CN108490051A - A kind of flexible miniature is from driving gas at normal temperature sensor and preparation method thereof - Google Patents
A kind of flexible miniature is from driving gas at normal temperature sensor and preparation method thereof Download PDFInfo
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- CN108490051A CN108490051A CN201810489743.8A CN201810489743A CN108490051A CN 108490051 A CN108490051 A CN 108490051A CN 201810489743 A CN201810489743 A CN 201810489743A CN 108490051 A CN108490051 A CN 108490051A
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- gas
- temperature sensor
- normal temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/307—Disposable laminated or multilayered electrodes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
Abstract
The invention discloses a kind of flexible miniatures to drive gas at normal temperature sensor and preparation method thereof certainly, belong to the preparing technical field of flexible electronic device, including flexible substrate, positioned at the flexible miniature capacitor based on film of poly pyrrole electrode material of substrate and the gas sensor based on multi-walled carbon nanotube/polyaniline composite material；Wherein, the capacitor collection liquid body is made of circular electrode and parallel pole respectively with gas sensors electrode structure, and film of poly pyrrole is deposited on circular electrode, and multi-walled carbon nanotube/polyaniline composite material is coated between parallel electrode.Power supply unit used in the present invention is ultracapacitor, and small, charging rate is fast, safe and convenient, can carry.Film of poly pyrrole prepared by electrodeposition process can form one layer of fine and close ultra-thin film in collection liquid surface, not only save material, but also can reduce contact resistance.The sensor at normal temperatures can be detected the concentration of alcohol gas, not need additional heating system.
Description
Technical field
The invention belongs to the preparing technical fields of flexible electronic device, and in particular to a kind of flexible miniature is from driving room temperature gas
Body sensor and preparation method thereof.
Background technology
In recent years, due to the rapid development of nano-fabrication technique, electronic device is towards flexibility, micromation, integrated
Direction shows powerful growth momentum during advancing, and has widened application field of the electronic device in mankind's daily life
And the form of expression.In numerous electronic devices, gas sensor plays an important role in occupation of important position, it can be with
The concentration of inflammable, the explosive even toxic gas generated in the monitoring daily production and living of people in real time.Therefore, it prepares a kind of micro-
Type portable energy storage-gas sensing device integrated device is particularly important.
Energy stores supply unit of the micro super capacitor (micro- capacitance) as flexible integration unit, with lithium ion battery
It compares, has the characteristics that power density is high, service life is long, the charging time is short, environmentally protective.Micro- capacitance mainly by three parts
Composition：Collector, electrode material and electrolyte.Wherein, it is to improve to improve the effective occupied area of electrode material on a current collector
The breach of capacitor performance.Electrode material is uniformly distributed and is mainly the following method on substrate：1, spraying/dipping
Method, the membranaceous electrode material that this method is formed is in uneven thickness, can cause the waste to material；2, spin-coating method, this method
Although the more uniform membranaceous electrode material of layer can be formed, a disconnecting is belonged between collector and electrode material
It touches, causes electric conductivity poor, the internal resistance of device is larger；3, print process, although this method can form one layer of fine and close film,
But the slurry that preparation can print is narrow to the selection of material harsh, cost is higher.
Functional unit of the gas sensor as integrated system can be detected effectively poisonous and harmful in air in real time
Gas concentration provides safeguard to keep the safety in production with life.Ethyl alcohol is as a kind of important organic solvent, in industry, medicine, paper
Towel, synthesis of perfume etc. are widely used.However, ethyl alcohol is also the main component of food and drug, and all the time, mistake
Degree, which is drunk, causes the accident of threat to life safety commonplace.Therefore, it is very to develop a kind of portable ethanol sensor
Significant.But common gas sensor is required for working at high temperature mostly now, and the sensitivity of sensor compared with
Low, response speed is also slow, it is difficult to realize efficiently rapidly gas-monitoring function.
In conclusion preparing the micro- capacitance of high-performance flexible at present, there are still certain difficulties with gas at normal temperature sensor aspect
Degree, it is necessary to develop a kind of novel flexible miniature from driving gas at normal temperature sensor integration system, with the production of further satisfactions
Living needs.
