CN113433173A - Flexible material with electrogenerated heat, humidity and VOC (volatile organic compound) sensing characteristics and preparation method thereof - Google Patents
Flexible material with electrogenerated heat, humidity and VOC (volatile organic compound) sensing characteristics and preparation method thereof Download PDFInfo
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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
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
- D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
- D21H23/22—Addition to the formed paper
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/04—Physical treatment, e.g. heating, irradiating
- D21H25/06—Physical treatment, e.g. heating, irradiating of impregnated or coated paper
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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
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Abstract
The invention provides a flexible material with the characteristics of electroluminescence, humidity and VOC sensing and a preparation method thereof, wherein the method comprises the steps of uniformly dispersing a dispersing agent, carbon black particles and graphene in deionized water, wherein the mass ratio of the dispersing agent to the carbon black particles to the graphene is (5-10): 2-6, so as to obtain a conductive dispersion liquid; then soaking the cellulose paper into the conductive dispersion liquid, and drying to obtain the cellulose paper coated with graphene and carbon black; and finally, repeating the obtained cellulose paper for a plurality of times until the resistance value of the obtained cellulose paper is stable, thereby obtaining the flexible material with the characteristics of electroheating, humidity and VOC sensing. The invention takes cellulose as a main component, has wide source, low cost, no pollution and simple preparation process, can realize the detection of VOC and water molecules, has good electrothermal performance and is expected to be applied to the field of flexible wearable electronic equipment.
Description
Technical Field
The invention relates to the technical field of flexible sensing, in particular to a flexible material with the characteristics of electroheating, humidity and VOC sensing and a preparation method thereof.
Technical Field
In modern life, people have higher and higher requirements on indoor environment, and are particularly sensitive to environmental temperature. Improper temperature has certain negative effects on the life and working environment of people. For environmental protection, an electric heating method is generally selected to convert electric energy into heat energy, so as to change the ambient temperature and provide comfortable temperature for people. The electrical heating can be applied precisely at precise points of high power concentration per unit area or volume. Compared to other forms, the advantages of the electrical heating method are quiet, clean and free of by-product emissions, precise control of achievable temperatures and uniform distribution of thermal energy. There were researchers who prepared MWCNT/m-aramid composite films by a solution casting method. For a composite film with 10.0 wt% MWCNTs, a maximum temperature of about 176 ℃ can be reached even at a low applied voltage of 10V. Specific published articles such as "Zhang, d.; sun, y.; li, P.; zhang, Y.simple simulation of MoS2-Modified SnO2 Hybrid Nanocomposite for ultrasensive Humidity sensing. ACS apple Mater Interfaces 2016,8(22),14142-9 ".
Humidity refers to the degree of atmospheric dryness, the moisture that is contained in a volume of air at a certain temperature. Too much or too little humidity can cause physical discomfort to the person. VOC (volatile organic compounds) is an abbreviation for volatile organic compounds. Common indoor volatile organic compounds are sourced from decoration building materials, furniture, coatings and the like, and the indoor VOC pollution degree is more serious than that of outdoor air. Humidity and VOC have a major impact on people's daily life and health safety. Therefore, real-time detection of humidity and VOCs is a crucial and challenging problem.
Cellulose substrate based flexible gas sensors are receiving wide attention due to their large potential applications in human-machine interfaces, health monitoring and robotic smart skin. Many researchers have explored this approach in order to meet the requirements of sensors that are low cost, portable, stable, environmentally friendly, good flexibility, high sensitivity, and fast response/recovery speed. For example, a gas sensor is made by printing crossed carbon electrodes on cellulose paper using commercial carbon ink, and fibers in the paper are utilizedThe inherent moisture absorption characteristic of the cellulose fiber can quantitatively detect the water-soluble gas in the atmosphere. The sensor exhibits high sensitivity to water-soluble gases, fast and reversible response, and is inexpensive. Specific published articles such as "Alkin K, Stockinger T, Zirkl M, et al, paper-based printed impedance sensors for water regulation and husbandry analysis [ J].Flexible&Printed Electronics,2017,2(1):21840-21849 "; preparing conductive yarn by adopting electrostatic spinning combined with in-situ solution polymerization, constructing an ammonia gas sensor, and measuring NH3And NO2Has high responsiveness and selectivity. The nano coaxial polyaniline/polyacrylonitrile nano fiber has higher specific surface area, can provide more adsorption sites and is beneficial to NH3Free diffusion of (2). Specific published articles such as "Lalit Kumar, Ishpal Rawal, Amarjeet Kaur, S.Annapororni. Flexible rock temperature sensor based on polyanaline [ J.].Sensors&Actuators:B.Chemical,2017,240:408-416”.
