A CN 108572199A CN 201810523581 A CN201810523581 A CN 201810523581A CN 108572199 A CN108572199 A CN 108572199A
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殷锡涛
汪琦
单科
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University of Science and Technology Liaoning USTL
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    • 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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Abstract

The invention discloses one kind being based on SnO2The method that base gas sensor realizes congeniality gas concentration simultaneous quantitative, first to single first gas, its response is measured using first gas gas sensor, establish the response of first gas and the relational expression of concentration, then the response of first gas is measured in the mixed gas comprising first gas and second gas, and above-mentioned relation formula is modified, obtain first gas response and first gas concentration and second gas concentration relationship formula in mixed gas；Similarly obtain second gas response with the relational expression simultaneous of first gas concentration and second gas concentration at equation group, you can to solve first gas and second gas respectively concentration.The present invention passes through rule and the mechanism of interacting between two kinds of congeniality gases, equation group is established in conjunction with two kinds of gas sensor responses and gas concentration, the respective concentration of two kinds of final gases is parsed, while to may be implemented congeniality gas concentration completely, accurate quantitative analysis.

Description

Based on SnO2The method that base gas sensor realizes congeniality gas concentration simultaneous quantitative
Technical field
The invention belongs to gas detection technology fields, and SnO is based on more particularly to one kind2Base gas sensor realizes the same sex The method of matter gas concentration simultaneous quantitative.
Background technology
T.Seiyama was developed into first oxide semiconductor gas sensor element in 1962；N.Taguchi is in 1968 Year realizes SnO2The commercialization of gas sensor.With artificial intelligence, the development of material science subject, gas sensor also takes Obtained significant progress；Atmospheric monitoring, toxic gas detection, the real time measure of vehicle exhaust, explosive safety inspection, Aerospace, military and national defense etc. increasingly show the important function of gas sensor.Wherein, SnO2In air-sensitive performance side Face is mainly aoxidized by the preparation of porous material, the preparation of nano structural material, the preparation of film, carried noble metal and doping The methods of object realizes raising and the shortening of response-recovery time of response；Meanwhile SnO2Based sensor has cost of manufacture Low, the features such as technological process is simple, it is widely used in the detection of reducibility gas and toxic gas.However, SnO2Base air-sensitive Greatest problem existing for sensor is selectively poor to object gas.Under a certain specific environment, often two or more have Evil gas exists simultaneously, and the response of such sensor is the comprehensive embodiment of several mixed gas, therefore can not be in mixed gas Each component or one-component accurate quantitative analysis.This is also a bottleneck for restricting this sensor development.Domestic and foreign scholars improve To the selectivity of object gas, it is summarized as following five big types：
1) selection of optimum working temperature：Based on sensor to the absorption of gas with the raising reduction of temperature activated gas Molecule increase with the raising of temperature between contradiction, there is " bell curve " distribution to the response of gas with temperature in sensor Feature, but the corresponding hump of gas with various appears in different temperature, so as to be used to improve material to object gas Selectivity.For example, W.J.Moon etc. is coated in SnO by CuO2The surfaces-ZnO, prepare sensor material；The sensor 200 It is 6 to the selectivity of CO when DEG C work；When working at 350 DEG C, to H2Selectivity be 4, this is the side that everybody generally uses Method.
2) temperature modulation method：It is different to the response and adsorption/desorption rate of gas with various based on sensor material, pass through Apply the temperature periodically by the tracks of line voltage variation, the response curve of gas with various will appear different shapes.Cause This, can distinguish gas by shape.For example, the method that J.R.Huang utilizes temperature modulation, realizes to CO and CH4Together When in the presence of differentiation.The quantifying of this method is necessarily dependent upon graphical display, and two kinds of gases are discernable.However, working as gaseous mixture When body occurs simultaneously, such sensor is extremely complex to the response curve of mixed gas, thus can not be to a certain gas therein Body is quantitative.
3) filter layer method：Based in filter layer active material or catalyst can selectivity with interference gas Reaction is learned, so as to realize the selective enumeration method to object gas.For example, A.Cabot etc. is in SnO2Add Pt above sensitive layer Or the mesopore silicon oxide of Pd loads is as Catalytic Layer, CO and CH4When existing simultaneously, the oxidation CO molecules of layer-selective are catalyzed, from And it improves to CH4Selectivity.However, since gas in the diffusion of filter layer needs certain time, the sound of material for gaseous Between seasonable and recovery time is elongated.