Invention content
The present invention, can be in view of the above-mentioned problems, provide a kind of flexible miniature from driving gas at normal temperature sensor integration system
Continuous room temperature, which quickly detects, to be realized to alcohol gas.The variation that itself electric property is shown as by perceiving gas concentration, into
And applied to the variation of monitoring human body alcohol content in real time.
The present invention is achieved through the following technical solutions：
A kind of flexible miniature driving gas at normal temperature sensor, including substrate, the capacitor collection liquid body positioned at substrate certainly
With gas sensors electrode structure, film of poly pyrrole and multi-walled carbon nanotube/polyaniline composite material；Wherein, the capacitance
Device collector is made of with gas sensors electrode structure circular electrode and parallel pole two parts, and film of poly pyrrole is deposited on
On circular electrode, multi-walled carbon nanotube/polyaniline composite material is coated between parallel electrode.
Further, the spacing of the circular electrode raceway groove is 100 μm.
Further, the distance between described parallel pole is 150 μm.
Further, the structure of the parallel pole is box-shaped, interdigitation or circle.
A kind of flexible miniature drives the preparation method of gas at normal temperature sensor certainly, is as follows：
(1), substrate is cleaned in ethyl alcohol and deionized water respectively, is then dried；
(2), spin coating photoresist, thickness 100nm-200nm on substrate, put mask plate, then photoetching, development are plated
Golden film is finally removed with acetone to get to capacitor collection liquid body and gas sensors electrode structure；Wherein, the structure of mask plate
It is made of circular electrode and parallel pole two parts；
(3), it is 30 μm -50 that electrodeposition process in-situ deposition film of poly pyrrole, thickness are used on the circular electrode after photoetching
μm, after having deposited film of poly pyrrole, solid electrolyte is coated, thickness is 500 μm -800 μm；2 parallel poles after photoetching
Between spin coating multi-walled carbon nanotube/polyaniline composite material, thickness be 200 nm-300nm.
Further, the thickness of the gold-plated film described in step (2) is at least 50nm.
Further, the time of the electro-deposition described in step (3) is 4-5min, and voltage 0-0.8V, method is that cycle lies prostrate
An Fa.
Further, it according to volume ratio is 5 that the polypyrrole described in step (3), which is by pyrrole monomer and sodium perchlorate,：100
It is configured to.
Further, the spin coating described in step (3), rotating speed are 500 revolution per seconds, and number is 2 times.
Further, multi-walled carbon nanotube/polyaniline composite material described in step (3), is prepared via a method which
It arrives, is as follows：
First, by multi-walled carbon nanotube and aniline monomer according to 1：2 mass ratio is added in 1M/L in perchloric acid solution,
It is stirred 30 minutes at 0 DEG C；Then, into above-mentioned solution with volume ratio 3:1 is added dropwise density as 6*10-3The ammonium persulfate of kg/L is molten
Liquid stirs mixed solution 24 hours under the conditions of 0 DEG C, and the polyaniline nano-rod array after polymerization is equably grown in carbon nanometer
Guan Shang；Finally, the multi-walled carbon nanotube polyaniline nano-composite material that will be obtained, is washed with deionized water, methanol and ethyl alcohol respectively
It washs, the nano material after washing is dried in vacuo 24 hours at 60 DEG C.
Further, the volume ratio of the mixed liquor and perchloric acid solution of the multi-walled carbon nanotube and aniline monomer is 1：
5。
Compared with prior art, advantages of the present invention is as follows：
(1) power supply unit used in the present invention is ultracapacitor, and small, charging rate is fast, safe and convenient, can be with
It carries.(2) film of poly pyrrole prepared by electrodeposition process can be formed one layer fine and close ultra-thin thin in collection liquid surface
Film not only saves material, but also can reduce contact resistance.(3) mask plate used in, the existing circular electrode for being suitable for capacitor
Structure, and have the parallel square electrode of matching gas sensor, both electrodes can simultaneously be obtained by a step photoetching process.