Flexible base materials, such as Polyimide (PI), Polydimethylsiloxane (PDMS), Polyester (PE), and polyethylene terephthalate (PET), have excellent flexibility and stability, but these organic substrates are difficult to degrade, resulting in electronic contamination. Weak affinity between the sensing materials and the organic substrate can cause the sensing materials to separate during deformation, affecting their durability.
Therefore, at present, no multifunctional flexible paper-based sensing material with characteristics of electric heating, degradability, strong bonding force and humidity and VOC sensing is available.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the flexible material with the characteristics of electroheating, humidity and VOC sensing and the preparation method thereof, the cellulose is used as the main component, the source is wide, the cost is low, no pollution is caused, the preparation process is simple, the detection of VOC and water molecules can be realized, and the flexible material has good electric heating performance and is expected to be applied to the field of flexible wearable electronic equipment.
The invention is realized by the following technical scheme:
the preparation method of the flexible material with the characteristics of electric heating, humidity and VOC sensing comprises the following steps,
step 1, uniformly dispersing a dispersing agent, carbon black particles and graphene in deionized water, wherein the mass ratio of the dispersing agent to the carbon black particles to the graphene is (5-10) to (2-6), and obtaining a conductive dispersion liquid;
and 3, repeating the cellulose paper obtained in the step 2 for a plurality of times according to the treatment mode of the step 2 until the resistance value of the obtained cellulose paper is stable, and obtaining the flexible material with the characteristics of electroluminescence, humidity and VOC sensing.
Preferably, the carbon black granules in step 1 are ground, sieved and dispersed in deionized water.
Further, the carbon black granules were ground and sieved with a 100-mesh classifying screen.
Preferably, the dispersant in step 1 is carboxymethyl cellulose, hydroxypropyl cellulose, polyacrylamide, polyvinyl alcohol or polyethylene glycol.
Preferably, the mass ratio of the graphene to the deionized water in the step 1 is (2-6): 150-500.
Preferably, in the step 2, the cellulose paper is immersed in the conductive dispersion liquid for 3-5 seconds and then dried.
Preferably, the drying in the step 2 is carried out at 40-90 ℃ for 5-50 min.
Preferably, the criterion for stabilizing the resistance value of the cellulose paper in step 3 is as follows:
the ratio of the difference of the resistance values of the last two cellulose papers to the resistance value of the last cellulose paper is less than 5%.
Preferably, the step 3 is repeated for 5-8 times by the treatment mode of the step 2 on the cellulose paper obtained in the step 2.
The flexible material with the characteristics of electroluminescence, humidity and VOC sensing is obtained by the preparation method of the flexible material with the characteristics of electroluminescence, humidity and VOC sensing.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the preparation method of the flexible material with the characteristics of electroheating, humidity and VOC sensing, firstly, the graphene and the carbon black can be uniformly dispersed in an aqueous solution by using a dispersing agent to prepare a conductive dispersion liquid, then the cellulose paper is immersed in the conductive dispersion liquid and dried, so that the graphene and the carbon black can be uniformly distributed on the surface of the paper, the uniformity of the material is improved, a conductive path can be formed between a graphene sheet and carbon black particles, and electronic conduction is realized. The single-layer dispersion liquid is coated on the paper strips, the content of the conductive material is too small, so that the resistance is too large to be beneficial to sensing, and the resistance can be stable by coating the dispersion liquid for many times, so that the sensing effect is achieved. The sensing material can form a structure in which graphene sheets and carbon black particles are overlapped with each other, so that gas molecules are adsorbed on the surface of the sensing material and react with oxygen ions under the condition of change of the content of water molecules or VOC molecules in the environment, holes are reduced, and finally resistance is increased, so that detection of the water molecules or the VOC molecules is realized. The carbon material conducting layer is formed by adopting a dipping coating method, the prepared composite conducting material is low in cost, pollution-free and simple to prepare, and water molecules or VOC (volatile organic compounds) molecules can be detected. Due to the excellent properties of graphene, a maximum temperature of about 130 ℃ can be reached even at a low applied voltage of 6V.
