CN111750975B - Flexible vibration sensor with piezoresistive effect and preparation method thereof - Google Patents
Flexible vibration sensor with piezoresistive effect and preparation method thereof Download PDFInfo
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- CN111750975B CN111750975B CN202010567988.5A CN202010567988A CN111750975B CN 111750975 B CN111750975 B CN 111750975B CN 202010567988 A CN202010567988 A CN 202010567988A CN 111750975 B CN111750975 B CN 111750975B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01H—MEASUREMENT OF MECHANICAL VIBRATIONS OR ULTRASONIC, SONIC OR INFRASONIC WAVES
- G01H11/00—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties
- G01H11/06—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties by electric means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- 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
Abstract
A flexible vibration sensor with piezoresistive effect belongs to the technical field of flexible functional electronic materials and novel sensors. The flexible vibration sensor comprises a sensitive material and a conductive electrode, wherein the sensitive material comprises a carbon nanotube film and zinc oxide particles attached to the carbon nanotube film, the thickness of the carbon nanotube film is 50-80 mu m, the size of the zinc oxide particles is 200-500 nm, and the mass ratio of the carbon nanotubes to the zinc oxide is (12-15): 1. The sensitive material of the sensor comprises a carbon nanotube film and zinc oxide particles. On one hand, the carbon nanotube film at the bottom layer has a three-dimensional conductive network structure, and the vibration of an object caused by impact causes the surface of the sensitive material to vibrate and deform, so that the resistance of the three-dimensional conductive network of the carbon nanotube is changed; on the other hand, zinc oxide has a piezoresistive effect, and the resistance of the zinc oxide layer can be changed due to the vibration of an object caused by impact, so that the sensitivity of the vibration sensor is effectively enhanced.
Description
Technical Field
The invention belongs to the technical field of flexible functional electronic materials and novel sensors, and particularly relates to a flexible vibration sensor with piezoresistive effect and distance measurement capability and a preparation method thereof.
Background
Mechanical sensors are sensors that convert mechanical signals into other detection signals, and mainly include metal foil strain gauges, piezoelectric wafers (typically lead zirconate titanate), optical fibers, electromagnetic acoustic transducers, and piezoelectric polymer-based sensors (e.g., polyvinylidene fluoride and its copolymers). The strain gauge and the piezoelectric polymer film type sensor only respond to low-frequency spectrum signals, and the sensitivity is low; the piezoelectric wafer cannot be bent and stretched, cannot be used for a curved surface or a complex surface, and has large weight and volume; optical fiber based sensors are fragile and embedding optical fibers in structures such as laminated composites not only complicates the manufacturing process but also reduces the local strength of the composite; polyvinylidene fluoride and its copolymers can achieve large area coverage and conform well to curved surfaces, but its piezoelectric coefficient is generally low, resulting in low sensitivity. Therefore, there is an urgent need to develop a new sensor that combines flexibility (adaptability to bending structures), weight (low additional mass to the inspection structure), bulk (negligible degradation to the mechanical properties of the inspection structure), and the like.
The flexible vibration sensor converts vibration into a detection signal, can be applied to voice recognition, azimuth measurement and distance measurement, and is one of mechanical sensors.
Disclosure of Invention
The invention aims to provide a flexible vibration sensor with piezoresistive effect, a preparation method thereof and application in azimuth measurement, aiming at solving the problems of the existing mechanical sensors in the background technology.
In order to achieve the purpose, the invention adopts the following technical scheme:
the flexible vibration sensor with the piezoresistive effect comprises a sensitive material and a conductive electrode, and is characterized in that the sensitive material comprises a carbon nanotube film and zinc oxide particles attached to the carbon nanotube film, wherein the thickness of the carbon nanotube film is 50-80 mu m, the size of the zinc oxide particles is 200-500 nm, and the mass ratio of the carbon nanotubes to the zinc oxide is (12-15): 1.
Further, the sensitive material is obtained by depositing zinc oxide on the carbon nanotube film after the surface plasma treatment by using an Atomic Layer Deposition (ALD) technology.
A preparation method of a flexible vibration sensor with piezoresistive effect is characterized by comprising the following steps:
2, depositing a zinc oxide layer on the carbon nanotube film processed in the step 1 by adopting an atomic layer deposition technology; taking diethyl zinc as a zinc source and deionized water as an oxygen source, wherein the deposition temperature is 140-160 ℃, and the cycle number is 100-500; wherein, a cycle includes: diethyl zinc pulse is carried out for 0.02s to 0.03s, nitrogen cleaning is carried out for 8 to 10s, deionized water pulse is carried out for 0.02s to 0.04s, and nitrogen cleaning is carried out for 8 to 10 s;
and 3, preparing an electrode to obtain the flexible vibration sensor.