4) preparation process and size controlling method：Size effect based on proposition, works as SnO2Grain size closer to 6nm when (SnO2Debye length be about 3nm), conductivity of material is high to the response of gas by intercrystalline neck control；And it is different Gas differs the depletion layer of material, to embody the selective difference to object gas.Therefore, Different Preparation The nano material for preparing grain size close to Debye length can improve selectivity and response to object gas to a certain extent Value.For example, T.Samerjai etc. is prepared for the WO of Pt loads by flame atomizing method3Sensitive layer；In CO, C2H4And C2H5OH is dry Gas is disturbed, when Pt contents are 1wt%, material works at 150 DEG C to H2There is preferable selectivity.
5) doping of element or load method：Under normal circumstances, the load or doping of element can cause material grains to refine, Therefore, the factor that influence of such method to selectivity is considered as should include the influence of granular size.H.J.Kim passes through solvent heat Method is prepared for the NiO materials of Cr doping, it is found that Cr doping can significantly improve the selective response to methyl.
The common feature of above-mentioned several method is the selectivity improved to object gas.But when two kinds of gases simultaneously In the presence of, individually a kind of sensor response is embodied to two kinds of the comprehensive of gas response；Therefore it can not obtain two kinds of gases respectively Concentration.
Invention content
In order to solve the deficiencies in the prior art, the present invention passes through rule and the machine of interacting between two kinds of congeniality gases Reason, obtains selective value of the corresponding two kinds of sensors to object gas, is built with gas concentration in conjunction with two kinds of sensor responses The thought of vertical equation group, parses the respective concentration of two kinds of final gases, determines while to realize congeniality gas concentration Amount.
The object of the present invention is to provide one kind being based on SnO2Base gas sensor realizes congeniality gas concentration simultaneous quantitative Method, detailed process is as follows：
S1：Pass through SnO2Base gas sensor is detected the first gas and second gas of same concentrations respectively, obtains To respective response, the ratio between the response of first gas and the response of second gas are in the presence of second gas to the first gas The selective value of body, is denoted as SS1/S2；The ratio between the response of second gas and the response of first gas are that first gas exists When to the selective value of second gas, be denoted as SS2/S1；
S2：To single first gas, the response R of first gas is measured using first gas gas sensorS1, first Shown in the response of gas and the relationship of concentration such as formula (1), the concentration C of first gas is determined by formula (1)S1；
Formula (1) is deformed, formula (2) is obtained,
In formula (1) and (2), RS1Response when indicating first gas gas sensor at the working temperature to first gas Value, k1Indicate the sensitivity coefficient of first gas gas sensor, CS1Indicate the concentration of first gas, n1Indicate that first gas is dense The power exponent of degree；
S3：To the mixed gas of connatural first gas and second gas, using SnO2The first gas air-sensitive of base passes Sensor measures the response R' of first gasS1, formula (2) is modified, the response of first gas in mixed gas is obtained R'S1With the relationship of first gas concentration and second gas concentration, specifically as shown in formula (3)；
In formula (3), CS1For the concentration of first gas；CS2For the concentration of second gas；R'S1In the presence of expression second gas The response of first gas, SS1/S2To the selective value of first gas in the presence of expression second gas；k1Indicate first gas gas The sensitivity coefficient of dependent sensor；n1Indicate the power exponent of first gas concentration；
S4：Similarly, using the method for S2~S3, using SnO2The second gas gas sensor of base, obtains mixed gas The response R' of middle second gasS2With the relationship of first gas concentration and second gas concentration, specifically as shown in formula (4)；
In formula (4), CS1For the concentration of first gas；CS2For the concentration of second gas；R'S2In the presence of expression first gas The response of second gas, SS2/S1To the selective value of second gas in the presence of expression first gas；k2Indicate second gas gas The sensitivity coefficient of dependent sensor；n2Indicate the power exponent of second gas concentration；
S5：By formula (3) and formula (4) simultaneous at equation group, first gas and the respective concentration of second gas are solved, such as formula (5) and shown in formula (6),
First gas and the second gas respective concentration in mixed gas are obtained by formula (5) and formula (6).
Preferably, the first gas is CO, and the second gas is H2。
Compared with prior art, the beneficial effects of the present invention are：
The present invention obtains corresponding two kinds of sensors pair by rule and the mechanism of interacting between two kinds of congeniality gases The selective value of object gas establishes equation group in conjunction with two kinds of sensor responses and gas concentration, parses final two kinds The respective concentration of gas, it is quantitative while to which congeniality gas concentration may be implemented completely.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention Some embodiments for those of ordinary skill in the art without creative efforts, can also basis These attached drawings obtain other attached drawings.
