CN111896593B - Asymmetric film type humidity sensor and preparation method thereof - Google Patents
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Abstract
The invention provides an asymmetric film type humidity sensor and a preparation method thereof, wherein the method comprises the following steps: step 1, carrying out suction filtration on a dispersion liquid of graphene oxide and nano-cellulose, wherein the mass fraction of the graphene oxide in the dispersion liquid is 2.5-10.0%, and nano-cellulose/graphene oxide gel is formed on a filter membrane; and 2, firstly placing a nylon net on the upper surface of the nano-cellulose/graphene oxide gel, stamping a patterned structure on the upper surface of the gel by the nylon net, and then drying to form an asymmetric film type humidity sensor between the filter membrane and the nylon net. The preparation process is simple, the price is low, the environment is protected, the humidity sensor is non-toxic and harmless, and the prepared humidity sensor has 2-5s quick linear humidity response.
Description
Technical Field
The invention relates to the technical field of humidity sensing, in particular to an asymmetric film type humidity sensor and a preparation method thereof.
Background
Humidity is an important physical quantity for measuring atmospheric dryness, and has very important influence in the fields of biomedicine, agricultural production, food and drug storage, aerospace and the like. As humidity detection devices, the most common humidity sensors at present mainly include resistance-type humidity sensors, capacitance-type humidity sensors, and colorimetric humidity sensors. Factors such as the need for sophisticated instrumentation, excessive subjective impact, etc. have limited further development of humidity sensors.
The curvature type humidity sensor has received much attention because of its simple equipment and manufacturing process. The main principle of the curvature type humidity sensor is that the film is used as a humidity sensitive element, and the two sides of the film are asymmetrically expanded after absorbing moisture to cause the directional deflection of the film.
So far, a great number of double-layer film curvature type humidity sensors are reported, and the sensing principle of the double-layer film curvature type humidity sensors is mainly based on different moisture absorption expansion coefficients of two layers of thin films, but the interlayer adhesion force of the double-layer film is weakened in the frequent bending and recovery deformation process, so that the application of the double-layer film in practice is hindered.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an asymmetric film type humidity sensor and a preparation method thereof, the preparation process is simple, the price is low, the sensor is green, environment-friendly, non-toxic and harmless, and the prepared humidity sensor has 2-5s rapid linear humidity response.
The invention is realized by the following technical scheme:
a method for preparing an asymmetric thin film type humidity sensor comprises the following steps:
step 1, carrying out suction filtration on a dispersion liquid of graphene oxide and nano-cellulose, wherein the mass fraction of the graphene oxide in the dispersion liquid is 2.5-10.0%, and forming nano-cellulose/graphene oxide gel on a filter membrane;
and 2, firstly placing a nylon net on the upper surface of the nano-cellulose/graphene oxide gel, impressing a patterned structure on the upper surface of the gel by the nylon net, then drying, and forming an asymmetric film type humidity sensor between the filter membrane and the nylon net.
Preferably, the asymmetric membrane-type humidity sensor is separated from the nylon net and the filter membrane in step 2, so as to obtain the asymmetric membrane-type humidity sensor.
Preferably, in the step 1, the graphene oxide solution is added into the nano-cellulose solution to obtain the dispersion liquid, and the concentration of each of the graphene oxide solution and the nano-cellulose solution is 0.01-1mg mL -1 。
Preferably, step 1, adding the graphene oxide solution into the nano-cellulose solution, dispersing the obtained mixed system at 25-35 ℃ to obtain the dispersion liquid,
further, the resulting mixed system is dispersed at this temperature range for 30-180min.
Preferably, in the step 2, a nylon net is placed on the upper surface of the nano-cellulose/graphene oxide gel and then is subjected to suction filtration for 0.5-6h.
Preferably, the mass of the nylon net in the step 2 is 0.06-0.08g.
Preferably, the humidity response time of the asymmetric thin film type humidity sensor formed in step 2 is 2-5s.
