CN110687169B - Humidity-sensitive carbon nano tube/graphene/organic composite flexible material, humidity sensor and preparation method thereof - Google Patents
Humidity-sensitive carbon nano tube/graphene/organic composite flexible material, humidity sensor and preparation method thereof Download PDFInfo
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Abstract
The invention provides a humidity-sensitive carbon nano tube/graphene/organic composite flexible material, a flexible humidity sensor and a preparation method thereof. The preparation method of the composite flexible material comprises the following steps: dispersing graphene oxide in an organic solvent I to prepare a graphene oxide dispersion liquid; dispersing the carbon nano tube in an organic solvent II to prepare a carbon nano tube dispersion liquid; soaking the flexible substrate in the graphene oxide dispersion liquid, and drying to obtain a flexible substrate coated by graphene oxide; and soaking the flexible substrate coated with the graphene oxide in the carbon nano tube dispersion liquid, and drying to obtain the carbon nano tube/graphene/organic composite flexible material sensitive to humidity. The composite flexible material has high sensitivity to humidity, and the preparation method is simple, low in production cost and high in efficiency, and can realize continuous and large-scale production.
Description
Technical Field
The invention belongs to the technical field of flexible functional electronic materials and flexible sensors, and particularly relates to a humidity-sensitive carbon nano tube/graphene/organic composite flexible material, a flexible humidity sensor and a preparation method thereof.
Background
The common humidity sensor works on the principle that the interaction between water molecules and organic polymers causes the change of dielectric constant or conductivity of the sensor, and the change of resistance or capacitance is measured to reflect the change of humidity. With the diversification of the application range of the sensor and the development of all countries in the world in the technical field of the sensor in recent years, the humidity sensor has wide application prospect in the fields of atmospheric monitoring, industrial production, biological medical treatment and the like. At present, a variety of sensors are largely used in many intelligent detection devices, and the application thereof has already penetrated aspects such as industrial production, ocean exploration, environmental protection, medical diagnosis, biological engineering, smart home and the like. With the increasing application demand of the information age, the expected values and the ideal requirements for various performance parameters such as the range, the precision and the stability of the measured information are gradually increased. For the measurement requirements of humidity in special environments and special signals, the novel sensor technology has developed towards the following trends: developing new materials, new processes and developing new sensors; the integration and the intellectualization of the sensor are realized; the microminiaturization of a hardware system and components of the sensing technology is realized. At the same time, it is desirable that the sensor also be transparent, flexible, extensible, freely bendable or even foldable, portable, wearable, etc. The traditional silicon-based semiconductor humidity sensor cannot be flexible, and is high in manufacturing cost and inconvenient to carry.
The prior art reports a method for preparing a humidity sensor by coating polyimide on silver cross electrodes by using an ink jet printing method, and the humidity sensor prepared by the method has a limited measurement range and poor humidity sensitivity although the resistance change range is large along with the humidity change. The prior art also discloses a method for preparing a humidity sensor by synthesizing a 2D nano material by stripping WS2 with tert-butyl lithium and then depositing the 2D nano material on an interdigital electrode of a conductive ceramic platform. In addition, there is a report on manufacturing a humidity sensor on a glass fiber substrate based on the principle that carboxymethyl cellulose (CMC) causes mechanical strain in response to a change in humidity, and although the sensor has high sensitivity, the applicable humidity range is narrow, and the application of the sensor is limited.
Disclosure of Invention
Aiming at the prior art, the invention provides a humidity-sensitive carbon nano tube/graphene/organic composite flexible material, and a flexible humidity sensor with high sensitivity and quick response can be prepared on the basis of the flexible material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the preparation method of the humidity-sensitive carbon nanotube/graphene/organic composite flexible material comprises the following steps:
s1: immersing graphene into mixed acid prepared from concentrated sulfuric acid and concentrated nitric acid according to a material-liquid ratio of 1g: 180-220 mL, treating for 6-8 h at 68-75 ℃, and then sequentially performing centrifugation, cleaning and drying to obtain graphene oxide;
s2: respectively dispersing graphene oxide and carbon nanotubes in a solvent to obtain graphene dispersion liquid and carbon nanotube dispersion liquid with the concentrations of 3-7 mg/mL;
s3: and (3) sequentially placing the flexible substrate in the graphene dispersion liquid and the carbon nano tube dispersion liquid for soaking to obtain the carbon nano tube/graphene/organic composite flexible material.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid in the mixed acid is 1: 1-5.
