CN118978723A - A flower-shaped ZnO/PEDOT:PSS composite film and preparation method thereof and the obtained flexible electronic skin sensor - Google Patents
A flower-shaped ZnO/PEDOT:PSS composite film and preparation method thereof and the obtained flexible electronic skin sensor Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 229920000144 PEDOT:PSS Polymers 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 31
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims abstract description 24
- 238000007639 printing Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 9
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 9
- 238000012544 monitoring process Methods 0.000 claims abstract description 9
- 210000002321 radial artery Anatomy 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 18
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 18
- 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 description 18
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 18
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 18
- 238000000137 annealing Methods 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000004044 response Effects 0.000 abstract description 10
- 238000001514 detection method Methods 0.000 abstract description 4
- 230000010354 integration Effects 0.000 abstract description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 94
- 239000011787 zinc oxide Substances 0.000 description 47
- 210000003491 skin Anatomy 0.000 description 32
- 229920000139 polyethylene terephthalate Polymers 0.000 description 28
- 239000005020 polyethylene terephthalate Substances 0.000 description 28
- 239000004734 Polyphenylene sulfide Substances 0.000 description 21
- 229920000069 polyphenylene sulfide Polymers 0.000 description 21
- 239000010410 layer Substances 0.000 description 16
- 230000035945 sensitivity Effects 0.000 description 4
- 244000137852 Petrea volubilis Species 0.000 description 3
- 239000004696 Poly ether ether ketone Substances 0.000 description 3
- 238000002493 microarray Methods 0.000 description 3
- 239000011664 nicotinic acid Substances 0.000 description 3
- 229920002530 polyetherether ketone Polymers 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 210000000707 wrist Anatomy 0.000 description 1
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- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/68—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The invention belongs to the technical field of flexible electronic skin sensors, and discloses a flower-shaped ZnO/PEDOT: PSS composite film, a preparation method thereof and a prepared flexible electronic skin sensor. The ZnO/PEDOT/PSS composite film is prepared by coating a mask on an ITO surface of an ITO/PET flexible substrate subjected to cleaning and drying treatment to perform magnetron sputtering ZnO, performing hydrothermal treatment at 80-90 ℃ and removing the mask to obtain a flower-shaped ZnO nano array; and preparing the PEDOT-PSS conductive layer on the flower-shaped ZnO nano array by a liquid drop printing method. The flexible electronic skin sensor prepared based on the ZnO/PEDOT/PSS composite film has the characteristics of high precision, wide detection range, high integration level, multiple response and the like, realizes the functions of pressure sense and touch sense similar to the skin of a human fingertip, and can be applied to the field of monitoring the pulse of the radial artery of a human body.
Description
Technical Field
The invention belongs to the technical field of flexible electronic skin sensors, and particularly relates to a flower-shaped ZnO/PEDOT/PSS composite film, a preparation method thereof and a prepared flexible electronic skin sensor.
Background
The pressure sensor is a device for detecting and transmitting pressure information, can convert pressure signals into electric signals or other forms of output signals according to a certain rule and mode, and has wide application prospects in the fields of aerospace, intelligent building, railway traffic, intelligent medical treatment and Internet of things. Traditional pressure sensors based on semiconductor materials, metal materials and piezoelectric crystals have the advantages of mature preparation process, high sensitivity, stable performance, wide detection range and the like, but are relatively large in volume and cannot bear large bending deformation, so that the application of the pressure sensors in the flexible wearable field is limited. In recent years, along with development of technology and improvement of demands of people, flexible pressure sensors based on functional materials are developed, and the flexible pressure sensors have the characteristics of light weight, small volume, flexibility, deformability and the like, can be attached to curved objects and human skin surfaces, and have great application potential in the fields of wearable electronics, soft robots, flexible display, electronic skin and the like. In order to meet the application requirements in these fields, flexible pressure sensors are required to have both high sensitivity and good bending characteristics. Therefore, it is of great importance to prepare an ultra-thin pressure-sensitive response layer having a surface microstructure and to use it for flexible electronic skin.
