CN113783462B - Microcapsule electret self-generating device and preparation and application thereof - Google Patents
Microcapsule electret self-generating device and preparation and application thereof Download PDFInfo
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
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- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 41
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 38
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 38
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 38
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 18
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
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- 239000002042 Silver nanowire Substances 0.000 claims abstract description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 6
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- 229910052709 silver Inorganic materials 0.000 claims abstract description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 9
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 9
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 claims description 9
- 239000003995 emulsifying agent Substances 0.000 claims description 6
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 239000007764 o/w emulsion Substances 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
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- 229910021641 deionized water Inorganic materials 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
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- 230000005611 electricity Effects 0.000 description 1
- 229920005570 flexible polymer Polymers 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
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- 230000010287 polarization Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- AVXLXFZNRNUCRP-UHFFFAOYSA-N trichloro(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctyl)silane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)[Si](Cl)(Cl)Cl AVXLXFZNRNUCRP-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
- H02N—ELECTRIC MACHINES NOT OTHERWISE PROVIDED FOR
- H02N1/00—Electrostatic generators or motors using a solid moving electrostatic charge carrier
- H02N1/06—Influence generators
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- Manufacturing Of Micro-Capsules (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention belongs to the field of electret sensors, and relates to a microcapsule electret self-generating device, and preparation and application thereof, wherein the microcapsule electret self-generating device comprises: attaching a conductive layer to the PTFE membrane; uniformly mixing PDMS base material and curing agent, and adding PTFE nano particles and charged microcapsule materials to form uncured microcapsule/PTFE/PDMS composite material; coating an uncured microcapsule/PTFE/PDMS composite material on the surface of a PTFE film, and curing to obtain the upper half part of the device; preparing a template with patterns, and coating a release agent on the template; injecting uncured PDMS prepolymer into a template, curing and demolding to obtain a PDMS film with patterns; sequentially loading an AgNWs coating and a metal silver film on the surface of the PDMS film to form a lower electrode; combining the upper half part of the device, the lower electrode and the bottom microstructure, and connecting a lead between the conductive fabric and the lower electrode. The prepared flexible microcapsule electret has stable and uniform externally-applied charges from the inside of the power generation device, better charge storage space closure and higher power generation efficiency.
Description
Technical Field
The invention belongs to the field of electret sensors, and particularly relates to preparation of a microcapsule electret self-generating device.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
With the development of flexible wearable electronics, many emerging applications have attracted a great deal of attention. However, due to their portability, the energy supply of such devices has become a major problem. In recent years, energy harvesting techniques that convert energy from the environment have attracted increasing attention as they can supplement the power of small electronic products, which may enable long-term and even sustainable operation.
Because of the built-in additional charge, the electrostatic flexible electret generates charge flow on the surface when the electret is deformed by external load, and has a power generation effect. The existing electret power generation device is a simple composite material without patterns, has low sensitivity, generates very small electric quantity under the action of external load, is insufficient for supporting the electric power required in the use process of small electronic products, and limits the wide application of the electret power generation device in industry.
Secondly, the electret piezoelectric sensor mainly utilizes the electrostatic effect of the electret, so that the electret needs to be polarized before a device is prepared, and the inside of the electret is subjected to an ultrahigh voltage charging process. However, this charging process is prone to damage to the material, and charges are prone to collect on the surface or near surface of the material, causing uneven distribution of electret space charges, and with increasing service time, loss of charges is prone to occur.
The prior electret schematic diagrams are shown in fig. 1 and 2:
1. the polymer is charged directly by high voltage to have additional charge inside.
2. A pattern for storing electric charges is prepared inside the polymer, and then the polymer is charged by high voltage to have additional electric charges inside.
Disclosure of Invention
The invention aims to provide a preparation method of a flexible microcapsule electret self-generating device with stable and uniform externally-added charges, better charge storage space sealing and higher generating efficiency, so as to solve at least one technical problem in the background technology.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
in a first aspect of the invention, a method for preparing a microcapsule electret self-generating device is provided, comprising the following steps:
attaching a conductive layer to the PTFE membrane;
uniformly mixing PDMS base material and curing agent, and adding PTFE nano particles and charged microcapsule materials to form uncured microcapsule/PTFE/PDMS composite material;
coating an uncured microcapsule/PTFE/PDMS composite material on the surface of a PTFE film, and curing to obtain the upper half part of the device;
preparing a template with patterns, and coating a release agent on the template;
injecting uncured PDMS prepolymer into a template, curing and demolding to obtain a PDMS film with patterns;
sequentially loading an AgNWs coating and a metal silver film on the surface of the PDMS film to form a lower electrode;
and combining the upper half part of the device, the lower electrode and the bottom microstructure, and connecting a lead between the conductive fabric and the lower electrode to obtain the microcapsule electret self-generating device.
