CN109557142A - A kind of resistance type humidity sensor of quick response and its preparation method and application - Google Patents
A kind of resistance type humidity sensor of quick response and its preparation method and application Download PDFInfo
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Abstract
The present invention provides resistance type humidity sensors of a kind of quick response and preparation method thereof, and are applied to real-time breathing detection system.Active material dispersion liquid is deposited to interdigital electrode surface by the methods of drop coating, spraying, spin coating by the present invention, two electrode humidity sensors are obtained after drying, electrode connection resistance testing device just can be applied to the detection of humidity, which has fast response time, high sensitivity, detection range wide and good selective.The present invention passes through the humidity sensor using this quick response, the respiratory of real-time monitoring user, to realize the assessment of respiratory function and the diagnosis of disease.
Description
Technical field
The invention belongs to electrochemical sensing technical fields, and in particular to a kind of resistance type humidity sensor of quick response and
Preparation method and application.
Background technique
The respiratory of the mankind has very important significance for life and health, and the monitoring for breathing is a kind of disease
The effective means of prevention and diagnosis in sleep disordered breathing (SDB) and obstructive are slept especially to the monitoring of sleep-respiratory
Have great importance in the diagnosis of dormancy apnea (OSA) and centric sleep apnea (CSA).Although having been developed
A variety of commercialized monitoring devices, such as polysomnography (PSG), existing method are usually to pass through detection breathing
Fluctuating when flow velocity, nasal pressure, blood oxygen saturation and the chest and abdomen of gas breathe monitors breathing to obtain multi-signal jointly, but
It is that these methods can only obtain basic information, such as respiratory rate and depth of respiration, the dynamic process of breathing is difficult to
Monitoring in real time and record are carried out, which has limited application of the monitoring of respiration in health medical treatment and diagnosing human disease field.
Hydrone is essential basic substance in human body, is all play in most of metabolic process extremely important
Role, wherein the exhaled gas in respiratory is just along with the flowing of hydrone, therefore hydrone can be used as a prison
The important signaling molecule for surveying breathing, the monitoring that can be realized to respiratory is monitored to hydrone.Resistor-type gas
Sensor is the converter that a kind of gas concentration by air is converted to electric signal.In recent years, many humidity sensors are opened
Hair is utilized and is had been put into and commercially produces, but generally existing response speed is slow, sensitivity and detection range need into one
The problems such as step improves.Main humidity-sensitive material has following a few classes: metal-oxide semiconductor (MOS), cheap but response speed
Slowly, selectivity is poor；Conducting polymer is easy to functionalization, but long-time stability are inadequate；Electrolyte type humidity-sensitive material, price are low
It is honest and clean but often detection range is relatively narrow.Carbon-rich material is caused people in recent years and is greatly paid close attention to due to its structure controllability,
Great application prospect is presented in humidity sensor.
Summary of the invention
Goal of the invention: the first purpose of the invention is to provide a kind of resistance type humidity sensors of quick response.
The present invention constructs quick response humidity sensor using rich carbon humidity sensitive material, when having the response time and restoring
Between short advantage, be applied to breathing detection field, the real-time monitoring of the pneumodynamics process of user may be implemented, thus
Realize the assessment of respiratory function and the diagnosis of disease.
A second object of the present invention is to provide a kind of preparation methods of the resistance type humidity sensor of quick response.
Third object of the present invention is to provide a kind of applications of the resistance type humidity sensor of quick response.
Technical solution: to realize above-mentioned first purpose, a kind of the technical solution adopted by the present invention are as follows: electricity of quick response
Resistance type humidity sensor, the resistance type humidity sensor rich in hydroxyl, amino, carboxyl or contain other hydrophilic groups using surface
The two-dimensional material of group deposits to interdigital electrode surface as active material, by drop coating, spraying or spin coating method, is after dry
?.
Wherein, the active material is one or more of azotized carbon nano line, carbon nanotube, graphene or carbon black.
Wherein, the interdigital electrode is carbon interdigital electrode, golden interdigital electrode, silver-colored interdigital electrode or platinum interdigital electrode.
