CN102095784B - Carbon nano tube film three-electrode gas humidity sensor and humidity measuring method thereof - Google Patents
Carbon nano tube film three-electrode gas humidity sensor and humidity measuring method thereof Download PDFInfo
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- CN102095784B CN102095784B CN 201110039161 CN201110039161A CN102095784B CN 102095784 B CN102095784 B CN 102095784B CN 201110039161 CN201110039161 CN 201110039161 CN 201110039161 A CN201110039161 A CN 201110039161A CN 102095784 B CN102095784 B CN 102095784B
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Abstract
The invention discloses a carbon nano tube film three-electrode gas humidity sensor and a humidity measuring method thereof; the sensor comprises a first, a second and a third electrodes distributed in sequence; the first electrode is provided with an air vent, and the inner surface of the first electrode is bonded with a substrate distributed with a carbon nano tube film; the center of the second electrode is provided with an exist aperture; the surface of the third electrode is provided with a blind hole; and the three electrodes are separated from each other. The method comprises the following steps of: 1) arranging the air humidity sensor; 2) applying voltages on the electrodes; 3) measuring the sensor to output ion flow value; 4) forming a sample by detected value and gas humidity calibration value and constructing a gas humidity measuring database with a interpolation sample; 5) constructing a data fusion instrument and building a gas humidity measuring model; 6) inputting the measured value of the sensor to the measuring model, and obtaining the accurate measuring value of gas humidity. The working voltage of the gas humidity sensor is low, the flexibility of the measured gas humidity is high, the linearity is good, the precision is high, and the sensor and the device can be used for measuring the humidity of inflammable, explosive and poisonous gas.
Description
Technical field
The present invention relates to the gas humidity detection field, particularly a kind of three electrode gas humidity sensors and humidity measuring method thereof based on carbon nano-tube film and gas discharge principle.
Background technology
Along with all trades and professions gas detect in the urgent need to and the development of nanometer technology, nano-sensor has obtained considerable progress.Especially along with the discovery of carbon nano-tube in latter stage in 20th century, carbon nano-tube shows tempting application prospect in gas, temperature and humidity measure field.Carbon nano-tube film two electrode sensors in the carbon nano-tube moisture sensor, high with its detection sensitivity, detect the advantages such as gas wide ranges, response be fast, become the study hotspot of gas humidity detection field.Carbon nano-tube film two-electrode gas humidity sensor is based on gas discharge principle, with carbon nano-tube as sensitive material, have the irreplaceable advantage of conventional sensors: the one, the specific surface area of carbon nano-tube is large, in the situation that the sensor overall dimensions is less, can greatly improve the area of electrode; Two are based on the tip curvature radius of carbon nanotube level, and working sensor voltage is greatly reduced, and obtain extremely strong electric field intensity near the carbon nano-tube tip, make tested gas ionization under low-voltage; The 3rd, the size of greatly having dwindled sensor, dynamic response is fast.Therefore, it has development prospect widely at aspects such as biology, chemistry, machinery, aviation, military affairs, anti-terrorisms.
Existing carbon nano-tube film two-electrode gas humidity sensor is developed under the condition of 120 microns die openings by Hui Guohua, the Chen Yuquan professor of Zhejiang University's biomedical engineering and instrumental science institute, studied the wet sensitive characteristic (Fig. 1) of carbon nano-tube thin film cathode two electrode sensors, i.e. the relation of voltage breakdown and humidity in air.The voltage breakdown of this two electrode sensor and humidity have many-valued nonlinear characteristic, do not consist of carbon nano-tube film two electrode humidity sensors.
Therefore, to the research of carbon nano-tube film three electrode gas humidity sensors and humidity measuring method thereof, become the technical matters that needs to be resolved hurrily at present.
Summary of the invention
One of purpose of the present invention, be to provide a kind of carbon nano-tube film three electrode gas humidity sensors, the output current of conventional carbon nano-tube film two electrode sensors is divided into electron stream and ion current, set up the ion current of the present invention's three electrode gas wet sensor collectors collections and the single-valued relationship of gas humidity, overcome the many-valued nonlinear problem of carbon nano-tube film two electrode sensor wet sensitive characteristics.Sensor construction of the present invention is simple, and cost is low, and measurement gas humidity is highly sensitive.
