CN102109492B - Carbon nanometer tube film ionization type gas humidity sensor and humidity measurement method thereof - Google Patents
Carbon nanometer tube film ionization type gas humidity sensor and humidity measurement method thereof Download PDFInfo
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- CN102109492B CN102109492B CN 201110039229 CN201110039229A CN102109492B CN 102109492 B CN102109492 B CN 102109492B CN 201110039229 CN201110039229 CN 201110039229 CN 201110039229 A CN201110039229 A CN 201110039229A CN 102109492 B CN102109492 B CN 102109492B
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Abstract
The invention discloses a carbon nanometer tube film ionization type gas humidity sensor and a humidity measurement method thereof. The sensor comprises a first electrode, a second electrode and a third electrode which are distributed in sequence, wherein the first electrode is provided with a breather hole, and a metal film substrate on which carbon nanometer tube films are distributed is adhered onto the inner surface of the first electrode; a leading-out hole is formed in the center of the second electrode; a blind hole is formed on the plate surface of the third electrode; and the three electrodes are isolated from one another. The method comprises the following steps: firstly, placing the gas humidity sensor; secondly, applying a voltage on the electrodes; thirdly, measuring the values of ion flows outputted by the sensor; fourthly, making samples of the measured values and gas humidity calibration values, and establishing a gas humidity measurement database with the samples and interpolated samples; fifthly, establishing a data fusion instrument and a gas humidity measurement model; and sixthly, inputting the measured values of the sensor into the measurement model to obtain the accurate gas humidity measurement value. The gas humidity sensor has low working voltage, as well as high gas humidity measurement sensitivity, linearity and accuracy, and can be used for humidity measurement of various gases.
Description
Technical field
The present invention relates to the gas humidity detection field, particularly a kind of ionization type gas humidity sensor 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 ionizing transducers 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 ionization type gas humidity sensors are 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 ionization type gas humidity sensors are 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 ionization type humidity sensors.
Therefore, to the research of carbon nanometer tube film ionization type gas sensor 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 nanometer tube film ionization type gas sensor, 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 ionization type gas wet sensor collector collection of the present invention 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 the carbon nanometer tube film ionization type gas sensor, by carbon nanometer tube film ionization type gas sensor measurement gas humidity to be measured; 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.
The carbon nanometer tube film ionization type gas sensor, 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 adheres to by inside surface the metallic film base that the carbon nano-tube film that distributing is arranged 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, adjacent two interelectrode die openings are 30 ~ 250 μ m; Described the first electrode and the second electrode pad are 0.01 ~ 170mm 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, and growth or screen printing are brushed with carbon nano-tube film on the metallic film base that the electrode inner surface adheres to;
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 the carbon nanometer tube film ionization type gas sensor, and the method comprises the steps:
(1) select the die opening of adjacent two electrodes in three electrodes to be set as the carbon nanometer tube film ionization type gas sensor of 30 ~ 250 μ m;
(2) the carbon nanometer tube film ionization type gas sensor is placed in gas humidity environment to be measured;
(3) to the first electrode on-load voltage 0V of carbon nanometer tube film ionization type gas sensor, 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 nanometer tube film ionization type gas sensor, 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 when (7) the carbon nanometer tube film ionization type gas sensor being surveyed, 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 nanometer tube film ionization type gas sensor, 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 nanometer tube film ionization type gas sensor, by carbon nanometer tube film ionization type gas sensor measurement gas humidity to be measured; 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 humidity environment 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 the carbon nanometer tube film ionization type gas sensor 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.By regulating die opening and the electrode voltage of adjacent two electrodes of sensor electrode, 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 the carbon nanometer tube film ionization type gas sensor, carbon nano-tube film ionizing transducer 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 nanometer tube film ionization type gas sensor construction schematic diagram of the present invention;
Fig. 3 is carbon nanometer tube film ionization type gas three-dimensional sensor structure side view of the present invention;
Fig. 4 is the single valued relation of humidity in the gas discharge ion current of carbon nanometer tube film ionization type gas sensor of the present invention output 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, metallic film base; 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, this carbon nanometer tube film ionization type gas sensor, 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 adheres to by inside surface the metallic film base 5 that the carbon nano-tube film 6 that distributing is arranged 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 nanometer tube film ionization type gas 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 attached with metallic film base 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 ~ 4 fairlead, have provided in Fig. 2, Fig. 3 a fairlead to be set and fairlead is circular embodiment.Third electrode 3 collector blind holes are corresponding with the fairlead of the second electrode, and the quantity of blind hole is 1 ~ 4, 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 the first electrode 1 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 of the first electrode 1 and the both sides on the inboard golden film surface of third electrode 3.
