CN110095508B - Method and device for gas identification based on single sensor - Google Patents
Method and device for gas identification based on single sensor Download PDFInfo
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- CN110095508B CN110095508B CN201910443500.5A CN201910443500A CN110095508B CN 110095508 B CN110095508 B CN 110095508B CN 201910443500 A CN201910443500 A CN 201910443500A CN 110095508 B CN110095508 B CN 110095508B
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Abstract
The invention discloses a method and a device for identifying gas based on a single sensor, which comprises the following steps: and applying short-period pulse heating voltage to a single sensor, acquiring the test current of unknown gas, and respectively calculating the maximum time and the gas sensitive response value sequence. And determining the position of the gas in a concentration-maximum time relation curve in a pre-established gas characteristic identification library according to the maximum time, and preliminarily prejudging the possible type and concentration of the gas. And matching the closed envelope of the gas-sensitive response value sequence in the radar map with a closed envelope cluster in the radar map in a pre-established gas characteristic identification library, and finally identifying the type and concentration of the gas by combining preliminary prejudgment. The gas identification can be realized by adopting a single sensor, the gas identification device is simple and convenient and easy to operate, the scale of the sensor is greatly reduced, and meanwhile, the single sensor is periodically positioned at a plurality of experimental temperatures by adopting short-period thermal modulation treatment, so that a large amount of experimental data can be quickly acquired, and the working efficiency is further improved.
Description
Technical Field
The invention belongs to the field of detection of nano gas sensors, and particularly relates to a method and a device for identifying gas based on a single sensor, and a method and a device for establishing a gas characteristic identification library.
Background
Gas detection usually needs large-scale instruments such as a gas chromatography-mass spectrometer, but the method has high cost and is only suitable for gases with non-overlapping characteristic spectral lines, and the key is that the method is only limited to off-line detection. The gas sensor based on the nano material has the advantages of low cost, miniaturization, easy integration, high reliability and the like. As the most classical gas detection materials, Transition Metal Oxides (TMOs) have received much attention due to their good sensitivity characteristics to a variety of gases. However, in the prior art, the required operating temperature of the TMOs sensors is generally high, and continuous heating causes the power consumption of the sensors to increase. In addition, a sensor is responsive to a plurality of gases, and has cross-sensitivity characteristics, which is an important reason for limiting the application of the gas sensor. Traditionally, comparing the magnitude of the response of the sensor to the different gases is the most common but very crude method of selective evaluation, which is affected by factors such as gas concentration and operating temperature. The method is another common idea for solving the problem of cross sensitivity by adopting a plurality of sensors with different performances to construct an array. However, in order to measure the contents of the components in various mixed gases, the required array size is also enlarged, resulting in large array size and high cost.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method and a device for identifying gas based on a single sensor. The invention mainly adopts the following technical scheme:
a method for gas identification based on a single sensor, comprising:
s1, applying short-period pulse heating voltage to the first sensor to enable the first sensor to be periodically positioned at N' different temperature points; wherein the first sensor is disposed in the first test gas chamber.
And S2, introducing unknown gas into the first test gas chamber.
S3, acquiring test current I of the first sensor sensing unknown gas at N' different temperature pointst，ItThe test current at the corresponding moment in the current heating period.
S4, respectively calculating N' groups of test currents ItCurrent change rate D oftThen generate DtA curve cluster; obtaining DtD in the curve clustertMaximum value, calculated from the introduction of unknown gas to DtThe time between the maxima is recorded as the maximum time τm(ii) a Calculating a gas-sensitive response value sequence of the unknown gas at 1 to N' temperature points, taking logarithm of the gas-sensitive response value sequence, and generating a closed envelope curve in a radar map according to the time sequence of each temperature point in each period.
S5, determining the maximum time taumPreliminarily prejudging the position of unknown gas in the concentration-maximum time relation curve in the pre-established gas characteristic identification libraryThe possible species and concentrations of the body; and matching the closed envelope curve generated in the radar map with a closed envelope curve cluster in the radar map in a pre-established gas feature recognition library, and finally recognizing the type and concentration of the unknown gas by combining the prejudgment.
Based on the same inventive concept, the invention also provides a device for gas identification based on a single sensor, which comprises: the device comprises a first sensor, a first test air chamber, a first external power supply, a signal generating circuit, a first gas introducing unit, a first test current obtaining unit, a first calculating unit and a gas identifying unit; wherein the content of the first and second substances,
the first sensor is disposed in the first test gas chamber for sensing the unknown gas passing into the first test gas chamber.
And the first external power supply and signal generating circuit is used for applying short-period pulse heating voltage to the first sensor so that the first sensor is periodically positioned at N' different temperature points.
And the first gas introducing unit is used for introducing unknown gas into the first test gas chamber.
A first test current obtaining unit for obtaining test current I of the first sensor sensing unknown gas at N' different temperature pointst，ItThe test current at the corresponding moment in the current heating period.
A first calculating unit for calculating N' groups of test currents I respectivelytCurrent change rate D oftThen generate DtA curve cluster; obtaining DtD in the curve clustertMaximum value, calculated from the introduction of unknown gas to DtThe time between the maxima is recorded as the maximum time τm(ii) a Calculating a gas-sensitive response value sequence of the unknown gas at 1 to N' temperature points, taking logarithm of the gas-sensitive response value sequence, and generating a closed envelope curve in a radar map according to the time sequence of each temperature point in each period.
A gas identification unit for determining a maximum time τmPreliminarily prejudging the possibility of unknown gas at the position in the concentration-maximum time relation curve in the pre-established gas characteristic identification libraryThe type and concentration; and matching the closed envelope curve generated in the radar map with a closed envelope curve cluster in the radar map in a pre-established gas feature recognition library, and finally recognizing the type and concentration of the unknown gas by combining the prejudgment.
Based on the same inventive concept, the invention also provides a method for establishing the gas characteristic identification library, which comprises the following steps:
a1, applying short-period pulse heating voltage to the second sensor to make the second sensor be at N' different temperature points periodically; wherein the second sensor is disposed in the second test plenum.
A2, sequentially introducing n groups of test gases with the same type and different concentrations into a second test air chamber, and sequentially sensing the test gases with different concentrations by a second sensor; wherein n is defined by the user according to the actual situation.