(4) ethanol sensor at normal temperatures can be detected the concentration of alcohol gas, not need additional heating system.
(5) it is 2cm*4cm, substrate PET that flexible super capacitor prepared by, which integrates room temperature ethanol sensor integrated system total size,
It still can be worked normally in the case where generating certain deformation, there is great application potential in terms of wearable device.
Description of the drawings
Fig. 1 is the structural schematic diagram that a kind of flexible miniature of the present invention drives the electrode structure of gas at normal temperature sensor certainly；
Wherein, (a) is the optical structure chart of electrode structure, is (b) optical structure chart of the PET sheet of the electrode after photoetching；
Fig. 2 is the deposition process figure using electrodeposition process in-situ deposition of the present invention；
Wherein, platinum electrode 1, working electrode 2, reference electrode 3；
Fig. 3 is that the flexible miniature of the present invention drives the structural schematic diagram of gas at normal temperature sensor certainly；
Fig. 4 is the SEM figures for the film of poly pyrrole that the present invention uses；
Wherein, (a) is film of poly pyrrole exterior view, is (b) film of poly pyrrole cross-sectional view；
Fig. 5 is the SEM figures of multi-walled carbon nanotube/polyaniline composite material of the present invention；
Fig. 6 is that a kind of flexible miniature of the present invention carries out cyclic voltammetric and constant current charge-discharge from driving gas at normal temperature sensor
The chemical property figure of test；
Wherein, (a) is cyclic voltammetry curve of the flexible miniature capacitor devices under different scanning rates, is (b) flexibility
Constant current charge-discharge curve of the button capacitor device under different current densities.
Fig. 7 is that a kind of flexible miniature of the present invention tests its spirit to ethyl alcohol at normal temperatures from driving gas at normal temperature sensor
Acuity curve.
Fig. 8 is chemical property when a kind of flexible miniature of the present invention carries out differently curved from driving gas at normal temperature sensor
Change curve.
Specific implementation mode
The present invention is described further below in conjunction with the accompanying drawings.
Embodiment 1
A kind of flexible miniature driving gas at normal temperature sensor, including substrate, the capacitor collection liquid body positioned at substrate certainly
With gas sensors electrode structure, film of poly pyrrole and multi-walled carbon nanotube/polyaniline composite material；Wherein, the capacitance
Device collector is made of with gas sensors electrode structure circular electrode and parallel pole two parts, and film of poly pyrrole is deposited on
On circular electrode, multi-walled carbon nanotube/polyaniline composite material is coated on parallel electrode.
Further, the spacing of the circular electrode raceway groove is 100 μm.
Further, the distance between described parallel pole is 150 μm.
Further, the structure of the parallel pole is box-shaped, interdigitation or circle.
A kind of flexible miniature drives the preparation method of gas at normal temperature sensor certainly, is as follows：
(3), it is 30 μm -50 that electrodeposition process in-situ deposition film of poly pyrrole, thickness are used on the circular electrode after photoetching
μm, after having deposited film of poly pyrrole, solid electrolyte is coated, thickness is 500 μm -800 μm；2 parallel poles after photoetching
Upper spin coating multi-walled carbon nanotube/polyaniline composite material, thickness are 200 nm-300nm.
A. the cleaning of plastics PET：The plastic sheet for cutting one section of 2*4 centimetres of size, surpasses respectively in ethyl alcohol and deionized water
Sound cleans 20 minutes, is then placed in 60 degrees Celsius of baking ovens and dries.
B. circular electrode is prepared with parallel square electrode：First, one layer photoresist of spin coating, thickness are on PET sheet
100nm, 100 degrees Celsius dry 5 minutes.Then, it uses pattern shown in Fig. 1 (a) to carry out photoetching as mask plate, carries out later
Development, developing time 9s.Plated film is carried out after development, the thickness of plated film is 50nm, is removed with acetone after plated film, i.e.,
Circular electrode shown in Fig. 1 (b) and parallel square electrode can be obtained.
