CN114441527A - Nanofiber colorimetric humidity sensor and preparation method thereof - Google Patents
Nanofiber colorimetric humidity sensor and preparation method thereof Download PDFInfo
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- CN114441527A CN114441527A CN202011185609.2A CN202011185609A CN114441527A CN 114441527 A CN114441527 A CN 114441527A CN 202011185609 A CN202011185609 A CN 202011185609A CN 114441527 A CN114441527 A CN 114441527A
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims description 13
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 61
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims abstract description 31
- 239000012528 membrane Substances 0.000 claims abstract description 23
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 22
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 17
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 17
- 239000002390 adhesive tape Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000000835 fiber Substances 0.000 claims abstract description 10
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 8
- 230000005684 electric field Effects 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 33
- 239000002904 solvent Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 15
- 229920002799 BoPET Polymers 0.000 claims description 13
- 238000009987 spinning Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 230000000007 visual effect Effects 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/81—Indicating humidity
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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Abstract
A nano-fibre colorimetric humidity sensor is prepared from Polyacrylonitrile (PAN) as fibre-forming matrix material and CoCl2The color-changing agent is prepared by electrostatic spinning under electric field force to form nanometer fiber, collecting on grounded metal roller to obtain PAN/CoCl2A nanofiber membrane; then, the nanofiber membrane is used as a colorimetric humidity-sensitive material, and a PET (polyethylene terephthalate) membrane and a conductive adhesive tape are utilized to finally obtain PAN/CoCl2A nanofiber colorimetric sensor; the polyacrylonitrile/cobalt chloride nanofiber colorimetric humidity sensor has the advantages of direct visual observation, good flexibility, good stability, short response time, wide range and the like.
Description
Technical Field
The present invention relates to the field of humidity sensors, and more particularly to optical and resistive humidity sensors.
Background
Humidity has an inseparable relationship with people's daily life and work, and with the technological progress, humidity sensors play an increasingly important role in people's production and life, and have been widely applied to the fields of climate detection, article storage, industrial production, medical treatment and health, and the like;
the existing sensors are mainly classified into resistive, capacitive, acoustic wave and optical sensors, the adopted humidity-sensitive materials are mainly electrolytes, metal oxides, polymers and the like, the optical sensors can provide signals visible to the naked eye, but the sensors on the market are generally high in price at present, and the sensors with low price mainly comprise resistive and capacitive sensors, but have the defects of low reliability, poor stability, narrow humidity measuring range, long response time and the like.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing a colorimetric humidity sensor integrating optics and resistance, which takes Polyacrylonitrile (PAN) as a fiber-forming material and cobalt chloride (CoCl)2) The polyacrylonitrile/cobalt chloride nanofiber membrane is used as a color developing agent, is prepared by an electrostatic spinning method, and is adhered to a PET (polyethylene terephthalate) membrane by using a double-sided conductive adhesive tape, so that the polyacrylonitrile/cobalt chloride nanofiber colorimetric humidity sensor is obtained. This sensor not only can be exported the signal conversion to the signal of telecommunication, can also directly discern the change of humidity with the form of colour, and the person of facilitating the use judges with the quick making of naked eye to have advantages such as low cost, response are fast, stability is good, measuring range is wide.
The technical scheme adopted by the invention for solving the technical problems is as follows: a nanofiber colorimetric humidity sensor and a preparation method thereof are characterized in that: the nano-fiber colorimetric humidity sensor takes Polyacrylonitrile (PAN) as a fiber-forming matrix material and CoCl2The color-changing agent is prepared by electrostatic spinning under electric field force to form nanometer fiber, collecting on grounded metal roller to obtain PAN/CoCl2A nanofiber membrane; then, the nanofiber membrane is used as a colorimetric humidity-sensitive material, and a PET (polyethylene terephthalate) membrane and a conductive adhesive tape are utilized to finally obtain PAN/CoCl2A nanofiber colorimetric sensor.
Further, the electrostatic spinning is carried out by PAN and CoCl2And a spinning solvent N, N-dimethylformamide.
Further, the mass fraction of the PAN is 10-20%, and the CoCl is2The mass fraction of the solvent is 10-30 percentThe mass fraction is 70-85%.
Further, the preparation method comprises the following specific steps:
(1) preparing an electrostatic spinning solution: respectively using PAN powder and CoCl2Adding the solute particles into N, N-dimethylformamide as solvent, stirring to dissolve completely, and mixing the two solutions at different ratio to obtain final PAN/CoCl2A solution;
(2) preparing a nanofiber precursor: placing the electrostatic spinning solution in a needle cylinder, and volatilizing the solvent in electrostatic spinning under the force of an electric field to form nano-sized nanofibers;
(3) preparing a sensor: and drying the obtained nano-fibers, cutting the dried nano-fibers according to a certain size, and adhering the nano-fibers on a PET (polyethylene terephthalate) film by using a conductive adhesive tape to obtain the polyacrylonitrile/cobalt chloride nano-fiber colorimetric humidity sensor.