Zinc oxide has the advantages of good biocompatibility, low toxicity and simple preparation method, has been widely applied to various electronic devices and catalysis fields, but the preparation of flower-shaped ZnO/PEDOT: PSS film and the application of high-sensitivity ultrathin flexible electronic skin have not been reported at present.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the primary purpose of the invention is to provide a flower-shaped ZnO/PEDOT/PSS composite film. The composite film is provided with a micro array with a bionic structure, and the flexible electronic skin sensor with high integration level is manufactured based on the micro array.
Another object of the present invention is to provide a method for preparing the above-mentioned flower-shaped ZnO/PEDOT: PSS composite film, which uses indium tin oxide/polyethylene terephthalate (ITO/PET) as a flexible substrate and an electrode, to prepare a flower-shaped zinc oxide/poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonic acid), abbreviated as ZnO/PEDOT: PSS composite film.
Still another object of the present invention is to provide a flexible electronic skin sensor made of the above flower-shaped ZnO/PEDOT: PSS composite film, which achieves a response to external pressure and can monitor a human pulse signal.
The aim of the invention is achieved by the following technical scheme:
a flower-shaped ZnO/PEDOT/PSS composite film is prepared by coating a mask on an ITO surface of an ITO/PET flexible substrate subjected to cleaning and drying treatment to perform magnetron sputtering ZnO, performing hydrothermal treatment at 80-90 ℃ and removing the mask to obtain a flower-shaped ZnO nano array; and preparing the PEDOT-PSS conductive layer on the flower-shaped ZnO nano array by a liquid drop printing method.
Preferably, the time of the hydrothermal treatment is 1-2 hours.
The preparation method of the flower-shaped ZnO/PEDOT/PSS composite film comprises the following specific steps:
S1, after cleaning and drying an ITO/PET flexible substrate, coating a mask on the ITO surface of the ITO flexible substrate, performing magnetron sputtering deposition under the condition of 250-300W to obtain a ZnO seed crystal layer, performing hydrothermal treatment at the temperature of 80-90 ℃, and removing the mask to obtain a flower-shaped ZnO nano array;
S2, adopting a liquid drop printing system, wherein the temperature of a printing table is 40-45 ℃, the liquid drop distance is 10-12 mu m, placing a printed PEDOT-PSS film on the printing table for drying after printing, and then annealing at 90-100 ℃, and preparing a PEDOT-PSS conductive layer on the flower-shaped ZnO nano array to obtain the ZnO/PEDOT-PSS composite film.
Preferably, the time of the magnetron sputtering deposition in the step S1 is 25-30 seconds; the thickness of the ZnO seed crystal layer is 40-50 nm; the area of the flower-shaped ZnO nano-array is (150-200) mu m x (150-200) mu m.
Preferably, the drying time in the step S2 is 15-20 min, and the annealing time is 10-15 min.
A flexible electronic skin sensor is composed of a plurality of sensor units, wherein the structure of each sensor unit is abbreviated as PET/Cu-ITO/ZnO/PEDOT, PSS/ITO-Cu/PET/PDMS, and the flexible electronic skin sensor is composed of a ZnO/PEDOT/PSS composite film on an ITO/PET flexible substrate and a PDMS film on the ITO/PET flexible substrate, and then the ITO is connected by copper wires.
Preferably, the PDMS film on the ITO/PET flexible substrate is prepared by coating PDMS on a PET substrate of the ITO/PET flexible substrate and annealing at 90-100 ℃.
The flexible electronic skin sensor is applied to the pulse monitoring of the radial artery of a human body.
Compared with the prior art, the technical scheme has the following beneficial effects:
1. The flower-shaped ZnO/PEDOT/PSS composite film is prepared by taking indium tin oxide/polyethylene terephthalate (ITO/PET) as a flexible substrate and an electrode, and is abbreviated as ZnO/PEDOT/PSS composite film, and the flower-shaped ZnO nano array is prepared by adopting a hydrothermal method, the area of the nano array can be controlled within the range of (150-200) mu m x (150-200) mu m, the preparation cost is low, and the preparation of the flexible film with a surface microstructure increases the sensitivity of a sensor in the aspect of detecting shear force.
