CN113667291B - Super-hydrophobic material, preparation method thereof and sensor - Google Patents
Super-hydrophobic material, preparation method thereof and sensor Download PDFInfo
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- CN113667291B CN113667291B CN202110968514.6A CN202110968514A CN113667291B CN 113667291 B CN113667291 B CN 113667291B CN 202110968514 A CN202110968514 A CN 202110968514A CN 113667291 B CN113667291 B CN 113667291B
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- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
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- G01L1/18—Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
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- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
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- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
- G01L1/2287—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges constructional details of the strain gauges
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Abstract
The invention discloses a super-hydrophobic material, a preparation method thereof and a sensor. The super-hydrophobic material has super-hydrophobicity, can be applied to equipment with high requirements on water resistance, and has high market value. The preparation process of the super-hydrophobic material is simple, easy to operate, low in price of the selected raw materials, low in cost and suitable for large-scale production. The sensor has the characteristics of super-hydrophobicity, high sensitivity up to 3.8, accurate detection on micro pressure, quick response and the like, and has high market value.
Description
Technical Field
The invention relates to the field of materials, in particular to a super-hydrophobic material, a preparation method thereof and a sensor.
Background
High-performance piezoresistive materials have been one of the most important components in the fields of human-computer interaction, robots, electronic skins, wearable equipment and the like. However, the practical application scenario of piezoresistive materials is often complex, and piezoresistive materials with single function have gradually failed to meet the practical application requirements. For example, piezoresistive materials used in wearable devices are susceptible to attack by moisture or sweat in the air when in actual use. This not only can lead to signal distortion, influences wearable equipment's life, very easily causes the short circuit moreover, threatens user's personal safety.
The super-hydrophobic material depends on a specific micro-nano composite structure and surface modification of hydrophobic substances, and the preparation idea is simple and effective. Accordingly, more and more researchers are working on developing piezoresistive materials having superhydrophobicity. Researchers have proposed strategies for self-assembling graphene sheets on three-dimensional polymer scaffolds to prepare graphene sponges. However, the graphene sensor based on the polymer matrix has low sensitivity, a complex process and high cost, and few researches on the super-hydrophobic performance are realized, so that the application of the sensor is limited to a certain extent.
Disclosure of Invention
In order to overcome the problems of the prior art, the invention aims to provide a super-hydrophobic material.
The second purpose of the invention is to provide a preparation method of the super-hydrophobic material.
The invention also aims to provide application of the super-hydrophobic material in human-computer interaction, robots, electronic skins or wearable equipment.
The fourth purpose of the present invention is to provide a sensor comprising the above-mentioned superhydrophobic material.
In order to achieve the above object, a first aspect of the present invention adopts the following technical solutions: a superhydrophobic material comprising a reduced graphene oxide/polyurethane sponge composite.
Preferably, the superhydrophobic material has a water contact angle >150 °; further preferably, the water contact angle of the superhydrophobic material is >152 °.
The second aspect of the present invention provides a preparation method of the above super-hydrophobic material, which comprises the following steps:
s1: mixing the graphene oxide aggregate with polyurethane sponge to prepare composite sponge;
s2: freezing the composite sponge, and then reacting with a reducing agent to prepare the super-hydrophobic material.
Preferably, the preparation method of the graphene oxide aggregate comprises the following steps: and mixing the graphene oxide dispersion liquid with dodecyl glucoside for reaction to prepare the graphene oxide aggregate. According to the preparation method disclosed by the invention, although the surfactant is used, the prepared reduced graphene oxide/polyurethane sponge composite material can still realize super-hydrophobicity.
Preferably, the graphene oxide agglomerates are vesicular.
Preferably, the graphene oxide dispersion is sonicated prior to use.
Preferably, the ultrasonic treatment time is 24-54 min; further preferably, the ultrasonic treatment time is 30-45 min; still further preferably, the ultrasonic treatment time is 30-45 min.
Preferably, the ultrasonic treatment temperature is 22-34 ℃; further preferably, the ultrasonic treatment temperature is 25-30 ℃; still further preferably, the sonication temperature is 28 ℃.
