CN116558701A - Field emission flexible pressure sensing film with high sensitivity and high precision and preparation method thereof - Google Patents
Field emission flexible pressure sensing film with high sensitivity and high precision and preparation method thereof Download PDFInfo
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- CN116558701A CN116558701A CN202210106317.8A CN202210106317A CN116558701A CN 116558701 A CN116558701 A CN 116558701A CN 202210106317 A CN202210106317 A CN 202210106317A CN 116558701 A CN116558701 A CN 116558701A
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Classifications
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- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C16/26—Deposition of carbon only
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/0041—Transmitting or indicating the displacement of flexible diaphragms
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract
The invention provides a field emission flexible pressure sensing film with high sensitivity and high precision and a preparation method thereof, and the field emission flexible pressure sensing film with high sensitivity and high precision has the characteristics that the field emission flexible pressure sensing film with high sensitivity and high precision comprises: the resin-embedded conductive vertical nanotube array film and the ultrathin single-component polymer elastic film, wherein the thickness of the ultrathin single-component polymer elastic film is less than 1 mu m. The application introduces a field emission mechanism in the field of pressure sensing, and uses the polymer elastomer with only a single component as an induction layer of external pressure to greatly reduce the system error, and simultaneously realizes high precision and high sensitivity.
Description
Technical Field
The invention belongs to the technical field of preparation of flexible electronic materials, and particularly relates to a field emission flexible pressure sensing film with high sensitivity and high precision and a preparation method thereof.
Background
A flexible electronic material that is an electrical signal. Meanwhile, the pressure sensor with high sensitivity and high precision can quantitatively sense tiny pressure information, so that the manipulator is endowed with more precise manipulation capability, and meanwhile, the manipulator can bring greater application possibility to a human-machine interaction interface, so that more abundant interaction information is generated between an operator and a machine through touch. At the same time, this technology is also considered an essential part of future meta-cosmic deployments.
A major obstacle to achieving both of these characteristics with conventional flexible sensors is that they rely on complex material systems, such as micro-nano structures or composite materials, to achieve high sensitivity. However, as the complexity increases, the random error in the read signal in the system increases, resulting in reduced accuracy. However, if extremely simple sensing materials are used to reduce random errors, high sensitivity cannot be achieved based on conventional sensor design considerations.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide a field emission flexible pressure sensing film having both high sensitivity and high accuracy, and a method for manufacturing the same. In the invention, a field emission mechanism is introduced in the pressure sensing field for the first time, and a polymer elastomer with only a single component is used as an external pressure sensing layer, so that the system error is greatly reduced, and meanwhile, high precision and high sensitivity are realized.
The invention provides a field emission flexible pressure sensing film with high sensitivity and high precision, which has the characteristics that: the resin-embedded conductive vertical nanotube array film and the ultrathin single-component polymer elastic film, wherein the thickness of the ultrathin single-component polymer elastic film is less than 1 mu m.
The field emission flexible pressure sensing film with high sensitivity and high precision provided by the invention can also have the following characteristics: wherein, the ultrathin single-component polymer elastic film is used as the induction layer, and the purity of the component is more than 90 percent.
The field emission flexible pressure sensing film with high sensitivity and high precision provided by the invention can also have the following characteristics: the elastic modulus of the resin-embedded conductive vertical nanotube array film is more than 5 times of that of the ultrathin single-component polymer elastic film, and the resin-embedded conductive vertical nanotube array film is arranged on the upper surface of the ultrathin single-component polymer elastic film.