Further, the mass fraction of PAN in the step (1) is 10-20%, and CoCl2The mass fraction of the solvent is 10-30%, and the mass fraction of the solvent is 70-85%; CoCl2The mixing volume ratio of the solution to the PAN solution is between 0.2 and 0.6.
Further, the specific preparation method of the nanofiber precursor in the step (2) comprises the following steps: the electrostatic spinning solution is placed in a needle cylinder, the advancing speed of the spinning solution is 1.0-5.0 ml/h, the ambient temperature is 20-40 ℃, the diameter of a nozzle is 1.5-2.0 mm, the receiving distance is 10-20 cm, the spinning voltage is 15-20kV, and a grounded rotary cylinder is used for receiving the fiber.
Further, the drying in the step (3) is performed by vacuum drying, and the drying temperature is 55-60 ℃.
Further, the thickness of the PET film in the step (3) is 0.15-0.25mm, and the PET film is cut into a square shape and has certain thickness and flexibility.
Further, the conductive adhesive tape in the step (3) is a conductive double-sided adhesive tape, and is adhered to two sides of the PET film at a distance.
Further, the method is characterized in that any one of polyacrylonitrile-cobalt chloride nano-fiber in claims 1, 2 and 3 is used as a colorimetric humidity-sensitive material to form a nano-fiber colorimetric humidity sensor.
The invention has the beneficial effects that:
1. the polyacrylonitrile/cobalt chloride nanofiber colorimetric humidity sensor has the advantages of direct visual observation, good flexibility, good stability, short response time, wide measuring range and the like;
2. the method of the invention controls the CoCl mixed in the PAN solution2The concentration and the proportion of the colorimetric humidity-sensitive material, and the color rendering performance and the magnitude of an output signal of the colorimetric humidity-sensitive material are regulated and controlled; controlling the mechanical strength of the colorimetric humidity-sensitive material by controlling the concentration of PAN;
3. the method is simple and convenient, is easy to control, and can reduce the cost.
Drawings
FIG. 1 shows different PAN, CoCl embodiments in accordance with the invention2And the effect of dimethyl sulfoxide ratio on the nanofiber colorimetric humidity sensor.
Detailed Description
In order to make the technical solution of the present invention more apparent, the present invention is further described with reference to the following embodiments.
As shown in fig. 1, a nanofiber colorimetric humidity sensor and a method for manufacturing the same according to an embodiment of the present invention are characterized in that: the nano-fiber colorimetric humidity sensor takes Polyacrylonitrile (PAN) as a fiber-forming matrix material and CoCl2The color-changing agent is prepared by electrostatic spinning under electric field force to form nanometer fiber, collecting on grounded metal roller to obtain PAN/CoCl2A nanofiber membrane; then, the nanofiber membrane is used as a colorimetric humidity-sensitive material, and a PET (polyethylene terephthalate) membrane and a conductive adhesive tape are utilized to finally obtain PAN/CoCl2A nanofiber colorimetric sensor.
Further, the electrostatic spinning is performed by PAN and CoCl2And a spinning solvent N, N-dimethylformamide.
Further, the mass fraction of the PAN is 10-20%, and the CoCl is2The mass fraction of the solvent is 10-30%, and the mass fraction of the solvent is 70-85%.
Further, the preparation method comprises the following specific steps:
(1) preparing an electrostatic spinning solution: respectively using PAN powder and CoCl2Adding the solute particles into N, N-dimethylformamide as solvent, stirring to dissolve completely, and mixing the two solutions at different ratio to obtain final PAN/CoCl2A solution;
(2) preparing a nanofiber precursor: placing the electrostatic spinning solution in a needle cylinder, and volatilizing the solvent in electrostatic spinning under the force of an electric field to form nano-sized nanofibers;
(3) preparing a sensor: and drying the obtained nano-fibers, cutting the dried nano-fibers according to a certain size, and adhering the nano-fibers on a PET (polyethylene terephthalate) film by using a conductive adhesive tape to obtain the polyacrylonitrile/cobalt chloride nano-fiber colorimetric humidity sensor.
Further, in the step (1), the mass fraction of PAN is 10-20%, and CoCl2The mass fraction of the solvent is 10-30%, and the mass fraction of the solvent is 70-85%; CoCl2The mixing volume ratio of the solution to the PAN solution is between 0.2 and 0.6.