A3, respectively acquiring the test current I of each group of test gas sensed by the second sensor at N' different temperature pointst，ItThe test current at the corresponding moment in the current heating period.
A4, respectively calculating N' groups of test currents I corresponding to each group of test gasestThen generating the concentration-maximum time relation curve of the n groups of test gases with the same kind and different concentrations.
A5, respectively calculating a gas-sensitive response value sequence of each group of test gas at 1 to N' temperature points, respectively taking logarithm of each group of gas-sensitive response value sequence, and then generating a closed envelope line cluster of the N groups of test gas with the same type and different concentrations in a radar chart according to the time sequence of each temperature point in each period.
A6, releasing the gas in the second test gas chamber, introducing another different type of test gas, and repeatedly executing A1-A5 until concentration-maximum time relation curves of m groups of different types of gas and a closed envelope line cluster in a radar chart are generated; wherein m is defined by the user according to the actual situation.
A7, storing the concentration-maximum time relation curves of the m groups of different gases and the closed envelope line cluster in the radar chart.
Based on the same inventive concept, the invention also provides a device for establishing the gas characteristic identification library, which comprises a second sensor, a second test gas chamber, a second external power supply, a signal generating circuit, a second gas introducing unit, a second test current acquiring unit, a second calculating unit and a gas characteristic identification library, wherein the second external power supply is connected with the second test gas chamber; wherein the content of the first and second substances,
the second sensor is disposed in the second test plenum.
And the second external power supply and the signal generating circuit are used for applying short-period pulse heating voltage to the second sensor so that the second sensor is periodically positioned at N' different temperature points.
The second gas introducing unit is used for sequentially introducing n groups of test gases with the same type and different concentrations into a second test gas chamber, so that the second sensor sequentially senses the test gases with different concentrations; wherein n is defined by the user according to the actual situation.
A second test current obtaining unit for respectively obtaining the test current I of each group of test gas sensed by the second sensor at N' different temperature pointst，ItThe test current at the corresponding moment in the current heating period.
A second calculating unit for calculating N' groups of test currents I corresponding to each group of test gases respectivelytThen generating the concentration-maximum time relation curve of the n groups of test gases with the same type and different concentrations; respectively calculating gas-sensitive response value sequences of each group of test gas at 1 to N' temperature points, respectively taking logarithm of each group of gas-sensitive response value sequences, and then generating closed envelope line clusters of the N groups of test gas with the same type and different concentrations in a radar chart according to the time sequence of each temperature point in each period; and repeatedly executing the steps until generating concentration-maximum time relation curves of m groups of different types of gases and a closed envelope line cluster in a radar chart; wherein m is defined by the user according to the actual situation.
And the gas characteristic identification library is used for storing concentration-maximum time relation curves of m groups of different kinds of gases and closed envelope line clusters in the radar map.
Compared with the prior art, the invention has the beneficial technical effects that:
1. the method can be used for gas identification only by adopting a single sensor, and is simple and easy to implement, low in cost, short in time consumption and convenient to expand. Meanwhile, the single sensor has the advantages of small volume, low cost, easy integration, high reliability, strong anti-interference capability and the like.
2. The invention applies short-period pulse heating voltage to a single sensor to carry out thermal modulation processing, so that the sensor can be rapidly positioned in different temperature ranges, and the optimal working temperature of the single sensor responding to specific gas is conveniently researched. In addition, the mode can quickly obtain the response curve of a single sensor to the test gas (or unknown gas) at a plurality of temperature points, and the working efficiency is greatly improved.
3. The method for identifying the type and the concentration of the gas based on the short-period pulse thermal modulation technology can realize the aim of identifying the type and the concentration of the unknown gas based on a single sensor, is simple and easy to operate, has low cost, and greatly reduces the whole volume of a device compared with the traditional sensor array by the single sensor. In addition, the method can be widely applied to online monitoring of various gases.
4. Compared with the traditional constant voltage heating mode, the short-period pulse thermal modulation technology adopted by the invention has lower power consumption of the sensor, and experimental data under different conditions can be rapidly acquired by simply adjusting various parameters of the short-period pulse heating voltage.
Drawings
FIG. 1 is a schematic flow chart of a method for gas identification based on a single sensor according to an embodiment of the present invention;
FIG. 2(a) is a schematic diagram of a single sensor employed in one embodiment of the present invention;
FIG. 2(b) shows heating current I when a sinusoidal heating voltage is applied to a single sensor in one embodiment of the present inventionheatHeating temperature Temp and test current I passing through the sensortIn a heating cycleDrawing;
FIG. 3 is a flow chart of a method for creating a gas signature library according to an embodiment of the present invention;
FIG. 4(a) is a schematic representation of the introduction of 50ppm H into a test chamber in accordance with one embodiment of the present invention2S, a dynamic curve graph of the current collected by the sensor;
FIG. 4(b) is a schematic view of a test chamber with 50ppm SO in accordance with an embodiment of the present invention2A dynamic curve graph of the current collected by the time sensor;
FIG. 5(a) is a schematic representation of the introduction of 50ppm H into a test chamber in accordance with one embodiment of the present invention 28 groups of sampling current curve graphs with separated temperature when S is carried out;
FIG. 5(b) is a schematic view of a test chamber with 50ppm SO in accordance with an embodiment of the present invention 28 sets of temperature separated sampling current graphs;
FIG. 6(a) is a graph of 50ppm H for one embodiment of the present invention2D of StA graph cluster diagram;
FIG. 6(b) is a graph showing the correspondence of 50ppm SO in one embodiment of the present invention2D of (A)tA graph cluster diagram;
FIG. 7(a) is a graph showing 50ppm H in one embodiment of the present invention2S is a corresponding gas-sensitive response value sequence diagram;
FIG. 7(b) is a graph showing 50ppm SO in one example of the present invention2A corresponding gas-sensitive response value sequence chart;
FIG. 8(a) is a block diagram of the establishment of H in one embodiment of the present invention2S and SO2Testing current dynamic curve graphs corresponding to the gas with different concentrations in the gas characteristic identification library;
FIG. 8(b) is a drawing of an embodiment of the present invention H2S and SO2A concentration-maximum time relationship curve corresponding to the gas;
FIG. 8(c) is a graph of various concentrations H in one embodiment of the present invention2A closed envelope line cluster diagram formed in the radar diagram after logarithm is taken on the gas-sensitive response value sequence of S;
FIG. 8(d) is a graph of SO at various concentrations in one embodiment of the present invention2A closed envelope of the sequence of gas-sensitive response values of (A) is formed in the radar map after taking the logarithmA cluster map;
FIG. 9(a) is a graph of the current dynamics of 4 sets of unknown gases collected for the identification of unknown gases in one embodiment of the present invention;
FIG. 9(b) is a schematic diagram of the first step in identifying a gas, i.e., determining the location of the maximum time of an unknown gas in a concentration-maximum time relationship curve, in accordance with an embodiment of the present invention;
fig. 9(c) and 9(d) are schematic diagrams of the second step of identifying gas in an embodiment of the present invention, namely, matching the closed envelope in the radar map after determining the logarithm of the gas-sensitive response value sequence of unknown gas with the closed envelope cluster in the gas feature identification library.
