CN114062443B - Flexible sensor for monitoring humidity of package headspace - Google Patents
Flexible sensor for monitoring humidity of package headspace Download PDFInfo
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- CN114062443B CN114062443B CN202111330098.3A CN202111330098A CN114062443B CN 114062443 B CN114062443 B CN 114062443B CN 202111330098 A CN202111330098 A CN 202111330098A CN 114062443 B CN114062443 B CN 114062443B
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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
- G01N27/02—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
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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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
- G01N27/02—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
Abstract
A flexible sensor for monitoring humidity in a package headspace relates to the field of humidity monitoring. Firstly, printing an interdigital electrode substrate by using a flexible plastic film as a base material through a screen printing process, and covering the electrode with c-MWCNTs/GO/WS after drying 2 Moisture sensitive film formed of composite material wherein c-MWCNTs, GO, WS 2 The mass ratio of the three is (1-4): 1-8): 1-4, and the three are put into a baking oven for drying, thus obtaining the C-MWCNTs/GO/WS-based catalyst 2 Is provided. The sensor prepared by the method has a large humidity monitoring range, can rapidly and accurately monitor humidity change in the package, and has good repeatability.
Description
Technical Field
The invention relates to the field of humidity monitoring, in particular to a flexible sensor for monitoring the humidity of a package headspace.
Technical Field
Intelligent packaging of food is an emerging technology that reduces waste and protects consumer health and safety. Humidity is one of the most important factors affecting food quality, when the humidity is too high, microorganisms rapidly grow, food is rapidly spoiled, when the humidity is too low, food water loss and quality reduction can bring about the problems of safety and resource waste, and improper humidity atmosphere leads to high decay rate of food and related disease outbreak. The traditional packaging mainly plays roles of protection, isolation, quantification, decoration and description, but the traditional packaging technology lacks monitoring, recording and controlling of package headspace humidity because intelligent materials are not included, so that an intelligent humidity sensor is necessarily installed on the fruit and vegetable package to monitor the humidity inside the package in real time, and measures are taken in time to regulate and control the humidity range.
In recent years, two-dimensional layered transition metal chalcogenides (TMDCs) have been used in the field of gas, temperature, electronic and optoelectronic sensing as a low-cost, fast, directly printable 2D semiconductor material due to their excellent performance in nanoelectronics. TMDCs of the general formula MX 2 Wherein M may be tin, tungsten, molybdenum, vanadium, etc., and X may be S, se, te, etc. Tungsten disulfide (WS) 2 ) As one of two-dimensional layered transition metal chalcogenides, the two-dimensional layered transition metal chalcogenides have a layered structure similar to graphene, have large specific surface area and adjustable band gap, and have great application potential in the aspect of humidity-sensitive sensors.
Disclosure of Invention
In order to solve the technical problems, the main purpose of the invention is to provide a flexible humidity sensor capable of rapidly detecting and a preparation method thereof.
The invention aims at realizing the following technical scheme:
a flexible sensor for monitoring humidity of package headspace is characterized by comprising an interdigital electrode printed on a flexible substrate film base material, and a filling sensitive layer c-MWCNTs/GO/WS coated on the interdigital electrode 2 。
Preferably, the flexible substrate is PET or PI.
Further, the interdigital electrode is obtained by printing conductive silver paste or conductive carbon paste by a screen printing process, the interdigital pair number is 4-10, and the electrode line width is 0.1-0.5 mm.
The flexible sensor for monitoring the humidity of the package headspace is based on c-MWCNTs/GO/WS 2 The preparation method of the flexible humidity sensor specifically comprises the following steps:
(1) Printing interdigital electrodes on the surface of the flexible substrate through a screen printing process, and drying to obtain a sensor substrate electrode layer;
(2) Will c-MWCNTs, GO, WS 2 The mixed solution prepared in the step (1-4) is poured into a centrifuge tube according to the mass ratio of (1-4) to (1-8), and the prepared humidity-sensitive mixed solution is coated on the flexible electrode substrate prepared in the step (1) after ultrasonic dispersion for not less than 2 hours.
Further, the saidThe drying temperature in the step (1) is 65 ℃ and the time is 2 hours, and the dried material is naturally dried under the room temperature condition to form uniform c-MWCNTs/GO/WS 2 And (3) a film.
Further, the c-MWCNTs used in the step (2) have a length of 0.5-2 μm.
Conventional humidity sensors are mostly based on rigid ceramics or Si/SiO 2 The substrate limits the application of the humidity sensor in some emerging industries, and the flexible film is selected as the substrate, so that the prepared flexible humidity sensor has good flexibility, low cost and simple and convenient process flow, and can be applied in wider fields compared with the traditional rigid humidity sensor.
