CN108414584A - A kind of preparation method of flexible, wearable moisture sensor and its application in breathing detection - Google Patents
A kind of preparation method of flexible, wearable moisture sensor and its application in breathing detection Download PDFInfo
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- CN108414584A CN108414584A CN201810180633.3A CN201810180633A CN108414584A CN 108414584 A CN108414584 A CN 108414584A CN 201810180633 A CN201810180633 A CN 201810180633A CN 108414584 A CN108414584 A CN 108414584A
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/121—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid for determining moisture content, e.g. humidity, of the fluid
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- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/08—Detecting, measuring or recording devices for evaluating the respiratory organs
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/08—Detecting, measuring or recording devices for evaluating the respiratory organs
- A61B5/0816—Measuring devices for examining respiratory frequency
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Abstract
The invention discloses a kind of preparation method of flexible, wearable moisture sensor and its applications in breathing detection.The preparation method comprises the following steps：1) it is that template in-situ polymerization aniline monomer obtains water-soluble polyaniline using macromolecular acid；2) flexible interdigital electrode is printed on a flexible substrate by inkjet printing technology；3) water-soluble polyaniline slurries are coated in flexible interdigital electrode surface and form flexible sensing film；4) lead is picked out by conductive silver paste and obtains flexible, wearable moisture sensor.Flexible, the wearable moisture sensor that the present invention obtains has overdelicate response performance and very strong stability for health detection, and detection is not necessarily to additional condition at ambient temperature, have the characteristics that environmentally protective, can be used for breathing detection and health medical treatment diagnostic field.
Description
Technical field
The invention belongs to technical field of polymer composite materials, and in particular to a kind of water-soluble polyaniline thin film flexible wet sensitive
The production method of sensor, which, which is applied to wearable breathing detection equipment, can realize the reality to health
When medical treatment detect.
Background technology
Humidity has been widely used for work as one very important reference index of environment by the development of recent decades
The fields such as industry, agricultural production, aerospace, electronics, meteorology.In recent years, flexible conductive film is because it can be with potential application to can wear
It wears, cause the research boom of numerous scholars in flexible electronic product and display equipment.It is soft derived from various flexible conductive films
Property, transparent electronics have been obtained for more and more applying, such as touch screen, electronic skin and can be worn strain transducer
The pulse analyzer etc. worn.Flexible, wearable moisture sensor can be with potential application to portable flexible electronic device
It shows in equipment, real-time, overdelicate ambient humidity monitoring is provided, timely and conveniently reflects human skin sweat and expiratory air
The content of specific objective object in body.In addition, the extensive use of flexible wearable may be implemented under human body different motion state
Effective detection of humidity, and the medical diagnosis to specific respiratory disease.
Conventional silica-base material and organic semiconductor is widely used for flexible electronic, but their low stability with
It is less flexible to significantly limit further practical application (bibliography：Nature,2004,432(7016):488-492；
Advanced Materials,2002,14(2):99-117).The non-flexible moisture sensor of tradition based on interdigital electrode,
It is difficult to meet requirement of the potential application to wearable integrated circuit, therefore, develops flexible, stable, the wide humidity of performance and respond model
It encloses, feel wet ability by force and the moisture sensor of dehumidification ability, long life is increasingly important.In order to overcome these limitations, H.Ryu
Et al. a kind of stretchable wet sensitive is prepared for by the polyaniline of the growth fold shape in dimethyl silicone polymer (PDMS) substrate
Sensor, tensility is good, and maximum tension deformation quantity can reach 40% (bibliography：RSC Adv.2014,4(4),
39767-39770；Nano Research,2017,10(6):1-13).Tran Quang Trung et al. be prepared for it is transparent, can
It stretches, wearable moisture sensor, response time 3.5s, recovery time 7s, maximum tension variable reaches 60%, repeats 1000
Wet sensitive performance is stablized after secondary, which may be implemented wearable detection human peripheral's environment also with PDMS substrates
Humidity, but it is not involved with health medical treatment diagnosis (bibliography：Nano Research,2017,10(6):1-13).
Invention content
The purpose of the present invention is to provide a kind of preparation method of flexible, wearable moisture sensor and its in breathing detection
In application.
A kind of production method of flexible, wearable moisture sensor, which is characterized in that include the following steps：
1) it is that template in-situ polymerization aniline monomer obtains water-soluble polyaniline using macromolecular acid；
2) flexible interdigital electrode is printed on a flexible substrate by inkjet printing technology；
3) water-soluble polyaniline slurries are coated in flexible interdigital electrode surface and form flexible sensing film；
4) lead is picked out by conductive silver paste and obtains flexible, wearable moisture sensor.