Another object of the present invention is to provide a kind of humidity measuring method based on carbon nano-tube film three electrode gas humidity sensors, measures gas humidity to be measured by carbon nano-tube film three electrode gas humidity sensors; The hardware configuration that this humidity measuring method requires is simple, can measure inflammable and explosive and toxic gas humidity, adopts data anastomosing algorithm, and the accuracy of measurement gas humidity is high.
The objective of the invention is to realize by following technical proposals.
Carbon nano-tube film three electrode gas humidity sensors, it is characterized in that: comprise three the first electrode, the second electrode and third electrodes that distribute successively from top to bottom, the electrode that described the first electrode is bonded with the substrate of the carbon nano-tube film that distributing by inside surface and is provided with bleeder vent consists of; The second electrode is made of the extraction pole pole plate that the center is provided with fairlead; Third electrode is made of the collector that the plate face is provided with blind hole; These three electrodes are isolated mutually by insulation column respectively.
Architectural feature of the present invention also is:
In described three electrodes, the die opening of adjacent two electrodes is 30～250 μ m; Described the first electrode and the second electrode pad are 0.01～17mm over against area
2, the second electrode and third electrode pole plate are 0.01～190mm over against area
2
The bleeder vent of the electrode surface of described the first electrode is 1～4, is attached with carbon nano-tube film in the bonding substrate of electrode inner surface;
Described the second electrode extraction pole center is provided with 1～4 fairlead;
Described third electrode collector blind hole is corresponding with the fairlead of the second electrode, and the quantity of blind hole is 1～4.
The present invention gives a kind of gas humidity measuring method based on carbon nano-tube film three electrode gas humidity sensors, and the method comprises the steps:
(1) select the die opening of adjacent two electrodes in three electrodes to be set as carbon nano-tube film three electrode gas humidity sensors of 30～250 μ m;
(2) carbon nano-tube film three electrode gas humidity sensors are placed in gas humidity environment to be measured;
(3) to the first electrode on-load voltage 0V of carbon nano-tube film three electrode gas humidity sensors, second electrode on-load voltage 2～200V, third electrode on-load voltage 1～180V;
(4) in gas humidity measurement range to be measured, corresponding different humidity demarcating values, the gas discharge ion flow valuve of survey sensor output;
(5) with the sensor output ion flow valuve and corresponding humidity demarcating value that record in step (4), form different experimental calibration samples, then adopt the piecewise interpolation technology to carry out interpolation to the experimental calibration sample, obtain interpolated data, obtain interpolated sample, and set up the gas humidity measured database according to all samples that comprised experimental calibration sample and interpolated sample;
(6) adopt Data fusion technique, build the data fusion instrument, set up the moisture measurement model of carbon nano-tube film three electrode gas humidity sensors, respectively with input sample and the desired output sample of the data in the gas humidity measured database as the data fusion instrument, and train and check as training sample and the test samples of data fusion instrument respectively with data different in range ability, when assay satisfies the measurement error requirement, the humidity Measurement accuracy model of data fusion instrument output transducer;
The gas humidity measurement model that during (7) with carbon nano-tube film three electrode gas humidity sensor actual measurement, the ion flow valuve input step (6) of output obtains, the Measurement accuracy value of this model output gas humidity.
The inventive method feature also is:
In described carbon nano-tube film three electrode gas humidity sensors, the second electrode potential is higher than the first electrode potential, and the third electrode current potential is lower than the second electrode potential and higher than the first electrode potential.
Described establishment gas humidity measured database is that experimental calibration data and interpolated data are formed database, and sensor is exported ion flow valuve and interpolated data thereof as the input sample, with gas humidity calibration value and interpolated data thereof as the desired output sample.