Further, the specific preparation method of the nanofiber precursor in the step (2) comprises the following steps: placing the electrostatic spinning solution into a needle cylinder, wherein the advancing speed of the spinning solution is 1.0-5.0 ml/h, the ambient temperature is 20-40 ℃, the diameter of a nozzle is 1.5-2.0 mm, the receiving distance is 10-20 cm, the spinning voltage is 15-20kV, and a grounded rotary cylinder is used for receiving fibers.
Further, the drying in the step (3) is performed by vacuum drying, and the drying temperature is 55-60 ℃.
Further, the thickness of the PET film in the step (3) is 0.15-0.25mm, and the PET film is cut into a square shape and has certain thickness and flexibility.
Further, the conductive adhesive tape in the step (3) is a conductive double-sided adhesive tape, and is adhered to two sides of the PET film at a distance.
Further, the method is characterized in that any one of polyacrylonitrile-cobalt chloride nano-fiber in claims 1, 2 and 3 is used as a colorimetric humidity-sensitive material to form a nano-fiber colorimetric humidity sensor.
A polyacrylonitrile/cobalt chloride nanofiber colorimetric humidity sensor comprises PAN (polyacrylonitrile)/CoCl (cobalt chloride) with the mass fraction of 20 percent2The mass fraction of the polyacrylonitrile/cobalt chloride nano-fiber membrane is 15%, the two are mixed according to the volume ratio of 2:1, the mass fraction of N, N-dimethylformamide is 85%, spinning solution is obtained by stirring uniformly, the nano-fiber membrane obtained by the electrostatic spinning method is dried to obtain the polyacrylonitrile/cobalt chloride nano-fiber membrane, and the nano-fiber membrane can be used for colorimetric and humidity sensitive materials. Cutting the fiber membrane into 2 × 2cm, sticking the PET membrane and the conductive double-sided adhesive tape as supporting and auxiliary materials on two sides of the fiber membrane to form electrodes, and finally obtaining the polyacrylonitrile/cobalt chloride nanofiber colorimetric humidity sensor
The polyacrylonitrile/cobalt chloride nanofiber membrane is prepared by the following method:
(1) firstly, adding PAN powder into a solvent N, N-dimethylformamide, and stirring to dissolve the PAN powder uniformly; then adding CoCl2Adding a solvent N, N-dimethylformamide into the particles, and stirring to uniformly dissolve the N, N-dimethylformamide; finally, mixing the two solutions according to a certain volume ratio, and stirring to make them uniform to obtain spinning solution, wherein PAN and CoCl2And the content of N, N-dimethylformamide is shown in FIG. 1;
(2) preparing a nanofiber precursor: placing the electrostatic spinning solution into a needle cylinder, wherein the advancing speed of the spinning solution is 1.0 ml/h, the ambient temperature is 25 ℃, the diameter of a nozzle is 2.0 mm, the receiving distance is 15 cm, the spinning voltage is 20kV, and a grounded rotary cylinder is used for receiving fibers;
(3) preparing a nanofiber colorimetric humidity sensor: and drying the obtained nano-fiber in an oven at 60 ℃, then cutting the nano-fiber into 2 x 2cm, similarly cutting the PET film into 2 x 2cm, and adhering the PET film on the PET film by using a conductive adhesive tape to obtain the polyacrylonitrile/cobalt chloride nano-fiber colorimetric humidity sensor.
In order to determine the performance of the nanofiber membrane, color development photos of the polyacrylonitrile/cobalt chloride nanofiber colorimetric humidity-sensitive material in different humidity environments are shot; and (3) carrying out current test on the prepared polyacrylonitrile/cobalt chloride nanofiber colorimetric humidity sensor by adopting an electrochemical workstation.
Different PAN, CoCl2And solvent percentages are shown in fig. 1, and the resulting polyacrylonitrile/cobalt chloride nanofiber colorimetric humidity sensors have currents at 11%, 33%, 59%, 75%, and 98% humidity as shown in fig. 1.
The above embodiments may be combined with each other and further implemented without being mutually opposed.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A nanofiber colorimetric humidity sensor and a preparation method thereof are characterized in that: the nano-fiber colorimetric humidity sensor takes Polyacrylonitrile (PAN) as a fiber-forming matrix material and CoCl2The color-changing agent is prepared by electrostatic spinning under electric field force to form nanometer fiber, collecting on grounded metal roller to obtain PAN/CoCl2A nanofiber membrane; then, the nanofiber membrane is used as a colorimetric humidity-sensitive material, and a PET (polyethylene terephthalate) membrane and a conductive adhesive tape are utilized to finally obtain PAN/CoCl2A nanofiber colorimetric sensor.