Further, the conductive liquid dispersing agent is carboxymethyl cellulose, hydroxypropyl cellulose, polyacrylamide, polyvinyl alcohol or polyethylene glycol, and the substances can uniformly disperse carbon black and graphene in an aqueous solution, so that the carbon black and the graphene can be uniformly coated on cellulose paper, and the detection effect of the flexible sensing material is improved.
The flexible material has the characteristics of electroheating, humidity and VOC sensing, and in humidity sensing, when the sensing range is 33% -75% RH, the response time is 218s, and the recovery time is 230 s; in VOC sensing, fast and efficient response to methanol, ethanol and toluene can be realized. The response time of methanol was 76s and the recovery time was 115 s. The response time for ethanol was 225s and the recovery time was 245 s. The response time of the toluene is 447s, and the recovery time is 812s, so that compared with the existing flexible sensing material, the substrate material which takes natural polymer as raw material is pollution-free, and can sense quickly and sensitively.
Drawings
Fig. 1 is a preparation flow chart and a test schematic diagram of the paper-based flexible material and device with the characteristics of electroluminescence, humidity and VOC sensing.
Fig. 2 is an assembly schematic diagram of the paper-based flexible material with the characteristics of electric heating, humidity and VOC sensing and the device of the present invention.
FIG. 3 is a scanning electron microscope photograph of a plane of a conductive material prepared in example 3 of the present invention at 5 μm.
Fig. 4 is a temperature curve diagram of the paper-based flexible sensor with the characteristics of electroluminescence, humidity and VOC sensing according to embodiment 3 of the present invention under the condition that the applied voltage is 6 v.
Fig. 5 is a humidity sensing test effect diagram of the paper-based flexible sensor with the characteristics of electroluminescence, humidity and VOC sensing according to embodiment 3 of the present invention.
Fig. 6 is a graph of sensing sensitivity of the paper-based flexible sensor with the characteristics of electroluminescence, humidity and VOC in different VOC environments according to embodiment 3 of the present invention.
Fig. 7 is a diagram illustrating a methanol gas sensing effect corresponding to the paper-based flexible sensor with the characteristics of electroluminescence, humidity and VOC according to embodiment 3 of the present invention.
Fig. 8 is a graph of the sensing effect of the paper-based flexible sensor with the characteristics of electroluminescence, humidity and VOC in the environment where methanol gas and humidity act together in embodiment 3 of the present invention.
In the figure: the conductive adhesive comprises conductive dispersion liquid 1, paper strips 2, sensing materials 3, a test instrument bridge 4, a lead 5 and conductive adhesive 6.
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.
Compared with common flexible organic materials, the material composed of cellulose has the advantages of low price, rich raw material sources, mature manufacturing process, good mechanical flexibility and biocompatibility. Making cellulose a good choice as a flexible sensor substrate.
The invention relates to a preparation method of a paper-based flexible material with the characteristics of electroheating, humidity and VOC sensing, which comprises the following steps as shown in figure 1,
step 1, grinding carbon black particles, screening by using a 100-mesh grading sieve, adding a dispersing agent, graphene and deionized water in proportion, and performing ultrasonic treatment to obtain a uniform conductive dispersion liquid 1.