For the second electret in the background art, the solution of the invention uses microcapsules to replace the preparation of the charge storage space inside the polymer, compared with the technology, the space formed by the microcapsules is more stable, the space is larger, and the internal additional charge is more stable, but the preparation of the charge storage space inside the polymer is not mentioned in the background part.
In a second aspect of the invention, there is provided a microcapsule electret self-generating device prepared by any of the above methods.
In a third aspect of the present invention, there is provided a microcapsule electret self-generating device comprising: the device comprises an upper electrode, a PTFE layer, a microcapsule/PTFE/PDMS composite layer, a lower electrode and a bottom microstructure;
the upper electrode, the PTFE layer, the microcapsule/PTFE/PDMS composite layer, the lower electrode and the bottom microstructure are sequentially arranged from top to bottom, and the upper electrode is connected with the lower electrode through a wire.
The invention provides an application of the microcapsule electret self-generating device in preparing flexible wearable electronic equipment.
The invention has the beneficial effects that:
(1) Compared with the prior art, the microcapsule has larger storage space, better sealing property and more stable performance.
Annotation: the microcapsule can form a closed space, can provide more stable storage space for charges, and can control the charges inside the microcapsule without leakage even if the internal charges move actively under high temperature conditions.
(2) The power generation device prepared by the method has high power generation efficiency.
Annotation: the microstructure at the bottom of the electret ensures that the contact area of the device is changed greatly under the deformation condition, so that the sensitivity of the device is higher and the power generation efficiency is higher.
(3) The preparation method does not need a high-voltage charging process, is simpler, and greatly reduces the preparation cost of the flexible electret.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a schematic illustration of a first electret in the prior art;
FIG. 2 is a schematic diagram of a second electret in the prior art;
FIG. 3 is a schematic representation of the device of example 1 of the present invention, wherein 1. Upper electrode, 2.PTFE, 3.PDMS, 4. Microcapsules, 5.PTFE nanoparticles, 6. Lower electrode, 7. Bottom microstructure, 8. Wires;
FIG. 4 shows charged microcapsules prepared in example 1 of the present invention;
FIG. 5 is a schematic diagram of a mold in example 1 of the present invention;
FIG. 6 is a patterned PDMS of example 1 of the present invention;
fig. 7 is a graph showing the self-electricity-generating performance test of the microcapsule electret self-electricity-generating device in example 1 of the present invention.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Term interpretation:
PTFE: polytetrafluoroethylene, polymers, a dielectric material.
PDMS: polydimethyl siloxane, polymer, prepolymer and curing agent according to 10:1, and can be cured into flexible polymer after heating.
Electret: electrets are a general term for a class of dielectric materials capable of long-term charge storage. The prior art generally refers to a dielectric material having a function of storing electric charges by a polarization (charging) treatment, so that the electric charges are stored therein. Under the external load condition, an electric signal is generated due to the electrostatic effect, so that the effect of generating electricity is achieved.
A preparation method of a microcapsule electret self-generating device comprises the following steps:
attaching a conductive layer to the PTFE membrane;
uniformly mixing PDMS base material and curing agent, and adding PTFE nano particles and charged microcapsule materials to form uncured microcapsule/PTFE/PDMS composite material;
coating an uncured microcapsule/PTFE/PDMS composite material on the surface of a PTFE film, and curing to obtain the upper half part of the device;
preparing a template with patterns, and coating a release agent on the template;
injecting uncured PDMS prepolymer into a template, curing and demolding to obtain a PDMS film with patterns;
sequentially loading an AgNWs coating and a metal silver film on the surface of the PDMS film to form a lower electrode;
and combining the upper half part of the device, the lower electrode and the bottom microstructure, and connecting a lead between the conductive fabric and the lower electrode to obtain the microcapsule electret self-generating device.
In some embodiments, the method of making the charged microcapsules comprises:
uniformly mixing urea formaldehyde prepolymer and emulsifier to form water phase;
SiO is made of 2 Adding the sol material into dichloromethane, and uniformly mixing to form an oil phase;
adding the oil phase into the water phase for emulsification to form an oil-in-water emulsion;
acidifying the oil-in-water emulsion, adding resorcinol for reaction, collecting the product, washing, separating solid from liquid, and drying to obtain the charged microcapsule.
In some embodiments, the emulsifier is polyvinyl alcohol.
In some embodiments, the urea formaldehyde prepolymer is prepared by: uniformly mixing formaldehyde aqueous solution and urea, adding triethanolamine to adjust the pH of the mixed system to 8-9, and carrying out water bath heating reaction to obtain a transparent urea formaldehyde prepolymer; adding water, and cooling for standby.