Further, the graphene is single-layer graphene or multi-layer graphene; the carbon nanotube is a single-walled carbon nanotube or a multi-walled carbon nanotube.
Further, the cleaning solution used for cleaning in S1 is deionized water with pH not less than 6; the drying temperature is 55-65 ℃, and the drying time is 12-16 h.
Further, a solvent for dispersing the graphene oxide in the S2 is ethanol; the solvent for dispersing the carbon nano tube is N, N-dimethylformamide.
Further, the flexible substrate is ultrasonically cleaned for 10-30 min by absolute ethyl alcohol before being soaked.
Further, the flexible substrate is polypropylene, polyacrylonitrile, polyvinyl formal, polyamide, polyethylene terephthalate, polyamide or cyanoacrylate
Further, the flexible substrate is soaked in the graphene dispersion liquid for 4-7 min, dried at 60 ℃ for 10min after soaking, then soaked in the carbon nano tube dispersion liquid for 3-5 min, and then dried at 150 ℃ for 0.5h, so that the carbon nano tube/graphene/organic composite flexible material is obtained.
The method can be used for preparing the humidity-sensitive carbon nano tube/graphene/organic composite flexible material, and the flexible material can be cut into pieces and coated with electrodes to obtain the flexible humidity sensor.
The invention has the beneficial effects that:
1. according to the invention, the graphene oxide and the carbon nano tube are adopted to prepare the composite flexible layer, and strong hydrogen bonds and van der Waals force interaction can be formed between the graphene oxide and the carbon nano tube, so that the finally prepared carbon nano tube/graphene/organic composite multilayer material has the advantages of small resistance and stable performance for a sensor.
2. The humidity sensor features that a film made of humidity sensing material is coated on a substrate, and when water vapor in air is adsorbed onto the humidity sensing film, the resistivity and resistance of the element are changed. When the humidity in the air is increased, the concentration of water molecules is increased, more water molecules are absorbed by the humidity-sensitive film, the conductivity is enhanced, the resistivity is reduced, and the resistance is reduced. When the water molecules on the surface of the humidity sensitive film fall off, the resistance is recovered to the original value. However, due to the good hydrophilic property of graphene oxide, the time required for the water molecules to fall off is long, and the falling off of the water molecules can be accelerated after the carbon nanotubes are covered on the surface of the graphene oxide. The carbon nano tube is of a tubular structure and is inserted between the graphene lamellar structures, and the carbon nano tube has hydrophobicity, so that water molecules adsorbed by the graphene fall off when contacting the carbon nano tube, and the response recovery of the humidity-sensitive film is accelerated. Therefore, the resistance of the humidity sensitive membrane is rapidly reduced when the humidity change is detected, and when the humidity returns to the original value, the water molecules on the surface of the humidity sensitive membrane are dropped off, and the resistance is rapidly recovered. Therefore, the humidity sensor has the characteristics of high sensitivity and quick response recovery. The humidity response time of the humidity sensor provided by the invention is less than 2 seconds, and the recovery time is less than 10 seconds.
3. From the preparation process of the composite flexible conductive fabric, the adopted dipping and coating process is simple, the production cost is low, the efficiency is high, and the continuous and large-scale production is easy to realize.
Drawings
Fig. 1 is a humidity-resistance rapid response characteristic curve of a carbon nanotube/graphene/organic composite flexible material;
FIG. 2 is a humidity-resistance response recovery time characteristic curve of a sample with optimal sensitivity of a carbon nanotube/graphene/organic composite flexible material;
FIG. 3 is a surface SEM image of a carbon nanotube/graphene/organic composite flexible material;
FIG. 4 is a humidity gradient-resistance characteristic curve of a carbon nanotube/graphene/organic composite flexible material;
fig. 5 is a humidity point diagram of the carbon nanotube/graphene/organic composite flexible material.
Detailed Description
The materials used in the process of preparing the flexible self-adhesive cloth with the pressure/friction sensing function are as follows:
1. graphene: the graphene can be single-layer graphene or multi-layer graphene;
2. carbon nanotube: can be single-wall carbon nano-tubes or multi-wall carbon nano-tubes; the carbon nano-tube is preferably a multi-wall carbon nano-tube, and the average diameter of the multi-wall carbon nano-tube is 10-20 nm, and the average length of the multi-wall carbon nano-tube is 20 mu m.