Preferably, the macromolecular acid described in step 1) is polystyrolsulfon acid or polyacrylic acid.
Preferably, the flexible substrates described in step 2) are PET substrate, polyimide substrate
Or any one in dimethyl silicone polymer.
Preferably, the painting method in step 3) is spread coating or spin-coating method.
A kind of breathing detection equipment, which is characterized in that use flexible, wearable moisture sensor system obtained by the above method
The wearable breathing detection equipment obtained.
Beneficial effects of the present invention：
1. the water-soluble polyaniline of the present invention obtained by polymer acid template is water-soluble good, synthetic method letter
Single, performance is stablized, and the flexible base material processability used is strong, at low cost, and the flexible sensor prepared has hypersensitive
Response performance and very strong stability.
2. the breathing detection equipment of the flexible sensor prepared using the present invention is with the breath size of breather, electric signal
Variation is apparent, and response restores sensitive, and detection is not necessarily to additional condition at ambient temperature, has the characteristics that green safe environmental protection.
Description of the drawings
Fig. 1 is the SEM figures of water-soluble polyaniline powder made from embodiment 1.
Fig. 2 is the response-recovery in 11%RH~95%RH humidity ranges at room temperature of sense film made from embodiment 1
Curve.
Fig. 3 is humidity hysteresis loop line of the sensing membrane made from embodiment 1 at room temperature in 11%RH~95%RH humidity ranges.
Fig. 4 is flexible wearable wet sensitive device and breath test data at room temperature made from embodiment 2.
Fig. 5 is wireless transmission test data of the flexible wearable sensor made from embodiment 2 under the conditions of human body is dressed.
Fig. 6 is flexible electrode of the embodiment 1 by PET substrate made from inkjet printing.
Specific implementation mode
Below in conjunction with the drawings and specific embodiments for the apparent explanation present invention, but it is not intended to limit the present invention.
Embodiment 1：
First by 3.5g polystyrolsulfon acids (PSSA) aqueous solution in beaker 25mL deionized waters are added, above-mentioned in 1a.
200 μ L aniline monomers are added in solution, stir 1h.The APS for weighing 54.7mg is added in 10mL deionized waters, is uniformly dissolved.
Then the acid solution of APS is poured into the mixed solution of polystyrolsulfon acid and aniline, is shaken up, be put into cold compartment of refrigerator, at 5 DEG C
Under conditions of react 8h.The solution of acquisition is added in a large amount of acetone, is filtered, it is clean using acetone rinsing, under room temperature
Vacuum drying for 24 hours, obtains polyaniline powder.
1b. prints interdigital electrode, size in polyethylene terephthalate (PET) substrate using inkjet printing technology
8mm × 6mm, 200 μm of electrode spacing.
1c. takes green powder sample prepared by 1a in the clean small mortar of agate, and rubber head dropper is drawn deionized water and added
Enter, being ground to sample clockwise with grinding pestle becomes uniform paste, and picking pastes with small brushes is uniformly applied to flexibility
Electrode area surfaces form thin and smooth coat, and naturally dry is placed under 95%RH humidity aging for 24 hours.
The senser element prepared in 1c is picked out lead by 1d. by conductive silver paste, is connected to wet sensitive measuring and analysing meter.
Water-soluble polyaniline conductive film prepared by the present embodiment 1 is assembled on moisture sensitive device and carries out moisture-sensitive energy survey
Examination.
Performance detection：Test method is saturated salt solution method of testing.
The supersaturated solution for preparing 6 kinds of different salt provides opposite humidity environment for next test.LiCl saturated salts
Solution, relative humidity 11%RH；MgCl2Saturated salt solution, relative humidity 33%RH；Mg(NO3)2Saturated salt solution,
Its relative humidity is 54%RH；NaCl saturated salt solutions, relative humidity 75%RH；KCl saturated salt solutions, relative humidity
For 85%RH；KNO3Saturated salt solution, relative humidity 95%RH.
By device sealing in wide-mouth bottle, baseline scan is carried out, test response recovery curve and humidity hysteresis loop line after stablizing, with
And the linear relationship under different frequency.Response is defined as S=Δs R/R0, wherein Δ R is the resistance changed under different humidity, R0
For the resistance under initial humidity.
Water-soluble polyaniline conductive film flexible sensor manufactured in the present embodiment is used for wet sensitive performance detection, Neng Goushi
Existing quick response and recovery, have good stability, such as Fig. 2；Humidity hysteresis loop line is drawn by the resistance test under different humidity gradient, such as
Fig. 3.