An asymmetric thin-film type humidity sensor obtained by the method for manufacturing an asymmetric thin-film type humidity sensor according to any one of the above.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a preparation method of an asymmetric film type humidity sensor, which takes nano-cellulose and graphene oxide with excellent water dispersibility as raw materials, and carries out suction filtration on dispersion liquid of the nano-cellulose and the graphene oxide to obtain nano-cellulose/graphene oxide composite gel; and then, placing the nylon net on the upper surface of the nano-cellulose/graphene oxide composite gel, sinking into the composite gel by virtue of the self gravity of the nylon net, and drying at room temperature to obtain the single-side patterned nano-cellulose/graphene oxide composite membrane, namely the asymmetric thin-film humidity sensor. The patterning increases the roughness of the composite film, which in turn increases the hydrophilicity of the patterned side. When the humidity in the environment increases, the patterned side of the composite film absorbs water and swells more than the smooth side, so that the composite film deflects to the smooth side, and the curvature change of the composite film increases along with the increase of the humidity. The method combining suction filtration and surface imprinting has no special requirements on equipment, is simple and easy to master, is suitable for large-scale expanded production, and provides a brand new idea for the preparation of the asymmetric membrane type humidity sensor.
The asymmetric film type humidity sensor has excellent humidity response characteristic and good flexibility, and has wide application prospect in various fields of humidity sensing, proximity sensing, humidity actuating robots, optical devices and the like.
Drawings
Fig. 1 is a micrograph of a one-sided patterned nanocellulose/graphene oxide composite membrane obtained in example 1 of the present invention.
Fig. 2 is a real image of the nanocellulose/graphene oxide composite membrane according to embodiment 2 of the present invention after being rolled and unfolded.
Fig. 3 is a diagram showing transparency of the nanocellulose/graphene oxide composite membrane according to embodiment 3 of the present invention.
Fig. 4 is a humidity response curve of the nanocellulose/graphene oxide composite membrane according to example 3 of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
According to the preparation method of the asymmetric film type humidity sensor, the nano-cellulose which is one of raw materials is used as a biomass material, the preparation method has the characteristics of environmental friendliness, renewability, wide source and the like, and the excellent hydrophilicity is endowed to the nano-cellulose by the abundant hydrophilic groups such as hydroxyl, carboxyl and the like on the surface of the nano-cellulose. However, a single nano-cellulose film has poor mechanical strength under high humidity conditions, and a certain amount of graphene oxide is doped into nano-cellulose, so that the interaction of hydrogen bonds between the graphene oxide and the nano-cellulose can obviously improve the flexibility of an asymmetric film under the high humidity conditions. The preparation method comprises the following steps of,
step 1, adding a graphene oxide solution into a nano-cellulose solution, and performing ultrasonic dispersion for 30-180min at room temperature and 35 ℃, wherein the concentrations of the nano-cellulose solution and the graphene oxide solution are both 0.01-1mg mL -1 The content of graphene oxide in the mixed solution is 2.5-10.0wt%, so as to obtain a uniformly mixed nano-cellulose/graphene oxide solution;
10g of nano-cellulose dispersion with the mass fraction of 1.0wt% can be dispersed in deionized water, and stirred at room temperature to be fully redispersed to prepare 100mL of nano-cellulose dispersion with the mass concentration of 1mg mL -1 The nanocellulose solution of (2) is then dilutedThe release is 0.01-1mg mL -1 The nanocellulose solution of (1).
And 2, carrying out vacuum filtration on the solution until the nano-cellulose/graphene oxide composite solution forms a gel state, placing a nylon net on the surface of the nylon net, continuously carrying out vacuum filtration for 0.5-6h, carrying out surface imprinting on the nylon net, naturally sinking by virtue of the gravity of the nylon net, generally 0.06-0.08g to form a patterned structure, drying at room temperature, and sequentially uncovering the nylon net and a filter membrane to obtain a single-side patterned nano-cellulose/graphene oxide composite membrane, namely the asymmetric film type humidity sensor.
The film type humidity sensor prepared by the invention has good flexibility, transparency and humidity response characteristics.
Example 1
Step 1, 0.5mL of graphene oxide solution (0.01 mg mL) -1 ) Added to 19.5mL of the nanocellulose solution (0.01 mg mL) -1 ) Performing ultrasonic dispersion at room temperature for 30min, and uniformly mixing the two solutions to prepare a nano-cellulose/graphene oxide mixed solution with the graphene oxide content of 2.5 wt%;
step 2, preparing the nano-cellulose/graphene oxide mixed solution with the graphene oxide content of 2.5wt% into nano-cellulose/graphene oxide composite gel by means of a vacuum filtration method;
step 3, placing a nylon net on the surface of the nano-cellulose/graphene oxide composite gel, continuing to perform suction filtration for 0.5h to enable the nano-cellulose/graphene oxide composite gel to be sunk into the composite gel by virtue of the gravity of the nano-cellulose/graphene oxide composite gel, and slowly drying at room temperature;
and 4, after fully drying the nano-cellulose/graphene oxide composite gel, sequentially uncovering the nylon net and the filter membrane to obtain the single-side patterned nano-cellulose/graphene oxide composite membrane with the graphene oxide content of 2.5 wt%.
