CN114634710B - Flexible material and preparation method and application thereof - Google Patents
Flexible material and preparation method and application thereof Download PDFInfo
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- CN114634710B CN114634710B CN202210174828.3A CN202210174828A CN114634710B CN 114634710 B CN114634710 B CN 114634710B CN 202210174828 A CN202210174828 A CN 202210174828A CN 114634710 B CN114634710 B CN 114634710B
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- 239000000463 material Substances 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000004729 solvothermal method Methods 0.000 claims abstract description 21
- 239000004020 conductor Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 51
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 41
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 41
- -1 polytetrafluoroethylene Polymers 0.000 claims description 40
- 239000002041 carbon nanotube Substances 0.000 claims description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 28
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- 239000006260 foam Substances 0.000 claims description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 11
- 239000011148 porous material Substances 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 229920006254 polymer film Polymers 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 4
- 230000008878 coupling Effects 0.000 abstract description 3
- 238000010168 coupling process Methods 0.000 abstract description 3
- 238000005859 coupling reaction Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 238000005530 etching Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 14
- 238000001035 drying Methods 0.000 description 10
- 230000004044 response Effects 0.000 description 10
- 230000035945 sensitivity Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000001816 cooling Methods 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
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- 238000005303 weighing Methods 0.000 description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
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- 239000000758 substrate Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000005355 Hall effect Effects 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000011370 conductive nanoparticle Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
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- 239000002071 nanotube Substances 0.000 description 1
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- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
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- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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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
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
-
- 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
-
- 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
- G01L1/20—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
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a flexible material, a preparation method and application thereof, wherein the preparation method of the flexible material comprises the following steps: and carrying out solvothermal reaction on the template material, the siloxane oligomer, the curing agent and the conductive material to obtain the flexible material. The preparation method of the flexible material is simple, has low cost and is operated, the flexible material is prepared by a template solvothermal method, the template material is easy to separate, and the template material is not required to be removed by an etching process. In addition, the flexible material prepared by the method has extremely high biocompatibility and excellent electrical property and mechanical property, and solves the problem of coupling of the electrical property and the mechanical property caused by adding the conductive material into the siloxane oligomer in the prior art.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a flexible material and a preparation method and application thereof.
Background
The flexible electronic device can be attached to various curved surfaces, especially to the skin surface of a human body, so that the application scene of the flexible electronic device can be expanded to occasions which are not qualified by the traditional hard electronic device based on semiconductor silicon, such as the fields of man-machine interaction interfaces, electronic skin, human physiological signal monitoring, medical robots and the like, and the flexible electronic device has gained wide attention. The flexible sensors are flexible in application scene, low in production cost, light in weight, good in compatibility with the traditional large-area mass production technology, and capable of meeting the requirements of various application scenes that the electronic device is required to be well attached to the skin and experience is not affected.
Siloxane oligomers, such as Polydimethylsiloxane (PDMS), are a commonly used matrix material whose elasticity can be controlled by adjusting the ratio of curing agent to siloxane oligomer. The conductive fillers include various conductive nanoparticles and various nanotubes such as Au/Ag nanoparticles/nanowires, etc. By adjusting the concentration ratio of the filler in the matrix, the formation of just the conductive network inside the compound can be controlled, which is the so-called threshold point. But the electrical conductivity and mechanical elasticity of the composite tend to couple together. When the electrical conductivity of the composite is increased by increasing the ratio of conductive fillers, such as by increasing the volume fraction of metal particles, carbon black or carbon nanotubes in the matrix, the mechanical stiffness of the composite as a whole is also significantly increased. The coupling relation between the mechanical elasticity and the conductivity of the composite material leads to the competition relation between the linear interval and the sensitivity of the piezoresistive sensor of the sensing material taking the composite material as the core.
Disclosure of Invention
In order to overcome the problems of the prior art, one of the purposes of the present invention is to provide a method for preparing a flexible material.
It is a second object of the present invention to provide a flexible material.
It is a further object of the present invention to provide a flexible pressure sensor.
It is a fourth object of the present invention to provide a use of a flexible material in a sensor.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a first aspect of the present invention provides a method of preparing a flexible material, comprising the steps of: and carrying out solvothermal reaction on the template material, the siloxane oligomer, the curing agent and the conductive material to obtain the flexible material.