The invention provides a preparation method of a field emission flexible pressure sensing film with high sensitivity and high precision, which has the characteristics that the preparation method comprises the following steps: step 1, preparing a conductive material with a vertical nanotube array structure; step 2, embedding the conductive material in epoxy resin, and slowly curing in a vacuum environment to obtain an embedded block; step 3, ultrathin slicing the embedded block along the direction perpendicular to the nanotube fiber of the conductive material to obtain a conductive vertical nanotube array film; step 4, spreading the conductive vertical nanotube array film on the surface of a conductive metal foil or other conductive films, and cleaning the surface of the conductive vertical nanotube array film by utilizing a plasma cleaning technology; step 5, spin-coating a sacrificial layer on the surface of the flat hard substrate, growing a layer of conductive electrode on the sacrificial layer by utilizing a magnetron sputtering technology, spin-coating diluted polymer elastomer on the surface of the conductive electrode by utilizing a spin-coating technology, slowly volatilizing a solvent of the diluted polymer elastomer at a low temperature, and curing the polymer to form a film to obtain an ultrathin single-component polymer elastic film; step 6, attaching the cleaned conductive vertical nanotube array film on the upper surface of the ultrathin single-component polymer elastic film, wetting the attaching surface by using ethanol, and removing bubbles and ethanol in the attaching surface under a vacuum condition to obtain a pressure sensing film; and 7, after electrode wires are led out from the pressure sensing film, packaging the pressure sensing film to obtain the field emission flexible pressure sensing film with high sensitivity and high precision, wherein the field emission flexible pressure sensing film with high sensitivity and high precision is the field emission flexible pressure sensing film with high sensitivity and high precision.
The preparation method of the field emission flexible pressure sensing film with high sensitivity and high precision provided by the invention can also have the following characteristics: in the step 1, a chemical vapor deposition method is used to prepare a conductive material, wherein the nanotube of the conductive material comprises at least one of a single-arm carbon nanotube and a multi-wall carbon nanotube, and the diameter of the nanotube of the conductive material is 1nm-300nm.
The preparation method of the field emission flexible pressure sensing film with high sensitivity and high precision provided by the invention can also have the following characteristics: wherein, in the step 3, the thickness of the conductive vertical nanotube array film is 0.2 μm-20 μm.
The preparation method of the field emission flexible pressure sensing film with high sensitivity and high precision provided by the invention can also have the following characteristics: in step 5, the material of the sacrificial layer includes at least one of polyvinyl alcohol, polymethyl methacrylate and dextran.
The preparation method of the field emission flexible pressure sensing film with high sensitivity and high precision provided by the invention can also have the following characteristics: in step 5, the polymer elastomer is any one of polydimethylsiloxane, hydrogenated styrene-butadiene block copolymer and polyurethane.
The preparation method of the field emission flexible pressure sensing film with high sensitivity and high precision provided by the invention can also have the following characteristics: wherein in step 5, the elastic modulus of the polymer elastomer is less than 50MPa at 5% strain.
Effects and effects of the invention
According to the field emission flexible pressure sensing film with high sensitivity and high precision and the preparation method thereof, the field emission flexible pressure sensing film comprises a conductive vertical nanotube array film embedded by resin and an ultrathin single-component polymer elastic film, and the field emission flexible pressure sensing film is reasonably and optimally designed and provided with a specific electron transport channel, so that the whole system can work in an electrical environment with F-N tunneling current as a main component, and the extremely sensitive characteristic of the thickness of a dielectric layer (an induction layer in the system) is utilized by virtue of F-N tunneling effect, so that the extremely small compressive stress collected by the induction layer can be converted into a strong output signal change amount, thereby realizing extremely high sensing sensitivity.
In addition, when the system is subjected to external pressure, the integral deformation is mainly concentrated in the ultrathin single-component polymer elastic film (sensing layer), so that the deformation of the system is quite uniform, excessive random errors can not be generated, and the integral precision of the system is improved.
Furthermore, the thickness of the sensing layer which acts with external compressive stress is smaller than 1 mu m, the rebound stroke of the sensing system is only tens of nanometers, and the phenomenon of great elastic relaxation of the material is greatly avoided, so that the sensing system has the response rate of far-beyond general elastic material, and lays a foundation for collecting sensing information at high frequency.
In addition, through theoretical analysis, the sensitivity of the sensor can be greatly reduced along with the increase of the measured voltage, but the measuring range of the sensor can be greatly increased. By utilizing the characteristic, the sensitivity and the measuring range of the sensor can be dynamically changed in measurement, so that more flexible application is obtained. The sensing material of the system has the advantages of pure structure, simple process and good industrial application prospect.
