CN114689217B - Flexible pressure-sensitive layer, preparation method and application - Google Patents
Flexible pressure-sensitive layer, preparation method and application Download PDFInfo
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- CN114689217B CN114689217B CN202210328195.7A CN202210328195A CN114689217B CN 114689217 B CN114689217 B CN 114689217B CN 202210328195 A CN202210328195 A CN 202210328195A CN 114689217 B CN114689217 B CN 114689217B
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- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
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Classifications
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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
- G01L1/14—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators
- G01L1/142—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators using capacitors
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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
- G01L1/14—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators
- G01L1/142—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators using capacitors
- G01L1/148—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators using capacitors using semiconductive material, e.g. silicon
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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
- G01L1/16—Measuring force or stress, in general using properties of piezoelectric devices
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Abstract
The invention provides a flexible pressure sensitive layer, a preparation method and application thereof. The flexible pressure sensitive layer is prepared by the preparation method and is applied to the capacitive flexible pressure sensor. The invention utilizes the property that the piezoelectric ceramic with high dielectric coefficient can generate stronger polarized electric field, controls the arrangement of nano particles in the pressure sensitive layer under the condition of applying conventional voltage, and improves the dielectric constant of the pressure sensitive layer. The capacitive flexible pressure sensor which consists of the pressure sensitive layer and has high sensitivity and wide measuring range is obtained. The support is provided for developing the flexible pressure sensor with low power consumption, high performance and low cost which are needed in the fields of the Internet of things and the artificial intelligence.
Description
Technical Field
The invention relates to the technical field of pressure detection, in particular to the field of flexible sensors, and specifically relates to a flexible pressure-sensitive layer, a preparation method and application.
Background
Flexible pressure sensors generally include two flexible electrodes and a flexible pressure sensitive layer. The flexible pressure sensor has the advantages of high sensitivity, short response time, wide detection range and the like, and is widely applied to a plurality of emerging wearable flexible electronic devices in recent years, such as human body movement monitoring equipment, medical health equipment and the like. However, capacitive flexible pressure sensors composed of conventional metal and semiconductor materials as pressure sensitive layers are generally limited to lower toughness and flexibility, and are poor in wearing comfort, and are difficult to meet the demands of the fields of electronic skin, smart clothing, implantation equipment, and the like. Under the premise of development of new generation flexible materials and sensing technology, the pressure sensitive layer with good development adaptability, accurate sensitivity, good stability, high response and low cost gradually becomes the development direction of the flexible pressure sensor.
However, it remains difficult to manufacture flexible sensors with high resolution, accurate sensitivity, ultra-wide measurement range, rapid response, and the ability to detect complex signals at low cost. One common defect of the existing flexible pressure sensor is that the measurement range is small, after the pressure reaches a certain value, the slope of the sensitivity curve of the sensor is rapidly reduced, so that the linearity of the sensor is reduced, and the other defect is that the preparation process of the pressure sensitive layer is complex and has relatively large environmental pollution from the aspect of environmental protection. Therefore, it is necessary to further expand the measurement range of the flexible pressure sensor, improve the linearity thereof and simplify the preparation process and flow of the pressure sensitive layer thereof.
Disclosure of Invention
The invention provides a flexible pressure-sensitive layer, a preparation method and application thereof for solving the technical problems.
The invention is realized by adopting the following technical scheme:
a method of making a flexible pressure sensitive layer, the method comprising:
preparing a mold, wherein the mold comprises a side wall and a bottom wall, and a cavity is formed by the side wall and the bottom wall;
pasting piezoelectric ceramics in the die, respectively pasting the piezoelectric ceramics on one pair of opposite side walls of the die in the cavity, wherein the piezoelectric ceramics respectively comprise extraction electrodes penetrating through the side walls of the attached die;
preparing a blending solution, and mixing the nano particles, a solvent and a curing agent to obtain the blending solution;
transferring the blending liquid into the mould, dripping the blending liquid into the mould, and removing air in the blending liquid in the mould;
and solidifying the blending liquid, heating the blending liquid, and applying voltage through the piezoelectric ceramic until the blending liquid is solidified, so as to obtain the flexible pressure-sensitive layer.