Preferably, the mass of the conductive material is 0% -5% of the total mass of the siloxane oligomer and the curing agent, and is not 0%; further preferably, the mass of the conductive material is 1% -5% of the total mass of the siloxane oligomer and the curing agent; still further preferably, the mass of the conductive material is 2% to 5% of the total mass of the siloxane oligomer and the curing agent; still more preferably, the mass of the conductive material is 3% to 5% of the total mass of the siloxane oligomer and the curing agent.
Preferably, the mass ratio of the siloxane oligomer to the curing agent is (1-20): 1, a step of; further preferably, the mass ratio of the siloxane oligomer to the curing agent is (5 to 20): 1, a step of; still further preferably, the mass ratio of the siloxane oligomer to the curing agent is (8 to 15): 1, a step of; still more preferably, the mass ratio of the siloxane oligomer to the curing agent is (10 to 15): 1.
preferably, the siloxane oligomer comprises at least one of PDMS, polymethyltriethoxysilane, polymethyltrimethoxysiloxane; further preferably, the siloxane oligomer is PDMS.
Preferably, the PDMS is the a-host in the dakangnin 184.
Preferably, the curing agent is a B side agent in dakangnin 184.
According to the invention, the flexible material is prepared by adopting a solvothermal reaction, conductive particles can be gathered at the bottom of an elastic substrate formed after the siloxane oligomer is solidified by controlling the solvothermal reaction temperature and time, and small particles at the bottom of the elastic substrate of the siloxane oligomer are conductive particles, so that rigid conductive particles are separated from the flexible elastic substrate, and the flexible material with decoupled mechanical property and electrical property is obtained.
Preferably, the temperature of the solvothermal reaction is 90-160 ℃; further preferably, the temperature of the solvothermal reaction is 100-150 ℃; still more preferably, the solvothermal reaction temperature is 100-140 ℃.
Preferably, the solvothermal reaction time is 1-5 h; further preferably, the solvothermal reaction time is 1 to 3 hours; still further preferably, the solvothermal reaction time is 2 to 3 hours.
Preferably, the temperature rising rate of the solvothermal reaction is 270-480 ℃/h; further preferably, the temperature rising rate of the solvothermal reaction is 300-450 ℃/h; still more preferably, the solvothermal reaction has a heating rate of 300 to 400 ℃/h.
Preferably, the template material comprises at least one of foam iron, foam copper, foam cobalt, foam nickel and foam ruthenium; further preferably, the template material comprises at least one of foamed cobalt and foamed nickel; still further preferably, the template material is nickel foam.
Preferably, the pore diameter of the template material is 400-600 mu m; further preferably, the pore diameter of the template material is 450-600 μm; still more preferably, the pore size of the template material is 450 to 550 μm.
Preferably, the conductive material comprises at least one of carbon nanotubes, carbon black, and metal particles; further preferably, the conductive material is carbon nanotubes.
Preferably, the solvent of the solvothermal reaction is cyclohexane.
Preferably, the solvothermal reaction step is specifically: firstly, carrying out ultrasonic treatment on the solution containing the carbon nano tube for 20-40 min; the siloxane oligomer and curing agent are then added, mechanically mixed and reacted.
Preferably, the mechanical mixing comprises at least one of mechanical stirring and magnetic stirring. The mechanical stirring includes stirring using a stirring rod.
Preferably, the method further comprises a cool drying step.
Preferably, the cooling and drying step is natural cooling and drying in the shade.
Preferably, the natural cooling and drying time is 10-20 hours; further preferably, the natural cooling and drying time is 10-14 h; still more preferably, the natural cooling and drying time is 12-14 hours.
Preferably, the flexible material has micropores with a pore size of 0.1 to 5 μm; further preferably, the flexible material has micropores with a pore size of 0.5 to 2 μm; still more preferably, the flexible material has micropores with a pore size of 1 to 2 μm.
A second aspect of the present invention is to provide a flexible material, obtainable by the preparation method provided in the first aspect of the present invention; the flexible material has micropores with a pore diameter of 0.1-5 μm.
A third aspect of the invention is to provide a flexible pressure sensor comprising the flexible material provided in the second aspect of the invention.