Preferably, the mass-to-volume ratio of the graphene oxide dispersion liquid is 6.4-9.6 mg/ml; further preferably, the mass-to-volume ratio of the graphene oxide dispersion liquid is 7-8.5 mg/ml; still further preferably, the mass-to-volume ratio of the graphene oxide is 8 mg/ml.
Preferably, the addition amount of the dodecyl glucoside is 16-30 mg; further preferably, the addition amount of the dodecyl glucoside is 20-25 mg.
Preferably, the mixing reaction in the preparation method of the graphene oxide aggregate is at least one of stirring, ultrasound and shaking.
Preferably, the mixing reaction in the preparation method of the graphene oxide aggregate is mixed in a stirring manner.
Preferably, the stirring speed is 2000-3000 r/min; further preferably, the stirring speed is 2400-2800 r/min; still more preferably, the stirring speed is 2500-2700 r/min.
Preferably, the stirring time is 1-18 min; further preferably, the stirring time is 3-15 min.
Preferably, the polyurethane sponge is cleaned prior to use.
Preferably, the step S1 is specifically: adding the polyurethane sponge into the graphene oxide aggregate, and extruding the sponge.
Preferably, the step of squeezing the sponge is repeated not less than 2 times; further preferably, the step of squeezing the sponge is repeated 10 times or more.
Preferably, in step S2, the freezing step is freezing with liquid nitrogen.
Preferably, step S2 further includes a step of drying the composite sponge.
Preferably, the drying step is located after the freezing step and before the step of reacting with the reducing agent.
Preferably, the drying treatment is carried out by adopting a freeze drying method.
Preferably, the freeze-drying time is 1-24 h; further preferably, the freeze-drying time is 5-20 h; still further preferably, the freeze-drying time is 15-20 h;
preferably, the reducing agent is at least one of ascorbic acid, hydroiodic acid, sodium hydroxide, hydrazine hydrate, sodium sulfide and sodium borohydride; further preferably, the reducing agent is at least one of hydroiodic acid, hydrazine hydrate and ascorbic acid; still further preferably, the reducing agent is hydrazine hydrate; more preferably, the hydrazine hydrate is gaseous.
Preferably, the step S2 further includes a vacuum drying step, and the vacuum drying step is after the step of reacting with the reducing agent.
Preferably, in the step S2, the reaction temperature is 50-120 ℃; further preferably, in the step S2, the reaction temperature is 90-120 ℃; still more preferably, in the step S2, the reaction temperature is 100 to 120 ℃.
Preferably, in the step S2, the reaction time is 3-10 h; more preferably, in the step S2, the reaction time is 5 to 6 hours.
The invention provides the application of the super-hydrophobic material in human-computer interaction, robots, electronic skins or wearable equipment.
In a fourth aspect, the invention provides a sensor comprising the superhydrophobic material described above.
Preferably, the sensor further comprises two copper sheet electrodes and conductive silver paste, the two copper sheet electrodes are respectively located on two sides of the super-hydrophobic material, and the conductive silver paste is filled between the copper sheet electrodes and the super-hydrophobic material.
Preferably, the sensor is prepared by the following method: and coating conductive silver paste on two sides of the super-hydrophobic material, adhering copper sheet electrodes on the conductive silver paste, and packaging.
The invention has the beneficial effects that: the super-hydrophobic material has super-hydrophobicity, can be applied to equipment with high requirements on water resistance, and has high market value.
The preparation process of the super-hydrophobic material is simple, easy to operate, low in price of the selected raw materials, low in cost and suitable for large-scale production.
The sensor has the characteristics of super-hydrophobicity, sensitivity up to 3.8, accurate detection on micro pressure, quick response and the like, and has high market value.
Drawings
FIG. 1 is a graph showing the sensitivity of the sensors of example 4, comparative example 4 and comparative example 5.
FIG. 2 is a graph of the rate of change of resistance of the sensor in example 4 during loading and unloading.
FIG. 3 is a graph of the rate of change of resistance of the sensor during strain versus time in example 4.
FIG. 4 is a scanning electron micrograph of comparative example 1.