Further, the thickness of the carbon nanotube film is 50-80 microns.
Further, the power of the plasma treatment in the step 1 is 290-320W, the air pressure is 10-50 Pa, and the time is 10-15 min.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a flexible vibration sensor with piezoresistive effect, and the sensitive material of the flexible vibration sensor comprises a carbon nanotube film and zinc oxide particles attached to the carbon nanotube film. On one hand, the carbon nanotube film at the bottom layer has a three-dimensional conductive network structure, and the vibration of an object caused by impact causes the surface of the sensitive material to vibrate and deform, so that the resistance of the three-dimensional conductive network of the carbon nanotube is changed; on the other hand, zinc oxide has a piezoresistive effect, and the resistance of the zinc oxide layer can be changed due to the vibration of an object caused by impact, so that the sensitivity of the vibration sensor is effectively enhanced.
2. According to the invention, the zinc oxide layer is prepared by adopting an atomic layer deposition technology, the piezoresistive performance and the environmental adaptability of the carbon nano tube subjected to the atomic layer deposition treatment are greatly improved, and the piezoresistive effect of the sensitive material is enhanced.
Drawings
FIG. 1 is a resistance change rate curve of a flexible vibration sensor (b) obtained in the example and a vibration sensor (a) prepared by using the hydroxylated carbon nanotube film treated in the step 2 as a sensitive material;
FIG. 2 is a photograph of the contact angles of step 1 carbon nanotube film (a) and step 2 plasma treated hydroxylated carbon nanotube film (b);
FIG. 3 shows the result of the strain resistance test of the zinc oxide @ carbon nanotube film obtained in step 3 when the tensile length is 0.1mm, i.e., the strain is 0.5%;
FIG. 4 shows the result of the strain resistance test of the zinc oxide @ carbon nanotube film obtained in step 3 when the tensile length is 0.5mm, i.e., the strain is 2.5%;
FIG. 5 shows the result of the strain resistance test of the zinc oxide @ carbon nanotube film obtained in step 3 when the tensile length is 1mm, i.e., the strain is 5%;
FIG. 6 shows the results of the strain resistance test of the zinc oxide @ carbon nanotube film obtained in step 3 when the tensile length is 2mm, i.e., the strain is 10%;
FIG. 7 shows the results of the strain resistance test of the zinc oxide @ carbon nanotube film obtained in step 3 at a tensile length of 3mm, i.e., a strain of 15%;
FIG. 8 is a resistance change rate curve of the zinc oxide @ carbon nanotube film obtained in step 3 under different strains;
FIG. 9 is a graph showing the rate of change of resistance of the flexible vibration sensor obtained in the example when the sensor is impacted;
fig. 10 is a resistance change rate versus distance of the flexible vibration sensor according to the embodiment.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
Examples
A preparation method of a flexible vibration sensor with piezoresistive effect is characterized by comprising the following steps:
step 3, depositing a zinc oxide layer on the carbon nanotube film processed in the step 1 by adopting an atomic layer deposition technology to obtain a zinc oxide @ carbon nanotube film; diethyl zinc is used as a zinc source, deionized water is used as an oxygen source, the deposition temperature is 150 ℃, and the cycle number is 280. Wherein, a cycle includes: diethyl zinc pulses for 0.02s, nitrogen purging for 8s (to remove ethane generated by the reaction and diethyl zinc gas molecules not participating in the reaction), deionized water pulses for 0.02s, and nitrogen purging for 8s (to remove ethane generated by the reaction and water molecules not participating in the reaction); firstly, diethyl zinc enters a reaction cavity to perform substitution reaction with functional group hydroxyl on a carbon nanotube film to generate ethane, meanwhile, ethyl zinc is attached to the surface of the carbon nanotube through a zinc-oxygen bond, then deionized water enters the reaction cavity, the hydroxyl in the water and the ethyl on a zinc atom perform substitution reaction to generate ethane, and at the moment, a carbon-oxygen-zinc-hydroxyl structure is formed on a hydroxyl site on the surface of the carbon nanotube, so that the circulation process of one atomic layer is completed;
and 4, cutting the zinc oxide @ carbon nanotube film obtained in the step 3 into a certain shape, coating an electrode on the film, and welding a lead to obtain the flexible vibration sensor.