To realize above-mentioned second purpose, the technical solution adopted by the present invention are as follows: the present invention provides the electricity of quick response
The preparation method of resistance type humidity sensor, comprising the following steps:
1) it prepares azotized carbon nano line: nitridation carbon dust and sodium hydroxide solution being mixed, which are put into round bottom
Flask stirs 1-24h in 60 DEG C of -80 DEG C of oil baths, after reaction, reaction product is packed into bag filter (molecular cut off
In 1000-5000Da), with deionized water dialysis to neutrality, the azotized carbon nano line hydrolyzed；
2) preparation of humidity sensor: azotized carbon nano line dispersion liquid and conductive carbon material are mixed, and ultrasound makes it uniformly
Compound, 5-20 times of dilution is added drop-wise to the interdigital electrode surface cleaned, and is humidity sensor after dry.
Wherein, the sodium hydroxide solution 0.5-8mol/L.
Wherein, the mass volume ratio of the conductive carbon material and azotized carbon nano line dispersion liquid are as follows: 1:(0.05-1) mg/
mL.The concentration of the azotized carbon nano line dispersion liquid is 5mg/ml.
Wherein, the conductive carbon material is one of carbon nanotube, graphene or carbon black.
To realize above-mentioned third purpose, the present invention also provides the resistance type humidity sensors of the quick response to exist
Application in Humidity Detection.
Wherein, the resistance type humidity sensor of the quick response is connected resistance testing device, applied by the application
Voltage passes through the variation of the variation monitoring ambient humidity of material resistance.
Wherein, the resistance testing device is electrochemical workstation or numeric type multimeter.
Wherein, the application is by timing Amperometric or linear sweep voltammetry, to the resistance type humidity of quick response
Sensor applies a constant potential or linear potential, and the variation of material resistance value is calculated from the curent change detected, from
And learn the variation of ambient humidity.
Wherein, application of the invention further includes being placed on humidity sensor in the closed environment of different relative humidity, wet
Degree sensing element is connected by conducting wire with extraneous electrochemical workstation, is tested I-V curve by linear sweep voltammetry, is calculated
Slope obtains the resistance under different relative humidity, to obtain resistance-relative humidity standard curve.
Wherein, the content of present invention further includes testing the response time of sensor: the sensor of preparation is placed on high-purity gas
In the channel that body passes through, and it is connected with electrochemical workstation.It is taken in the closed container for holding deionized water with syringe a small amount of
Humidity is the air of 100%RH, and fast injection forms a pulse signal to the front in the channel for placing sensor.When there is tide
Humid air as pulse signal by humidity-sensitive material on sensor when, electric current rapid decrease, the response time in 50ms or so, and
And sensor sheet reveals good reproducibility.
Wherein, summary of the invention further includes being fixed on the sensor on test mask and being connected with electrochemical workstation, is allowed
Subject personnel take test mask, adjust electrode position.When the personnel of subject breathing, contain hydrone, gas in exhaled gas
When stream passes through sensing element, resistance is caused to increase electric current decline, so as to detect the respiratory state of subject personnel.
The working principle of the invention is: the difference of physicochemical property of the humidity sensitive material under different ambient humidities is led
The difference that resistance value is shown when applying voltage is caused, the present invention carries out the detection of different humidity using this characteristic.
The utility model has the advantages that compared with prior art, the present invention have the advantages that following characteristic and: the humidity sensor has good
Good sensitivity, wider detection range and excellent stability.Simultaneously because the design feature of material itself, causes to water
Molecule has faster adsorption desorption effect, to have the advantages that fast response time.This advantage in the present invention further by
It is used in the detection of human body respiration, this method not only can detecte the information that traditional breathing detection equipment obtains, such as breathing frequency
Rate, depth of respiration etc., and due to the faster response speed of the sensor, the higher breathing I-t curve of resolution ratio can be obtained,
To monitor the details of the process of breathing, the assessment of respiratory function and the diagnosis of disease are realized.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of azotized carbon nano line；
Fig. 2 is current -voltage curve of the humidity sensor under different humidity；
Fig. 3 is resistance variations figure of the humidity sensor under different humidity；
Fig. 4 is the quick response current versus time curve of humidity sensor；
Fig. 5 is the stability curve of humidity sensor；
Fig. 6 is breathing detection current versus time curve.