Preferably, the sensor further comprises a polymer film and interdigitated electrodes; the flexible material is positioned between the polymer film and the interdigitated electrodes.
Preferably, the polymer film is a waterproof film.
Preferably, the polymer film is a PS film.
Preferably, the polymer film, the interdigital electrode and the flexible material are encapsulated by adhesive materials.
Preferably, the adhesive material comprises double sided tape.
Preferably, the sensitivity of the flexible pressure sensor is 0.5-0.7 kPa -1 The method comprises the steps of carrying out a first treatment on the surface of the Further preferably, the sensitivity of the flexible pressure sensor is 0.55 to 0.65kPa -1 The method comprises the steps of carrying out a first treatment on the surface of the Still further preferably, the flexible pressure sensor has a sensitivity of 0.6kPa -1 。
A fourth aspect of the invention provides the use of the flexible material provided in the second aspect of the invention in a sensor.
The beneficial effects of the invention are as follows: the preparation method of the flexible material is simple, has low cost and is operated, the flexible material is prepared by a template solvothermal method, the template material is easy to separate, and the template material is not required to be removed by an etching process. In addition, the flexible material prepared by the method has extremely high biocompatibility and excellent electrical property and mechanical property, and solves the problem of coupling of the electrical property and the mechanical property caused by adding the conductive material in the prior art.
In addition, the flexible material has a micropore structure, is light in weight, and is beneficial to improving the sensitivity of the sensor. The flexible material of the invention is manufactured into a flexible pressure sensor, which has high sensitivity (the sensitivity reaches 0.6 kPa) -1 ) The linear interval is large, the cycling stability is good, and the sensitivity of the device to various types of pressure is excellent.
Drawings
Fig. 1 is a schematic flow chart of a method for producing a flexible material in example 1.
Fig. 2 is a schematic structural diagram of the flexible pressure sensor in embodiment 1.
Fig. 3 is a raman spectrum of the flexible material in example 1.
Fig. 4 is a physical view of the flexible material in example 9.
Fig. 5 is a cross-sectional view of the flexible material in example 8.
Fig. 6 is a surface structural view of the flexible material in example 8.
FIG. 7 is a graph showing mechanical properties of the flexible materials in examples 10 to 15.
Fig. 8 is a stress-strain diagram of the flexible material in examples 9 to 16.
Fig. 9 is a sheet resistance test chart of the flexible material in examples 1 to 8.
Fig. 10 is a response graph of the flexible pressure sensor in example 1.
FIG. 11 is a graph of response curves of the flexible pressure sensor of example 1 at different mechanical strengths.
Fig. 12 is a graph of the response of the flexible pressure sensor of example 1 at 45 ° and 90 ° finger bending.
Detailed Description
Specific embodiments of the present invention will be described in further detail below with reference to the drawings and examples, but the practice and protection of the present invention are not limited thereto. It should be noted that the following processes, unless otherwise specified, are all realized or understood by those skilled in the art with reference to the prior art. The reagents or apparatus used were not manufacturer-specific and were considered conventional products commercially available.
Example 1
The flexible material in this example was prepared using the following preparation method, which comprises the steps of:
(1) Weighing polydimethylsiloxane (Dow Corning 184, wherein the mass ratio of the main agent A to the auxiliary agent B is 10:1) as 3g of solute, adding the solute into a beaker, then adding carbon nano tubes with the dosage of 0.6% of the total mass of the polydimethylsiloxane into the beaker, weighing 15g of solvent n-hexane, adding the solvent n-hexane into the beaker, magnetically stirring and mixing for 2h, and carrying out ultrasonic treatment for 30min at an ultrasonic frequency of 80 KHz; a mixed solution was obtained.
(2) The foam nickel having a porous structure and a pore diameter of 500 μm was cut into 5cm using scissors 2 The wafer of (2) is placed at the bottom of the polytetrafluoroethylene lining of the hydrothermal reaction kettle, meanwhile, the mixed solution is poured into the polytetrafluoroethylene lining of the hydrothermal reaction kettle, the filling amount is ensured to be not more than 70% of the polytetrafluoroethylene lining of the hydrothermal reaction kettle, and then the lining of the hydrothermal reaction kettle is placed into the stainless steel shell.