Wherein the dispersant is one of carboxymethyl cellulose, hydroxypropyl cellulose, polyacrylamide, polyvinyl alcohol and polyethylene glycol. The mass ratio of the dispersing agent to the sieved carbon black particles to the graphene to the deionized water is (5-10) to (2-6) to (150-500).
And 2, cutting the cellulose paper into paper strips 2 with the length of 2cm and the width of 1 cm.
And 3, completely soaking the paper slip 2 into the conductive dispersion liquid 1, taking out the paper slip 2 after soaking for 3-5 seconds, and drying for 5-50 minutes at 40-90 ℃ in a blast drying oven to obtain the single-layer coated paper slip. A small amount of conductive liquid exists on the surface of the paper slip obtained by single-layer coating, and the resistance can not be measured through a universal meter, so that the sensing test can not be realized.
And 4, repeating the step 3 until the resistance value is stable. When the resistance change amount of the sensing material is less than 5% when the number of applications is more, i.e., the ratio of the difference between the resistance values of the last two cellulose papers to the resistance value of the last cellulose paper is less than 5%, the resistance is stabilized, and the number of applications at this time is defined as the optimum number of applications. The sensing material 3 is obtained through five to eight times of coating, conductive paths are formed on the surfaces of the cellulose paper by the conductive layers formed by overlapping the graphene and the carbon black, and the electronic transfer in the sensing process can be realized, so that the humidity and VOC sensing material taking the cellulose paper as a flexible substrate material is obtained.
In the humidity sensing test, MgCl was prepared separately in erlenmeyer flasks2、K2CO3、Mg(NO3)2NaCl and KNO3And left for 24 hours to obtain a humidity environment having a Relative humidity (Relative humidity) of 33%, 43%, 54%, 75% and 95% in this order.
For VOC detection, calculated volumes of methanol, ethanol, toluene, dichloromethane, acetone and petroleum ether were transferred to a 250mL flask and left for several minutes to allow the organic solvent to diffuse to obtain the desired VOC concentration.
One end of the sensing material 3 is placed in the manufactured humidity or VOC gas environment, the other end of the sensing material is connected with a testing instrument bridge 4, and a resistance change signal along with time can be output through a computer end.
As shown in fig. 2, the sensing material 3 prepared by the above preparation method is cut into a rectangle, and both ends of the sensing material are connected with the conductive adhesive 6 through the conducting wire 5, so that the flexible gas sensor can be obtained. The sensor can realize the detection of water molecules or VOC molecules.
In humidity sensing, when the sensing range is 33% -75% RH, the response time is 218s, and the recovery time is 230 s; in VOC sensing, fast and efficient response to methanol, ethanol and toluene can be achieved. The response time of methanol was 76s and the recovery time was 115 s. The response time for ethanol was 225s and the recovery time was 245 s. The toluene response time was 447s and the recovery time was 812 s. In the electrothermal test, heat was generated at various direct current voltages, and a maximum temperature of about 130 to 3min was reached even at a low applied voltage of 6V.
Example 1
The invention relates to a preparation method of a paper-based flexible material with the characteristics of electroheating, humidity and VOC (volatile organic compounds) sensing, which comprises the following steps,
step 1, grinding carbon black particles, screening by using a 100-mesh grading screen, selecting polyvinyl alcohol as a dispersing agent, adding the polyvinyl alcohol according to the mass ratio of 7:5:2:400, and uniformly dispersing a conductive material in deionized water by using the screened carbon black particles, graphene and deionized water. The uniform conductive dispersion liquid is obtained by stirring and ultrasonic processing for 30 min.
And 2, cutting the cellulose paper into small paper strips with the length of 2cm and the width of 1cm, and completely immersing the paper strips into the conductive dispersion liquid. The paper strips were immersed for three seconds, removed, hung in a forced air drying cabinet at 80 ℃ and, after 30 minutes, single-coated paper strips were obtained. And repeating the dipping and drying operations for seven times to obtain a multi-layer coated paper strip, and connecting two ends of the multi-layer coated paper strip with the conductive adhesive through a lead to obtain the flexible gas sensor.