Embodiment 2
2a：Polyacrylic acid (PAA) solution is configured, is obtained secretly with reference to the method in-situ polymerization aniline monomer of 1a in embodiment 1
The water-soluble polyaniline powder of green.
2b：Referring to 1b steps in embodiment 1, inkjet printing is flexible in polyethylene terephthalate (PET) substrate
The interdigital electrode of substrate.
2c：In deionized water by the dirty-green powder prepared in 2a dissolving hairbrush is used referring to 1c steps in embodiment 1
It picks pastes and is uniformly applied to flexible electrode region surface and form thin and smooth coat, naturally dry is placed on 95%
Aging is for 24 hours under RH humidity.
2d：Referring to 1d steps in embodiment 1, the senser element of preparation is picked out into lead by conductive silver paste, is attached to mask
Detection such as Fig. 4 of respiratory disease is carried out above.
Water-soluble polyaniline conductive film manufactured in the present embodiment is assembled on moisture sensitive device and carries out moisture-sensitive energy test.
Performance detection：Test method is saturated salt solution method of testing.
The supersaturated solution for preparing 6 kinds of different salt provides opposite humidity environment for next test.LiCl saturated salts
Solution, relative humidity 11%RH；MgCl2Saturated salt solution, relative humidity 33%RH；Mg(NO3)2Saturated salt solution,
Its relative humidity is 54%RH；NaCl saturated salt solutions, relative humidity 75%RH；KCl saturated salt solutions, relative humidity
For 85%RH；KNO3Saturated salt solution, relative humidity 95%RH.
By device sealing in wide-mouth bottle, baseline scan is carried out, test response recovery curve and humidity hysteresis loop line after stablizing, with
And the linear relationship under different frequency.Response is defined as S=Δs R/R0, wherein Δ R is the resistance changed under different humidity, R0
For the resistance under initial humidity.
Device is fixed on mask, lead is connected to semiconductor test analyzer, test breathing law curve, such as Fig. 4.
By test it was found that when taking mask breathing, electric current obviously rises, with the increase of even breathing number, stability
Well；Secondly it can be found that a rule, each respiratory intervals time is about 4s.Respiratory intensity is different, and electric signal accordingly also becomes
Change obviously, as shown in Fig. 4, shallow breathing, eupnea and deep breathing sensitivity difference are notable, this can be used as health medical treatment
The important evidence of diagnosis.
Embodiment 3
3a：Polystyrolsulfon acid (PSSA) aqueous solution is configured, according to the method in-situ polymerization aniline monomer of 1a in embodiment 1
Obtain the water-soluble polyaniline powder of dirty-green.
3b：Referring to 1b steps in embodiment 1, the interdigital electricity of inkjet printing flexible substrates in polyimides (PI) substrate
Pole.
3c：It in deionized water by the dirty-green powder dissolving of preparation is picked with hairbrush referring to 1c steps in embodiment 1
Pastes is uniformly applied to flexible electrode region surface and forms thin and smooth coat, and it is wet that naturally dry is placed on 95%RH
The lower aging of degree is for 24 hours.
3d：Referring to 1d steps in embodiment 1, the senser element of preparation is picked out into lead by conductive silver paste, is connected to wet
The wet sensitive performance data of flexible sensor is tested above quick detecting instrument；Device is connected to above mask to frequency of not shared a common fate
The detection of rate and different respiratory intensities.
Water-soluble polyaniline conductive film manufactured in the present embodiment is assembled on moisture sensitive device and carries out moisture-sensitive energy test.
Performance detection：Test method is saturated salt solution method of testing.
The supersaturated solution for preparing 6 kinds of different salt provides opposite humidity environment for next test.LiCl saturated salts
Solution, relative humidity 11%RH；MgCl2Saturated salt solution, relative humidity 33%RH；Mg(NO3)2Saturated salt solution,
Its relative humidity is 54%RH；NaCl saturated salt solutions, relative humidity 75%RH；KCl saturated salt solutions, relative humidity
For 85%RH；KNO3Saturated salt solution, relative humidity 95%RH.
By device sealing in wide-mouth bottle, baseline scan is carried out, test response recovery curve and humidity hysteresis loop line after stablizing, with
And the linear relationship under different frequency.Response is defined as S=Δs R/R0, wherein Δ R is the resistance changed under different humidity, R0
For the resistance under initial humidity.