Detailed Description
The invention is described in detail below with reference to the drawings and examples, but the invention is not limited thereto.
In one embodiment, as shown in fig. 1, the present disclosure discloses a method for gas identification based on a single sensor, comprising:
s1, applying short-period pulse heating voltage to the first sensor to enable the first sensor to be periodically positioned at N' different temperature points; wherein the first sensor is disposed in the first test gas chamber.
And S2, introducing unknown gas into the first test gas chamber.
S3, acquiring test current I of the first sensor sensing unknown gas at N' different temperature pointstObtaining N' test currents ItAnd testing the current I for each grouptGenerating a corresponding test current dynamic curve, ItThe test current at the corresponding moment in the current heating period.
S4, respectively calculating N' groups of test currents ltCurrent change rate D oftThen generate DtA curve cluster; obtaining DtD in the curve clustertMaximum value, calculated from the introduction of unknown gas to DtThe time between the maxima is recorded as the maximum time τm(ii) a Calculating the gas-sensitive response value sequence of the unknown gas at 1 to N' temperature points, taking the logarithm of the gas-sensitive response value sequence, and obtaining the logarithm of the gas-sensitive response value sequenceThe time sequence of the temperature points within each cycle generates a closed envelope in the radar map.
S5, determining the maximum time taumPreliminarily prejudging the possible types and concentrations of unknown gases at the position in a concentration-maximum time relation curve in a pre-established gas characteristic identification library; and matching the closed envelope curve generated in the radar map with a closed envelope curve cluster in the radar map in a pre-established gas feature recognition library, and finally recognizing the type and concentration of the unknown gas by combining the prejudgment.
By applying the technical scheme of the embodiment of the disclosure, the method at least has the following beneficial effects:
1. the method can be used for gas identification by adopting a single sensor, and is simple and easy to implement, low in cost, short in time consumption and convenient to expand.
2. The invention applies short-period pulse heating voltage to a single sensor to perform thermal modulation processing, so that the single sensor can be rapidly positioned in different temperature ranges, and the optimal working temperature of the single sensor responding to specific gas is conveniently researched. In addition, the response curve of a single sensor to unknown gas at a plurality of temperature points can be rapidly obtained by the method, and the working efficiency is greatly improved.
3. The method for identifying the type and the concentration of the gas based on the short-period pulse thermal modulation technology can realize the aim of identifying the type and the concentration of the unknown gas based on a single sensor, is simple and easy to operate, has low cost, and greatly reduces the whole volume of a device compared with the traditional sensor array by the single sensor. In addition, the method can be widely applied to online monitoring of various gases.
4. Compared with the traditional constant voltage heating mode, the short-period pulse thermal modulation technology adopted by the invention has the advantages that the power consumption of the sensor is reduced, and experimental data under different conditions can be rapidly acquired by simply adjusting various parameters of the applied pulse heating voltage.
In another embodiment, in step S4, the N' sets of test currents I are calculated separately bytCurrent change rate D oft；
Wherein, ItFor the test current at the corresponding instant in the current heating cycle, It-N′The current is the test current at the corresponding moment in the previous heating period, and N' is the number of current sampling points in each heating period.
In another embodiment, in step S4, the calculation is performed from the time of the unknown gas introduction to DtThe time between the maxima is recorded as the maximum time τmThe formula is as follows:
wherein the above formula (2) represents the maximum time τmGet Dτ(1)，Dt(2)，…，Dt(N') average of the abscissas corresponding to the maximum value, argmaxDt(N) represents a correspondence Dt(N) the abscissa when the maximum value is taken.
In this embodiment, after the unknown gas is introduced, the resistance of the sensor changes due to the adsorption of the unknown gas with the nanomaterial coated on the surface of the first sensor, and the test current I is measuredtChanges occur, but the response current changes with the change speed of the ventilation time from the introduction of unknown gas to DtThe time between the maxima is the period of rapid increase in current change and is recorded as the maximum time τm. Introducing unknown gases with different types and different concentrations, corresponding to taumThe range is different, the maximum time tau ismAs a characteristic quantity for gas identification.
In another embodiment, in step S4, a gas-sensitive response value sequence of the unknown gas at 1-N' temperature points is calculated, and the sampling currents I corresponding to different temperature points are calculatedNThe variation in the process of introducing unknown gas is also different, i.e. the response at different temperatures is different. Calculating a gas-sensitive response value sequence of the unknown gas at 1 to N' temperature points, wherein a gas-sensitive response value formula is defined as follows:
SN＝IgN/IcN(3)
wherein, IgNFor measuring the saturation current through the first sensor under the atmosphere, IgNIs the current through the first sensor in a background atmosphere. Calculating a gas-sensitive response value sequence S under 1 to N' temperature points according to the formula1，S2，…，SN’The logarithm of the sequence of gas-sensitive response values is taken, and then a closed envelope curve in the radar map is formed in the time sequence of the temperature points in each period, and the closed envelope curve is used as another characteristic quantity for gas identification.