The flexible vibration sensor obtained in example and the vibration sensor prepared by using the hydroxylated carbon nanotube film treated in step 2 only as a sensitive material were tested for piezoresistive effect, the flexible sensor was placed in a pressure gauge ZQ-770, a periodic triangular wave force (0-4kgf) was applied, and the resistance data of the sample was recorded using a digital source meter 2450. FIG. 1 is a resistance change rate curve of a flexible vibration sensor (b) obtained in the example and a vibration sensor (a) prepared by using the hydroxylated carbon nanotube film treated in the step 2 as a sensitive material; as can be seen from fig. 1, with the increase of pressure, the resistance of the vibration sensor prepared by using the hydroxylated carbon nanotube film processed in step 2 as the sensitive material is rapidly decreased, the pressure is gradually removed, the resistance is recovered, and a periodic peak in the graph is formed, and the resistance change rate is calculated to be 1.99%, while the resistance change rate of the flexible vibration sensor obtained in the example is 5.12%. Meanwhile, the initial value of the zero load resistance of the carbon nanotube film is 52.7 ohms, and the zero load resistance of the zinc oxide @ carbon nanotube film is increased to 69.3 ohms, which shows that the zinc oxide is successfully deposited on the carbon nanotube film, so that the resistance of the zinc oxide @ carbon nanotube film is increased, and the piezoresistive effect is increased.
FIG. 2 is a photograph of the contact angles of step 1 carbon nanotube film (a) and step 2 plasma treated hydroxylated carbon nanotube film (b); as can be seen from fig. 2, the contact angle of the carbon nanotube film before plasma treatment was 125 °, which shows good superhydrophobic property, while the contact angle of the hydroxylated carbon nanotube film after plasma treatment was 50 °, which indicates that the plasma treatment improved the hydrophilicity of the carbon nanotube film and introduced hydrophilic functional group hydroxyl.
And (3) performing a strain resistance test on the zinc oxide @ carbon nanotube film (cut into a square of 2cm multiplied by 2 cm) obtained in the step (3) by using a stress meter ZQ-990. The zinc oxide @ carbon nanotube film is fixed on a lower knob iron block of a stress gauge, two ends of the zinc oxide @ carbon nanotube film are connected to a digital source meter 2450 through leads so as to measure the resistance value of the film while applying stress, and the test process is as follows: the upper knob iron block stretches the film at a constant speed of 50mm/min upwards until reaching the set stretching length, and then compresses the film to the original length at a constant speed of 50mm/min downwards.
FIG. 3 shows the result of the strain resistance test of the zinc oxide @ carbon nanotube film obtained in step 3 when the tensile length is 0.1mm, i.e., the strain is 0.5%; the resistance of the film rises during stretching and falls during compression, and the ratio of the resistance value of the wave crest to the resistance value of the wave trough is subtracted by 1 to obtain the resistance change rate of the film under the stretching length. As can be seen from fig. 3, the zinc oxide @ carbon nanotube film obtained in step 3 had a resistance change rate of 0.33% at a tensile length of 0.1mm, i.e., a strain of 0.5%.
FIG. 4 shows the result of the strain resistance test of the zinc oxide @ carbon nanotube film obtained in step 3 when the tensile length is 0.5mm, i.e., the strain is 2.5%; as can be seen from fig. 4, the zinc oxide @ carbon nanotube film obtained in step 3 had a resistance change rate of 0.376% at a tensile length of 0.5mm, i.e., a strain of 2.5%.
FIG. 5 shows the result of the strain resistance test of the zinc oxide @ carbon nanotube film obtained in step 3 when the tensile length is 1mm, i.e., the strain is 5%; as can be seen from fig. 5, the zinc oxide @ carbon nanotube film obtained in step 3 had a resistance change rate of 0.46% when the tensile length was 1mm, i.e., when the strain was 5%.
FIG. 6 shows the results of the strain resistance test of the zinc oxide @ carbon nanotube film obtained in step 3 when the tensile length is 2mm, i.e., the strain is 10%; as can be seen from fig. 6, the zinc oxide @ carbon nanotube film obtained in step 3 had a resistance change rate of 0.56% when the tensile length was 2mm, i.e., when the strain was 10%.
FIG. 7 shows the results of the strain resistance test of the zinc oxide @ carbon nanotube film obtained in step 3 at a tensile length of 3mm, i.e., a strain of 15%; as can be seen from fig. 7, the zinc oxide @ carbon nanotube film obtained in step 3 had a rate of change in resistance of 1.17% when the tensile length was 3mm, i.e., when the strain was 15%.
Fig. 8 is a resistance change rate curve of the zinc oxide @ carbon nanotube film obtained in step 3 under different strains, and it can be seen from fig. 8 that the strain-resistance sensitivity of the zinc oxide @ carbon nanotube film is 0.0307 when the strain is in the range of 0.5% to 10%; the rate of change of resistance is more stable at strains less than 10% and increases sharply at strains of 15%, probably because the conductive network structure of the film is destroyed by the greater strain and the destruction process is irreversible, resulting in a sharp increase in the rate of change of resistance. In this example, the film was broken when the strain was 20%.