Specific embodiment
With reference to the accompanying drawings and examples, technical solution of the present invention is described in detail.
Embodiment 1 prepares azotized carbon nano line
1, material and instrument: dicyandiamide, sodium hydroxide, bag filter, Muffle furnace, IKA temperature control stirring device, the silent winged pure water system of match
System；
2, method: weighing 5g dicyandiamide and be put into crucible, and crucible is put into 550 DEG C of high-temperature process 4h in Muffle furnace, then certainly
It is so cooled to room temperature, product is ground to obtain CN powder with agate mortar.It weighs 300mgCN powder and is added to 50mL with magneton
In round-bottomed flask, 20mLNaOH solution (concentration 3mol/L) then is added into flask, by the mixed liquor in 70 DEG C of oil baths
Stir 6h.After reaction, dispersion liquid is fitted into the bag filter of 3500Da molecular cut off, with deionized water dialysis into
Property.
3, result: the azotized carbon nano line of uniform stable dispersion has been prepared, as shown in Figure 1, being seen with transmission electron microscope
Its pattern is examined, shows to be successfully prepared a few micrometers of wide about 10-20nm long of nanofiber.
Embodiment 2 prepares azotized carbon nano line
Essentially the same with embodiment 1, different is, the NaOH solution concentration is 0.5mol/L, the oil bath temperature
Degree is 80 DEG C, and the molecular cut off 1000Da of the bag filter, the azotized carbon nano line being prepared is the same as embodiment 1.
Embodiment 3 prepares azotized carbon nano line
Essentially the same with embodiment 1, different is, the NaOH solution concentration is 8mol/L, the oil bath temperature
It is 60 DEG C, the molecular cut off 5000Da of the bag filter, the azotized carbon nano line being prepared is described to be prepared
Azotized carbon nano line is the same as embodiment 1.
The preparation of 4 humidity sensor of embodiment
5mg/ml azotized carbon nano line dispersion liquid 0.2mL and carbon nanotube 1mg prepared by embodiment 1 is mixed, and ultrasound makes
It is uniformly compound, and 5 μ l is taken to be added drop-wise to the golden interdigital electrode surface cleaned, and is humidity sensor after dry.
The preparation of 5 humidity sensor of embodiment
5mg/ml azotized carbon nano line dispersion liquid 0.05mL and graphene 1mg prepared by embodiment 2 is mixed, and ultrasound makes it
It is uniformly compound, it takes 5 μ l to spray to the carbon interdigital electrode surface cleaned, is humidity sensor after dry.
The preparation of 6 humidity sensor of embodiment
5mg/ml azotized carbon nano line dispersion liquid 1mL and carbon black 1mg prepared by embodiment 3 is mixed, and ultrasound makes it uniformly
It is compound, it takes 5 μ l to be spun to the silver-colored interdigital electrode surface cleaned, is humidity sensor after dry.
The preparation of 7 humidity sensor of embodiment
5mg/ml azotized carbon nano line dispersion liquid 0.5mL and carbon nanotube 1mg prepared by embodiment 1 is mixed, and ultrasound makes
It is uniformly compound, and 5 μ l is taken to be added drop-wise to the platinum interdigital electrode surface cleaned, and is humidity sensor after dry.
Current-voltage (I-V) curve and humidity-sensitive material of 8 humidity sensor of embodiment under different humidity are in different humidity
Under resistance variations figure
1, instrument: GamryReference600 electrochemical workstation；
2, material: golden interdigital electrode (Micrux), azotized carbon nano line, carbon nanotube, the concentrated sulfuric acid, saturation LiCl solution,
It is saturated MgCl2Solution is saturated Mg (NO3)2Solution is saturated NaCl solution, is saturated KCl solution, deionized water.