Optionally, in the process of preparing the blend, the mass of the nanoparticles is 2% -35% of the mass of the solvent.
Optionally, in the process of preparing the blend, the nanoparticles are nano-metal particles or nano-dielectrics; the solvent is polydimethylsiloxane, polyester resin, epoxy resin, polyester resin, polyamide resin, unsaturated polyester resin, organic silicon resin, polyimide, rubber or ethylene-vinyl acetate copolymer.
Optionally, in the process of transferring the blending liquid into the mold, placing the mold into which the blending liquid is dripped into a vacuum kettle, vacuumizing the vacuum kettle, and removing air in the blending liquid in the mold.
Optionally, in the process of solidifying the blending liquid, an electric heating plate is adopted to heat the blending liquid, and the temperature of the electric heating plate is kept at 25-80 ℃ to heat the blending liquid in the die for 2-12 hours.
Optionally, in the process of solidifying the blending liquid, the value of the voltage applied by the piezoelectric ceramic is 1-4KV. The voltage is applied to the piezoelectric ceramic by applying a voltage to the extraction electrode on the piezoelectric ceramic. The invention also provides a flexible pressure-sensitive layer, which is prepared by adopting the method for preparing the flexible pressure-sensitive layer.
Optionally, the pressure-sensitive layer is a flexible substrate to which nanoparticles are added, and the nanoparticles are distributed in a chain shape in the flexible substrate.
The invention also provides a capacitive flexible pressure sensor which comprises an upper electrode, a pressure-sensitive layer and a lower electrode which are sequentially laminated, wherein the pressure-sensitive layer is prepared by adopting the preparation method of the flexible pressure-sensitive layer.
Optionally, the upper electrode and the lower electrode are made of metal materials and conductive organic materials.
The beneficial effects of the invention include: compared with the prior art, the invention utilizes the property that the piezoelectric ceramic with high dielectric coefficient can generate strong polarized electric field, and under the condition that conventional voltage is applied to the piezoelectric ceramic with high dielectric coefficient, the high dielectric ceramic provides strong electric field to control the distribution of nano particles doped in the pressure sensitive layer, so that the nano particles are orderly distributed in the pressure sensitive layer in a chain manner, the nano particles orderly distributed in the pressure sensitive layer enhance the coupling effect of the pressure sensitive layer under the action of pressure, thereby improving the dielectric property and the pressure sensitive property of the sensor formed by the pressure sensitive layer, and remarkably improving the sensitivity and the measurement range of the sensor.
Drawings
FIG. 1 is a perspective view of the internal structure of a mold for a capacitive flexible pressure sensor according to the present invention;
FIG. 2 is a cross-sectional view taken along section A-A of FIG. 1;
FIG. 3 is a top view of a mold in a capacitive flexible pressure sensor of the present invention;
fig. 4 is a flow chart of the preparation of a flexible pressure sensitive layer of the invention.
Description of the drawings
1. A first lead 2, a first layer of piezoceramic 3, a pressure sensitive layer 4, a second layer of piezoceramic
5. Second conducting wire
Detailed Description
In the following, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
As shown in fig. 4, a method of preparing a flexible pressure sensitive layer, the method of preparing comprising,
preparing a mold, wherein the mold comprises a side wall and a bottom wall, and a cavity is formed by the side wall and the bottom wall;
in this example, as shown in fig. 1 to 3, the mold is printed using a 3D printer, for example, and the size of the mold is 2cm×2cm×0.5cm. And through holes are formed in the opposite side walls and are used for leading out electrode leads for applying an electric field, and a cavity surrounded by the side walls and the bottom wall is used for containing the prepared blending liquid.