FIG. 5 is a scanning electron micrograph of comparative example 2.
FIG. 6 is a SEM image of example 1.
FIG. 7 is a static hydrophobic angle measurement as in example 1.
FIG. 8 is a static hydrophobic angle measurement of comparative example 3.
Detailed Description
The following description of the embodiments of the present invention is provided in connection with the accompanying drawings and examples, but the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
The super-hydrophobic material in this embodiment includes a reduced graphene oxide/polyurethane sponge composite.
The preparation method of the super-hydrophobic material comprises the following steps:
(1) dispersing 0.4g of graphene oxide in 50mL of deionized water, and performing ultrasonic treatment at 50kHz for 45min to obtain a graphene oxide dispersion liquid, which is marked as a dispersion liquid A (the concentration of the graphene oxide dispersion liquid in the embodiment is 8 mg/mL); adding 20mg of dodecyl glucoside into the dispersion liquid A, and shearing the dispersion liquid A for 3min at 2500r/min to generate uniform microbubbles so as to obtain graphene oxide microbubble aggregates B; ultrasonically cleaning a polyurethane sponge cube (15mm multiplied by 15mm) by acetone and absolute ethyl alcohol respectively, drying at 80 ℃ to remove water in the sponge, and completely immersing the sponge cube into graphene oxide microbubble aggregates B to prepare a composite sponge;
(2) freezing the composite sponge in the step (1) in liquid nitrogen at-196 ℃, and then immediately freeze-drying for 12h at-50 ℃ to obtain graphene oxide/polyurethane composite sponge;
(3) and (3) reducing the graphene oxide/polyurethane composite sponge in the step (2) in hydrazine hydrate steam at 90 ℃ for 5h, and drying in vacuum to obtain the super-hydrophobic reduced graphene oxide/polyurethane sponge composite material.
Example 2
The super-hydrophobic material in this embodiment includes a reduced graphene oxide/polyurethane sponge composite.
The preparation method of the super-hydrophobic material comprises the following steps:
(1) dispersing 0.4g of graphene oxide in 50mL of deionized water, and performing ultrasonic treatment at 50kHz for 45min to obtain a graphene oxide dispersion liquid, which is marked as a dispersion liquid A (the concentration of the graphene oxide dispersion liquid in the embodiment is 8 mg/mL); adding 20mg of dodecyl glucoside into the dispersion liquid A, and then shearing the dispersion liquid A for 3min at 2500r/min to uniformly generate microbubbles so as to obtain graphene oxide microbubble aggregates B; ultrasonically cleaning a polyurethane sponge cube (15mm multiplied by 15mm) by acetone and absolute ethyl alcohol respectively, drying at 80 ℃ to remove water in the sponge, and completely immersing the sponge cube into graphene oxide microbubble aggregates B to prepare a composite sponge;
(2) freezing the composite sponge in the step (1) in liquid nitrogen at the freezing temperature of-196 ℃, and then carrying out freeze drying for 12h at the temperature of-50 ℃ of a freeze-dried machine cold trap to obtain graphene oxide/polyurethane composite sponge through freeze drying;
(3) and (3) reducing the graphene oxide/polyurethane composite sponge in the step (2) in hydrazine hydrate steam at the temperature of 80 ℃ for 10h, and drying in vacuum to obtain the super-hydrophobic reduced graphene oxide/polyurethane sponge composite material.
Example 3
The super-hydrophobic material in this embodiment includes a reduced graphene oxide/polyurethane sponge composite.