Based on the gas humidity measuring method of carbon nano-tube film three electrode gas humidity sensors, measure gas humidity to be measured by carbon nano-tube film three electrode gas humidity sensors; Powered by the sensor electrical potential source; Exported by pA level current measurement system detecting sensor; Adjust electrode separation, adjust electrode voltage, carry out the calibration experiment of sensor in gas to be measured; Based on the piecewise interpolation technology, the experimental calibration data are carried out interpolation, obtain interpolated data; All data that will comprise experimental calibration data and interpolated data form the gas humidity measured database, obtain the monodrome humidity sensitive characteristic of sensor; According to the data in the gas humidity measured database, the based on data integration technology is set up the humidity Measurement accuracy model of gas humidity sensor; During with actual measurement, the gas humidity measurement model is inputted in the output of sensor in real time, just can obtain the measured result of gas humidity.This gas humidity measuring method has overcome carbon nano-tube film two electrode sensor operating voltage height and the many-valued nonlinear problems of wet sensitive characteristic, the hardware configuration that requires is simple, can measure inflammable, explosive and toxic gas humidity, and cost is low, measurement gas humidity is highly sensitive, accuracy is high, is suitable for promoting the use of.
The present invention can realize the measurement of various gas humidities owing to having taked carbon nano-tube film three electrode gas humidity sensors to measure humidity, and accuracy is 1%.The sensor of this structure adopts carbon nano-tube film to do electrode, can realize working sensor voltage is down to safe and practical scope below 200 volts with the tip curvature radius of carbon nanotube level.Die opening and the inter-electrode voltage of adjacent two electrodes by regulating three-electrode structure, in the moisture measurement scope, can solve in prior art that carbon nano-tube film two electrode sensor operating voltage are high, the many-valued nonlinear problem of wet sensitive characteristic, can be used for the measurement of humidity in inflammable, explosive, toxic gas environment.The present invention is due to the humidity measuring method of having taked based on carbon nano-tube film three electrode gas humidity sensors, carbon nano-tube film three electrode sensor technology, pA level current measurement techniques, piecewise interpolation technology and Data fusion technique are integrated, can realize the Measurement accuracy of gas humidity.
Description of drawings
Fig. 1 is the many-valued non-linear humidity sensitive characteristic of prior art carbon nano-tube film two electrode humidity sensors.
Fig. 2 is carbon nano-tube film three electrode gas humidity sensor structural representations of the present invention;
Fig. 3 is carbon nano-tube film three electrode gas humidity sensor spatial structure side views of the present invention;
Fig. 4 is the single valued relation of humidity in the gas discharge ion current of carbon nano-tube film of the present invention three electrode gas humidity sensors outputs and nitrogen environment.
In figure: 1, the first electrode; 2, the second electrode; 3, third electrode; 4, be provided with the electrode of bleeder vent; 5, carbon nano-tube film substrate; 6, carbon nano-tube film; 7, insulation column.
Embodiment
The present invention will be further described below in conjunction with drawings and the specific embodiments.
As shown in Figure 2 and Figure 3, these carbon nano-tube film three electrode gas humidity sensors, comprise by three electrodes that mutually superpose from top to bottom successively and consisting of, these three mutual overlay electrodes are respectively the first electrode 1, the second electrode 2 and third electrode 3, and the electrode 4 that its first electrode 1 is bonded with the substrate 5 of the carbon nano-tube film 6 that distributing by inside surface and is provided with bleeder vent consists of; The second electrode 2 is made of the extraction pole pole plate that the center is provided with fairlead; Third electrode 3 is made of the collector that the battery lead plate face is provided with blind hole; These three electrodes are isolated mutually by insulation column 7 respectively.