The paper-based flexible sensor with the characteristics of electroheating, humidity and VOC sensing obtained in the embodiment can be used for detecting water molecules or VOC. In humidity sensing, when the sensing range is 33-43% RH, the response time is 130s, and the recovery time is 170 s; in VOC sensing, fast and efficient response to methanol, ethanol and toluene can be realized. The response time of methanol was 23s and the recovery time was 35 s. The response time of ethanol was 85s and the recovery time was 75 s. The response time for toluene was 217s and the recovery time was 512 s. In the electrothermal test, a maximum temperature of about 120 to 3min was reached even at a low applied voltage of 6V.
Example 2
The invention relates to a preparation method of a paper-based flexible material with the characteristics of electroheating, humidity and VOC (volatile organic compounds) sensing, which comprises the following steps,
step 1, grinding carbon black particles, screening by using a 100-mesh grading sieve, adding polyvinyl alcohol according to the ratio of 8:4:2:350, and uniformly dispersing the conductive material in deionized water by using the screened carbon black particles, graphene and deionized water. The uniform conductive dispersion liquid is obtained by stirring and ultrasonic processing for 30 min.
And 2, cutting the cellulose paper into small paper strips with the length of 2cm and the width of 1cm, and completely immersing the paper strips into the conductive dispersion liquid. The paper strips were dipped for three seconds and taken out, hung in a 90 ℃ forced air drying cabinet and after 30 minutes single-coated paper strips were obtained. And repeating the dipping and drying operations for seven times to obtain a paper strip 3 coated with multiple layers, and connecting two ends of the paper strip coated with multiple layers with conductive adhesive through leads to obtain the flexible gas sensor.
The paper-based flexible sensor with the characteristics of electrogenerated heat, humidity and VOC sensing can detect water molecules or VOC. In humidity sensing, when the sensing range is 33-55% RH, the response time is 250s, and the recovery time is 270 s; in VOC sensing, fast and efficient response to methanol, ethanol and toluene can be realized. The response time of methanol was 100s and the recovery time was 120 s. The response time of ethanol was 275s and the recovery time was 315 s. The response time for toluene was 537s and the recovery time was 801 s. In the electrothermal test, a maximum temperature of about 130 to about 130 was reached within 3min even at a low applied voltage of 6V.
Example 3
The invention relates to a preparation method of a paper-based flexible material with the characteristics of electroheating, humidity and VOC (volatile organic compounds) sensing, which comprises the following steps,
step 1, grinding carbon black particles, sieving by using a 100-mesh grading sieve, adding carboxymethyl cellulose according to the proportion of 7:4:3:280, stirring the sieved carbon black particles, graphene and deionized water, and performing ultrasonic treatment for 30min to obtain a uniform conductive dispersion liquid.
And 2, cutting the cellulose paper into small paper strips with the length of 2cm and the width of 1cm, and completely immersing the paper strips into the conductive dispersion liquid. The paper strips were immersed for three seconds, removed, hung in a forced air drying cabinet at 80 ℃ and, after 30 minutes, single-coated paper strips were obtained. And repeating the dipping and drying operations for eight times to obtain a paper strip with multiple layers of coatings, and connecting two ends of the paper strip with the multiple layers of coatings with conductive adhesive through a lead to obtain the flexible gas sensor.
The paper-based flexible sensor with the characteristics of electroheating, humidity and VOC sensing obtained in the embodiment can be used for detecting water molecules or VOC. In humidity sensing, when the sensing range is 33-75% RH, the response time is 218s, and the recovery time is 230 s; in VOC sensing, fast and efficient response to methanol, ethanol and toluene can be realized. The response time of methanol was 76s and the recovery time was 115 s. The response time for ethanol was 225s and the recovery time was 245 s. The toluene response time was 447s and the recovery time was 812 s. In the electrothermal test, a maximum temperature of about 130 to about 130 was reached within 3min even at a low applied voltage of 6V. Compared with the existing flexible sensing material, the substrate material taking natural macromolecules as raw materials is pollution-free, and can be used for sensing quickly and sensitively.