Pasting piezoelectric ceramics in the die, respectively pasting the piezoelectric ceramics on one pair of opposite side walls of the die in the cavity, wherein the piezoelectric ceramics respectively comprise extraction electrodes penetrating through the side walls of the attached die;
in this embodiment, as shown in fig. 1 to 3, the first piezoelectric ceramic 2 and the second piezoelectric ceramic 4 are respectively adhered to the inner wall of the mold, and the side of the piezoelectric ceramic having the metal coating is adhered to the inner wall of the mold, and then the first lead wire 1 and the second lead wire 5 are respectively connected to the metal layer of the first piezoelectric ceramic sheet 2 and the metal layer of the second piezoelectric ceramic sheet 4, and the first lead wire 1 and the second lead wire 5 are electrode leads for applying an electric field to the first piezoelectric ceramic 2 and the second piezoelectric ceramic 4.
Preparing a blending solution, and mixing the nano particles, a solvent and a curing agent to obtain the blending solution;
in this example, the nanoparticles, solvent and curing agent were mixed and stirred uniformly using a glass rod to obtain a blend. The mass of the nano particles is 2% -35% of the mass of the solvent. In the range of the mass ratio, the higher the doping mass ratio of the nano particles is, the larger the dielectric coefficient of the prepared pressure-sensitive layer is under the action of pressure, and the higher the dielectric coefficient is, so that the sensitivity of the sensor formed by the pressure-sensitive layer is higher. Such as nano-metal particles or nano-dielectrics; the solvent is polydimethylsiloxane, polyester resin, epoxy resin, polyester resin, polyamide resin, unsaturated polyester resin, organic silicon resin, polyimide, rubber or ethylene-vinyl acetate copolymer. In this embodiment, when the nanoparticles are nano metal particles, the mass of the nano metal particles is in the range of 2% -35% of the mass of the solvent, and the sensor composed of the pressure sensitive layer is a capacitive pressure sensor, and the smaller the ratio of the nano metal particles mass to the solvent mass, the more the sensor composed of the pressure sensitive layer tends to be a capacitive pressure sensor. When the mass of the nano metal particles exceeds the range of 2% -35% of the mass of the solvent, the sensor composed of the pressure sensitive layer is converted into a resistive pressure sensor. Thus in this embodiment, the mass of the nano-metal particles is limited to 2% -35% of the mass of the solvent. In this embodiment, the mass of the nano-metal particles is 2% of the mass of the solvent. The solvent is a flexible, malleable film material, so any of the above materials is selected, in this embodiment, the solvent is polydimethylsiloxane.
Transferring the blending liquid into the mould, dripping the blending liquid into the mould, and removing air in the blending liquid in the mould;
in this embodiment, as shown in fig. 1 to 3, the blending liquid is dripped into the cavity of the mold by using a rubber head dropper, the mold dripped with the blending liquid is placed into a vacuum kettle, and the vacuum kettle is vacuumized by using an air pump, so that air in the blending liquid in the mold is removed.
And solidifying the blending liquid, heating the blending liquid, and applying voltage through the piezoelectric ceramic until the blending liquid is solidified, so as to obtain the flexible pressure-sensitive layer.
And heating the blending liquid in the die for 2-12 hours by adopting an electric heating plate in the process of curing the blending liquid and keeping the temperature of the electric heating plate at 25-80 ℃. The higher the temperature of the electric heating plate, the shorter the time required for the blend to cure.
And in the process of solidifying the blending liquid, the applied voltage value of the piezoelectric ceramic is 1-4KV. The larger the value of the applied voltage to the piezoelectric ceramic, the shorter the time required for curing the blend. According to the property that the piezoelectric ceramic can generate a high polarization electric field, the piezoelectric ceramic with the value of the applied voltage of 1.5KV provides the effect of controlling the arrangement of the nano particles in the pressure sensitive layer by the strong electric field, and is better than the effect of controlling the arrangement of the nano particles in the pressure sensitive layer by the high voltage with the value of the applied voltage of 10KV of a common electrode.