2. The ZnO/PEDOT-PSS composite film with the flower-shaped structure has the sensor response layer film microarray with the bionic structure, and the flexible electronic skin sensor is prepared based on the ZnO/PEDOT-PSS composite film with the flower-shaped structure, has high integration, realizes the functions of pressure sense and touch sense similar to the skin of a human fingertip, and improves the accuracy of detecting the external pressure distribution of the electronic skin and identifying the texture of the surface of an object. The flexible electronic skin sensor has the characteristics of high sensitivity and wide detection range, more than 100kPa -1, object surface texture detection limit of less than 10 mu m, high integration level, multiple response and the like, realizes the pressure sense and touch sense functions similar to the skin of human fingertips, has the characteristics of light weight, softness, comfort and the like, can reduce the burden and discomfort of wearing by users, is used for monitoring the pulse signals of the radial artery of the human body, responds to the external pressure, and has wide application prospect in the fields of motion analysis and health management.
Drawings
FIG. 1 is a flow chart of the preparation of the flower-shaped ZnO/PEDOT-PSS composite film and the flexible electronic skin sensor prepared by the same;
FIG. 2 shows the surface morphology of the ZnO/PEDOT/PSS composite film prepared in example 1;
FIG. 3 is an external pressure response chart of the flexible electronic skin sensor of application example 1;
Fig. 4 is a human radial artery pulse signal monitoring using the flexible electronic skin sensor of example 1.
Detailed Description
The technical solutions according to the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the embodiments described herein are only for illustrating and explaining the present invention, but should not be construed as limiting the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
1. Cleaning an ITO/PET flexible substrate, drying at 60 ℃ for 30min, coating a mask on the ITO surface of the ITO flexible substrate, performing magnetron sputtering deposition at 300W for 30 seconds to obtain a 40nm ZnO seed crystal layer, performing hydrothermal treatment at 90 ℃ for 1h, and removing the mask to obtain a flower-shaped ZnO nano array;
2. And adopting a liquid drop printing system, wherein the temperature of a printing table is 40 ℃, the liquid drop distance is 10 mu m, preparing a PEDOT (polyether-ether-ketone) PSS conductive layer on the surface of the flower-shaped ZnO nano array, printing a film with 1-5 stacking layers for reducing sheet resistance, placing the printed PEDOT PSS film on the printing table, drying for 15min, and then annealing at 90 ℃ for 10min to prepare the flower-shaped ZnO/PEDOT PSS composite film on the ITO/PET flexible substrate, wherein the effective area of the flower-shaped ZnO/PEDOT PSS composite film is 200 mu m multiplied by 200 mu m, as shown in figure 1.
FIG. 2 shows the surface morphology of the ZnO/PEDOT/PSS composite film prepared in example 1. Wherein, (a) is the surface morphology of the flower-shaped ZnO nano material. And (b) the surface morphology of the ZnO/PEDOT/PSS composite film. As can be seen from fig. 2, a flower-shaped ZnO nano-array was prepared on an ITO/PET flexible substrate, and a PEDOT: PSS conductive layer was prepared thereon by a droplet printing method, to obtain a ZnO/PEDOT: PSS film having a bionic structure.
Example 2
1. Cleaning an ITO/PET flexible substrate, drying at 60 ℃ for 30min, coating a mask on the ITO surface of the ITO flexible substrate, performing magnetron sputtering deposition at 250W for 30 seconds to obtain a 45nm ZnO seed crystal layer, performing hydrothermal treatment at 80 ℃ for 1h, and removing the mask to obtain a flower-shaped ZnO nano array;
2. and adopting a liquid drop printing system, wherein the temperature of a printing table is 45 ℃, the liquid drop distance is 12 mu m, preparing a PEDOT (polyether-ether-ketone) PSS conductive layer on the surface of the flower-shaped ZnO nano array, printing a film with 1-5 stacking layers for reducing sheet resistance, placing the printed PEDOT PSS film on the printing table, drying for 15min, and then annealing at 100 ℃ for 8min to prepare the flower-shaped ZnO/PEDOT PSS composite film on the ITO/PET flexible substrate, wherein the effective area of the flower-shaped ZnO/PEDOT PSS composite film is 150 mu m multiplied by 150 mu m.