The present invention's the first electrode 1 adopts silicon sheet material to make, and a side surface of the first electrode 1 is attached with metallic film base 5; 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 on metallic film base 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 of the first electrode 1 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 detected and enter electrode gap; Metallic film base 5 is attached to the first electrode 1 one side surfaces, has conductive capability; On the second electrode 2, fairlead is arranged; Third electrode 3 collectors can be collected the positive ion stream that gas ionization produces.Between the first electrode 1 and the second electrode 2, 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 the carbon nanometer tube film ionization type gas sensor 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 the output of carbon nanometer tube film ionization type gas sensor, apply at the second electrode on the basis of certain voltage, present single valued relation (shown in Figure 4).By piecewise interpolation and data fusion, realized the accuracy of measurement of gas humidity 1%.Carbon nano-tube film ionizing transducer 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 nanometer tube film ionization type gas sensor measurement gas humidity of the present invention is described further.
Adopt the fixing carbon nanometer tube film ionization type gas sensor 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 nanometer tube film ionization type gas sensor shown in Figure 4 detects in the embodiment of nitrogen environment humidity, and the experimental situation condition is 20.8 ~ 21.8 ℃ of temperature, atmospheric pressure 93.6 ~ 100KPa.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 170mm 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 25.8 ~ 100%RH humidity range, 25 groups of experimental calibration data have been obtained.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 0.5%RH as step-length in 25.8 ~ 100%RH humidity range, obtain 150 groups of interpolated datas, and form database with 25 groups of experimental calibration data.Select 45 groups of interpolated datas as training sample, 25 groups of experimental calibration data are as test samples, and input data fusion instrument is checked by training, obtains moisture measurement model in nitrogen.The linearity of this moisture measurement model is that the assay fiducial error maximal value of 0.15%, 25 group of test samples is 0.2%, has reached 1% moisture measurement accuracy.
The present embodiment basic structure is with embodiment 1, difference is: in three electrodes of carbon nanometer tube film ionization type gas 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 carbon nanometer tube film ionization type gas 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 nanometer tube film ionization type gas 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 carbon nanometer tube film ionization type gas 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 nanometer tube film ionization type gas sensor, 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 faint ion current of pA level; The pA level ion 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 nanometer tube film ionization type gas sensor, 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 adheres to by inside surface the metallic film base that the carbon nano-tube film that distributing is arranged 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, adjacent two interelectrode die openings are 30 ~ 250 μ m; Described the first electrode and the second electrode pad are 10 ~ 170mm 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, and growth or screen printing are brushed with carbon nano-tube film on the metallic film base that the electrode inner surface adheres to;
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 nanometer tube film ionization type gas sensor 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 the carbon nanometer tube film ionization type gas sensor of 30 ~ 250 μ m;
(2) the carbon nanometer tube film ionization type gas sensor is placed in gas humidity environment to be measured;
(3) to the first electrode on-load voltage 0V of carbon nanometer tube film ionization type gas sensor, 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 nanometer tube film ionization type gas sensor, 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 when (7) the carbon nanometer tube film ionization type gas sensor being surveyed, 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 the carbon nanometer tube film ionization type gas sensor according to claim 2, it is characterized in that: in described carbon nanometer tube film ionization type gas sensor, 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 the carbon nanometer tube film ionization type gas sensor 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, with gas humidity calibration value and interpolated data thereof as the desired output sample.
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| CN102095789B (en) * | 2011-02-16 | 2013-07-10 | 西安交通大学 | Carbon nanotube film ionizing sensor and method for detecting concentration of bi-component gas |
| CN102081067B (en) * | 2011-02-16 | 2013-01-02 | 西安交通大学 | Carbon nanotube (CNT) film based ionization nitrogen dioxide sensor and method for measuring concentration by adopting same |
| CN103236429B (en) * | 2013-05-14 | 2015-09-09 | 哈尔滨工业大学 | With the Miniature carbon nano pipe humidity sensor chip of heating unit |
| CN107525825A (en) * | 2016-06-21 | 2017-12-29 | 天津理工大学 | It is prepared by a kind of gas sensor based on screen printing technique |
| CN106198714B (en) * | 2016-08-03 | 2019-04-12 | 西安交通大学 | A kind of gold-plated carbon nano-tube film ionization type methane transducer |
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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 |
| CN102081072A (en) * | 2011-02-16 | 2011-06-01 | 西安交通大学 | Carbon nanotube (CNT) film based ionization nitric oxide (NO) sensor and method for measuring concentration by adopting same |
| CN102175756A (en) * | 2011-02-16 | 2011-09-07 | 西安交通大学 | Carbon nanotube film ionizing sulphur dioxide sensor and concentration measuring method by utilizing same |
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| JP2006220513A (en) * | 2005-02-09 | 2006-08-24 | Fujitsu Ltd | Target detection device, its manufacturing method and target detection method |
| CN102095781B (en) * | 2011-02-16 | 2012-09-05 | 西安交通大学 | Carbon nano tube film ionizing sensor and method for detecting concentration of single gas based on same |
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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 |
| CN102081072A (en) * | 2011-02-16 | 2011-06-01 | 西安交通大学 | Carbon nanotube (CNT) film based ionization nitric oxide (NO) sensor and method for measuring concentration by adopting same |
| CN102175756A (en) * | 2011-02-16 | 2011-09-07 | 西安交通大学 | Carbon nanotube film ionizing sulphur dioxide sensor and concentration measuring method by utilizing same |
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