3, humidity sensor prepared by embodiment 4 is placed in different saturated solutions (saturation LiCl solution, saturation
MgCl2Solution is saturated Mg (NO3)2Solution, be saturated NaCl solution, be saturated KCl solution) closed container top, with obtain not
Same ambient humidity, humidity sensing element are connected by conducting wire with the external world.It is subsequently attached on electrochemical workstation, passes through
Linear sweep voltammetry tests I-V curve, and scanning range is 0.3V to -0.3V, and sweeping speed is 50mV/s.
4, result: being shown in Fig. 2, obtains the I-V curve under varying environment humidity.As shown in Figure 1, I-V curve is a process
The straight line of origin shows that material shows typical Ohmic resistance behavior.With the raising of relative humidity, electric current becomes smaller, will not
It is converted to resistance with the electric current under humidity, as shown in figure 3, the resistance and ambient humidity of material are presented within the scope of 0-100%RH
Good corresponding relationship out.
The quick response current versus time curve of 9 humidity sensor of embodiment
1, instrument: GamryReference600 electrochemical workstation；
2, material: golden interdigital electrode (Micrux), azotized carbon nano line, carbon nanotube, high pure air, deionized water.
3, the humidity sensor is placed on the channel that high-purity gas passes through by the humidity sensor prepared using embodiment 4
In, and be connected with electrochemical workstation.Taking a small amount of humidity in the closed container for holding deionized water with syringe is 100%RH
Air, fast injection to place sensing element channel front, form a pulse signal.It is tested by timing Amperometric
Constant voltage 0.3V, sampling time interval 0.001s is arranged in I-t curve.
4, result: being shown in Fig. 4, and when there is humid air as pulse signal, sensing material resistance increases, under electric current is quick
Drop, then restores, the response time shows good reproducibility in 50ms or so.
The stability of 10 humidity sensor of embodiment
1, instrument: GamryReference600 electrochemical workstation；
2, material: golden interdigital electrode (Micrux), azotized carbon nano line, carbon nanotube, high pure air, deionized water.
3, the humidity sensor is placed on the closed environment of different humidity by the humidity sensor prepared using embodiment 4
In, control ambient humidity switches between 5%RH and 55%RH, tests I-t curve by timing Amperometric, constant voltage is arranged
0.001V, sampling time interval 0.1s.
4, result: being shown in Fig. 5, and initial environment humidity is 5%RH, and when humidity increases to 55%RH, electric current rapid decrease is simultaneously
It keeps stablizing, when switching back into 5%RH, electric current is restored to initial current level again, and so several times, humidity sensor shows circulation
Good stability and repeatability out.
The breathing detection current versus time curve of 11 humidity sensor of embodiment
1, instrument: GamryReference600 electrochemical workstation；
2, material: golden interdigital electrode (Micrux), azotized carbon nano line, carbon nanotube；
3, the humidity sensor prepared using embodiment 4, by the humidity sensor be fixed on test mask on and with electrification
It learns work station to be connected, allows subject personnel to take test mask, adjust electrode position.I-t curve is tested by timing Amperometric,
Constant voltage 0.3V, sampling time interval 0.001s are set.
4, result: being shown in Fig. 6, when the personnel of subject breathing, contains hydrone in exhaled gas, air-flow passes through sensing element
When, cause resistance to increase electric current decline, so as to detect the respiratory state of subject personnel.It can be seen from the figure that this method
It not only can detecte the information that traditional breathing detection equipment obtains, such as respiratory rate, depth of respiration, and due to the sensing
The faster response speed of device obtains the breathing I-t curve of higher resolution to monitor the details of the process of breathing, these information
There is important relation with respiratory disorders such as asthma, pneumonia and disordered breathings, medically the judgement of disease is needed by a variety of
Means of testing Combining diagnosis provides possibility for the measurement of the breathing of more details and the accurate medical treatment of respiratory disorder.
Obviously, the above embodiment is merely an example for clearly illustrating the present invention, and is not to of the invention
The restriction of embodiment.For those of ordinary skill in the art, it can also be made on the basis of the above description
Its various forms of variation or variation, there is no necessity and possibility to exhaust all the enbodiments, these changes extended out
Change or change and is also among protection scope of the present invention.