Water-soluble polyaniline conductive film flexible sensor manufactured in the present embodiment is used for wet sensitive performance detection, Neng Goushi
Existing quick response and recovery, have good stability；Humidity hysteresis loop line is drawn by the resistance test under different humidity gradient.
Device is fixed on mask, lead is connected to semiconductor test analyzer, test breathing law curve.Pass through survey
It was found that when taking mask breathing, electric current obviously rises, and with the increase of even breathing number, has good stability for examination；Its
Secondary to can be found that a rule, each respiratory intervals time is about 3.8s.Respiratory intensity is different, and electric signal accordingly also changes bright
Aobvious, shallow breathing, eupnea and deep breathing sensitivity difference are notable, this important evidence that can be diagnosed as health medical treatment.
Embodiment 4
4a：Polystyrolsulfon acid (PSSA) aqueous solution is configured, according to the method in-situ polymerization aniline monomer of 1a in embodiment 1
Obtain the water-soluble polyaniline powder of dirty-green.
4b：Interdigital electrode is printed in dimethyl silicone polymer (PDMS) flexible substrates.184 silicon rubbers of DOW CORNING SYLGARD
Glue is made of basis (A) and curing agent (B), by 10:1 mass ratio mixes, and 20 DEG C~150 DEG C solidification 1h, obtaining flexibility can
Dimethyl silicone polymer (PDMS) substrate of stretching.Referring to 1b steps in embodiment 1, in dimethyl silicone polymer (PDMS) substrate
The interdigital electrode of upper inkjet printing flexible substrates.
4c：It in deionized water by the dirty-green powder dissolving of preparation is picked with hairbrush referring to 1c steps in embodiment 1
Pastes is uniformly applied to flexible electrode region surface and forms thin and smooth coat, and it is wet that naturally dry is placed on 95%RH
The lower aging of degree is for 24 hours.
4d：Referring to 1d steps in embodiment 1, the senser element of preparation is picked out into lead by conductive silver paste, is connected to wet
The wet sensitive performance data of flexible sensor is tested above quick detecting instrument；Device is connected to above mask to frequency of not shared a common fate
The detection of rate and different respiratory intensities.
Water-soluble polyaniline conductive film manufactured in the present embodiment is assembled on moisture sensitive device and carries out moisture-sensitive energy test.
Performance detection：Test method is saturated salt solution method of testing.
The supersaturated solution for preparing 6 kinds of different salt provides opposite humidity environment for next test.LiCl saturated salts
Solution, relative humidity 11%RH；MgCl2Saturated salt solution, relative humidity 33%RH；Mg(NO3)2Saturated salt solution,
Its relative humidity is 54%RH；NaCl saturated salt solutions, relative humidity 75%RH；KCl saturated salt solutions, relative humidity
For 85%RH；KNO3Saturated salt solution, relative humidity 95%RH.
By device sealing in wide-mouth bottle, baseline scan is carried out, test response recovery curve and humidity hysteresis loop line after stablizing, with
And the linear relationship under different frequency.Response is defined as S=Δs R/R0, wherein Δ R is the resistance changed under different humidity, R0
For the resistance under initial humidity.
Water-soluble polyaniline conductive film flexible sensor manufactured in the present embodiment is used for wet sensitive performance detection, Neng Goushi
Existing quick response and recovery, have good stability；Humidity hysteresis loop line is drawn by the resistance test under different humidity gradient.
Device is fixed on mask, lead is connected to semiconductor test analyzer, test breathing law curve.Pass through survey
It was found that when taking mask breathing, electric current obviously rises, and with the increase of even breathing number, has good stability for examination；Its
Secondary to can be found that a rule, each respiratory intervals time is about 4s.Respiratory intensity is different, and accordingly also variation is apparent for electric signal,
Shallow breathing, eupnea and deep breathing sensitivity difference are notable, this important evidence that can be diagnosed as health medical treatment.
Embodiment 5：
5a：Referring to 1a steps in embodiment 1, the water-soluble polyaniline powder of dirty-green is obtained.
5b：Referring to 1b steps in embodiment 1, inkjet printing is flexible in polyethylene terephthalate (PET) substrate
The interdigital electrode of substrate.
5c：Referring to 1c steps in embodiment 1, the dirty-green powder of preparation is dissolved in a certain amount of deionized water, use is even
Water-soluble polyaniline solution is spin-coated on flexible electrode region by glue machine, and naturally dry is placed under 95%RH humidity aging for 24 hours.