GO is an excellent nanomaterial consisting of epoxy (-O), hydroxyl (-OH) and carboxyl (-COOH) groups coated on the surface and edges. GO has proven to be an excellent sensing layer due to its humidity sensing capability, its hydrophilicity being derived from its dangling bonds. However, when the humidity of the pure GO is reduced, the time for removing the water molecules is long, so that the c-MWCNTs with hydrophobicity can be compounded, the time for removing the water molecules can be shortened, interaction force exists between the GO and delocalized electrons on benzene rings of the c-MWCNTs due to pi-pi accumulation, and electrostatic repulsive force exists between the GO molecules, so that the c-MWCNTs can be well dissolved in the GO solution. c-MWCNTs/GO/WS 2 The humidity sensor is exposed to a humid environment, and adsorbed water molecules are directed to c-MWCNTs, GO and WS 2 Electrons are injected into the surface. Thus, n-type WS 2 The number of electrons in (a) increases and the concentration of holes in (b) p-type GO decreases, resulting in further expansion of the depletion layer, followed by c-MWCNTs/GO/WS 2 The resistance of the humidity sensor changes.
Drawings
FIG. 1 is a c-MWCNTs/GO/WS-based image of the invention 2 An electrode size schematic of a flexible humidity sensor;
FIG. 2 is a schematic illustration of humidity sensor flexibility;
FIG. 3 is a response curve of the flexible humidity sensor in a humidity environment of 11-98% RH;
fig. 4 is a graph of the repeatability of the flexible humidity sensor switching back and forth between 11% humidity and 98% rh.
Detailed Description
Based on c-MWCNTs/GO/WS 2 Comprises a flexible substrate, interdigital electrodes and c-MWCNTs/GO/WS covered on the surface of the flexible substrate 2 Composite material, wherein the length of the c-MWCNTs is 0.5-2 mu m, c-MWCNTs, GO, WS 2 The mass ratio is (1-4)/(1-8)/(1-4).
The invention will be further illustrated by the following examples, which are intended to be illustrative of the invention and are not to be construed as limiting the invention in any way, i.e., the examples described are merely illustrative of some, but not all, of the examples.
Example 1: in this embodiment, c-MWCNTs/GO/WS 2 The humidity sensor is manufactured by the following method:
step 1) preparing a sensitive solution: adopting a solution method, taking c-MWCNTs with certain mass, dispersing in GO solution after ultrasonic treatment for 2 hours, and then taking WS with set mass 2 Mixing, performing ultrasonic treatment for 2h again, and mixing with vortex mixer for 30min to obtain c-MWCNTs/GO/WS 2 Composite solution in which c-MWCNTs/GO/WS 2 The mass ratio of (2) is 4:2:1.
Step 2) preparing an interdigital electrode: pretreating the flexible substrate, ultrasonically cleaning for 15min, cleaning with deionized water, and drying in a 75 ℃ oven. And (3) customizing 8 pairs of interdigital pairs, sequentially printing conductive silver paste on a base film by using a screen printing machine, and placing the printed electrodes into a baking oven, drying at 75 ℃ for 60min, and naturally drying at room temperature for later use.
Step 3) preprocessing the interdigital electrode obtained in the step 2), cleaning the surface of the electrode by deionized water and absolute ethyl alcohol in sequence, fully drying in a nitrogen environment, and then adopting a dripping method to obtain the c-MWCNTs/GO/WS obtained in the step 1) 2 The composite solution is coated on the surface of the interdigital electrode in a dripping way to form a composite gas-sensitive film, and finally the electrode with the composite gas-sensitive film is put into a drying box for drying at the temperature of 65 ℃ for 2 hours, and the temperature is kept at room temperature after dryingNaturally drying to obtain c-MWCNTs/GO/WS 2 A humidity sensor.
The prepared flexible humidity sensor is placed in a humidity atmosphere of 11% RH, 23% RH, 33% RH, 43% RH, 59% RH, 75% RH, 85% RH and 98% RH obtained by a saturated salt solution method, a lead copper wire is contacted with a universal meter, and a real-time resistance value of the sensor under different humidity environments is recorded by the universal meter connected with a computer.
Fig. 3 is a response curve of the fabricated flexible humidity sensor at different humidities, and it can be seen that the sensor has a good response in the range of 11-98% rh.
Fig. 4 is the resistance data of the manufactured flexible humidity sensor for nine consecutive adsorption-desorption processes between 11% rh and 98% rh, and it can be seen that the sensor has better stability and repeatability.
In this embodiment, the flexible substrate is PET.