In another embodiment, in step S1, the short-period pulse heating voltage VheatThe signal waveform of (A) is one of a rectangular wave, a triangular wave or a sine wave, and the period T heat5 to 10s, and 0.5 to 1.75V peak-to-peak voltage.
In this embodiment, the method for applying the short-period pulse heating voltage to the first sensor to perform the thermal modulation processing includes: the method comprises the steps of applying short-period pulse heating voltage to a heating layer substrate of a first sensor, and achieving the effect of obtaining 5-20 dynamic response curves (namely under 5-20 different working temperature points) in each pulse heating period by setting the pulse heating period and the data sampling period. Heating voltage VheatWith a heating current I flowing through the heated layer substrateheatIn phase. The first sensor is controlled to be at different working temperatures by changing the amplitude of the applied pulse heating voltage, and a large amount of experimental data can be obtained in a short time. In the embodiment, the power consumption required by temperature adjustment is between 10 and 200 mW.
Test current ItThe sampling frequency f of (2) is 0.5-2 Hz. Under the action of periodic pulse heating voltage, testing current ItAlso present as periodic and having a period corresponding to the period of the applied pulsed heating voltage, the test current I contained in each periodtThe number of data of (2) is f x TheatDenoted N 'represents the current data through a single sensor at N' different temperatures acquired per cycle.
In order to ensure that the applied heating voltage enables the first sensor to be in a proper working temperature range, the peak-to-peak value of the applied pulse heating voltage is selected to be 0.5-1.75V.
To avoid the cause of test current ItToo small results in larger test error, and the bias voltage is set to be 100-600 mV.
In order to acquire stable and effective data quickly, the sampling period is set to be 0.5-1 s.
In order to quickly acquire gas-sensitive response data of a plurality of temperature points, a short period of pulse heating voltage needs to be set so that the first sensor is quickly positioned at the plurality of temperature points, and the period of the applied pulse heating voltage is selected to be 5-10 s.
In another embodiment, the method identifies the type of the unknown gas as at least one, and the value of N' is in a range of 5-20.
Based on the same inventive concept, the present disclosure also discloses a device for gas identification based on a single sensor, comprising: the device comprises a first sensor, a first test air chamber, a first external power supply, a signal generating circuit, a first gas introducing unit, a first test current obtaining unit, a first calculating unit and a gas identifying unit. Wherein the content of the first and second substances,
the first sensor is disposed in the first test gas chamber for sensing the unknown gas passing into the first test gas chamber.
And the first external power supply and signal generating circuit is used for applying short-period pulse heating voltage to the first sensor so that the first sensor is periodically positioned at N' different temperature points.
And the first gas introducing unit is used for introducing unknown gas into the first test gas chamber.
A first test current obtaining unit for obtaining test current I of the first sensor sensing unknown gas at N' different temperature pointstObtaining N' test currents ItAnd testing the current I for each grouptGenerating a corresponding test current dynamic curve, ItThe test current at the corresponding moment in the current heating period.
A first calculating unit for calculating N' groups of test currents I respectivelytCurrent change rate D oftThen generate DtAnd (4) clustering curves. Obtaining DtCurve clusterD in (1)tMaximum value, calculated from the introduction of unknown gas to DtThe time between the maxima is recorded as the maximum time τm. Calculating a gas-sensitive response value sequence of the unknown gas at 1 to N' temperature points, taking logarithm of the gas-sensitive response value sequence, and generating a closed envelope curve in a radar map according to the time sequence of each temperature point in each period.
A gas identification unit for determining a maximum time τmAnd preliminarily prejudging the possible types and concentrations of unknown gases at the positions in the concentration-maximum time relation curve in the pre-established gas characteristic identification library. And matching the closed envelope curve generated in the radar map with a closed envelope curve cluster in the radar map in a pre-established gas feature recognition library, and finally recognizing the type and concentration of the unknown gas by combining the prejudgment.
By applying the technical scheme of the embodiment of the disclosure, the method at least has the following beneficial effects:
1. the method can be used for gas identification by adopting a single sensor, and is simple and easy to implement, low in cost, short in time consumption and convenient to expand.
2. The invention applies short-period pulse heating voltage to a single sensor to perform thermal modulation processing, so that the single sensor can be rapidly positioned in different temperature ranges, and the optimal working temperature of the single sensor responding to specific gas is conveniently researched. In addition, the response curve of a single sensor to unknown gas at a plurality of temperature points can be rapidly obtained by the method, and the working efficiency is greatly improved.
3. The method for identifying the type and the concentration of the gas based on the short-period pulse thermal modulation technology can realize the aim of identifying the type and the concentration of the unknown gas based on a single sensor, is simple and easy to operate, has low cost, and greatly reduces the whole volume of a device compared with the traditional sensor array by the single sensor. In addition, the method can be widely applied to online monitoring of various gases.
4. Compared with the traditional constant voltage heating mode, the short-period pulse thermal modulation technology adopted by the invention has the advantages that the power consumption of the sensor is reduced, and experimental data under different conditions can be rapidly acquired by simply adjusting various parameters of the applied pulse heating voltage.
In another embodiment, as shown in fig. 2(a), the first sensor includes a test layer 1, a substrate 2, and a heating layer 3, which are sequentially disposed from top to bottom. The test layer comprises a test electrode, the surface of the test electrode is coated with a nano gas-sensitive film, and the heating layer comprises a heating electrode and a heating material.
In this embodiment, the first sensor made of the nano gas-sensitive material has the advantages of small volume, low cost, easy integration, high reliability, strong anti-interference capability and the like.
In another embodiment, the volume of the substrate is 10.0 × 5.0.0 5.0 × 0.2.2 mm, the heater electrodes are serpentine electrodes, the electrode size is 3.0 × 4.0.0 mm, the electrode thickness is 100nm the test electrodes are interdigitated electrodes with a finger pitch of 100 μm and an electrode thickness of 100 nm.
In another embodiment, the first sensor is prepared as follows:
and forming a test electrode on the upper surface of the substrate through an electron beam evaporation coating process and a photoetching process, and simultaneously leading out a test electrode lead 4.
A heating electrode and a heating material are formed on the lower surface of the substrate while a heating electrode lead 5 is drawn out.