In some embodiments, the conductive layer is composed of a conductive fabric or a conductive film, preferably made of at least one of a deposited metal film, a metal nanowire, a conductive polymer.
In some embodiments, the pattern is at least one of a cone, a pyramid, a micron-sized cylinder.
In some embodiments, the PTFE film has a thickness of 0.03 to 0.1mm.
The invention will now be described in further detail with reference to the following specific examples, which should be construed as illustrative rather than limiting.
In the following examples, the curative was a us doukangnin 184 silicone rubber, and two bottles were dispensed, one bottle being the prepolymer substrate and the other bottle being the curative. When stored alone, the rubber is a flowable liquid, and after mixing, the rubber solidifies into a flexible solid rubber material.
Example 1:
1. preparation of charged microcapsule materials:
1. preparation of capsule shell urea formaldehyde prepolymer
The formaldehyde aqueous solution (37%) and urea were added to the beaker in a mass ratio of 1:1 and mixed well, the magnetic stirrer speed was set to 300rpm, and stirring was carried out until complete dissolution. Adding analytically pure triethanolamine to regulate the pH value of the mixed system to 8-9. The reaction system is heated for 60min in water bath at 70 ℃ to obtain transparent urea formaldehyde prepolymer. And weighing the mass of the obtained urea formaldehyde prepolymer, slowly adding 2 times of deionized water at room temperature into the prepolymer, and waiting for natural cooling for standby.
2. Preparation of aqueous phase
50ml of deionized water is heated to 50 ℃, 1.6g of PVA powder is added in multiple times under the rotation speed of 500rpm of a magnetic stirrer, then the temperature is heated to 80 ℃ and stirring is continued until the PVA powder is completely dissolved, and then the PVA powder is cooled to room temperature to serve as an emulsifier for standby. 10.8g of the prepared prepolymer was added to an emulsifier and uniformly mixed to obtain an aqueous phase.
3. Preparation of the oil phase
1g of SiO 2 The sol material was added to 30g of methylene chloride as an oil phase.
4. Preparation of charged microcapsules
7.5g of the oil phase was added to 62.4g of the water phase and emulsified for 5min with stirring at 800rpm to give an oil-in-water emulsion. After the emulsification is successful, 0.1mol/L dilute hydrochloric acid is used to gradually adjust the pH of the solution to 3, and the acidification process is controlled to be about 2 hours. 0.5g of analytically pure resorcinol was added to the acidified solution, the solution temperature was raised to 60℃and heated at constant temperature for 1h. Repeatedly washing the obtained product with deionized water for 6 times, standing, removing supernatant, and oven drying at 60deg.C to obtain dried charged microcapsule.
2. Preparation of a flexible microcapsule electret self-generating device:
1. preparation of the upper half of the device:
(1) First, an upper electrode (e.g., a conductive fabric or other conductive film such as a deposited metal film, metal nanowires, conductive polymer, etc., having a thickness of about 100 μm) is attached to a PTFE film (the thickness of the PTFE film may be 0.03 to 0.1mm, and this embodiment employs 0.1 mm).
(2) Mixing PDMS base material and curing agent according to a weight ratio of 10: mixing the materials according to the mass ratio of 1; the PTFE nanoparticle and the prepared charged microcapsule material were then mixed at 1:1:1 to the mixture.
(3) The uncured microcapsule/PTFE/PDMS composite was spin coated onto the surface of the PTFE film (thickness about 1 mm) by a spin coater.
(4) The composite was placed in an oven and cured at 80 ℃ for 1 hour, the diameter of the microcapsules after curing being 20-100 microns, wherein the PTFE particles were approximately 200 nanometers in diameter.
2. Preparation of the lower half of the device:
(1) Templates (which may be cones, pyramids, micro-scale cylinders, etc.) of the acrylates were prepared by a stereolithography 3D printer.
(2) A low surface energy release agent (e.g., polytetrafluoroethylene, perfluorooctyl trichlorosilane, etc.) is spin coated onto the surface of the template to aid in release.
(3) Uncured PDMS prepolymer (10:1 ratio of binder to curing agent) was injected into the template, placed in a vacuum oven and degassed for 10 minutes to remove air bubbles, and then cured at a temperature of 80 ℃ for 1 hour. And then separating the PDMS film with the conical pattern on the surface from the template after curing.
(4) A dispersion of AgNWs (silver nanowires) in alcohol was diluted to 0.5mg/mL and spin coated onto a PDMS surface with a conical pattern (PDMS substrate about 1 mm).