C. the preparation of electro-deposition polypyrrole solution：According to volume ratio it is 5 by pyrrole monomer and sodium perchlorate：100 are configured to
The solution of 20ml is stirred at room temperature to solution and clarifies.
D. electrochemical deposition process：The solution prepared in c importing is poured into electrolytic cell, as shown in Figure 2.Then electrification is used
It learns work station (CHI 760e series) to be deposited, method is cyclic voltammetry, and deposition voltage 0.8V, sedimentation time is 5 points
Clock, deposition thickness are 30 μm.
E. spin coating multi-walled carbon nanotube/polyaniline gas sensitive between the parallel pole shown in the lower sections Fig. 1 (b), rotating speed
For 500 revolution per seconds, spin coating 2 times.Spin coating next time could be carried out after needing equal solvent to volatilize completely after the completion of each spin coating process, it is thick
Degree is 200nm.
2 electrochemical property test of embodiment
When test, the positive electrode of electrochemical workstation is clipped in two parallel square electrodes of device respectively with negative electrode
On, then carry out cyclic voltammetry and constant current charge-discharge test respectively, environment temperature when test is 25 DEG C.
By Fig. 6 (a) it is found that the optimal voltage range of a kind of flexible miniature of the present invention from driving gas at normal temperature sensor is
0~0.8V.By the test of different voltages sweep speed (0.1 volt per second~3 volts per second), counted maximum area specific capacitance is counted
Value is 45mF/cm2.Meanwhile capacitor has carried out the constant currents of different current densities within the scope of the voltage window of 0~0.8V and has filled
Discharge test, such as Fig. 6 (b).It is 0.1mA/cm in current density2, the discharge time of capacitor can reach 850 seconds, show
Excellent chemical property.Subsequently to have laid a good foundation to gas sensor power supply.
3 electrochemical property test of embodiment
As shown in Figure 7,1.15 can be reached to the sensitivity of the ethyl alcohol of 50ppm under the gas sensor room temperature, resistance value
Increase with the increase of concentration of alcohol.It is 13s, recovery time 4.5s to the response time of ethyl alcohol under room temperature.This is under room temperature
Quickly detection concentration of alcohol provides possibility.
4 bending property of embodiment is tested
Flexible miniature is placed on from driving gas at normal temperature sensor on the device that one can be bent, as shown in Figure 8.It utilizes
Bending apparatus in Fig. 8 tests the change curve and stability of its electric property under differently curved angle.Wherein, sensor by
Initial angle is bent to different angle, then restores again to initial.
As can be seen from Figure 8, the maximum bending angle of the sensor is 120 degree, when carrying out constant current charge-discharge test,
Curve obtained is consistent substantially with the constant current charge-discharge curve before bending, has absolutely proved device in chemical property with curved
The variation of bent angle does not occur significantly to change, and illustrates that the sensor has good mechanical bend performance, this makes the biography
Sensor has that room temperature ethanol sensor integrated system is small, quality is small with portable characteristic, takes offence body for wearable self-powered
The further practical application of sensor provides guarantee.
Claims (10)
1. a kind of flexible miniature drives gas at normal temperature sensor certainly, which is characterized in that including flexible substrate, positioned at substrate
Polypyrrole ultracapacitor and the gas sensor based on multi-walled carbon nanotube/polyaniline composite material；Wherein, the capacitance
Device collector is made of circular electrode and parallel pole respectively with gas sensors electrode structure, and film of poly pyrrole is deposited on
On circular electrode, multi-walled carbon nanotube/polyaniline composite material is coated between parallel electrode.
2. a kind of flexible miniature as described in claim 1 drives gas at normal temperature sensor certainly, which is characterized in that the circle
The spacing of electrode raceway groove is 100 μm.
3. a kind of flexible miniature as described in claim 1 drives gas at normal temperature sensor certainly, which is characterized in that described is parallel
The distance between electrode is 150 μm.
4. a kind of flexible miniature as described in claim 1 drives gas at normal temperature sensor certainly, which is characterized in that described is parallel
The structure of electrode is box-shaped.