(3) Putting the hydrothermal reaction kettle into an oven, and setting the temperature rise rate of experimental parameters as follows: raising the temperature from room temperature to 140 ℃ within 1h, and preserving the heat for 3h; naturally cooling and drying in the shade for 12 hours, and removing foam nickel to obtain a PDMS-CNTs material which does not contain solvent and has holes with micropores of 1-2 mu m; and (3) soaking for many times by using cyclohexane to remove unreacted monomers and surface impurities thereof, and naturally drying in the shade for 12 hours to prepare the flexible material (PDMS-CNTs) with the controllable electrical property of the Carbon Nanotubes (CNTs) embedded in Polydimethylsiloxane (PDMS). A schematic flow chart of the preparation method of the flexible material in this example is shown in FIG. 1.
The flexible material (PDMS-CNTs) was cut into 3mm x 3mm sensing units with a knife, and the flexible pressure sensor in this example was fabricated using PS film and double sided tape with a center cut size of 4mm x 4mm to encapsulate on the interdigital electrodes. A schematic structural diagram of the flexible pressure sensor in this example is shown in fig. 2.
Example 2:
the addition amount of the carbon nanotubes in the flexible material of this example is different from that of example 1, specifically: the carbon nanotubes were added in an amount of 1% by weight based on the total mass of polydimethylsiloxane, and the other raw materials and the preparation method were the same as in example 1.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 1.
Example 3:
the addition amount of the carbon nanotubes in the flexible material of this example is different from that of example 1, specifically: the carbon nanotubes were added in an amount of 1.3% by weight based on the total mass of polydimethylsiloxane, and the other raw materials and the preparation method were the same as in example 1.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 1.
Example 4:
the addition amount of the carbon nanotubes in the flexible material of this example is different from that of example 1, specifically: the carbon nanotubes were added in an amount of 1.6% by weight based on the total mass of polydimethylsiloxane, and the other raw materials and the preparation method were the same as in example 1.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 1.
Example 5:
the addition amount of the carbon nanotubes in the flexible material of this example is different from that of example 1, specifically: the carbon nanotubes were added in an amount of 2% by weight based on the total mass of polydimethylsiloxane, and the other raw materials and the preparation method were the same as in example 1.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 1.
Example 6:
the addition amount of the carbon nanotubes in the flexible material of this example is different from that of example 1, specifically: the carbon nanotube was added in an amount of 2.4% based on the total mass of polydimethylsiloxane, and other raw materials and preparation methods were the same as in example 1.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 1.
Example 7:
the addition amount of the carbon nanotubes in the flexible material of this example is different from that of example 1, specifically: the carbon nanotube was added in an amount of 2.6% based on the total mass of polydimethylsiloxane, and other raw materials and preparation methods were the same as in example 1.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 1.
Example 8:
the addition amount of the carbon nanotubes in the flexible pressure sensor in this example is different from that in example 1, specifically: the carbon nanotubes were added in an amount of 3% by mass based on the total mass of polydimethylsiloxane, and the other raw materials and the preparation method were the same as in example 1.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 1.
Example 9
The flexible material in this example was prepared using the following preparation method, which comprises the steps of:
(1) Weighing polydimethylsiloxane (Dow Corning 184, wherein the mass ratio of the main agent A to the auxiliary agent B is 5:1) as 3g of solute, the dosage of the carbon nano tube is 3% of the total mass of the polydimethylsiloxane, adding the carbon nano tube and the polydimethylsiloxane into a beaker, weighing 15g of solvent n-hexane, adding into the beaker, magnetically stirring and mixing for 2h, and carrying out ultrasonic treatment for 30min at an ultrasonic frequency of 80 KHz; a mixed solution was obtained.
(2) The foam nickel having a porous structure and a pore diameter of 500 μm was cut into 5cm using scissors 2 The wafer of (2) is placed at the bottom of the polytetrafluoroethylene lining of the hydrothermal reaction kettle, meanwhile, the mixed solution is poured into the polytetrafluoroethylene lining of the hydrothermal reaction kettle, the filling amount is ensured to be not more than 70% of the polytetrafluoroethylene lining of the hydrothermal reaction kettle, and then the lining of the hydrothermal reaction kettle is placed into the stainless steel shell.