As shown in fig. 3, a scanning electron micrograph of a plane of a conductive material prepared in example 3 of the present invention. The surface of the paper slip after being dipped and coated for many times forms a conductive layer formed by overlapping graphene and carbon black, so that the conductivity of the material is improved, and the detection of water molecules and VOC molecules can be realized.
Fig. 4 is a temperature curve diagram of the paper-based flexible sensing material with the characteristics of electroluminescence, humidity and VOC sensing in the state of a dc voltage of 6v according to embodiment 3 of the present invention. The prepared paper-based flexible sensing material has good electrothermal property, and can generate heat to 120 ℃ within 150s under the applied voltage of 6 v. And a stable heat generation temperature is maintained. And returned to room temperature within a period of 20s after the applied voltage was turned off.
Fig. 5 is a humidity sensing test effect diagram of the paper-based flexible sensor with the characteristics of electroluminescence, humidity and VOC sensing according to embodiment 3 of the present invention. The sensor can monitor corresponding resistance by using an instrument, shows the sensitivity of the gas sensor to the resistance change in the environment from 33% RH to 75% RH, has lower resistance in a low humidity state, increases the resistance along with the increase of the humidity, and can see that the resistance changes periodically along with the monitoring time through continuous humidity change. Sensor performance is defined by the following equation: s can be represented by0Where Δ is relative to the original resistance R0Increase in resistance of R0Is the resistance of the sensor in air. To explore the response time and recovery time of paper based gas sensors, the sampling time for the sensor to reach equilibrium was 30 minutes. It can be seen that the response time is 218s and the recovery time is 230 s.
Fig. 6 is a graph of sensing sensitivity of the paper-based flexible sensor with the characteristics of electroluminescence, humidity and VOC in different VOC environments according to embodiment 3 of the present invention. It can be seen that in many VOCs, the sensor has high sensitivity to the response of methanol, ethanol, and toluene.
Fig. 7 is a diagram illustrating a methanol gas sensing effect corresponding to the paper-based flexible sensor with the characteristics of electroluminescence, humidity and VOC according to embodiment 3 of the present invention. The resistance of the sensor exhibits a periodic variation with the addition and release of gas. The response time was 76s and the recovery time was 115s for a 30 minute sample time.
Fig. 8 is a graph of the sensing effect of the paper-based flexible sensor with the characteristics of electroluminescence, humidity and VOC in the environment where methanol gas and humidity act together in embodiment 3 of the present invention. Under the combined influence of a humidity environment and a methanol gas environment, the resistance of the sensor changes. In the presence of water molecules, the methanol gas can still be adsorbed to the surface of the sensing material and undergo electron transfer. While maintaining a methanol gas environment of 5000ppm, the relative humidity was increased from 43% RH to 54% RH while recording the change in the output signal. The high peak in the output signal indicates that the sensor has good sensitivity to methanol vapor under high humidity conditions. When the RH changes but the VOC level remains unchanged, the response recovery time decreases. This means that the sensor can distinguish well between environmental changes, humidity environments and VOC gas environments.
Example 4
The invention relates to a preparation method of a paper-based flexible material with the characteristics of electroheating, humidity and VOC (volatile organic compounds) sensing, which comprises the following steps,
step 1, grinding carbon black particles, screening by using a 100-mesh grading sieve, adding polyethylene glycol according to the ratio of 8:2:3:400, and uniformly dispersing the conductive material in deionized water by using the screened carbon black particles, graphene and deionized water by using the polyethylene glycol. The uniform conductive dispersion liquid is obtained by stirring and ultrasonic processing for 30 min.
And 2, cutting the cellulose paper into small paper strips with the length of 3cm and the width of 1cm, and completely immersing the paper strips into the conductive dispersion liquid. The strips were immersed for three seconds and then removed and hung in a forced air drying oven at 70 c for 40 minutes to obtain single coated strips. And repeating the dipping and drying operations for seven times to obtain a multi-layer coated paper strip, and connecting two ends of the multi-layer coated paper strip with the conductive adhesive through a lead to obtain the flexible gas sensor.