2. The nanofiber colorimetric humidity sensor and the preparation method thereof according to claim 1, wherein the humidity sensor comprises: the electrostatic spinning is carried out by PAN and CoCl2And a spinning solvent N, N-dimethylformamide.
3. The nanofiber colorimetric humidity sensor and the preparation method thereof according to claim 1, wherein the humidity sensor comprises: the mass fraction of the PAN is 10-20%, and the CoCl2The mass fraction of the solvent is 10-30%, and the mass fraction of the solvent is 70-85%.
4. The nanofiber colorimetric humidity sensor and the preparation method thereof according to claims 1, 2 and 3, wherein the humidity sensor comprises: the preparation method comprises the following specific steps:
(1) preparing an electrostatic spinning solution: respectively using PAN powder and CoCl2Adding the solute particles into N, N-dimethylformamide as solvent, stirring to dissolve completely, and mixing the two solutions at different ratio to obtain final PAN/CoCl2A solution;
(2) preparing a nanofiber precursor: placing the electrostatic spinning solution in a needle cylinder, and volatilizing the solvent in electrostatic spinning under the force of an electric field to form nano-sized nanofibers;
(3) preparing a sensor: and drying the obtained nano-fibers, cutting the dried nano-fibers according to a certain size, and adhering the nano-fibers on a PET (polyethylene terephthalate) film by using a conductive adhesive tape to obtain the polyacrylonitrile/cobalt chloride nano-fiber colorimetric humidity sensor.
5. The method of manufacturing according to claim 4, characterized in that: the mass fraction of PAN in the step (1) is 10-20%, and CoCl2The mass fraction of the solvent is 10-30%, and the mass fraction of the solvent is 70-85%; CoCl2The mixing volume ratio of the solution to the PAN solution is between 0.2 and 0.6.
6. The method of claim 4, wherein: the specific preparation method of the nanofiber precursor in the step (2) comprises the following steps: placing the electrostatic spinning solution into a needle cylinder, wherein the advancing speed of the spinning solution is 1.0-5.0 ml/h, the ambient temperature is 20-40 ℃, the diameter of a nozzle is 1.5-2.0 mm, the receiving distance is 10-20 cm, the spinning voltage is 15-20kV, and a grounded rotary cylinder is used for receiving fibers.
7. The method of claim 4, wherein: the drying in the step (3) is carried out by vacuum drying, and the drying temperature is 55-60 ℃.
8. The method of claim 4, wherein: the thickness of the PET film in the step (3) is 0.15-0.25mm, and the PET film is cut into a square shape and has certain thickness and flexibility.
9. The method of claim 4, wherein: the conductive adhesive tape in the step (3) is a conductive double-sided adhesive tape, is adhered to two sides of the PET film and is separated from the PET film by a certain distance.
10. The method of claim 4, wherein: the method takes any polyacrylonitrile-cobalt chloride nano fiber in claims 1, 2 and 3 as a colorimetric humidity-sensitive material to form a nano fiber colorimetric humidity sensor.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102954848A (en) * | 2011-08-16 | 2013-03-06 | 中国科学技术大学 | Novel flexible mechanical sensor and preparation method thereof |
| CN105568557A (en) * | 2015-12-22 | 2016-05-11 | 青岛大学 | Humidity-sensitive electrospun cobalt chloride micro-nanofiber membrane as well as preparation method and application thereof |
| CN109655492A (en) * | 2018-11-12 | 2019-04-19 | 浙江大学 | A kind of humidity sensor and its method based on friction nanometer power generator |
| CN109855782A (en) * | 2019-02-21 | 2019-06-07 | 电子科技大学 | Sensor compliant conductive composite membrane and preparation method thereof and flexible sensor |
| 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 |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102954848A (en) * | 2011-08-16 | 2013-03-06 | 中国科学技术大学 | Novel flexible mechanical sensor and preparation method thereof |
| CN105568557A (en) * | 2015-12-22 | 2016-05-11 | 青岛大学 | Humidity-sensitive electrospun cobalt chloride micro-nanofiber membrane as well as preparation method and application thereof |
| CN109655492A (en) * | 2018-11-12 | 2019-04-19 | 浙江大学 | A kind of humidity sensor and its method based on friction nanometer power generator |
| CN109855782A (en) * | 2019-02-21 | 2019-06-07 | 电子科技大学 | Sensor compliant conductive composite membrane and preparation method thereof and flexible sensor |
| 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 |
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