In carbon nano-tube film three electrode gas humidity sensor embodiment shown in Figure 2, the bleeder vent of the electrode surface of the first electrode 1 has 2, and bleeder vent is circular; Inner surface at this first electrode 1 is bonded with carbon nano-tube film substrate 5, is distributed with carbon nano-tube film 6 on it, and this carbon nano-tube mouth of pipe is downward.The second electrode 2 centers are provided with 1 fairlead and fairlead for circular.Third electrode 3 collector blind holes are corresponding with the fairlead of the second electrode, provided in Fig. 2, Fig. 3 a blind hole to be set and blind hole is the embodiment of cylindrical structure.Insulation column 7 is separately positioned between carbon nano-tube film substrate 5 and the second electrode 2, between the second electrode 2 and third electrode 3, namely insulation column 7 is distributed in the second electrode 2 over against the surperficial both sides at the carbon nano-tube film substrate two ends of the first electrode 1 and the both sides of the inner surface of third electrode 3.
The present invention is provided with electrode 4 plate faces and the carbon nano-tube film substrate 5 of bleeder vent and all adopts silicon sheet material to make; Described carbon nano-tube film 6 can adopt FePC as catalyzer, and adopts carbon source, and carbon nano-tube film 6 is made in growth in substrate 5, and perhaps the serigraphy carbon nano-tube film 6.The second electrode 2 and third electrode 3 all adopt silicon wafer to manufacture.The two sides that are provided with the electrode 4 of bleeder vent and third electrode 3 medial surfaces, the second electrode 2 are equipped with metal film.
On electrode in the present invention's the first electrode 1,2 bleeder vents are arranged, be convenient to gas to be measured and enter electrode gap; Growth has conductive capability at the bottom of the silicon wafer-based of carbon nano-tube film is arranged, and strong bond is at the first electrode 1 inner surface; Through the fairlead of the second electrode 2, third electrode 3 collectors can be collected the positive ion stream that gas ionization produces.Between the first electrode 1 and the second electrode 3, mutually isolate by insulation column 7 between the second electrode 2 and third electrode 3; Tested gas enters in the gap of adjacent two electrodes of sensor by the gap between the sensor peripheral electrode.
The present invention takes carbon nano-tube film three electrode gas humidity sensors of said structure when measurement gas humidity, and the second electrode potential is higher than the first electrode potential, and the third electrode current potential is lower than the second electrode potential and higher than the first electrode potential.The second electrode and the first electrode form the electron stream loop, and third electrode and the first electrode form the ion current loop, and realization separates electron stream with ion current.Between the ion current and gas humidity of carbon nano-tube film three electrode gas humidity sensor outputs, apply at the second electrode on the basis of certain voltage, present single valued relation (Fig. 4).By piecewise interpolation and data fusion, realized the accuracy of measurement of gas humidity 1%.Carbon nano-tube film three electrode sensor technology, pA level current measurement techniques, piecewise interpolation technology and Data fusion technique are the features of humidity measuring method of the present invention.
Below by an instantiation, the method for carbon nano-tube film three electrode gas humidity sensor measurement gas humidity of the present invention is described further.
Adopt fixing carbon nano-tube film three electrode gas humidity sensors of die opening, experiment has obtained the monodrome humidity characteristic (shown in Figure 4) in nitrogen, the moisture measurement model that the ion current input data fusion of sensor output is set up has obtained fiducial error less than the moisture measurement value in 1% nitrogen.
Carbon nano-tube film three electrode gas humidity sensors shown in Figure 4 detect in the embodiment of the humidity in nitrogen, and the experimental situation condition is temperature 23.7%RH, atmospheric pressure 93.7KPa.Sensor the first electrode 1 and the second electrode 2 die openings are that 200 μ m, the second electrode 2 are 100 μ m with third electrode 3 die openings; The first electrode 1 and the second electrode 2 pole plates are 17mm over against area
2, the second electrode 2 is 190mm with third electrode 3 pole plates over against area
2The first electrode 1 cathode voltage is 0V, the second electrode 2 extraction pole on-load voltage 90V, third electrode 3 collector on-load voltage 10V.Along with the rising of humidity, the ion current that collector is collected increases, and presents monodrome rising relation between ion current and humidity.In 30～100%RH humidity range, obtain 36 groups of experimental calibration data.Humidity sensor ion flow valuve is as the input sample, and the humidity demarcating value is as the desired output sample data.Adopt linear interpolation, carry out equidistant interpolation take step-length as 0.1%RH in 30～100%RH humidity range, obtain 798 groups of interpolated datas, and form database with 36 groups of experimental calibration data.Select 57 groups of interpolated datas and 25 groups of experimental calibration data as training sample, 11 groups of experimental calibration data that are different from training sample and 2 groups as the experimental calibration data of training sample totally 13 groups of data together as test samples, input data fusion instrument, check by training, obtain moisture measurement model in nitrogen.The linearity of this moisture measurement model is that the assay fiducial error maximal value of 0.07%, 7 group of test samples is 0.42%, has reached 1% moisture measurement accuracy.