And fully grinding the nano gas-sensitive material, dispersing the nano gas-sensitive material by ethanol or isopropanol, and uniformly coating the nano gas-sensitive material on the center of the upper surface of the test electrode to form the nano gas-sensitive film.
In another embodiment, the test electrode is made of one of gold, platinum or silver-palladium alloy. The nano gas-sensitive material is one of cerium oxide, gold-doped cerium oxide, indium oxide, tungsten oxide or zinc oxide, the coating mode is one of spray coating, spin coating or drop coating, and the coating thickness is 50 nm-2 mu m. The heating electrode is made of gold-nickel alloy or platinum, and the heating material is ruthenium dioxide. The preparation material of the substrate is one of silicon dioxide, silicon nitride or aluminum oxide.
In another embodiment, since the substrate is used to separate the heating layer from the testing layer and support the first sensor, an insulating material with good hardness is required to be used as the material for preparing the substrate, and in this embodiment, silicon nitride is used as the material for preparing the substrate.
In another embodiment, since the heating layer is used for bearing different pulse heating voltages to adjust the temperature of the first sensor, platinum is selected as the material for preparing the heating electrode in the embodiment, and ruthenium dioxide with good thermal conductivity and high melting point is selected as the heating material.
In another embodiment, gold with excellent conductivity is selected as the test electrode preparation material for good conductivity.
In another embodiment, to obtain a stable and more sensitive sensor, it is preferred to obtain a sensor by doping gold with cerium oxide (Au-CeO)2) The nano gas-sensitive film is formed on the surface of the testing electrode of the first sensor in a spinning way, and the thickness of the film is 1 mu m.
Based on the same inventive concept, as shown in fig. 3, the present disclosure further discloses a method for establishing a gas feature recognition library, including:
a1, applying short-period pulse heating voltage to the second sensor to make the second sensor be at N' different temperature points periodically; wherein the second sensor is disposed in the second test plenum.
A2, sequentially introducing n groups of test gases with the same type and different concentrations into a second test air chamber, and sequentially sensing the test gases with different concentrations by a second sensor; wherein n is defined by the user according to the actual situation.
A3, respectively acquiring the test current I of each group of test gas sensed by the second sensor at N' different temperature pointstObtaining N' groups of test currents I corresponding to each group of test gasestAnd testing the current I for each grouptGenerating a corresponding test current dynamic curve, ItThe test current at the corresponding moment in the current heating period.
A4, respectively calculating N' groups of test currents I corresponding to each group of test gasestThen generating the concentration-maximum time relation curve of the n groups of test gases with the same kind and different concentrations. Wherein each group of test gas corresponds toN' set of test currents ItThe maximum time calculation method comprises the following steps: respectively calculating N' groups of test currents ItCurrent change rate D oftThen generate DtA curve cluster; obtaining DtD in the curve clustertMaximum value, calculated from the start of the introduction of the set of test gases to DtThe time between the maxima is recorded as the maximum time τmObtaining N' sets of test currents I corresponding to the set of test gasestMaximum time τ ofm。
A5, respectively calculating a gas-sensitive response value sequence of each group of test gas at 1 to N' temperature points, respectively taking logarithm of each group of gas-sensitive response value sequence, and then generating a closed envelope line cluster of the N groups of test gas with the same type and different concentrations in a radar chart according to the time sequence of each temperature point in each period.
A6, releasing the gas in the second test gas chamber, introducing another different type of test gas, and repeatedly executing A1-A5 until concentration-maximum time relation curves of m groups of different types of gas and a closed envelope line cluster in a radar chart are generated; wherein m is defined by the user according to the actual situation.
A7, storing concentration-maximum time relation curves of m groups of different gases and a closed envelope line cluster in a radar chart.
In this embodiment, the N' sets of test currents I are calculatedtCurrent change rate D oftCalculating the maximum time τmAnd the formula for calculating the gas-sensitive response value sequence is consistent with the formula described in the above gas identification method embodiment, which is not repeated herein, for details, please refer to the related description of the above embodiment.
Based on the same inventive concept, the disclosure also discloses a device for establishing the gas characteristic identification library, which comprises a second sensor, a second test gas chamber, a second external power supply, a signal generating circuit, a second gas introducing unit, a second test current acquiring unit, a second calculating unit and a gas characteristic identification library. Wherein the content of the first and second substances,
the second sensor is disposed in the second test plenum.
And the second external power supply and the signal generating circuit are used for applying short-period pulse heating voltage to the second sensor so that the second sensor is periodically positioned at N' different temperature points.
The second gas introducing unit is used for sequentially introducing n groups of test gases with the same type and different concentrations into a second test gas chamber, so that the second sensor sequentially senses the test gases with different concentrations; wherein n is defined by the user according to the actual situation.
A second test current obtaining unit for respectively obtaining the test current I of each group of test gas sensed by the second sensor at N' different temperature pointstObtaining N' groups of test currents I corresponding to each group of test gasestAnd testing the current I for each grouptGenerating a corresponding test current dynamic curve, ItThe test current at the corresponding moment in the current heating period.
A second calculating unit for calculating N' groups of test currents I corresponding to each group of test gases respectivelytThen generating the concentration-maximum time relation curve of the N groups of test gases with the same kind and different concentrations (wherein, each group of test gases corresponds to N' groups of test currents I)tThe maximum time calculation method comprises the following steps: respectively calculating N' groups of test currents ItCurrent change rate D oftThen generate DtA curve cluster; obtaining DtD in the curve clustertMaximum value, calculated from the start of the introduction of the set of test gases to DtThe time between the maxima is recorded as the maximum time τmObtaining N' sets of test currents I corresponding to the set of test gasestMaximum time τ ofm) (ii) a Respectively calculating gas-sensitive response value sequences of each group of test gas at 1 to N' temperature points, respectively taking logarithm of each group of gas-sensitive response value sequences, and then generating closed envelope line clusters of the N groups of test gas with the same type and different concentrations in a radar chart according to the time sequence of each temperature point in each period; and repeatedly executing the steps until generating concentration-maximum time relation curves of m groups of different types of gases and a closed envelope line cluster in a radar chart; wherein m is defined by the userThe self-definition is carried out according to the actual situation.