Claims (10)
1. a kind of resistance type humidity sensor of quick response, which is characterized in that the resistance type humidity sensor utilizes surface
Rich in hydroxyl, amino, carboxyl or the two-dimensional material for containing other hydrophilic radicals as active material, pass through drop coating, spraying or rotation
Coating method deposits to interdigital electrode surface, after drying to obtain the final product.
2. a kind of resistance type humidity sensor of quick response according to claim 1, which is characterized in that the active matter
Matter is azotized carbon nano line, carbon nanotube or one or more of graphene or carbon black.
3. a kind of resistance type humidity sensor of quick response according to claim 1, which is characterized in that the interdigital electricity
Extremely carbon interdigital electrode, golden interdigital electrode, silver-colored interdigital electrode or platinum interdigital electrode.
4. the preparation method of the resistance type humidity sensor of the described in any item quick responses of claim 1 ~ 3, which is characterized in that
The following steps are included:
It prepares azotized carbon nano line: nitridation carbon dust and sodium hydroxide solution being mixed, which are put into round-bottomed flask,
1-24h is stirred in 60 DEG C of -80 DEG C of oil baths, after reaction, reaction product is fitted into bag filter, with deionized water dialysis into
Property, the azotized carbon nano line hydrolyzed；
The preparation of humidity sensor: azotized carbon nano line dispersion liquid and conductive carbon material are mixed, and ultrasound keeps it uniformly compound, dilute
It releases 5-20 times and is added drop-wise to the interdigital electrode surface cleaned, be humidity sensor after dry.
5. the preparation method of the resistance type humidity sensor of quick response according to claim 4, which is characterized in that described
Sodium hydroxide solution 0.5-8mol/L.
6. the preparation method of the resistance type humidity sensor of quick response according to claim 4, which is characterized in that described
The conductive carbon material of step 2 and the mass volume ratio of azotized carbon nano line dispersion liquid are 1:0.05-1mg/mL.
7. application of the resistance type humidity sensor of the described in any item quick responses of claim 1 ~ 3 in Humidity Detection.
8. application according to claim 4, which is characterized in that connect the resistance type humidity sensor of the quick response
Resistance testing device applies voltage, passes through the variation of the variation monitoring ambient humidity of material resistance.
9. application according to claim 5, which is characterized in that the resistance testing device is electrochemical workstation or number
Type multimeter.
10. application according to claim 4, which is characterized in that the application is by timing Amperometric or linear scan
Voltammetry applies a constant potential or linear potential to the resistance type humidity sensor of quick response, becomes from the electric current detected
Change the variation that material resistance value is calculated, to learn the variation of ambient humidity.
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| CN110849941A (en) * | 2019-12-17 | 2020-02-28 | 大连理工大学 | Preparation method of resistance-type humidity sensing device based on loose carbon structure and hydrophilic polymer material composition |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110568025A (en) * | 2019-09-24 | 2019-12-13 | 无锡物联网创新中心有限公司 | humidity sensor based on candle ash nanoparticle layer and preparation method thereof |
| CN110941213A (en) * | 2019-11-18 | 2020-03-31 | 无锡物联网创新中心有限公司 | Non-contact key system |
| CN110849941A (en) * | 2019-12-17 | 2020-02-28 | 大连理工大学 | Preparation method of resistance-type humidity sensing device based on loose carbon structure and hydrophilic polymer material composition |
| CN110849941B (en) * | 2019-12-17 | 2021-11-02 | 大连理工大学 | Preparation method of resistance-type humidity sensing device based on loose carbon structure and hydrophilic polymer material composition |
| CN111704155A (en) * | 2020-01-20 | 2020-09-25 | 中国石油大学(华东) | CeO (CeO)2/g-C3N4Humidity sensor of hybrid membrane and preparation method and application thereof |
| CN111704155B (en) * | 2020-01-20 | 2021-04-27 | 中国石油大学(华东) | CeO (CeO)2/g-C3N4Humidity sensor of hybrid membrane and preparation method and application thereof |
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