Example 2: in this embodiment, c-MWCNTs/GO/WS 2 The humidity sensor is manufactured by the following method:
step 1) preparing a sensitive solution: adopting a solution method, taking c-MWCNTs with certain mass, dispersing in GO solution after ultrasonic treatment for 2 hours, and then taking WS with set mass 2 Mixing, performing ultrasonic treatment for 2h again, and mixing with vortex mixer for 30min to obtain c-MWCNTs/GO/WS 2 Composite solution in which c-MWCNTs/GO/WS 2 The mass ratio of (2) to (1).
Step 2) preparing an interdigital electrode: pretreating the flexible substrate, ultrasonically cleaning for 15min, cleaning with deionized water, and drying in a 75 ℃ oven. And (3) customizing 8 pairs of interdigital pairs, sequentially printing conductive carbon paste on a base film PI by using a screen printing machine, putting the printed electrodes into a baking oven, drying at 75 ℃ for 60min, and naturally drying at room temperature for later use.
Step 3) preprocessing the interdigital electrode obtained in the step 2), cleaning the surface of the electrode by deionized water and absolute ethyl alcohol in sequence, fully drying in a nitrogen environment, and then adopting a spraying method to obtain the c-MWCNTs/GO/WS obtained in the step 1) 2 Composite solventSpraying the liquid on the surface of the interdigital electrode to form a composite gas-sensitive film, and finally placing the electrode with the composite gas-sensitive film into a drying oven for drying at 65 ℃ for 2 hours, and naturally drying at room temperature after drying to prepare the c-MWCNTs/GO/WS 2 A humidity sensor.
Example 3: in this embodiment, c-MWCNTs/GO/WS 2 The humidity sensor is manufactured by the following method:
step 1) preparing a sensitive solution: adopting a solution method, taking c-MWCNTs with certain mass, dispersing in GO solution after ultrasonic treatment for 2 hours, and then taking WS with set mass 2 Mixing, performing ultrasonic treatment for 2h again, and mixing with vortex mixer for 30min to obtain c-MWCNTs/GO/WS 2 Composite solution in which c-MWCNTs/GO/WS 2 The mass ratio of (2) is 1:4:1.
Step 2) preparing an interdigital electrode: pretreating the flexible substrate, ultrasonically cleaning for 15min, cleaning with deionized water, and drying in a 75 ℃ oven. 10 pairs of interdigital pairs are customized, a silk screen plate with the electrode line width of 0.2mm is used for sequentially printing conductive carbon paste on a base film PET by a silk screen printer, the printed electrodes are put into a baking oven, and are dried at 75 ℃ for 60min and then are dried naturally at room temperature for standby.
Step 3) preprocessing the interdigital electrode obtained in the step 2), cleaning the surface of the electrode by deionized water and absolute ethyl alcohol in sequence, fully drying in a nitrogen environment, and then adopting a dripping method to obtain the c-MWCNTs/GO/WS obtained in the step 1) 2 Coating the composite solution on the surface of the interdigital electrode to form a composite gas-sensitive film, and finally placing the electrode with the composite gas-sensitive film into a drying oven for drying at 65 ℃ for 2 hours, and naturally drying at room temperature after drying to prepare the c-MWCNTs/GO/WS 2 A humidity sensor.
Finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention.
Claims (7)
1. A flexible sensor for monitoring humidity of package headspace is characterized by comprising an interdigital electrode printed on a flexible substrate film base material, and a filling sensitive layer c-MWCNTs/GO/WS coated on the interdigital electrode 2 。
2. A flexible sensor for package headspace humidity monitoring according to claim 1, wherein said flexible substrate is PET or PI.
3. A flexible sensor for monitoring humidity in a package headspace according to claim 1, wherein the interdigital electrode is obtained by printing conductive silver paste or conductive carbon paste by a screen printing process, the interdigital pair number is 4-10, and the electrode line width is 0.1-0.5 mm.
4. A method for manufacturing a flexible sensor for monitoring the humidity of a package headspace according to any of claims 1 to 3, comprising the steps of:
(1) Printing interdigital electrodes on the surface of the flexible substrate through a screen printing process, and drying to obtain a sensor substrate electrode layer;
(2) Will c-MWCNTs, GO, WS 2 The doped solution prepared in the step (1-4) is poured into a centrifuge tube according to the mass ratio of (1-4), and the prepared wet-sensitive mixed solution is dripped on the flexible interdigital electrode substrate prepared in the step (1) after ultrasonic dispersion is carried out for not less than 2 hours.
5. The process according to claim 4, wherein the drying temperature in step (1) is 65℃for 2 hours, and the drying is carried out naturally at room temperature to form uniform c-MWCNTs/GO/WS 2 And (3) a film.
6. The process according to claim 4, wherein the c-MWCNTs used in step (2) have a length of 0.5-2. Mu.m.
7. Use of a flexible sensor for package headspace humidity monitoring as claimed in any of claims 1-3 for monitoring food package headspace humidity.
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