Drawings
FIG. 1 is a physical view of a conductive material prepared by a chemical vapor deposition method in example 1 of the present invention;
FIG. 2 is a topography under a scanning electron microscope of the electrically conductive material of example 1 of the present invention;
FIG. 3 is an optical photograph of an embedded block in example 1 of the present invention;
FIG. 4 is a microscopic topography of the washed conductive vertical nanotube array film of example 1 of the present invention;
FIG. 5 is a photograph of polydimethylsiloxane diluted in cyclohexane in example 1 of the present invention;
FIG. 6 is an atomic force microscope topography of an ultrathin single component polymeric elastic film of example 1 of the present invention;
FIG. 7 is an optical photograph of a flexible pressure-sensitive film for field emission in example 1 of the present invention, which has both high sensitivity and high accuracy;
FIG. 8 is a graph of resistance versus pressure and a graph of sensitivity versus pressure for a flexible pressure sensing film of field emission with both high sensitivity and high accuracy in example 1 of the present invention;
FIG. 9 is the maximum and minimum deviation ranges of the accuracy of the output signal after repeated measurement of 20 times of the field emission flexible pressure sensing film of example 1 of the present invention having both high sensitivity and high accuracy;
FIG. 10 is a relaxation response curve of a flexible pressure-sensitive film for field emission in example 2 of the present invention, which has both high sensitivity and high accuracy;
FIG. 11 is a fatigue response test curve of a flexible pressure sensing film with high sensitivity and high accuracy for field emission in example 2 of the present invention;
FIG. 12 is a graph showing the relationship between sensitivity and measuring range of the flexible pressure sensor film of example 2 of the present invention with high sensitivity and high accuracy.
Detailed Description
The invention provides a field emission flexible pressure sensing film with high sensitivity and high precision and a preparation method thereof.
The preparation method of the field emission flexible pressure sensing film with high sensitivity and high precision comprises the following steps:
step 1, preparing a conductive material with a vertical nanotube array structure by using a chemical vapor deposition method or other methods. The process of preparing electrically conductive materials with vertical nanotube array structures is prior art. The nanotube of the conductive material comprises at least one of a single-arm carbon nanotube and a multi-wall carbon nanotube, and the diameter of the nanotube is 1nm-300nm.
And 2, embedding the conductive material into epoxy resin, and slowly curing in a vacuum environment to obtain an embedded block.
And 3, ultrathin slicing the embedded block along the direction perpendicular to the nanotube fiber of the conductive material to obtain the conductive vertical nanotube array film with the preset thickness. Wherein the predetermined thickness is 0.2 μm to 20 μm.
And 4, spreading the conductive vertical nanotube array film on the surface of a conductive metal foil or other conductive films, and cleaning the surface of the conductive vertical nanotube array film by utilizing a plasma (oxygen or argon) cleaning technology.
And 5, spin-coating a sacrificial layer on the surface of the flat hard substrate, growing a layer of conductive electrode on the sacrificial layer by utilizing a magnetron sputtering technology, spin-coating diluted polymer elastomer on the surface of the conductive electrode by utilizing a spin-coating technology, slowly volatilizing a solvent at a low temperature, and curing the polymer to form a film to obtain the ultrathin single-component polymer elastic film. The hard substrate is, for example, a silicon wafer, a quartz wafer or the like; the material of the sacrificial layer comprises at least one of polyvinyl alcohol, polymethyl methacrylate and dextran; the polymer elastomer is any one of polydimethylsiloxane, hydrogenated styrene-butadiene block copolymer and polyurethane, and the elastic modulus of the polymer elastomer is less than 50MPa when the polymer elastomer is strained at 5%. The ultra-thin single component polymeric elastic film has a thickness of less than 1 μm and a purity of more than 90% as a sensing layer.
And 6, attaching the conductive vertical nanotube array film cleaned in the step 4 on the upper surface of the ultrathin single-component polymer elastic film, wetting the attaching surface by using ethanol, and removing bubbles and ethanol in the attaching surface under a vacuum condition to obtain the pressure sensing film.
And 7, after electrode wires are led out from the pressure sensing film, packaging the pressure sensing film to obtain the field emission flexible pressure sensing film with high sensitivity and high precision.
The field emission flexible pressure sensing film with high sensitivity and high precision comprises a conductive vertical nanotube array film embedded by resin and an ultrathin single-component polymer elastic film, wherein the conductive vertical nanotube array film embedded by resin is arranged on the upper surface of the ultrathin single-component polymer elastic film.