5. a kind of flexible miniature as described in claim 1 is from the preparation method for driving gas at normal temperature sensor, specific steps are such as
Under：
(1), flexible substrate is cleaned in ethyl alcohol and deionized water respectively, is then dried；
(2), spin coating photoresist on substrate after cleaning, thickness 100nm-200nm, put mask plate, photoetching, development, so
Gold-plated film afterwards is finally removed with acetone to get to capacitor collection liquid body and gas sensors electrode structure；Wherein, mask plate
Structure is made of circular electrode and parallel pole two parts；
(3), it is 30 μm -50 μm that electrodeposition process in-situ deposition film of poly pyrrole, thickness are used on the circular electrode after photoetching, is sunk
After the good film of poly pyrrole of product, solid electrolyte is coated, thickness is 500 μm -800 μm, the power unit as gas sensor；
Spin coating multi-walled carbon nanotube/polyaniline composite material between two parallel poles after photoetching, thickness 200nm-300nm are complete
At the preparation from driving gas at normal temperature sensor.
6. a kind of flexible miniature as claimed in claim 5 drives the preparation method of gas at normal temperature sensor certainly, which is characterized in that
The thickness of gold-plated film described in step (2) is at least 50nm.
7. a kind of flexible miniature as claimed in claim 5 drives the preparation method of gas at normal temperature sensor certainly, which is characterized in that
The time of electro-deposition described in step (3) is 4-5min, and voltage 0-0.8V, method is cyclic voltammetry.
8. a kind of flexible miniature as claimed in claim 5 drives the preparation method of gas at normal temperature sensor certainly, which is characterized in that
It according to volume ratio is 5 that polypyrrole described in step (3), which is by pyrrole monomer and sodium perchlorate,：100 are configured to.
9. a kind of flexible miniature as claimed in claim 5 drives the preparation method of gas at normal temperature sensor certainly, which is characterized in that
Spin coating described in step (3), rotating speed are 500 revolution per seconds, and number is 2 times.
10. a kind of flexible miniature as claimed in claim 5 is from the preparation method for driving gas at normal temperature sensor, feature exists
In multi-walled carbon nanotube/polyaniline composite material described in step (3) is prepared via a method which to obtain, and specific steps are such as
Under：
First, by multi-walled carbon nanotube and aniline monomer according to 1：2 mass ratio is added in 1M/L in perchloric acid solution, 0 DEG C
Lower stirring 30 minutes；Then, into above-mentioned solution with volume ratio 3:1 is added dropwise density as 6*10-3The ammonium persulfate solution of kg/L, will
Mixed solution stirs 24 hours under the conditions of 0 DEG C, and the polyaniline nano-rod array after polymerization is equably grown on the carbon nanotubes；
Finally, the multi-walled carbon nanotube polyaniline nano-composite material that will be obtained, is washed with deionized water, methanol and ethyl alcohol, is washed respectively
Nano material after washing is dried in vacuo 24 hours at 60 DEG C；The mixed liquor of the multi-walled carbon nanotube and aniline monomer and height
The volume ratio of solution chlorate is 1：5.
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| CN110297027A (en) * | 2019-08-06 | 2019-10-01 | 西交利物浦大学 | Porous polymer film, gas sensor and its preparation method and application |
| CN111505062A (en) * | 2020-04-27 | 2020-08-07 | 电子科技大学 | Photovoltaic self-driven flexible gas sensor based on organic-inorganic heterojunction and preparation method thereof |
| CN112763548A (en) * | 2020-12-16 | 2021-05-07 | 北京无线电计量测试研究所 | Carbon monoxide detection method and system based on polymer composite film |
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| CN112763548A (en) * | 2020-12-16 | 2021-05-07 | 北京无线电计量测试研究所 | Carbon monoxide detection method and system based on polymer composite film |
| CN113161158A (en) * | 2021-04-30 | 2021-07-23 | 中国科学院半导体研究所 | Flexible micro capacitor and preparation method thereof |
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