Fig. 1 is SnO under different calcination temperatures2To H2Response curve；
Fig. 2 is SnO under different calcination temperatures2To H2Response and concentration relationship figure；
Fig. 3 is SnO2Base gas sensor is to CO and H2Response curve；
Fig. 4 is the response curve of two kinds of gas of respective sensor pair in application example.
Specific implementation mode
In order to enable those skilled in the art to more fully understand, technical scheme of the present invention is practiced, with reference to specific The invention will be further described for embodiment, but illustrated embodiment is not as a limitation of the invention.
It should be noted that the object detected in the present invention is concentration of component in the mixed gas that congeniality gas forms Quantitative approach, the accurate quantitative analysis of two or more congeniality gas mixtures may be implemented, between them at a temperature of detection There is no chemical reactions.We are just using CO as first gas below, H2As second gas, the solution of the present invention is carried out detailed Thin explanation.
It should be further noted that in the present invention, about gas component dosing process in two kinds of congeniality gaseous mixtures In, pass through SnO2Quantitative parameter when base under test gas gas sensor is to gasometry to be measured is determining by the following method 's：
The SnO made under different calcination temperatures is measured respectively2Response of the base under test gas gas sensor under test gas Curve；The relationship empirical formula of under test gas response and under test gas concentration is established by measurement result：Wherein, i indicates first gas S1 or second gas S2, RiIndicate the response of under test gas.
Logarithm, intercept and slope is taken to respectively represent k at formula both ends aboveiValue and ni values.It obtains under different calcination temperatures The SnO of making2Base under test gas gas sensor to the linear relationship of the response and under test gas concentration of under test gas, wherein kiValue indicates the sensitivity coefficient of under test gas gas sensor；Ni indicates that the power exponent of under test gas concentration, these data are To necessary parameter when two kinds of congeniality gas simultaneous quantitatives in mixed gas.
We are H under test gas2For, the above process is specifically illustrated；
500 DEG C, 600 DEG C, 700 DEG C, the SnO that makes under 800 DEG C of calcination temperatures are measured respectively2Base H2Gas sensor is to H2 Response curve, it is specific as shown in Figure 1；H is established by said determination result2Response and H2The relationship empirical formula of concentration：Logarithm, intercept and slope is taken to respectively represent k at the formula both ends2Value and n2Value, S2 indicate the second gas Body H2, SnO under different calcination temperatures2Base H2Gas sensor is to H2Response and concentration relationship figure, it is specific as shown in Figure 2.
Likewise, we by taking under test gas is CO as an example, obtain the relationship empirical formula of CO responses and CO concentration：We obtain formula (2) to deforming formula (1), specific as follows：
In formula (1) and (2), S1 indicates first gas CO, RS1Response when indicating CO sensors at the working temperature to CO Value, k1Indicate the sensitivity coefficient of CO gas sensors, CS1Indicate the concentration of CO, n1Indicate the power exponent of CO concentration.
In the following, we are with CO and H2For the mixed gas of composition, using method provided by the invention in mixed gas CO and H2Concentration carries out simultaneous quantitative, and detailed process is as follows：
In gaseous mixture, we measure corresponding gas sensor to CO and H2Response curve, it is specific as shown in figure 3, by Fig. 3, which can be seen that, is first passed through CO it may be seen that there is 7.4 response, and is passed through H2Afterwards, in H2In the presence of, we see It is still to have 7.4 response, therefore may determine that CO, CO and H2Between be not present chemical reaction process.In addition, we study It was found that CO sensors are to CO and H2N values it is identical, i.e., CO is to H2Selectivity be steady state value.In consideration of it, we carry out formula (2) It corrects, is added on formula (2) left side and contain H2The item of concentration obtains the response R' of CO in mixed gasS1With CO concentration and H2It is dense The relationship of degree, specifically as shown in formula (3)；
In formula (3), CS1For the concentration of CO；CS2For H2Concentration；R'S1Indicate H2In the presence of CO response, SS1/S2It indicates H2In the presence of to the selective value of CO；k1Indicate the sensitivity coefficient of CO gas sensors；n1Indicate the power exponent of CO concentration；
Similarly, we obtain H in mixed gas using the above method2Response R'S2With CO concentration and H2The pass of concentration System, specifically as shown in formula (4)；
In formula (4), CS2For H2Concentration；CS1For the concentration of CO；R'S2H in the presence of expression CO2Response, SS2/S1It indicates To H in the presence of CO2Selective value；k2Indicate H2The sensitivity coefficient of gas sensor；n2Indicate H2The power exponent of concentration；
S5：By formula (3) and formula (4) simultaneous at equation group, CO and H are solved2Respective concentration, such as formula (5) and formula (6) institute Show,
CO and H are obtained by formula (5) and formula (6)2The respective concentration in mixed gas.