In the process of solidifying the blend, the temperature of the electric heating plate and the value of the voltage applied by the piezoelectric ceramics are kept constant.
In this embodiment, the electric heating plate is used to heat the blending solution, the value of the voltage applied by the piezoelectric ceramic is 1KV under the condition of selecting room temperature, that is, under the condition that the heating plate is kept at 25 ℃, and under the condition that the temperature of the heating plate is kept constant at 25 ℃ and the value of the voltage applied by the piezoelectric ceramic is 1KV, the curing of the blending solution needs 12 hours to be completely cured, and the completely cured blending solution is taken out from the mold, so as to obtain the flexible pressure-sensitive layer.
In this embodiment, as shown in fig. 1 to 3, by the above preparation method, a flexible pressure-sensitive layer 3 is obtained, the pressure-sensitive layer 3 is a flexible substrate to which nanoparticles are added, and the nanoparticles are distributed in a chain shape in the flexible substrate.
In this embodiment, a capacitive flexible pressure sensor is formed by obtaining a flexible pressure-sensitive layer, which includes an upper electrode, a pressure-sensitive layer 3, and a lower electrode laminated in this order, the pressure-sensitive layer being manufactured by a method of manufacturing a flexible pressure-sensitive layer. The upper electrode and the lower electrode are made of metal materials and conductive organic materials. In this embodiment, the lower electrode and the upper electrode are made of copper foil materials, have good conductivity and anti-static shielding characteristics, and are adhered to the upper surface and the lower surface of the pressure sensitive layer 3 to form a flexible capacitive pressure sensor structure.
In the preparation process, the arrangement of the nano particles in the pressure sensitive layer is controlled by utilizing the high dielectric coefficient enhanced electric field of the piezoelectric ceramic plate, so that the nano particles are distributed in the pressure sensitive layer in a chain shape. The principle of dielectric polarized particle coupling is utilized to explain that the pressure-sensitive layer with the nano particles distributed in a chain shape has higher dielectric strain coefficient compared with the conventional pressure-sensitive layer. Under the action of external pressure, the distance between electric dipoles formed by nano particles in the pressure-sensitive layer is reduced, when the distance is reduced to a certain degree, the polarization directions of the nano particles tend to be in the same direction, and the coupling effect between the dipoles is obviously enhanced, so that the dielectric strain coefficient of the pressure-sensitive layer is increased. Thereby achieving an improvement in the sensitivity of the sensor composed of the pressure-sensitive layer. Under the action of pressure, the thickness of the pressure-sensitive layer is reduced, and simultaneously the dielectric coefficient of the equivalent pressure-sensitive layer is increased, so that the capacitance value of the sensor formed by the pressure-sensitive layer is increased. Thus, the sensitivity and pressure measurement range of the capacitive flexible pressure sensor composed of the pressure sensitive layer will be significantly improved.
The pressure sensitive layer can be prepared by the combined action of the two aspects, and the sensitivity of the capacitive flexible pressure sensor formed by the pressure sensitive layer is higher than that of a plurality of existing capacitive flexible pressure sensors, and the linearity is obviously better than that of other capacitive flexible pressure sensors, so that the pressure measuring range of the capacitive flexible pressure sensor formed by the pressure sensitive layer is expanded; the high sensitivity test range of the flexible pressure sensor in the prior report is generally 0-10kPa, and the measurement range of the capacitive flexible pressure sensor formed by the pressure sensitive layer can reach at least 250kPa.
Example 2
The embodiment provides a flexible pressure-sensitive layer, a preparation method and application thereof. This embodiment 2 differs from embodiment 1 in that:
in the process of preparing the blend, the nano particles are selected as nano dielectrics, the mass of the nano dielectrics is 25% of the mass of the solvent, and the solvent is epoxy resin.