Wherein, the elastic modulus of the conductive vertical nanotube array film embedded by the resin is more than 5 times of that of the ultrathin single-component polymer elastic film. The thickness of the ultrathin single-component polymer elastic film is less than 1 mu m. The ultra-thin single-component polymer elastic film is used as the sensing layer, and the purity of the component is more than 90%.
In order to make the technical means, creation characteristics, achievement purposes and effects of the present invention easy to understand, the following embodiments specifically describe the field emission flexible pressure sensing film with high sensitivity and high precision and the preparation method thereof with reference to the accompanying drawings.
Example 1 ]
Embodiment 1 provides a field emission flexible pressure sensing film with high sensitivity and high precision and a preparation method thereof.
The preparation method of the field emission flexible pressure sensing film with high sensitivity and high precision in the embodiment 1 comprises the following steps:
step 1, preparing a conductive material with a vertical nanotube array structure by using a chemical vapor deposition method. The nanotubes of the electrically conductive material are multiwall carbon nanotubes.
FIG. 1 is a physical view of a conductive material prepared by a chemical vapor deposition method in example 1 of the present invention; fig. 2 is a topography under a scanning electron microscope of the electrically conductive material of example 1 of the present invention.
As shown in fig. 1 to 2, the diameter of the nanotube of the conductive material is 15nm, and the interval is about 15nm.
And 2, embedding the conductive material into epoxy resin, and slowly curing in a vacuum environment to obtain an embedded block.
Wherein step 2 comprises the sub-steps of:
step 2-1, configuring the SPON812 epoxy resin. And (3) fully stirring and mixing 2ml of the SPON812 resin, 0.65ml of 2-dodecenyl-succinic anhydride and 1.2ml of methyl nadic anhydride for 2 hours, then adding 0.06ml of DMP-30 curing agent, fully stirring for 30 minutes again, and placing in a vacuum environment for defoaming to obtain the SPON812 epoxy resin.
And 2-1, pouring the prepared SPON812 epoxy resin onto the conductive material, placing the conductive material in a vacuum oven, curing for 96 hours at 50 ℃, soaking the cured sample in 5% hydrofluoric acid aqueous solution for 30 minutes to remove the silicon substrate supporting the conductive material, and obtaining an embedded block (shown in figure 3).
And 3, ultrathin slicing the embedded block along the direction perpendicular to the nanotube fiber of the conductive material by using an ultrathin slicer to obtain the conductive vertical nanotube array film with the thickness of 500 nm.
And 4, spreading the conductive vertical nanotube array film on the surface of an aluminum foil, integrally transferring the film into an oxygen plasma cleaner, and cleaning for 1min under the conditions of 300cc/min of oxygen flow and 50w of power.
FIG. 4 is a microscopic topography of the washed conductive vertical nanotube array film of example 1 of the present invention.
And 5, spin-coating a sacrificial layer on the surface of the flat silicon wafer, growing a layer of conductive electrode on the sacrificial layer by utilizing a magnetron sputtering technology, spin-coating diluted polymer elastomer on the surface of the conductive electrode by utilizing a spin-coating technology, slowly volatilizing a solvent of the diluted polymer elastomer at a low temperature, and curing the polymer to form a film to obtain the ultrathin single-component polymer elastic film.
Wherein, step 5 comprises the following sub-steps:
and 5-1, spin coating a sacrificial layer on the surface of the flat silicon wafer. The specific process comprises the following steps:
a flat silicon wafer was subjected to ultrasonic cleaning in acetone, ethanol and deionized water for 6min, respectively, and then a dextran aqueous solution of 10% mass concentration was spin-coated on the upper surface thereof at a speed of 1500rpm for 20s. And baking the silicon wafer on a hot plate at 80 ℃ for 30min, and then placing the silicon wafer on the hot plate at 150 ℃ for 30min to sufficiently remove the moisture in the silicon wafer.
And 5-2, sputtering an Al layer with the thickness of 800nm on the upper surface of the silicon wafer spin-coated with the sacrificial layer by utilizing a magnetron sputtering technology.