The preparation method of the super-hydrophobic material comprises the following steps:
(1) dispersing 0.4g of graphene oxide in 50mL of deionized water, and performing ultrasonic treatment at 50kHz for 45min to obtain a graphene oxide dispersion liquid, which is marked as a dispersion liquid A (the concentration of the graphene oxide dispersion liquid in the embodiment is 8 mg/mL); adding 20mg of dodecyl glucoside into the dispersion liquid A, and then shearing the dispersion liquid A for 3min at 2500r/min to uniformly generate microbubbles so as to obtain graphene oxide microbubble aggregates B; ultrasonically cleaning a polyurethane sponge cube (15mm multiplied by 15mm) by acetone and absolute ethyl alcohol respectively, drying at 80 ℃ to remove water in the sponge, and completely immersing the sponge cube into graphene oxide microbubble aggregates B to prepare a composite sponge;
(2) immediately freezing the composite sponge in the step (1) in liquid nitrogen at-196 ℃, and then carrying out freeze drying for 12h at-50 ℃ to obtain graphene oxide/polyurethane composite sponge;
(3) and (3) placing the graphene oxide/polyurethane composite sponge in the step (2) in hydrazine hydrate steam at 120 ℃ for reduction for 2h, and drying in vacuum to obtain the super-hydrophobic reduced graphene oxide/polyurethane composite material.
Example 4
A sensor comprises the super-hydrophobic material prepared in embodiment 1, and further comprises two copper sheet electrodes and conductive silver paste, wherein the two copper sheet electrodes are respectively located on two sides of the super-hydrophobic material, and the conductive silver paste is filled between the copper sheet electrodes and the super-hydrophobic material.
The sensor is prepared by adopting the following preparation method: and coating conductive silver paste on two opposite surfaces of the super-hydrophobic material, bonding a copper sheet electrode, and packaging to obtain the sensor, wherein the sensor is a super-hydrophobic reduced graphene oxide/polyurethane sponge stress strain sensor.
Comparative example 1
The preparation method of the reduced graphene oxide/polyurethane composite material in comparative example 1 is substantially the same as that of example 1, except that the freezing temperature of comparative example 1 in step (2) is-10 ℃, and the remaining steps are the same as those of example 1.
Comparative example 2
The reduced graphene oxide/polyurethane composite of comparative example 2 was prepared in substantially the same manner as in example 1, except that the freezing temperature of comparative example 2 in step (2) was-80 ℃, and the remaining steps were the same as in example 1.
Comparative example 3
The method for preparing the reduced graphene oxide/polyurethane composite material in comparative example 3 is substantially the same as that of example 1, except that the reducing agent and the reduction manner are different, that is, in comparative example 3, ascorbic acid is added as the reducing agent in step (2), and the reduction temperature and the reduction time in step (3) are used, and the rest of the steps are the same as those of example 1.
Comparative example 4
A sensor comprises the reduced graphene oxide/polyurethane composite material prepared in the comparative example 1, and further comprises two copper sheet electrodes and conductive silver paste, wherein the two copper sheet electrodes are respectively located on two sides of the reduced graphene oxide/polyurethane composite material, and the conductive silver paste is filled between the copper sheet electrodes and the reduced graphene oxide/polyurethane composite material.
The sensor is prepared by adopting the following preparation method: and coating conductive silver paste on two opposite surfaces of the reduced graphene oxide/polyurethane composite material, bonding a copper sheet electrode, and packaging to obtain the sensor, wherein the sensor is a reduced graphene oxide/polyurethane sponge stress-strain sensor.
Comparative example 5
A sensor comprises the reduced graphene oxide/polyurethane composite material prepared in the comparative example 2, and further comprises two copper sheet electrodes and conductive silver paste, wherein the two copper sheet electrodes are respectively located on two sides of the reduced graphene oxide/polyurethane composite material, and the conductive silver paste is filled between the copper sheet electrodes and the reduced graphene oxide/polyurethane composite material.
The sensor is prepared by adopting the following preparation method: and coating conductive silver paste on two opposite surfaces of the reduced graphene oxide/polyurethane composite material, bonding a copper sheet electrode, and packaging to obtain the sensor, wherein the sensor is a reduced graphene oxide/polyurethane sponge stress-strain sensor.
Comparative example 6
A sensor comprises the reduced graphene oxide/polyurethane composite material prepared in the comparative example 3, and further comprises two copper sheet electrodes and conductive silver paste, wherein the two copper sheet electrodes are respectively located on two sides of the reduced graphene oxide/polyurethane composite material, and the conductive silver paste is filled between the copper sheet electrodes and the reduced graphene oxide/polyurethane composite material.