And the gas characteristic identification library is used for storing concentration-maximum time relation curves of m groups of different kinds of gases and closed envelope line clusters in the radar map.
It should be noted that, in the implementation, the first sensor and the second sensor described in this disclosure may be the same sensor or different sensors. Meanwhile, the first sensor and the second sensor are the same type of sensors with the same function. Therefore, the composition structure and the manufacturing method of the second sensor are not repeated herein, and refer to the related description of the first sensor embodiment.
Similarly, the second test air chamber and the first test air chamber, the second external power supply and the signal generating circuit and the first external power supply and the signal generating circuit, the second gas introducing unit and the first gas introducing unit, the second test current obtaining unit and the first test current obtaining unit, and the second calculating unit and the first calculating unit described in the present disclosure may be the same unit or different units.
In the above embodiments of the present disclosure, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The following is a detailed description of the gas identification using a single sensor in the present disclosure with reference to specific embodiments, but not intended to limit the disclosure.
Hydrogen sulfide (H)2S) and sulfur dioxide (SO)2) The gas is common gas in industrial production, is colorless, toxic and corrosive, and is an atmospheric pollutant. In many industrial scenarios (e.g. flue gas generated by oil refineries, sulphur hexafluoride (SF)6) Decomposition products, etc.) exist at the same time, and the detection of the types and concentrations of the two gases has clear application value for the state evaluation of equipment. Therefore, this embodiment uses H2S and SO2For example, a method of implementing gas identification using a single sensor is described.
In this embodiment, the method for applying a short-period pulse heating voltage to a single sensor to perform thermal modulation processing is to apply a short-period pulse heating voltage to the heating layer substrate of the single sensor, and set a pulse heating period and a data sampling period to achieve an effect of obtaining 8 dynamic response curves (i.e., at different working temperatures) in each pulse heating period. In the embodiment, the power consumption required by temperature adjustment is between 10 and 200 mW.
In order to ensure that the applied heating voltage enables a single sensor to be in a proper working temperature range, the peak-to-peak value of the applied pulse heating voltage is selected to be 0.5-1.75V.
In order to avoid larger test error caused by too small test current, the bias voltage is set to be 100-600 mV.
In order to acquire stable and effective data quickly, the sampling period is set to be 0.5-1 s.
In order to rapidly acquire gas-sensitive response data of a plurality of temperature points, the pulse heating voltage is required to be set to have a short period so that a single sensor can be rapidly positioned at the plurality of temperature points, and the period of the applied pulse heating voltage is selected to be 5-10 s.
In a specific embodiment, the waveform of the pulse heating voltage is selected from a sine wave, the peak-to-peak value is 1V, the period is 8s, the direct-current voltage is offset by 600mV, and the power consumption required by temperature regulation is about 10 mW.
Heating current I corresponding to single pulse heating voltage periodheatTemperature point of the individual sensor and test current I through the test electrode of the sensortAs shown in fig. 2 (b).
In particular embodiments, SO is selected2And H2S is used as test gas, and SO with different concentrations are sequentially introduced into a test gas chamber2And H2And S, carrying out gas-sensitive test.
FIG. 4(a) and FIG. 4(b) are each a diagram showing the introduction of 50ppm H into a test gas chamber2S and 50ppm SO2The dynamic curve of the test current collected by a single sensor.
The collected test current ItGrouping according to 8 temperature points in each heating cycle, obtaining electricity passing through a single sensor at 8 different temperaturesFlow, i.e. sampling current INFIG. 5(a) and FIG. 5(b) are each a case where 50ppm of H was introduced2S and 50ppm SO2Corresponding to 8 sets of temperature separation curves.
Each set of test currents ItThe logarithm of the time t is taken and then the derivative is obtained to obtain the current change rate DtThen generate DtAnd (4) clustering curves. Obtaining DtD in the curve clustertMaximum value, calculated from the start of the test gas introduction to DtThe time between the maxima is recorded as the maximum time τmIs recorded as a maximum time τmIntroducing different kinds of test gases with different concentrations and corresponding taumThe difference is that the maximum time is used as a characteristic quantity of gas identification, and 50ppm H is respectively corresponding to FIG. 6(a) and FIG. 6(b)2S and 50ppm SO2D of (A)tCurve cluster (corresponding maximum time tau is marked on the graph)m)。
Sampling current I corresponding to different temperature pointsNThe variation in the process of passing the test gas is also different, i.e. the response at different temperatures is different, and the gas-sensitive responses at 1 to 8 temperature points are calculated. 50ppm H2S and 50ppm SO2The corresponding gas response value sequences are shown in fig. 7(a) and fig. 7(b), respectively.
The following describes the method for establishing the gas characteristic identification library and the step of identifying the unknown gas in detail with reference to the embodiments.
Establishment of SO2And H2The method of the S gas feature identification library is as follows:
1) testing multiple SO concentrations by single sensor2And H2The current change of S is based on the current change characteristics and the maximum time τ in the graph, as shown in FIG. 8(a)mThe concentration-maximum time curve is plotted as shown in FIG. 8 (b).
2) Calculating a gas-sensitive response value sequence of 1-8 temperature points according to the test current, taking logarithm of the gas-sensitive response value sequence, and then drawing a closed envelope line cluster in the radar map according to the time sequence of each temperature point in a period, wherein the same test gas with different concentrations corresponds to a similar envelope line cluster in the radar map. Envelope line clusters in radar maps of different kinds of test gasesThe shapes are different in size. Multiple different concentrations of H2S and SO2The sequence of gas-sensitive response values of (a) is plotted as a closed envelope cluster in a radar chart after taking the logarithm as shown in fig. 8(c) and fig. 8 (d).
Above, regarding SO2And H2And S gas is established by a gas characteristic identification library which is formed by two groups of characteristic quantities, namely an envelope line cluster of a concentration-maximum time relation curve and a temperature-gas sensitive response value sequence in a radar chart of a characteristic library.
To test the reliability of the proposed method for identifying gases, 4 sets of current curves of single sensors under unknown atmosphere were measured, as shown in fig. 9(a), and the proposed method was used to identify the type and concentration of gases. The method for identifying the type and concentration of the gas comprises two steps:
1) the first step is as follows: and preliminarily judging possible gas types and concentrations by using the position of the obtained maximum time in a concentration-maximum time relation curve of the gas characteristic identification library.