Step 5-3, a polydimethylsiloxane diluted in cyclohexane (dakangnin 184) (a: b=14:1, mass ratio) was spin-coated on the Al layer at a mass concentration of 9.5%.
FIG. 5 is a photograph of polydimethylsiloxane diluted in cyclohexane in example 1 of the present invention.
And 5-4, placing the whole sample in a vacuum oven at 80 ℃ for curing for 3 hours to obtain an elastomer film sensing layer loaded on the surface of the electrode, wherein the elastomer film sensing layer is an ultrathin single-component polymer elastic film. The ultrathin single-component polymer elastic film has a thickness of less than 1 mu m and a purity of more than 90 percent.
FIG. 6 is an atomic force microscope topography of an ultrathin, single component polymeric elastic film of example 1 of the present invention.
As shown in FIG. 6, the ultrathin single-component polymer elastic film has a very flat surface, is convenient for the subsequent lamination process, and has the surface roughness of only 0.455nm as measured by an atomic force microscope.
In this embodiment, the elastic modulus of the resin-embedded conductive vertical nanotube array film is 5 times or more that of the ultrathin single-component polymer elastic film.
And 6, attaching the conductive vertical nanotube array film cleaned in the step 4 to the upper surface of the ultrathin single-component polymer elastic film obtained in the step 5, wetting the attaching surface by ethanol, and then placing the film in a vacuum oven to remove air and ethanol in the attaching surface to obtain the pressure sensing film.
And 7, after electrode wires are led out from the pressure sensing film, packaging the electrode wires by using pre-cured PDMS, and thus obtaining the field emission flexible pressure sensing film with high sensitivity and high precision (shown in figure 7).
Fig. 8 is a resistance-pressure curve and a sensitivity-pressure curve of the field emission flexible pressure sensing film of example 1 of the present invention having both high sensitivity and high accuracy.
As can be seen from FIG. 8, the field emission flexible pressure sensing film having both high sensitivity and high accuracy has a sensitivity of more than 1kPa-1 in the pressure range of 0 to 950Pa, and the highest sensitivity reaches about 300kPa-1, showing extremely excellent high sensitivity characteristics.
Fig. 9 shows the maximum and minimum deviation ranges of the accuracy of the output signal after repeated measurement of 20 times of the field emission flexible pressure sensing film having both high sensitivity and high accuracy in example 1 of the present invention.
As can be seen from fig. 9, the readout signal error of the field emission flexible pressure sensing film having both high sensitivity and high accuracy is less than 2% in 20 measurements, and excellent accuracy is exhibited. And as can be seen from fig. 8 and fig. 9, the field emission flexible pressure sensing film (sensor) with high sensitivity and high precision prepared by this embodiment has the characteristics of high sensitivity and high precision.
Example 2 ]
Example 2 provides a field emission flexible pressure sensing film with high sensitivity and high precision and a preparation method thereof.
The preparation method of the field emission flexible pressure sensing film with high sensitivity and high precision in the embodiment 2 comprises the following steps:
step 1, preparing a conductive material with a vertical nanotube array structure by using a chemical vapor deposition method. The nanotubes of the electrically conductive material are multiwall carbon nanotubes. The diameter of the nanotube of the conductive material is 10nm, and the distance is about 25nm.
And 2, embedding the conductive material into epoxy resin, and slowly curing in a vacuum environment to obtain an embedded block.
Wherein step 2 comprises the sub-steps of:
step 2-1, configuring the SPON812 epoxy resin. After 2ml of SPON812 resin, 0.95ml of 2-dodecenyl-succinic anhydride and 0.8ml of methyl nadic anhydride are fully stirred and mixed for 2 hours, 0.07ml of DMP-30 curing agent is added, and the mixture is fully stirred for 30 minutes again and placed in a vacuum environment for defoaming, so that the SPON812 epoxy resin can be obtained.
And 2-1, pouring the prepared SPON812 epoxy resin onto the conductive material, placing the conductive material in a vacuum oven, curing the conductive material for 72 hours at the temperature of 60 ℃, and soaking the cured sample in 5% hydrofluoric acid aqueous solution for 30 minutes to remove the silicon substrate supporting the conductive material, thereby obtaining the embedded block.