The present embodiment basic structure is with embodiment 1, difference is: in three electrodes of carbon nano-tube film three electrode gas humidity sensor, adjacent two interelectrode die openings are respectively 250 μ m, 30 μ m, and the first electrode 1 and the second electrode 2 pole plates are 0.01mm over against area
2, the second electrode 2 is 0.01mm with third electrode 3 pole plates over against area
2
The bleeder vent of the electrode surface of the first electrode 1 has 1, and bleeder vent is quadrilateral, pentagon or hexagon; The second electrode 2 center fairleads are 4, and fairlead is quadrilateral, pentagon or hexagon; The quantity of third electrode 3 blind holes is 4, and blind hole is 3～6 prisms or pyramid.
The humidity measuring method of the present embodiment is substantially the same manner as Example 1, and difference is:
The first electrode cathode voltage of sensor is 0V, the second electrode extraction pole on-load voltage 2V, third electrode collector on-load voltage 1V.
The present embodiment basic structure is with embodiment 1, difference is: in three electrodes of carbon nano-tube film three electrode gas humidity sensor, adjacent two interelectrode die openings are respectively 250 μ m, 30 μ m, and the first electrode 1 and the second electrode 2 pole plates are 10mm over against area
2, the second electrode 2 is 100mm with third electrode 3 pole plates over against area
2
The bleeder vent of the electrode surface of the first electrode 1 has 4, and bleeder vent is quadrilateral, pentagon or hexagon; The second electrode 2 center fairleads are 2, and fairlead is quadrilateral, pentagon or hexagon; The quantity of third electrode 3 blind holes is 2, and blind hole is 3～6 prisms or pyramid.
The humidity measuring method of the present embodiment is substantially the same manner as Example 1, and difference is:
The first electrode cathode voltage of sensor is 0V, the second electrode extraction pole on-load voltage 200V, third electrode collector on-load voltage 180V.
The present invention is by carbon nano-tube film three electrode gas humidity sensors, the output of pA level current measurement system detecting sensor, piecewise interpolation and data fusion method, form a kind of novel, can measure various gas humidities to be measured, the linearity is good, accuracy is high gas humidity measuring method.The direct measurement gas humidity of sensor of the present invention is also exported the above weak current of pA level; The pA level electric current of pA level current measurement system detectable gas humidity sensor output; Piecewise interpolation and data fusion method can obtain the high gas humidity measured value of accuracy.
Although the present invention has made detailed description with above-mentioned preferred embodiment to the present invention, above-described embodiment is not intended to limit the present invention.In the situation that do not break away from the given technical characterictic of technical solution of the present invention and range of structures, the increase that technical characterictic is done, distortion or with the replacement of the same content in this area all should belong to protection scope of the present invention.
Claims (4)
1. carbon nano-tube film three electrode gas humidity sensors, it is characterized in that: comprise three the first electrode, the second electrode and third electrodes that distribute successively from top to bottom, the electrode that described the first electrode is bonded with the substrate of the carbon nano-tube film that distributing by inside surface and is provided with bleeder vent consists of; The second electrode is made of the extraction pole pole plate that the center is provided with fairlead; Third electrode is made of the collector that the plate face is provided with blind hole; These three electrodes are isolated mutually by insulation column respectively;
In described three electrodes, the die opening of adjacent two electrodes is 100 ~ 200 μ m; Described the first electrode and the second electrode pad are 10 ~ 17mm over against area
2, the second electrode and third electrode pole plate are 0.01 ~ 190mm over against area
2
The bleeder vent of the electrode surface of described the first electrode is 1 ~ 4, is attached with carbon nano-tube film in the bonding substrate of electrode inner surface;
Described the second electrode extraction pole center is provided with 1 ~ 4 fairlead;
Described third electrode collector blind hole is corresponding with the fairlead of the second electrode, and the quantity of blind hole is 1 ~ 4.