(3) Putting the hydrothermal reaction kettle into an oven, and setting the temperature rise rate of experimental parameters as follows: raising the temperature from room temperature to 140 ℃ within 1h, and preserving the heat for 3h; naturally cooling and drying in the shade for 12 hours, and removing foam nickel to obtain a PDMS-CNTs material which does not contain solvent and has uniform holes with micropores of 1 mu m; and (3) soaking for many times by using cyclohexane to remove unreacted monomers and surface impurities thereof, and naturally drying in the shade for 12 hours to prepare the flexible material (PDMS-CNTs) with the controllable electrical property of the Carbon Nanotubes (CNTs) embedded in Polydimethylsiloxane (PDMS).
The flexible pressure sensor in this example was fabricated by cutting flexible materials (PDMS-CNTs) with a knife into 3mm x 3mm sensing units, and encapsulating the sensing units on interdigital electrodes using PS film and double sided tape with a center cut size of 4mm x 4 mm.
Example 10:
the amount of polydimethylsiloxane in the flexible material of this example was different from that of example 9, and specifically: the total mass of polydimethylsiloxane (Dow Corning 184, A main agent, B side agent) was 3g, wherein the mass ratio of the A main agent to the B side agent was 6:1, and the other raw materials and preparation methods were the same as in example 9.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 9.
Example 11:
the amount of polydimethylsiloxane in the flexible material of this example was different from that of example 9, and specifically: the total mass of polydimethylsiloxane (Dow Corning 184, A main agent, B side agent) was 3g, wherein the mass ratio of the A main agent to the B side agent was 7:1, and the other raw materials and preparation methods were the same as in example 9.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 9.
Example 12:
the amount of polydimethylsiloxane in the flexible material of this example was different from that of example 9, and specifically: the total mass of polydimethylsiloxane (Dow Corning 184, A main agent, B side agent) was 3g, wherein the mass ratio of the A main agent to the B side agent was 8:1, and the other raw materials and preparation methods were the same as in example 9.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 9.
Example 13:
the amount of polydimethylsiloxane in the flexible material of this example was different from that of example 9, and specifically: the total mass of polydimethylsiloxane (Dow Corning 184, A main agent, B side agent) was 3g, wherein the mass ratio of the A main agent to the B side agent was 9:1, and the other raw materials and preparation methods were the same as in example 9.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 9.
Example 14:
the amount of polydimethylsiloxane in the flexible material of this example was different from that of example 9, and specifically: the total mass of polydimethylsiloxane (Dow Corning 184, A main agent, B side agent) was 3g, wherein the mass ratio of the A main agent to the B side agent was 10:1, and the other raw materials and preparation methods were the same as in example 9.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 9.
Example 15:
the amount of polydimethylsiloxane in the flexible material of this example was different from that of example 9, and specifically: the total mass of polydimethylsiloxane (Dow Corning 184, A main agent, B side agent) was 3g, wherein the mass ratio of the A main agent to the B side agent was 11:1, and the other raw materials and preparation methods were the same as in example 9.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 9.
Example 16:
the amount of polydimethylsiloxane in the flexible material of this example was different from that of example 9, and specifically: the total mass of the polydimethylsiloxane (Dow Corning 184, A main agent, B side agent) was 3g, wherein the mass ratio of the A main agent to the B side agent was 12:1, and the other raw materials and preparation methods were the same as in example 9.
The flexible pressure sensor in this example was prepared with reference to the preparation method of example 9.
Performance test:
(1) Raman scattering properties
The raman scattering spectrum of the flexible material in example 1 was measured by a raman spectrum analyzer, as shown in fig. 3, wherein D, G and 2D in fig. 3 are both raman diffraction peaks of the carbon nanotubes. From fig. 3, a peak of carbon nanotubes and a peak of PDMS can be observed, indicating successful embedding of carbon nanotubes in PDMS.
(2) Topography testing
The flexible material prepared in example 9 was columnar in shape and its physical diagram is shown in fig. 4.
The flexible material of example 8 was tested using a scanning electron microscope for a cross-sectional view as shown in fig. 5 and a surface structure as shown in fig. 6. As can be seen from fig. 5 and 6: example 8 a flexible material with a porous structure on the surface was successfully synthesized.