The paper-based flexible sensor with the characteristics of electrogenerated heat, humidity and VOC sensing can detect water molecules or VOC. In humidity sensing, when the sensing range is 33-75% RH, the response time is 200s, and the recovery time is 215 s; in VOC sensing, the rapid and efficient response to methanol can be realized, the response time is 67s, and the recovery time is 85 s. After heating, the temperature may reach 100 ℃.
Example 5
The invention relates to a preparation method of a paper-based flexible material with the characteristics of electroheating, humidity and VOC (volatile organic compounds) sensing, which comprises the following steps,
step 1, grinding carbon black particles, screening by using a 100-mesh grading sieve, adding polyethylene glycol according to the ratio of 8:4:3:150, stirring the screened carbon black particles, graphene and deionized water, and performing ultrasonic treatment for 30min to obtain a uniform conductive dispersion liquid.
And 2, cutting the cellulose paper into small paper strips with the length of 4cm and the width of 3cm, and completely immersing the paper strips into the conductive dispersion liquid. The paper strips were dipped for three seconds and taken out, hung in a 90 ℃ forced air drying cabinet and after 25 minutes single-coated paper strips were obtained. And repeating the dipping and drying operations for seven times to obtain a multi-layer coated paper strip, and connecting two ends of the multi-layer coated paper strip with the conductive adhesive through a lead to obtain the flexible gas sensor.
The paper-based flexible sensor with the characteristics of electrogenerated heat, humidity and VOC sensing can detect water molecules or VOC. In humidity sensing, when the sensing range is 33-65% RH, the response time is 180s, and the recovery time is 185 s;
in VOC sensing, fast and efficient response to methanol, ethanol and toluene can be realized. The response time of methanol was 54s and the recovery time was 75 s. The response time for ethanol was 165s and the recovery time was 195 s. The response time for toluene was 413 and recovery time was 756 s. In the electrothermal test, a maximum temperature of about 90 reached within 3min was reached even at a low applied voltage of 6V.
Example 6
The invention relates to a preparation method of a paper-based flexible material with the characteristics of electroheating, humidity and VOC (volatile organic compounds) sensing, which comprises the following steps,
step 1, grinding carbon black particles, sieving by using a 100-mesh grading sieve, adding hydroxypropyl cellulose according to the proportion of 8:5:3:300, stirring the sieved carbon black particles, graphene and deionized water, and performing ultrasonic treatment for 30min to obtain a uniform conductive dispersion liquid.
And 2, cutting the cellulose paper into small paper strips with the length of 4cm and the width of 1cm, and completely immersing the paper strips into the conductive dispersion liquid. The paper strips were dipped for three seconds and taken out, hung in a 90 ℃ forced air drying cabinet and after 20 minutes single-coated paper strips were obtained. And repeating the dipping and drying operations for seven times to obtain a multi-layer coated paper strip, and connecting two ends of the multi-layer coated paper strip with the conductive adhesive through a lead to obtain the flexible gas sensor.
The paper-based flexible sensor with the characteristics of electroheating, humidity and VOC sensing obtained in the embodiment can be used for detecting water molecules or VOC. In humidity sensing, when the sensing range is 33-54% RH, the response time is 210s, and the recovery time is 234 s;
in VOC sensing, fast and efficient response to methanol, ethanol and toluene can be realized. The response time of methanol was 63s and the recovery time was 79 s. The response time for ethanol was 205s and the recovery time was 231 s. The response time for toluene was 397s and the recovery time was 692 s. In the electrothermal test, a maximum temperature of about 80 reached within 3min was reached even at a low applied voltage of 6V.
Example 7
The invention relates to a preparation method of a paper-based flexible material with the characteristics of electroheating, humidity and VOC (volatile organic compounds) sensing, which comprises the following steps,
step 1, grinding carbon black particles, screening by using a 100-mesh grading sieve, adding polyacrylamide according to the proportion of 7:6:3:500, and uniformly dispersing the conductive material in deionized water by using the screened carbon black particles, graphene and deionized water by using the polyacrylamide. The uniform conductive dispersion liquid is obtained by stirring and ultrasonic processing for 30 min.