The sensor obtained in the embodiment is fixed on the plate to be tested, and the two ends of the sensor are connected with the digital source meter 2450 by leads to measure the resistance value. And marking points at intervals of 5cm from the sensor, placing a plastic pipe vertically fixed by an iron stand, and using a mode of dropping iron columns or glass beads from the free falling body of the plastic pipe to knock the iron plate as a vibration source. A point was taken 20cm from the sensor radius and the resistance was recorded with a digital source meter 2450 while falling (iron pillar).
Fig. 9 is a graph showing the rate of change of the resistance of the flexible vibration sensor obtained in the example at the time of impact. As can be seen from fig. 9, the resistance change rates at points on the same circumference 15cm from the sensor are very close, and the mean square deviation of the resistance change rates was calculated to be 3.96%. The smaller the mean square error, the higher the sensitivity of the sensor.
The sensor obtained in the embodiment is fixed on the plate to be tested, and the two ends of the sensor are connected with the digital source meter 2450 by leads to measure the resistance value. And marking points at intervals of 5cm from the sensor, placing a plastic pipe vertically fixed by an iron stand, and using a mode of dropping iron columns or glass beads from the free falling body of the plastic pipe to knock the iron plate as a vibration source. Respectively taking 5cm, 10cm and 15cm of the distance sensor as falling points at intervals of 5cm, and researching the relation between the piezoresistive effect and the distance of the flexible vibration sensor by impacting a single point for 5 times of averaging.
Fig. 10 is a resistance change rate versus distance of the flexible vibration sensor according to the embodiment. The falling body is small balls, when the sensor is 5cm, 10cm and 15cm away from the falling point, the resistance change rate is respectively 8.72%, 6.31% and 4.06%, and the resistance change rate of the sensor and the distance show good inverse proportion linear relation; for far excitation, the sensor response is small, while for near excitation, the sensor response is large. The rate of change of resistance of the sensor decreases with increasing distance, which can be used as a basis for practical ranging applications.
Claims (4)
1. A flexible vibration sensor with piezoresistive effect comprises a sensitive material and a conductive electrode, and is characterized in that the sensitive material comprises a carbon nanotube film and zinc oxide particles attached to the carbon nanotube film, wherein the thickness of the carbon nanotube film is 50-80 μm, the size of the zinc oxide particles is 200-500 nm, and the mass ratio of carbon nanotubes to zinc oxide is (12-15): 1;
the flexible vibration sensor with piezoresistive effect is prepared by adopting the following method:
step 1, preparing a carbon nanotube film by adopting a chemical vapor deposition method, and carrying out plasma treatment;
2, depositing a zinc oxide layer on the carbon nanotube film processed in the step 1 by adopting an atomic layer deposition technology; taking diethyl zinc as a zinc source and deionized water as an oxygen source, wherein the deposition temperature is 140-160 ℃, and the cycle number is 100-500; wherein, a cycle includes: diethyl zinc pulse is carried out for 0.02s to 0.03s, nitrogen cleaning is carried out for 8 to 10s, deionized water pulse is carried out for 0.02s to 0.04s, and nitrogen cleaning is carried out for 8 to 10 s;
and 3, preparing an electrode to obtain the flexible vibration sensor.
2. The flexible vibration sensor with piezoresistive effect according to claim 1, wherein the sensitive material is obtained by depositing zinc oxide on the carbon nanotube film after surface plasma treatment by atomic layer deposition technique.
3. A preparation method of a flexible vibration sensor with piezoresistive effect is characterized by comprising the following steps:
step 1, preparing a carbon nanotube film by adopting a chemical vapor deposition method, and carrying out plasma treatment;
2, depositing a zinc oxide layer on the carbon nanotube film processed in the step 1 by adopting an atomic layer deposition technology; taking diethyl zinc as a zinc source and deionized water as an oxygen source, wherein the deposition temperature is 140-160 ℃, and the cycle number is 100-500; wherein, a cycle includes: diethyl zinc pulse is carried out for 0.02s to 0.03s, nitrogen cleaning is carried out for 8 to 10s, deionized water pulse is carried out for 0.02s to 0.04s, and nitrogen cleaning is carried out for 8 to 10 s;
and 3, preparing an electrode to obtain the flexible vibration sensor.
4. The method for preparing a flexible vibration sensor with piezoresistive effect according to claim 3, wherein the plasma treatment power in step 1 is 290-320W, the air pressure is 10-50 Pa, and the time is 10-15 min.
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