(3) Mechanical property test
The mechanical properties required for the flexible materials in examples 10 to 15 under the same compression set (compression set of 2 mm) were respectively tested using a universal pressure tester, and the specific test results are shown in fig. 7. As can be seen from fig. 7, as the mass ratio of the a main agent and the B sub agent in the polydimethylsiloxane increases, the pressure required for compression becomes smaller and smaller under the same compression set, indicating the enhanced flexibility of the flexible materials prepared in examples 10 to 15.
The flexible materials of examples 9 to 16 were each tested for stress strain using a universal tensile machine, and the specific test results are shown in fig. 8. As can be seen from fig. 8, as the mass ratio of the a main agent and the B auxiliary agent in the polydimethylsiloxane increases, the stress gradually decreases, and the elongation gradually increases, indicating that the flexibility of the flexible materials prepared in examples 9 to 16 increases, and the materials gradually become soft.
(4) Electrical property test
The square resistance test of the flexible materials in examples 1 to 8 was tested by using an HL-550 hall effect tester and a four-probe test method, and the specific test results are shown in fig. 9, and as can be seen from fig. 9, the resistance of the flexible material gradually decreases with increasing carbon nanotube addition, indicating that: with the increase of the addition amount of the carbon nano tube, the electrical property of the flexible material is improved.
(5) Sensing performance test
The response curve of the flexible pressure sensor of example 1 was tested by cyclic loading and unloading of pressure at 220kPa using a universal tensile tester and a figure 2400 source of time, and the specific test results are shown in fig. 10. As can be seen from fig. 10, the flexible pressure sensor in example 1 has excellent response stability when cyclically loading and unloading pressure.
The flexible pressure sensor of example 1 was tested for its response properties at different mechanical strengths using a universal tensile tester and a reference 2400 digital source meter, and the specific test results are shown in fig. 11, where the ordinate of fig. 11 is the current at a current change rate that is greater when the initial dead load is pressureless, meaning that the current changes more when the pressure is applied. As can be seen from fig. 11: the flexible pressure sensor of example 1 had good linearity within 250kPa at increasing applied pressure, and the slope-dependent sensitivity was maintained at 0.6kPa -1 I.e. with excellent sensitivity.
The response curves of the flexible pressure sensor of example 1 were tested at 45 ° and 90 ° finger bending, respectively, see in particular fig. 12. As can be seen from fig. 12: the flexible pressure sensor in embodiment 1 can accurately and rapidly obtain different response curves when the bending degree of the finger is different.
In summary, the flexible material of the present invention prepares a flexible material with decoupled mechanical and electrical properties by embedding the carbon nanotubes into polydimethylsiloxane, namely: the mechanical property and the electrical property of the flexible material have the characteristic of being separately controllable. According to the invention, the flexible material is prepared into the flexible pressure sensor, so that the response of different fingers can be accurately identified, different response curves are provided under different pressures, and the flexible pressure sensor has good circulation stability and programmable potential to an integrated circuit.
While the embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes may be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (3)
1. A flexible pressure sensor, wherein the sensor comprises a flexible material, the flexible material being made by a method of preparation comprising the steps of:
carrying out solvothermal reaction on a template material, a siloxane oligomer, a curing agent and a conductive material, and removing the template material to prepare the flexible material; the template material is placed at the bottom of the inner liner of polytetrafluoroethylene of the hydrothermal reaction kettle in the solvothermal reaction,
the siloxane oligomer is a main agent A in the dakangnin 184, and the curing agent is a side agent B in the dakangnin 184; the template material is foam nickel; the conductive material is a carbon nanotube;
the temperature of the solvothermal reaction is 90-160 ℃; the solvothermal reaction time is 1-5 h; the addition amount of the conductive material is 0.6% of the total mass of the polydimethylsiloxane; the mass ratio of the siloxane oligomer to the curing agent is 10:1.
2. the flexible pressure sensor of claim 1, wherein: the flexible material is provided with micropores with the pore diameter of 0.1-5 mu m.
3. The flexible pressure sensor of claim 1, wherein: the sensor further comprises a polymer film and interdigital electrodes; the flexible material is positioned between the polymer film and the interdigitated electrodes.
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