And 2, cutting the cellulose paper into small paper strips with the length of 3cm and the width of 2cm, and completely immersing the paper strips into the conductive dispersion liquid. The strips were immersed for three seconds and then removed and hung in a forced air drying oven at 70 c for 40 minutes to obtain single coated strips. And repeating the dipping and drying operations five times to obtain a multi-layer coated paper strip, and connecting two ends of the multi-layer coated paper strip with the conductive adhesive through a lead to obtain the flexible gas sensor.
The paper-based flexible sensor with the characteristics of electroheating, humidity and VOC sensing obtained in the embodiment can be used for detecting water molecules or VOC. In humidity sensing, when the sensing range is 33-75% RH, the response time is 250s, and the recovery time is 233 s;
in VOC sensing, fast and efficient response to methanol, ethanol and toluene can be realized. The response time of methanol was 86s and the recovery time was 97 s. The response time of ethanol was 239s and the recovery time was 258 s. The response time for toluene was 474s and the recovery time was 829 s. In the electrothermal test, a maximum temperature of about 110 ℃ was reached within 3min even at a low applied voltage of 6V.
Claims (10)
1. The preparation method of the flexible material with the characteristics of electric heating, humidity and VOC sensing is characterized by comprising the following steps,
step 1, uniformly dispersing a dispersing agent, carbon black particles and graphene in deionized water, wherein the mass ratio of the dispersing agent to the carbon black particles to the graphene is (5-10) to (2-6), and obtaining a conductive dispersion liquid;
step 2, soaking the cellulose paper into the conductive dispersion liquid, and then drying to obtain the cellulose paper coated with graphene and carbon black;
and 3, repeating the cellulose paper obtained in the step 2 for a plurality of times according to the treatment mode of the step 2 until the resistance value of the obtained cellulose paper is stable, and obtaining the flexible material with the characteristics of electroluminescence, humidity and VOC sensing.
2. The method for preparing a flexible material with electrothermal, humidity and VOC sensing characteristics as claimed in claim 1, wherein the carbon black particles in step 1 are ground, screened, and dispersed in deionized water.
3. The method of claim 2, wherein the carbon black particles are ground and screened through a 100 mesh sizing screen.
4. The method for preparing a flexible material having electrothermal, humidity and VOC sensing properties according to claim 1, wherein the dispersant in step 1 is carboxymethyl cellulose, hydroxypropyl cellulose, polyacrylamide, polyvinyl alcohol or polyethylene glycol.
5. The method for preparing the flexible material with the characteristics of electroluminescence, humidity and VOC sensing as claimed in claim 1, wherein the mass ratio of the graphene to the deionized water in the step 1 is (2-6): (150-500).
6. The method for preparing the flexible material with the characteristics of electroluminescence, humidity and VOC sensing according to claim 1, wherein the cellulose paper is immersed in the conductive dispersion liquid for 3-5 seconds and then dried in the step 2.
7. The method for preparing a flexible material with electrothermal, humidity and VOC sensing characteristics as claimed in claim 1, wherein the drying in step 2 is performed at 40-90 ℃ for 5-50 min.
8. The method for preparing a flexible material having electrothermal, humidity and VOC sensing properties according to claim 1, wherein the resistance value of the cellulose paper in step 3 is stabilized as follows:
the ratio of the difference of the resistance values of the last two cellulose papers to the resistance value of the last cellulose paper is less than 5%.
9. The method for preparing the flexible material with the characteristics of electroluminescence, humidity and VOC sensing according to claim 1, wherein the step 3 is repeated for 5-8 times by the cellulose paper obtained in the step 2 according to the treatment mode of the step 2.
10. The flexible material with the characteristics of electric heating, humidity and VOC sensing obtained by the preparation method of the flexible material with the characteristics of electric heating, humidity and VOC sensing of any one of claims 1-9.
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