Example 2
Step 1, 1.0mL of graphene oxide solution (0.1 mg mL) -1 ) Added to 19.0mL of the nanocellulose solution (0.1 mg mL) -1 ) Performing ultrasonic dispersion at 30 ℃ for 60min to uniformly mix the two to prepare a nano-cellulose/graphene oxide mixed solution with the content of graphene oxide of 5.0 wt%;
step 2, preparing the nano-cellulose/graphene oxide mixed solution with the graphene oxide content of 5.0wt% into nano-cellulose/graphene oxide composite gel by means of a vacuum filtration method;
step 3, placing a nylon net on the surface of the nano-cellulose/graphene oxide composite gel, continuously performing suction filtration for 1 hour to enable the nano-cellulose/graphene oxide composite gel to be sunk into the composite gel by virtue of the gravity of the nano-cellulose/graphene oxide composite gel, and slowly drying the nano-cellulose/graphene oxide composite gel at room temperature;
and 4, after fully drying the nano-cellulose/graphene oxide composite gel, sequentially uncovering the nylon net and the filter membrane to obtain the single-side patterned nano-cellulose/graphene oxide composite membrane with the graphene oxide content of 5.0 wt%.
Example 3
Step 1, 1.5mL of graphene oxide solution (0.5 mg mL) -1 ) Added to 18.5mL of nanocellulose solution (0.5 mg mL) -1 ) Performing ultrasonic dispersion at 35 ℃ for 180min to uniformly mix the two to prepare a nano-cellulose/graphene oxide mixed solution with the content of graphene oxide of 7.5 wt%;
step 2, preparing the nano-cellulose/graphene oxide mixed solution with the graphene oxide content of 7.5wt% into nano-cellulose/graphene oxide composite gel by means of a vacuum filtration method;
step 3, placing a nylon net on the surface of the nano-cellulose/graphene oxide composite gel, continuously performing suction filtration for 3 hours to enable the nano-cellulose/graphene oxide composite gel to be sunk into the composite gel by virtue of the gravity of the nano-cellulose/graphene oxide composite gel, and slowly drying the nano-cellulose/graphene oxide composite gel at room temperature;
and 4, after fully drying the nano-cellulose/graphene oxide composite gel, sequentially uncovering the nylon net and the filter membrane to obtain the single-side patterned nano-cellulose/graphene oxide composite membrane with the graphene oxide content of 7.5 wt%.
Example 4
Step 1, 2.0mL of graphene oxide solution (1.0 mg mL) -1 ) Added to 18.0mL of nanocellulose solution (1.0 mg mL) -1 ) Performing ultrasonic dispersion at room temperature for 60min, and mixing the two uniformly to prepare a nano-cellulose/graphene oxide mixed solution with the graphene oxide content of 10.0 wt%;
step 2, preparing a nano-cellulose/graphene oxide composite gel from a nano-cellulose/graphene oxide mixed solution with the graphene oxide content of 10.0wt% by means of a vacuum filtration method;
step 3, placing a nylon net on the surface of the nano-cellulose/graphene oxide composite gel, continuously performing suction filtration for 6 hours to enable the nano-cellulose/graphene oxide composite gel to be sunk into the composite gel by means of the gravity of the nano-cellulose/graphene oxide composite gel, and slowly drying the nano-cellulose/graphene oxide composite gel at room temperature;
and 4, after fully drying the nano-cellulose/graphene oxide composite gel, sequentially uncovering the nylon net and the filter membrane to obtain the single-side patterned nano-cellulose/graphene oxide composite membrane with the graphene oxide content of 10.0 wt%.
The one-sided patterned nanocellulose/graphene oxide composite films formed in examples 1 to 4 had good flexibility, transparency, and humidity response characteristics.