Calculating the current change rate D corresponding to the test current curvetAnd generates DtCurve cluster for obtaining maximum time tau corresponding to four groups of testsm. test-1: 48.1s, and referring to its position in the concentration-time maximum curve, as shown in FIG. 9(b), it can be seen that test-1 corresponds to a gas that may be 22ppmH2S or 67ppm SO2(ii) a test-2: 63.47s, corresponding to a gas of 9ppmH2S; similarly, the gas in test-3 may be 28ppm H2S or 97ppm SO2The corresponding gas in test 4 may be 26ppm H2S or 84ppm SO2。
2) The second step is that: in order to further determine the gases in test-1, test-3 and test-4, logarithm is taken on the gas-sensitive response value sequence of the unknown gas, a closed envelope generated in a radar map according to the time sequence of each temperature point in a period is matched with a closed envelope cluster in the radar map of a gas feature recognition library, and judgment and recognition are carried out by combining the primary pre-judgment result of the first step, so that the type and the concentration of the unknown gas are finally obtained.
The positions of closed envelopes formed by a sequence of gas-sensitive response values of unknown gas in a radar chart are shown in figure 9(a), (b)c) FIG. 9 (d). For example, the closed envelope of test-2 in FIG. 9(c) is at 5 to 10ppmH2S between the closed envelopes, and SO in FIG. 9(d)2Are not matched in shape. In combination with the preliminary judgment of the first step, the gas in test-2 can be determined to be 9ppmH2S, with actual introduction of gas (9 ppmH)2S) are completely matched. Similarly, the gas in test-1, test-3 and test-4 can be respectively judged to be 22ppmH2S、97ppmSO2And 84ppm SO2。
The results of judging and identifying 4 groups of unknown gases and the actual types of the introduced gases, and the inspection errors are shown in the following table 1.
TABLE 1
The combination of the test results of the embodiment proves that the method for realizing gas identification by adopting a single sensor is simple and effective, and compared with the existing sensor array, the method for realizing gas identification by adopting a single sensor has the advantages of small volume, simple structure, low power consumption, convenience in integration and potential for popularization to various application occasions.
The principle and implementation of the present disclosure are explained in detail by applying specific embodiments in the present disclosure, and the application of the above embodiments is only used to help understanding the using method and the idea of the present disclosure, and does not limit the application scenario of the present disclosure. The present disclosure may be modified in the specific embodiments and applications according to the actual situations, and the addition, modification or replacement of technical features with those of the present disclosure should fall within the protection scope of the present disclosure without departing from the technical features of the present disclosure.
Claims (9)
1. A method for gas identification based on a single sensor, comprising:
s1, applying short-period pulse heating voltage to the first sensor to enable the first sensor to be periodically positioned at N' different temperature points; wherein the first sensor is disposed in a first test gas chamber; the signal waveform of the short-period pulse heating voltage is one of rectangular wave, triangular wave or sine wave; the period is 5-10s, so that the first sensor is rapidly located at a plurality of temperature points, and gas-sensitive response data of the plurality of temperature points are rapidly acquired; the peak-to-peak value of the pulse heating voltage is 0.5-1.75V, so that the applied heating voltage is ensured to enable the first sensor to be in a proper working temperature range;
s2, introducing unknown gas into the first test gas chamber;
s3, obtaining the test current I of the first sensor sensing the unknown gas at N' different temperature pointst，ItThe current is the test current at the corresponding moment in the current heating period;
s4, respectively calculating N' groups of test currents ItCurrent change rate D oftThen generate DtA curve cluster; obtaining DtD in the curve clustertMaximum value, calculated from the introduction of unknown gas to DtThe time between the maxima is recorded as the maximum time τm(ii) a Calculating a gas-sensitive response value sequence of unknown gas at 1 to N' temperature points, taking logarithm of the gas-sensitive response value sequence, and generating a closed envelope curve in a radar map according to the time sequence of each temperature point in each period;
s5, determining the maximum time taumPreliminarily prejudging the possible types and concentrations of unknown gases at the position in a concentration-maximum time relation curve in a pre-established gas characteristic identification library; matching the closed envelope curve generated in the radar map with a closed envelope curve cluster in the radar map in a pre-established gas feature recognition library, and finally recognizing the type and concentration of unknown gas by combining the prejudgment;
wherein the identified unknown gases include hydrogen sulfide and sulfur dioxide.
2. The method according to claim 1, wherein in step S4, the N' sets of test currents I are respectively calculated by the following formulatCurrent change rate D oft；
Wherein, It-N′The test current at the corresponding instant in the previous heating cycle.
3. The method according to claim 2, wherein in step S4, the calculation is performed from the time of introducing the unknown gas to DtThe time between the maxima is recorded as the maximum time τmThe formula is as follows:
wherein the above formula represents the maximum time τmGet Dt(1)，Dt(2)，…，Dt(N') average of the abscissas corresponding to the maximum value, argmaxDt(N) represents a correspondence Dt(N) the abscissa when the maximum value is taken.
4. The method according to claim 1, wherein in step S4, a gas sensitivity response value sequence of the unknown gas at 1 to N' temperature points is calculated, wherein the gas sensitivity response value formula is defined as follows:
SN＝IgN/IaN
wherein, IgNFor measuring the saturation current through the first sensor under the atmosphere, IaNAnd respectively calculating gas-sensitive response values of 1 to N' temperature points according to the formula for the current passing through the first sensor under the background atmosphere to obtain a gas-sensitive response value sequence.
5. The method according to any one of claims 1 to 4, wherein the method identifies at least one type of unknown gas, and the value of N' is in the range of 5-20.