And 3, ultrathin slicing the embedded block along the direction perpendicular to the nanotube fiber of the conductive material by using an ultrathin slicer to obtain the conductive vertical nanotube array film with the thickness of 600 nm.
And 4, spreading the conductive vertical nanotube array film on the surface of an aluminum foil, integrally transferring the film into an oxygen plasma cleaner, and cleaning for 1min under the conditions of 300cc/min of oxygen flow and 50w of power.
And 5, spin-coating a sacrificial layer on the surface of the flat silicon wafer, growing a layer of conductive electrode on the sacrificial layer by utilizing a magnetron sputtering technology, spin-coating diluted polymer elastomer on the surface of the conductive electrode by utilizing a spin-coating technology, slowly volatilizing a solvent of the diluted polymer elastomer at a low temperature, and curing the polymer to form a film to obtain the ultrathin single-component polymer elastic film.
Wherein, step 5 comprises the following sub-steps:
and 5-1, spin coating a sacrificial layer on the surface of the flat silicon wafer. The specific process comprises the following steps:
a flat silicon wafer was subjected to ultrasonic cleaning in acetone, ethanol and deionized water for 6min, respectively, and then a dextran aqueous solution of 10% mass concentration was spin-coated on the upper surface thereof at a speed of 1500rpm for 20s. And baking the silicon wafer on a hot plate at 80 ℃ for 30min, and then placing the silicon wafer on the hot plate at 150 ℃ for 30min to sufficiently remove the moisture in the silicon wafer.
And 5-2, sputtering a 1500nm thick Al layer on the upper surface of the silicon wafer spin-coated with the sacrificial layer by utilizing a magnetron sputtering technology.
Step 5-3, a polydimethylsiloxane diluted in cyclohexane (dakangnin 184) (a: b=14:1, mass ratio) was spin-coated on the Al layer at a mass concentration of 11.3%.
And 5-4, placing the whole sample in a vacuum oven at 80 ℃ for curing for 3 hours to obtain an elastomer film sensing layer loaded on the surface of the electrode, wherein the elastomer film sensing layer is an ultrathin single-component polymer elastic film. The ultrathin single-component polymer elastic film has a thickness of less than 1 mu m and a purity of more than 90 percent.
In this embodiment, the elastic modulus of the resin-embedded conductive vertical nanotube array film is 5 times or more that of the ultrathin single-component polymer elastic film.
And 6, attaching the conductive vertical nanotube array film cleaned in the step 4 to the upper surface of the ultrathin single-component polymer elastic film obtained in the step 5, wetting the attaching surface by ethanol, and then placing the film in a vacuum oven to remove air and ethanol in the attaching surface to obtain the pressure sensing film.
And 7, after the electrode lead is led out from the pressure sensing film, packaging the electrode lead by using pre-cured PDMS, and thus obtaining the field emission flexible pressure sensing film with high sensitivity and high precision.
FIG. 10 is a relaxation response curve of a flexible pressure-sensitive film for field emission in example 2 of the present invention, which has both high sensitivity and high accuracy.
As can be seen from fig. 10, after receiving the external pressure, the field emission flexible pressure sensing film (sensor) with high sensitivity and high precision realizes the stabilization of the signal only through 3.327ms, and detects the specific external pressure condition, thus the sensor has very rapid response time.
FIG. 11 is a fatigue response test curve of a field emission flexible pressure sensing film of example 2 of the present invention having both high sensitivity and high accuracy.
As can be seen from fig. 11, the field emission flexible pressure sensing film (sensor) having both high sensitivity and high accuracy has very accurate response to pressures of 40Pa and 400Pa, respectively, during 5000 cycles of testing, and the overall error thereof is very small. And so many cycles, the output signal of the sensor has no sign of any drift, demonstrating the excellent anti-fatigue properties of the sensor.
FIG. 12 is a graph showing the relationship between sensitivity and measuring range of the flexible pressure sensor film of example 2 of the present invention with high sensitivity and high accuracy.