The sensor is prepared by adopting the following preparation method: and coating conductive silver paste on two opposite surfaces of the reduced graphene oxide/polyurethane composite material, bonding a copper sheet electrode, and packaging to obtain the sensor, wherein the sensor is a reduced graphene oxide/polyurethane sponge stress-strain sensor.
Implementing effect verification
(1) And (3) testing the sensitivity of the sensor:
the graphs of the resistance change rate with respect to strain at a constant rate of 10mm/min of the sensors of example 4, comparative example 4 and comparative example 5 were recorded using an electronic universal tester model KJ-1065 of china kokey ltd, and the test results are shown in fig. 1. The sensitivity of the reduced graphene oxide/polyurethane sponge stress-strain sensor prepared at the freezing temperature of-10 ℃ and-80 ℃ is 0.2-0.5 when the three groups of samples are subjected to micro pressure (the strain epsilon is less than 10%), and the maximum sensitivity of the reduced graphene oxide/polyurethane sponge stress-strain sensor at the freezing temperature of-196 ℃ can reach 3.8.
FIG. 2 is a graph of the rate of change of resistance of the sensor in example 4 during loading and unloading. When the sensor prepared in embodiment 4 is compressed to 10% strain, 30% strain and 50% strain, the rate of change of the resistance is approximately linearly and continuously changed along with the change of the strain, and the resistance value after unloading corresponds to the resistance value in the initial state, which indicates that the sensor can monitor different strains, so that the stress-strain sensor based on reduced graphene oxide/polyurethane sponge can meet the application requirements in different scenes.
FIG. 3 is a graph of the rate of change of resistance of the sensor during strain versus time in example 4. FIG. 3 also includes a partial enlarged view of the resistance change rate curve over time between 5.32 and 5.42. As can be seen from fig. 3, the response time of the sensor is as low as 45ms when the strain reaches 40%, which indicates that the sensor has the characteristic of fast response to the strain.
(2) And (3) micro-morphology testing:
fig. 4, 5, and 6 are scanning electron micrographs of example 1, comparative example 1, and comparative example 2, respectively. As can be seen from fig. 4 and 5, the reduced graphene oxide/polyurethane sponge composite prepared at the freezing temperature of-10 ℃ and-80 ℃ still can be observed to form agglomerated reduced graphene oxide after the micro-bubbles are broken due to the insufficient cooling rate. And when the freeze-drying temperature is-196 ℃, the cooling rate is fast enough, and the microbubble structure of the graphene oxide is almost completely fixed by the ice crystals.
(3) And (3) hydrophobic property test:
FIG. 7 is a static hydrophobic angle measurement pattern of example 1, and FIG. 8 is a static hydrophobic angle measurement pattern of comparative example 3. As can be seen from fig. 7 and 8: the water drops are spherical on the surface of the reduced graphene oxide/polyurethane sponge composite material in example 1, the static water contact angle is measured to be 152.5 degrees, and the reduced graphene oxide/polyurethane sponge composite material in example 2 and example 3 is super-hydrophobic (more than 150 degrees). And the water drop is hemispherical on the surface of the reduced graphene oxide/polyurethane sponge composite material in the comparative example 3, and the static water contact angle is 121.6 degrees, so that the composite material is hydrophobic but has no super-hydrophobicity.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (1)
1. A sensor, characterized by: the sensor comprises a superhydrophobic material; the super-hydrophobic material comprises a reduced graphene oxide/polyurethane sponge composite material; the water contact angle of the superhydrophobic material is >150 °; the preparation method of the super-hydrophobic material comprises the following steps: s1: mixing the graphene oxide aggregate with polyurethane sponge to prepare composite sponge; s2: freezing the composite sponge, and then reacting with a reducing agent to prepare the super-hydrophobic material; the preparation method of the graphene oxide aggregate comprises the following steps: mixing and reacting the graphene oxide dispersion liquid with dodecyl glucoside to prepare a graphene oxide aggregate; the graphene oxide aggregate is in a micro-bubble shape; the freezing step in the step S2 is to freeze by adopting liquid nitrogen; the reducing agent is hydrazine hydrate; in the step S2, the reaction temperature is 50-120 ℃.
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