6. An apparatus for gas identification based on a single sensor, comprising: the device comprises a first sensor, a first test air chamber, a first external power supply, a signal generating circuit, a first gas introducing unit, a first test current obtaining unit, a first calculating unit and a gas identifying unit; wherein the content of the first and second substances,
the first sensor is arranged in the first testing gas chamber and used for sensing unknown gas introduced into the first testing gas chamber;
the first external power supply and signal generating circuit is used for applying short-period pulse heating voltage to the first sensor to enable the first sensor to be periodically positioned at N' different temperature points; the signal waveform of the short-period pulse heating voltage is one of rectangular wave, triangular wave or sine wave; the period is 5-10s, so that the first sensor is rapidly located at a plurality of temperature points, and gas-sensitive response data of the plurality of temperature points are rapidly acquired; the peak-to-peak value of the pulse heating voltage is 0.5-1.75V, so that the applied heating voltage is ensured to enable the first sensor to be in a proper working temperature range;
the first gas introducing unit is used for introducing unknown gas into the first test gas chamber;
the first test current acquisition unit is used for acquiring test current I of the unknown gas sensed by the first sensor at N' different temperature pointst，ItThe current is the test current at the corresponding moment in the current heating period;
the first calculating unit is used for respectively calculating N' groups of test currents ItCurrent change rate D oftThen generate DtA curve cluster; obtaining DtD in the curve clustertMaximum value, calculated from the introduction of unknown gas to DtThe time between the maxima is recorded as the maximum time τm(ii) a Calculating a gas-sensitive response value sequence of unknown gas at 1 to N' temperature points, taking logarithm of the gas-sensitive response value sequence, and generating a closed envelope curve in a radar map according to the time sequence of each temperature point in each period;
the gas identification unit for determining the maximum time τmPreliminarily prejudging the possible types and concentrations of unknown gases at the position in a concentration-maximum time relation curve in a pre-established gas characteristic identification library; the closed envelope generated in the radar map is compared withMatching closed envelope line clusters in radar maps in a pre-established gas characteristic identification library, and finally identifying the type and concentration of unknown gas by combining the prejudgment;
wherein the identified unknown gases include hydrogen sulfide and sulfur dioxide.
7. The apparatus of claim 6, wherein the first sensor comprises a test layer, a substrate, and a heating layer, disposed in sequence from top to bottom; the test layer comprises a test electrode, and the surface of the test electrode is coated with a nano gas-sensitive film; the heating layer includes a heating electrode and a heating material.
8. A method for establishing a gas feature recognition library comprises the following steps:
a1, applying short-period pulse heating voltage to the second sensor to make the second sensor be at N' different temperature points periodically; wherein the second sensor is disposed in a second test plenum; the signal waveform of the short-period pulse heating voltage is one of rectangular wave, triangular wave or sine wave; the period is 5-10s, so that the second sensor is located at a plurality of temperature points quickly, and gas-sensitive response data of the temperature points are acquired quickly; the peak-to-peak value of the pulse heating voltage is 0.5-1.75V, so that the applied heating voltage is ensured to enable the second sensor to be in a proper working temperature range;
a2, sequentially introducing n groups of test gases with the same type and different concentrations into a second test air chamber, so that the second sensor sequentially senses the test gases with different concentrations; wherein n is defined by a user according to the actual situation;
a3, respectively acquiring the test current I of each group of test gases sensed by the second sensor at N' different temperature pointst，ItThe current is the test current at the corresponding moment in the current heating period;
a4, respectively calculating N' groups of test currents I corresponding to each group of test gasestThen generating the concentration-maximum time relation curve of the n groups of test gases with the same type and different concentrations;
a5, respectively calculating a gas-sensitive response value sequence of each group of test gas at 1-N' temperature points, respectively taking logarithm of each group of gas-sensitive response value sequence, and then generating closed envelope line clusters of the N groups of test gas with the same type and different concentrations in a radar chart according to the time sequence of each temperature point in each period;
a6, releasing the gas in the second test gas chamber, introducing another different type of test gas, and repeatedly executing A1-A5 until concentration-maximum time relation curves of m groups of different types of gas and a closed envelope line cluster in a radar chart are generated; wherein m is defined by the user according to the actual situation;
a7, storing concentration-maximum time relation curves of the m groups of different gases and a closed envelope line cluster in a radar chart;
wherein the test gas comprises hydrogen sulfide and sulfur dioxide.
9. A device for establishing a gas characteristic identification library comprises a second sensor, a second test gas chamber, a second external power supply, a signal generating circuit, a second gas introducing unit, a second test current acquiring unit, a second calculating unit and a gas characteristic identification library; wherein the content of the first and second substances,
the second sensor is arranged in the second testing air chamber;
the second external power supply and signal generating circuit is used for applying short-period pulse heating voltage to the second sensor to enable the second sensor to be periodically positioned at N' different temperature points; the signal waveform of the short-period pulse heating voltage is one of rectangular wave, triangular wave or sine wave; the period is 5-10s, so that the second sensor is located at a plurality of temperature points quickly, and gas-sensitive response data of the temperature points are acquired quickly; the peak-to-peak value of the pulse heating voltage is 0.5-1.75V, so that the applied heating voltage is ensured to enable the second sensor to be in a proper working temperature range;
the second gas introducing unit is used for sequentially introducing n groups of test gases with the same type and different concentrations into a second test gas chamber, so that the second sensor sequentially senses the test gases with different concentrations; wherein n is defined by a user according to the actual situation;
the second test current acquisition unit is used for respectively acquiring the test current I of each group of test gas sensed by the second sensor at N' different temperature pointst，ItThe current is the test current at the corresponding moment in the current heating period;
the second calculating unit is used for calculating N' groups of test currents I corresponding to each group of test gases respectivelytThen generating the concentration-maximum time relation curve of the n groups of test gases with the same type and different concentrations; respectively calculating gas-sensitive response value sequences of each group of test gas at 1 to N' temperature points, respectively taking logarithm of each group of gas-sensitive response value sequences, and then generating closed envelope line clusters of the N groups of test gas with the same type and different concentrations in a radar chart according to the time sequence of each temperature point in each period; and repeatedly executing the steps until generating concentration-maximum time relation curves of m groups of different types of gases and a closed envelope line cluster in a radar chart; wherein m is defined by the user according to the actual situation;
the gas characteristic identification library is used for storing concentration-maximum time relation curves of the m groups of different gases and a closed envelope line cluster in a radar map;
wherein the test gas comprises hydrogen sulfide and sulfur dioxide.
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