2. based on the gas humidity measuring method of carbon nano-tube film three electrode gas humidity sensors claimed in claim 1, it is characterized in that, the method comprises the steps:
(1) select the die opening of adjacent two electrodes in three electrodes to be set as carbon nano-tube film three electrode gas humidity sensors of 100 ~ 200 μ m;
(2) carbon nano-tube film three electrode gas humidity sensors are placed in gas humidity environment to be measured;
(3) to the first electrode on-load voltage 0V of carbon nano-tube film three electrode gas humidity sensors, second electrode on-load voltage 2 ~ 200V, third electrode on-load voltage 1 ~ 180V;
(4) in gas humidity measurement range to be measured, corresponding different humidity demarcating values, the gas discharge ion flow valuve of survey sensor output;
(5) with the sensor output ion flow valuve and corresponding humidity demarcating value that record in step (4), form different experimental calibration samples, then adopt the piecewise interpolation technology to carry out interpolation to the experimental calibration sample, obtain interpolated data, obtain interpolated sample, and set up the gas humidity measured database according to all samples that comprised experimental calibration sample and interpolated sample;
(6) adopt Data fusion technique, build the data fusion instrument, set up the moisture measurement model of carbon nano-tube film three electrode gas humidity sensors, respectively with input sample and the desired output sample of the data in the gas humidity measured database as the data fusion instrument, and train and check as training sample and the test samples of data fusion instrument respectively with data different in range ability, when assay satisfies the measurement error requirement, the humidity Measurement accuracy model of data fusion instrument output transducer;
The gas humidity measurement model that during (7) with carbon nano-tube film three electrode gas humidity sensor actual measurement, the ion flow valuve input step (6) of output obtains, the Measurement accuracy value of this model output gas humidity.
3. the gas humidity measuring method based on carbon nano-tube film three electrode gas humidity sensors according to claim 2, it is characterized in that: in described carbon nano-tube film three electrode gas humidity sensors, the second electrode potential is higher than the first electrode potential, and the third electrode current potential is lower than the second electrode potential and higher than the first electrode potential.
4. the gas humidity measuring method based on carbon nano-tube film three electrode gas humidity sensors according to claim 2, it is characterized in that: described establishment gas humidity measured database, that experimental calibration data and interpolated data are formed database, sensor is exported ion flow valuve and interpolated data thereof as the input sample, gas humidity is demarcated and the interpolated data value as the desired output sample.
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| CN112229878B (en) * | 2020-01-07 | 2021-08-10 | 南通大学 | Humidity sensor chip with three-electrode structure |
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| CN101363807A (en) * | 2008-09-11 | 2009-02-11 | 电子科技大学 | Organic gas sensor and method for making same |
| CN102081068A (en) * | 2011-02-16 | 2011-06-01 | 西安交通大学 | Three-electrode sulfur dioxide sensor of carbon nanotube film and concentration measurement method thereof |
| CN102175343A (en) * | 2011-02-16 | 2011-09-07 | 西安交通大学 | Carbon nanotube film three-electrode gas temperature sensor and temperature measuring method thereof |
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| CN101363807A (en) * | 2008-09-11 | 2009-02-11 | 电子科技大学 | Organic gas sensor and method for making same |
| CN102081068A (en) * | 2011-02-16 | 2011-06-01 | 西安交通大学 | Three-electrode sulfur dioxide sensor of carbon nanotube film and concentration measurement method thereof |
| CN102175343A (en) * | 2011-02-16 | 2011-09-07 | 西安交通大学 | Carbon nanotube film three-electrode gas temperature sensor and temperature measuring method thereof |
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