3. A flexible substrate: the flexible substrate has a width of 2cm and a length of 10cm, and is made of high polymer such as polypropylene, polyacrylonitrile, polyvinyl formal, polyamide, polyethylene terephthalate, polyamide or cyanoacrylate.
The following examples are provided to illustrate specific embodiments of the present invention.
Example one
A method for preparing a humidity-sensitive carbon nanotube/graphene/organic composite flexible material comprises the following steps:
s1: taking 150mL of concentrated sulfuric acid (98%) and 50mL of concentrated nitric acid (65%), and mixing the concentrated sulfuric acid and the concentrated nitric acid to obtain 200mL of mixed acid; and adding 1g of multilayer graphene into the mixed acid, uniformly stirring, heating to 70 ℃, and keeping the reaction for 7 hours. After the reaction system is cooled, centrifuging at 6000rpm for 3min, then washing with deionized water with the pH value of more than or equal to 6 for 4 times, and drying at 60 ℃ for 14h to prepare graphene oxide;
s2: dispersing the prepared graphene oxide in absolute ethyl alcohol to obtain graphene oxide dispersion liquid with the concentration of 5 mg/mL; dispersing the multi-wall carbon nano tube in N, N-Dimethylformamide (DMF) to obtain carbon nano tube dispersion liquid with the concentration of 5 mg/mL;
s3: ultrasonically cleaning the two sides of the polypropylene non-woven fabric for 10min by absolute ethyl alcohol;
s4: placing the cleaned polypropylene nonwoven fabric in graphene oxide dispersion liquid to be soaked for 5min, and then drying at 60 ℃ for 10min to obtain graphene oxide coated nonwoven fabric;
s5: and (3) soaking the obtained graphene oxide coated non-woven fabric in a carbon nano tube dispersion liquid for 20s, and then drying at 150 ℃ for 0.5h to prepare the carbon nano tube/graphene/organic composite multilayer coated non-woven fabric.
Example two
A method for preparing a humidity-sensitive carbon nanotube/graphene/organic composite flexible material comprises the steps of soaking a graphene oxide-coated non-woven fabric in a carbon nanotube dispersion liquid for 1min, and carrying out the same operation as the embodiment.
EXAMPLE III
A method for preparing a humidity-sensitive carbon nanotube/graphene/organic composite flexible material comprises the steps of soaking a graphene oxide-coated non-woven fabric in a carbon nanotube dispersion liquid for 3min, and carrying out the same operation as the embodiment.
Example four
A method for preparing a humidity-sensitive carbon nanotube/graphene/organic composite flexible material comprises the steps of soaking a graphene oxide-coated non-woven fabric in a carbon nanotube dispersion liquid for 10min, and carrying out the same operation as the embodiment except for the step of soaking.
EXAMPLE five
A method for preparing a humidity-sensitive carbon nanotube/graphene/organic composite flexible material comprises the steps of soaking a graphene oxide-coated non-woven fabric in a carbon nanotube dispersion liquid for 5min, and carrying out the same operation as the embodiment.
Fig. 1 is a humidity-resistance quick response characteristic curve of a carbon nanotube/graphene/organic composite flexible material, and a to E are humidity-resistance response characteristic curves of flexible materials obtained in the first to fifth embodiments, respectively. As can be seen from fig. 1, the resistance value of the carbon nanotube/graphene/organic composite flexible material decreases with the increase of the relative humidity, and the sensitivity is high; as can be seen from curves a to C and E in fig. 1, as the soaking time of the graphene oxide-coated nonwoven fabric in the carbon nanotube dispersion liquid is prolonged, the resistance-humidity change sensitivity of the graphene oxide-coated nonwoven fabric is increased; from the curve D in fig. 1, it can be seen that the resistance change rate of the carbon nanotube/graphene/organic composite flexible material is greatly reduced, but the resistance-humidity change sensitivity of the carbon nanotube/graphene/organic composite flexible material is still increased, and this result shows that the hydrophobic property of the surface of the humidity-sensitive membrane is already strong, and the hydrophilicity of the humidity-sensitive membrane is destroyed and has the hydrophobic property after the soaking time is further prolonged.