(5) And depositing a layer of metal silver film (the thickness of the metal layer is about 1 micron) on the surface of the AgNWs coating by a vacuum evaporation technology, and forming the lower electrode together.
Finally, the upper part and the lower part are combined together to form the microcapsule electret self-generating device.
The performance of the microcapsule electret self-generating device prepared as described above was tested and the result is that the device produced an alternating current of about 9 microamps at maximum under pressing conditions as shown in fig. 7.
Finally, it should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited to the above-mentioned embodiments, but may be modified or substituted for some of them by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the microcapsule electret self-generating device is characterized by comprising the following steps of:
attaching a conductive layer to the PTFE membrane;
uniformly mixing PDMS base material and curing agent, and adding PTFE nano particles and charged microcapsule materials to form uncured microcapsule/PTFE/PDMS composite material;
coating an uncured microcapsule/PTFE/PDMS composite material on the surface of a PTFE film, and curing to obtain the upper half part of the device;
preparing a template with patterns, and coating a release agent on the template;
injecting uncured PDMS prepolymer into a template, curing and demolding to obtain a PDMS film with patterns;
sequentially loading an AgNWs coating and a metal silver film on the surface of the PDMS film to form a lower electrode;
combining the upper half part of the device, the lower electrode and the bottom microstructure, and connecting a lead between the upper electrode and the lower electrode to obtain a microcapsule electret self-generating device;
the preparation method of the charged microcapsule comprises the following steps:
uniformly mixing urea formaldehyde prepolymer and emulsifier to form water phase;
SiO is made of 2 Adding the sol material into dichloromethane, and uniformly mixing to form an oil phase;
adding the oil phase into the water phase for emulsification to form an oil-in-water emulsion;
acidifying the oil-in-water emulsion, adding resorcinol for reaction, collecting the product, washing, separating solid from liquid, and drying to obtain the charged microcapsule.
2. The method for preparing a microcapsule electret self-generating device according to claim 1, wherein the emulsifier is polyvinyl alcohol.
3. The method for preparing the microcapsule electret self-generating device of claim 1, wherein the method for preparing the urea formaldehyde prepolymer is as follows: uniformly mixing formaldehyde aqueous solution and urea, adding triethanolamine to adjust the pH of the mixed system to 8-9, and carrying out water bath heating reaction to obtain a transparent urea formaldehyde prepolymer; adding water, and cooling for standby.
4. The method of claim 1, wherein the conductive layer is made of a conductive fabric or a conductive film.
5. The method of claim 4, wherein the conductive film is made of at least one of a deposited metal film, a metal nanowire, and a conductive polymer.
6. The method for preparing a microcapsule electret self-generating device according to claim 1, wherein the pattern is at least one of cone, pyramid, and micron-sized cylinder.
7. A microcapsule electret self-generating device made by the method of any of claims 1-6.
8. A microcapsule electret self-generating device, comprising: the device comprises an upper electrode, a PTFE layer, a charged microcapsule/PTFE/PDMS composite layer, a lower electrode and a bottom microstructure;
the upper electrode, the PTFE layer, the charged microcapsule/PTFE/PDMS composite layer, the lower electrode and the bottom microstructure are sequentially arranged from top to bottom, and the upper electrode is connected with the lower electrode through a wire.
9. The microcapsule electret self-generating device of claim 8 wherein the PTFE film has a thickness of 0.03 to 0.1mm.
10. Use of the microcapsule electret self-generating device of any one of claims 7-9 in the manufacture of a flexible wearable electronic device.
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| CN103682083A (en) * | 2012-08-31 | 2014-03-26 | 纳米新能源（唐山）有限责任公司 | Piezoelectric electret film and preparation method thereof |
| CN103700761A (en) * | 2013-11-27 | 2014-04-02 | 深圳市豪恩声学股份有限公司 | Piezoelectret structure and preparation method thereof |
| CN108063183A (en) * | 2017-11-30 | 2018-05-22 | 西安交通大学 | A kind of method that closing porous piezoelectric electret energy accumulator is prepared based on nano impression |
| CN111327224A (en) * | 2018-12-17 | 2020-06-23 | 北京纳米能源与系统研究所 | Waterproof electret material, electret method and friction nano-generator |
| CN110455443A (en) * | 2019-08-23 | 2019-11-15 | 北京航空航天大学 | A kind of flexible capacitive sensor and preparation method thereof using the preparation of silver nanowires flexible electrode |
| CN111682099A (en) * | 2020-06-01 | 2020-09-18 | 华中科技大学 | Flexible polymer piezoelectric film and preparation method thereof |
| CN113108953A (en) * | 2021-03-29 | 2021-07-13 | 山东大学 | Flexible microcapsule piezoelectric sensor and preparation method thereof |
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