The curing conditions employed during curing of the blend are different. Specifically, under the condition that the heating plate is kept at 60 ℃, the value of the voltage applied to the extraction electrode on the piezoelectric ceramic is 2.5KV, under the condition that the temperature of the heating plate at 60 ℃ and the value of the voltage applied to the piezoelectric ceramic are kept constant and are 2.5KV, 4 hours are required for curing the blending liquid to be completely cured, and the completely cured blending liquid is taken out of the die, so that the flexible pressure-sensitive layer is obtained.
Example 3
The embodiment provides a flexible pressure-sensitive layer, a preparation method and application thereof. This embodiment 3 differs from embodiment 2 in that:
in the process of preparing the blending liquid, the nano particles are selected as nano metal particles, the mass of the nano metal particles is 5% of the mass of the solvent, and the solvent is polyester resin.
The curing conditions employed during curing of the blend are different. Specifically, under the condition that the heating plate is kept at 80 ℃, the value of the voltage applied by the piezoelectric ceramic is 4KV, the temperature of the heating plate at 80 ℃ is kept constant, and under the condition that the value of the voltage applied by the piezoelectric ceramic is 4KV, the curing of the blending liquid takes 2 hours to be completely cured, and the completely cured blending liquid is taken out of the die, so that the flexible pressure-sensitive layer is obtained.
While the fundamental and principal features of the invention and advantages of the invention have been shown and described, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. A method of preparing a flexible pressure sensitive layer, the method comprising:
preparing a mold, wherein the mold comprises a side wall and a bottom wall, and a cavity is formed by the side wall and the bottom wall;
pasting piezoelectric ceramics in the die, respectively pasting the piezoelectric ceramics on one pair of opposite side walls of the die in the cavity, wherein the piezoelectric ceramics respectively comprise extraction electrodes penetrating through the side walls of the attached die;
preparing a blending solution, and mixing the nano particles, a solvent and a curing agent to obtain the blending solution;
transferring the blending liquid into the mould, dripping the blending liquid into the mould, and removing air in the blending liquid in the mould;
and solidifying the blending liquid, heating the blending liquid, and applying voltage through the piezoelectric ceramic until the blending liquid is solidified, so as to obtain the flexible pressure-sensitive layer.
2. The method for preparing a flexible pressure sensitive layer according to claim 1, wherein the mass of the nanoparticles is 2% -35% of the mass of the solvent in the process of preparing the blend.
3. The method for preparing a flexible pressure sensitive layer according to claim 1, wherein in the process of preparing the blend, the nanoparticles are nano metal particles or nano dielectrics; the solvent is polydimethylsiloxane, polyester resin, epoxy resin, polyester resin, polyamide resin, unsaturated polyester resin, organic silicon resin, polyimide, rubber or ethylene-vinyl acetate copolymer.
4. The method for producing a flexible pressure-sensitive layer according to claim 1, wherein in transferring the blend into the mold, the mold into which the blend is dropped is placed into a vacuum vessel, and the vacuum vessel is evacuated to remove air in the blend in the mold.
5. The method for preparing a flexible pressure-sensitive layer according to claim 1, wherein the blend is heated by an electric plate during curing the blend, and the blend in the mold is heated for 2 to 12 hours while maintaining the temperature of the electric plate at 25 to 80 ℃.
6. The method for producing a flexible pressure-sensitive layer according to claim 1, wherein the piezoelectric ceramic has a value of applied voltage of 1 to 4KV during curing of the blend.
7. A flexible pressure sensitive layer, characterized in that it is produced by the method for producing a flexible pressure sensitive layer according to any one of claims 1 to 6.
8. The flexible pressure sensitive layer of claim 7, wherein the pressure sensitive layer is a flexible substrate to which nanoparticles are added, the nanoparticles being distributed in a chain in the flexible substrate.
9. A capacitive flexible pressure sensor comprising an upper electrode, a pressure sensitive layer and a lower electrode laminated in this order, the pressure sensitive layer being produced by the method for producing a flexible pressure sensitive layer according to any one of claims 1 to 6.
10. The capacitive flexible pressure sensor of claim 9, wherein said upper and lower electrodes are made of a metallic material or a conductive organic material.
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