As can be seen from fig. 12, with the rise of the test voltage (from 2.3V to 3.1V), the highest sensitivity of the field emission flexible pressure sensing film (sensor) with high sensitivity and high accuracy is rapidly reduced, and the measuring range is rapidly increased, so that the sensor can realize the adjustment of sensitivity and measuring range only by adjusting the measurement voltage during the use process, and has very objective flexible application prospect.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.
Claims (9)
1. A field emission flexible pressure sensing film having both high sensitivity and high accuracy, comprising:
a resin-embedded conductive vertical nanotube array film and an ultrathin single-component polymer elastic film,
wherein the ultra-thin single component polymeric elastic film has a thickness of less than 1 μm.
2. The flexible pressure sensing film of field emission with both high sensitivity and high accuracy according to claim 1, wherein:
wherein, the ultrathin single-component polymer elastic film is used as an induction layer, and the purity of the component is more than 90 percent.
3. The flexible pressure sensing film of field emission with both high sensitivity and high accuracy according to claim 1, wherein:
wherein the elastic modulus of the resin-embedded conductive vertical nanotube array film is more than 5 times of that of the ultrathin single-component polymer elastic film,
the resin-embedded conductive vertical nanotube array film is disposed on the upper surface of the ultra-thin single-component polymer elastic film.
4. The preparation method of the field emission flexible pressure sensing film with high sensitivity and high precision is characterized by comprising the following steps:
step 1, preparing a conductive material with a vertical nanotube array structure;
step 2, embedding the conductive material into epoxy resin, and slowly curing in a vacuum environment to obtain an embedded block;
step 3, ultrathin slicing the embedded block along the direction perpendicular to the nanotube fiber of the conductive material to obtain a conductive vertical nanotube array film;
step 4, the conductive vertical nanotube array film is flatly paved on the surface of a conductive metal foil or other conductive films, and the surface of the conductive vertical nanotube array film is cleaned by utilizing a plasma cleaning technology;
step 5, spin-coating a sacrificial layer on the surface of the flat hard substrate, growing a layer of conductive electrode on the sacrificial layer by utilizing a magnetron sputtering technology, spin-coating diluted polymer elastomer on the surface of the conductive electrode by utilizing a spin-coating technology, slowly volatilizing a solvent of the diluted polymer elastomer at a low temperature, and curing the polymer to form a film to obtain an ultrathin single-component polymer elastic film;
step 6, attaching the cleaned conductive vertical nanotube array film on the upper surface of the ultrathin single-component polymer elastic film, wetting the attaching surface by using ethanol, and removing bubbles and ethanol in the attaching surface under a vacuum condition to obtain a pressure sensing film;
step 7, after electrode wires are led out from the pressure sensing film, the pressure sensing film is packaged to obtain the field emission flexible pressure sensing film with high sensitivity and high precision,
wherein the high-sensitivity and high-precision field emission flexible pressure sensing film is the high-sensitivity and high-precision field emission flexible pressure sensing film according to any one of claims 1 to 3.
5. The method for preparing the field emission flexible pressure sensing film with high sensitivity and high precision according to claim 4, which is characterized in that:
wherein in step 1, the conductive material is prepared by using a chemical vapor deposition method,
the nanotubes of electrically conductive material comprise at least one of single-walled carbon nanotubes and multi-walled carbon nanotubes,
the diameter of the nanotube of the conductive material is 1nm-300nm.
6. The method for preparing the field emission flexible pressure sensing film with high sensitivity and high precision according to claim 4, which is characterized in that:
in the step 3, the thickness of the conductive vertical nanotube array film is 0.2 μm-20 μm.
7. The method for preparing the field emission flexible pressure sensing film with high sensitivity and high precision according to claim 4, which is characterized in that:
in step 5, the material of the sacrificial layer includes at least one of polyvinyl alcohol, polymethyl methacrylate and dextran.
8. The method for preparing the field emission flexible pressure sensing film with high sensitivity and high precision according to claim 4, which is characterized in that:
in step 5, the polymer elastomer is any one of polydimethylsiloxane, hydrogenated styrene-butadiene block copolymer and polyurethane.
9. The method for preparing the field emission flexible pressure sensing film with high sensitivity and high precision according to claim 4, which is characterized in that:
in step 5, the elastic modulus of the polymer elastomer is less than 50MPa at 5% strain.
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