Fig. 2 shows that the sensitivity of the humidity sensor is optimized, the response time is 1s, the recovery time is 7s, and the response recovery curve is shown in fig. 2, for the carbon nanotube/graphene/organic composite flexible material prepared in the fifth embodiment.
Fig. 3 is a surface SEM image of the carbon nanotube/graphene/organic composite flexible material prepared in example two. As can be seen from the figure, the carbon nanotubes and graphene form a conductive network with a certain continuity.
Fig. 4 is a humidity gradient-resistance characteristic curve of the carbon nanotube/graphene/organic composite flexible material. It can be seen from the figure that the resistance value of the humidity-sensitive membrane resistance at the corresponding humidity does not change too much by changing the humidity of the testing environment for many times, which indicates that the composite humidity-sensitive material has good stability.
Fig. 5 is a humidity point diagram of the carbon nanotube/graphene/organic composite flexible material. It can be seen from the graph that the sensitivity in the low humidity region is higher than that in the high humidity region, and the resistance change amplitude is larger. From a relative humidity of 45% RH to 95% RH, the resistance drops by 436k Ω per 1% RH rise on average.
While the present invention has been described in detail with reference to the embodiments, it should not be construed as limited to the scope of the patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (8)
1. A preparation method of a humidity-sensitive carbon nano tube/graphene/organic substrate composite flexible material is characterized by comprising the following steps:
s1: immersing graphene into mixed acid prepared from concentrated sulfuric acid and concentrated nitric acid according to a material-liquid ratio of 1g: 180-220 mL, treating for 6-8 h at 68-75 ℃, and then sequentially performing centrifugation, cleaning and drying to obtain graphene oxide;
s2: respectively dispersing graphene oxide and carbon nanotubes in a solvent to obtain graphene oxide dispersion liquid and carbon nanotube dispersion liquid with the concentrations of 3-7 mg/mL; wherein the solvent for dispersing the graphene oxide is ethanol; the solvent for dispersing the carbon nano tube is N, N-dimethylformamide;
s3: sequentially placing the flexible substrate in graphene oxide dispersion liquid and carbon nanotube dispersion liquid for soaking to obtain a carbon nanotube/graphene oxide/organic substrate composite flexible material; the flexible substrate is soaked in the graphene oxide dispersion liquid for 4-7 min, dried at 60 ℃ for 10min after soaking, then soaked in the carbon nano tube dispersion liquid for 5min, and then dried at 150 ℃ for 0.5 h.
2. The method of claim 1, wherein: the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid in the mixed acid is 1-5: 1.
3. The method of claim 1, wherein: the graphene is single-layer graphene or multi-layer graphene; the carbon nano tube is a single-wall carbon nano tube or a multi-wall carbon nano tube.
4. The method of claim 1, wherein: the cleaning liquid used for cleaning in the S1 is deionized water with the pH value more than or equal to 6; the drying temperature is 55-65 ℃, and the drying time is 12-16 h.
5. The method of claim 1, wherein: and ultrasonically cleaning the flexible substrate with absolute ethyl alcohol for 10-30 min before soaking.
6. The production method according to claim 1 or 5, characterized in that: the flexible substrate is polypropylene, polyacrylonitrile, polyvinyl formal, polyamide or polyethylene terephthalate.
7. The humidity-sensitive carbon nanotube/graphene oxide/organic substrate composite flexible material prepared by the preparation method of any one of claims 1 to 6.
8. A flexible humidity sensor comprising the flexible material of claim 7.
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| CN114062443B (en) * | 2021-11-10 | 2023-10-03 | 北京印刷学院 | Flexible sensor for monitoring humidity of package headspace |
| JP2023092739A (en) * | 2021-12-22 | 2023-07-04 | Tdk株式会社 | humidity sensor |
| CN114752093A (en) * | 2022-05-06 | 2022-07-15 | 绍兴兆丽新材料科技有限公司 | High-strength high-toughness flexible sensing fiber composite membrane and preparation method thereof |
| CN115005804A (en) * | 2022-06-06 | 2022-09-06 | 华东师范大学 | Breathing monitoring device of flexible all-carbon-based humidity sensor |
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