Example 1 single-sided patterning of a nanocellulose/graphene oxide composite membrane as shown in fig. 1, it is clear from the micrograph that the composite membrane surface has a regular pattern.
As an example, example 2 demonstrates the good flexibility of the prepared nanocellulose/graphene oxide composite membrane, as shown in fig. 2, the single-sided patterned composite membrane still maintains the integrity of the membrane after being rolled or bent 20 times.
The transparency of the nanocellulose/graphene oxide composite membrane of example 3 is shown in fig. 3, and it can be seen from the figure that the word "huminity sensor" printed on the following paper can be clearly seen through the nanocellulose/graphene oxide thin film, indicating that it has excellent transparency.
The nanocellulose/graphene oxide composite membrane of embodiment 3 is directly placed in the air, the ambient humidity is changed, the change of the deflection angle of the composite membrane under different humidities is measured, and according to the formula:
and (4) calculating the curvature of the composite membrane under different humidities to obtain a humidity response curve. Due to the fact that abundant hydrophilic groups (such as hydroxyl, carboxyl and the like) on the surfaces of the nano-cellulose and the graphene oxide endow the composite membrane with good hydrophilic characteristics, the roughness of the composite membrane is increased through patterning, and the speed of combination of the composite membrane and water is further increased. Therefore, under the same environmental humidity, the expansion degrees of the two sides of the composite film after moisture absorption are different, when the humidity is increased, the patterned side has a faster moisture absorption rate, the expansion degree is greater than that of the smooth side, and the composite film deflects to the smooth side. As shown in fig. 4, the curvature of the single-sided patterned composite film increases with an increase in relative humidity in the environment, and the two have a better linear relationship. Therefore, the single-side patterned nano-cellulose/graphene oxide composite film has excellent humidity response performance as a novel humidity sensor.
Claims (9)
1. A preparation method of an asymmetric thin film type humidity sensor is characterized by comprising the following steps:
step 1, carrying out suction filtration on a dispersion liquid of graphene oxide and nano-cellulose, wherein the mass fraction of the graphene oxide in the dispersion liquid is 2.5-10.0%, and nano-cellulose/graphene oxide gel is formed on a filter membrane;
and 2, firstly placing a nylon net on the upper surface of the nano-cellulose/graphene oxide gel, stamping a patterned structure on the upper surface of the gel by the nylon net, drying, and forming a single-side patterned nano-cellulose/graphene oxide composite film between the filter membrane and the nylon net to form the asymmetric thin-film type humidity sensor, wherein the water absorption expansion degree of the patterned side of the composite film is greater than that of the smooth side, so that the curvature change of the composite film is increased along with the increase of humidity.
2. The method of manufacturing an asymmetric membrane-type humidity sensor according to claim 1, wherein the asymmetric membrane-type humidity sensor is separated from the nylon net and the filter membrane in the step 2 to obtain the asymmetric membrane-type humidity sensor.
3. According toThe method of claim 1, wherein in step 1, the graphene oxide solution is added to the nanocellulose solution to obtain the dispersion, and the concentration of each of the graphene oxide solution and the nanocellulose solution is 0.01-1mg mL -1 。
4. The method for preparing an asymmetric membrane-type humidity sensor according to claim 3, wherein the graphene oxide solution is added into the nano-cellulose solution in step 1, and the obtained mixed system is dispersed at 25-35 ℃ to obtain the dispersion liquid.
5. The method of manufacturing an asymmetric membrane type humidity sensor according to claim 4, wherein the obtained mixed system is dispersed at the temperature range for 30-180min.
6. The method for manufacturing an asymmetric thin-film type humidity sensor according to claim 1, wherein step 2 comprises placing a nylon mesh on the upper surface of the nanocellulose/graphene oxide gel, performing suction filtration for 0.5-6h, embossing a patterned structure on the upper surface of the gel with the nylon mesh, and drying.
7. The method for manufacturing an asymmetric membrane type humidity sensor according to claim 1, wherein the nylon mesh mass in step 2 is 0.06-0.08g.
8. The method for manufacturing an asymmetric thin film type humidity sensor according to claim 1, wherein the humidity response time of the asymmetric thin film type humidity sensor formed in the step 2 is 2-5s.
9. An asymmetric membrane type humidity sensor obtained by the method of manufacturing an asymmetric membrane type humidity sensor according to any one of claims 1 to 8.
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