5d：Referring to 1d steps in embodiment 1, the senser element of preparation is picked out into lead by conductive silver paste, is connected to wet
The wet sensitive performance data of flexible sensor is tested above quick detecting instrument；Device is connected to above mask to frequency of not shared a common fate
The detection of rate and different respiratory intensities.
Performance detection：Test method is saturated salt solution method of testing.
The supersaturated solution for preparing 6 kinds of different salt provides opposite humidity environment for next test.LiCl saturated salts
Solution, relative humidity 11%RH；MgCl2Saturated salt solution, relative humidity 33%RH；Mg(NO3)2Saturated salt solution,
Its relative humidity is 54%RH；NaCl saturated salt solutions, relative humidity 75%RH；KCl saturated salt solutions, relative humidity
For 85%RH；KNO3Saturated salt solution, relative humidity 95%RH.
By device sealing in wide-mouth bottle, baseline scan is carried out, test response recovery curve and humidity hysteresis loop line after stablizing, with
And the linear relationship under different frequency.Response is defined as S=Δs R/R0, wherein Δ R is the resistance changed under different humidity, R0
For the resistance under initial humidity.
Water-soluble polyaniline conductive film flexible sensor manufactured in the present embodiment is used for wet sensitive performance detection, Neng Goushi
Existing quick response and recovery, have good stability；Humidity hysteresis loop line is drawn by the resistance test under different humidity gradient.It can send out
Existing, different device methods processed have an impact wet sensitive performance, the layer/polyaniline conductive film that spin coating obtains evenly, wet sensitive stability
It is better than the device brushed and prepared.
Simple simulation test has been carried out to apnea syndrome using the flexible wearable sensor of preparation, has found effect
Fruit is apparent, and corresponding and recovery time is short, and performance is stablized.The disease is related with respiratory rate and respiratory intensity, passes through breathing
Non-electrical signal is converted into electric signal output and shown, may be implemented to human body by the difference of time interval or the difference of respiratory intensity
The real-time detection of respiratory health situation, this is provided to further senser element is applied in portable, wearable circuit
Possibility has a extensive future.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, however the present invention is not limited thereto.For those skilled in the art, in the essence for not departing from the present invention
In the case of refreshing and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (5)
1. a kind of production method of flexible, wearable moisture sensor, which is characterized in that include the following steps：
1) it is that template in-situ polymerization aniline monomer obtains water-soluble polyaniline using macromolecular acid；
2) flexible interdigital electrode is printed on a flexible substrate by inkjet printing technology；
3) water-soluble polyaniline slurries are coated in flexible interdigital electrode surface and form flexible sensing film；
4) lead is picked out by conductive silver paste and obtains flexible, wearable moisture sensor.
2. a kind of production method of flexible, wearable moisture sensor according to claim 1, which is characterized in that step
1) the macromolecular acid described in is polystyrolsulfon acid or polyacrylic acid.
3. a kind of production method of flexible, wearable moisture sensor according to claim 2, which is characterized in that step
2) flexible substrates described in are in PET substrate, polyimide substrate or dimethyl silicone polymer
Any one.
4. a kind of production method of flexible, wearable moisture sensor according to claim 3, which is characterized in that step
3) painting method in is spread coating or spin-coating method.
5. a kind of breathing detection equipment, which is characterized in that using flexible, wearable described in any one in claim 1-4
Wearable breathing detection equipment made from moisture sensor.
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| CN110856678A (en) * | 2018-08-22 | 2020-03-03 | 胡衍荣 | Intelligent moisture absorption sensing material, humidity management system and application thereof |
| CN109613075A (en) * | 2019-01-07 | 2019-04-12 | 电子科技大学 | A kind of flexible humidity sensor and preparation method thereof based on fibroin |
| CN110455871A (en) * | 2019-07-25 | 2019-11-15 | 湘潭大学 | A kind of bimodulus humidity sensor and preparation method thereof based on nickel iodide |
| CN110440996A (en) * | 2019-08-16 | 2019-11-12 | 哈工程先进技术研究院(招远)有限公司 | A kind of dipping detector, manufacturing method and its working method |
| CN111657862A (en) * | 2020-06-08 | 2020-09-15 | 浙江理工大学 | Washable integrated flexible fabric array sensor and method thereof and intelligent mattress |
| CN112924316A (en) * | 2021-02-09 | 2021-06-08 | 中国石油大学(华东) | Humidity-sensitive film based on chitosan and polypyrrole and preparation method and application thereof |
| CN112924316B (en) * | 2021-02-09 | 2023-03-31 | 中国石油大学(华东) | Humidity-sensitive film based on chitosan and polypyrrole and preparation method and application thereof |
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