In above process, it should be further noted that SS1/S2And SS2/S1It obtains by the following method：Pass through Corresponding SnO2CO and H of the base gas sensor to same concentrations2Be detected respectively, obtain respective response, the response of CO and H2The ratio between response be H2In the presence of to the selective value of CO, be denoted as SS1/S2；H2Response and CO the ratio between response i.e. For in the presence of CO to H2Selective value, be denoted as SS2/S1。
Application example
We are respectively by the H of the CO of 3000ppm and 4000ppm2It after mixing, is quantified using the above method, is adopted respectively Use SnO2Base CO gas sensors and SnO2Base H2Gas sensor measures, respectively to the response curve of object gas such as Fig. 4 It is shown, as seen from Figure 4, SnO2Base CO gas sensors are 34.2, SnO to the response of CO2Base H2Gas sensor is to H2 Response be 43.8, k1And k2It is 1, n1It is 1, n2It is 0.5, SS1/S2It is 4, SS2/S1It is 5；Bring these numerical value into formula respectively (5) and in formula (6), H is obtained2Concentration value 3033ppm, CO concentration value 3865ppm, it can be achieved that in mixed gas two kinds of gas it is same Shi Dingliang, accuracy are high.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies Within, then the present invention is also intended to include these modifications and variations.Embodiment described above is only to absolutely prove the present invention And the preferred embodiment lifted, protection domain are without being limited thereto.Those skilled in the art institute on the basis of the present invention The equivalent substitute of work or transformation, within protection scope of the present invention, protection scope of the present invention is subject to claims.

Claims (2)

1. one kind being based on SnO2The method that base gas sensor realizes congeniality gas concentration simultaneous quantitative, which is characterized in that specific Process is as follows：
S1：Pass through SnO2Base gas sensor is detected the first gas and second gas of same concentrations respectively, obtains respectively Response, the ratio between the response of first gas and the response of second gas are choosing to first gas in the presence of second gas Selecting property value, is denoted as SS1/S2；The ratio between the response of second gas and the response of first gas are in the presence of first gas to the The selective value of two gases, is denoted as SS2/S1；
S2：To single first gas, the response R of first gas is measured using first gas gas sensorS1, first gas Response and concentration relationship such as formula (1) shown in, the concentration C of first gas is determined by formula (1)S1；
Formula (1) is deformed, formula (2) is obtained,
In formula (1) and (2), RS1To the response of first gas, k when indicating first gas gas sensor at the working temperature1 Indicate the sensitivity coefficient of first gas gas sensor, CS1Indicate the concentration of first gas, n1Indicate first gas concentration Power exponent；
S3：To the mixed gas of connatural first gas and second gas, using SnO2The first gas gas sensor of base is surveyed Determine the response R' of first gasS1, formula (2) is modified, the response R' of first gas in mixed gas is obtainedS1With The relationship of one gas concentration and second gas concentration, specifically as shown in formula (3)；
In formula (3), CS1For the concentration of first gas；CS2For the concentration of second gas；R'S1First in the presence of expression second gas The response of gas, SS1/S2To the selective value of first gas in the presence of expression second gas；k1Indicate that first gas air-sensitive passes The sensitivity coefficient of sensor；n1Indicate the power exponent of first gas concentration；
S4：Similarly, using the method for S2~S3, using SnO2The second gas gas sensor of base, obtains second in mixed gas The response R' of gasS2With the relationship of first gas concentration and second gas concentration, specifically as shown in formula (4)；
In formula (4), CS1For the concentration of first gas；CS2For the concentration of second gas；R'S2Second in the presence of expression first gas The response of gas, SS2/S1To the selective value of second gas in the presence of expression first gas；k2Indicate that second gas air-sensitive passes The sensitivity coefficient of sensor；n2Indicate the power exponent of second gas concentration；
S5：By formula (3) and formula (4) simultaneous at equation group, solve first gas and the respective concentration of second gas, such as formula (5) and Shown in formula (6),
First gas and the second gas respective concentration in mixed gas are obtained by formula (5) and formula (6).
2. according to claim 1 be based on SnO2The method that base gas sensor realizes congeniality gas concentration simultaneous quantitative, It is characterized in that, the first gas is CO, the second gas is H2。
CN201810523581.5A 2018-05-28 2018-05-28 Based on SnO2The method that base gas sensor realizes congeniality gas concentration simultaneous quantitative Pending CN108572199A (en)

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