Application example 1
1. PDMS (purchased from Dow Corning company) solution is coated on a 120-mesh sand paper template, a layer of ITO/PET substrate is covered, a roller rod auxiliary pressing process is used for preparing a uniform PDMS film between the sand paper and the ITO/PET substrate, the microstructure of the PDMS film has a gradient structure imitating the skin surface layer to the dermis layer of human skin, the PDMS film is heated and cured for 1h at 90 ℃, and after the sand paper template is removed, the microstructure PDMS film is prepared on the ITO/PET substrate. Annealing at 100 ℃ to tightly combine PDMS and PET together to obtain an ITO/PET/PDMS film;
2. The ZnO/PEDOT: PSS composite film and the ITO/PET/PDMS film combination are prepared on an ITO/PET flexible substrate in the embodiment 1, two ITO are connected by copper wires and respectively used as a top electrode and a bottom electrode to prepare a flexible electronic skin sensor unit, the structure is abbreviated as PET/Cu-ITO/ZnO/PEDOT: PSS/ITO-Cu/PET/PDMS, and a plurality of sensor units are combined into the flexible electronic skin sensor as shown in figure 1.
Fig. 3 is an external pressure response chart of the flexible electronic skin sensor of application example 1. Wherein (a) is a change in current generated by the flexible electronic skin sensor at a pressure of 200 Pa. (b) Is a change in current produced by a flexible electronic skin sensor at a pressure of 1 kPa. As can be seen from FIG. 3, the single-point pressure sensor based on the ZnO/PEDOT: PSS response layer film realizes good external pressure response. The flexible electronic skin sensor can respond to external pressure, and current changes along with the external pressure under different external pressure conditions. The surface of the PET flexible substrate is attached with a PDMS film, a human fingerprint microstructure is simulated, and the flexible electronic skin sensor is fixed on a test bench and used for detecting responses generated by different pressures. The flexible electronic skin sensor can be applied to monitoring of the pulse signals of the radial artery of a human body, and is fixed at the pulse position of the radial artery of the wrist of a tester (a healthy male) and used for monitoring the pulse signals of the human body. Fig. 4 is a human radial artery pulse signal monitoring using the flexible electronic skin sensor of example 1. As can be seen from fig. 4, the flexible electronic skin sensor is capable of monitoring the pulse signal of the human body, the monitored pulse frequency being about 60 times per minute, in accordance with the expected value of a healthy male aged 20 years.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (8)
1. A flower-shaped ZnO/PEDOT-PSS composite film is characterized in that the ZnO/PEDOT-PSS composite film is prepared by coating a mask on an ITO surface of an ITO/PET flexible substrate which is cleaned and dried, performing magnetron sputtering ZnO, performing hydrothermal treatment at 80-90 ℃ and removing the mask to obtain a flower-shaped ZnO nano array; and preparing the PEDOT-PSS conductive layer on the flower-shaped ZnO nano array by a liquid drop printing method.
2. The flower-shaped ZnO/PEDOT: PSS composite film according to claim 1, wherein the time of the hydrothermal treatment is 1 to 2 hours.
3. The preparation method of the flower-shaped ZnO/PEDOT/PSS composite film according to claim 1 or 2, which is characterized by comprising the following specific steps:
S1, after cleaning and drying an ITO/PET flexible substrate, coating a mask on the ITO surface of the ITO flexible substrate, performing magnetron sputtering deposition under the condition of 250-300W to obtain a ZnO seed crystal layer, performing hydrothermal treatment at the temperature of 80-90 ℃, and removing the mask to obtain a flower-shaped ZnO nano array;
S2, adopting a liquid drop printing system, wherein the temperature of a printing table is 40-45 ℃, the liquid drop distance is 10-12 mu m, placing a printed PEDOT-PSS film on the printing table for drying after printing, and then annealing at 90-100 ℃, and preparing a PEDOT-PSS conductive layer on the flower-shaped ZnO nano array to obtain the ZnO/PEDOT-PSS composite film.
4. The method for preparing a flower-shaped ZnO/PEDOT: PSS composite film according to claim 3, characterized in that the magnetron sputtering deposition time in step S1 is 25 to 30 seconds; the thickness of the ZnO seed crystal layer is 40-50 nm; the area of the flower-shaped ZnO nano-array is (150-200) mu m x (150-200) mu m.
5. The method for producing a flower-shaped ZnO/PEDOT: PSS composite film according to claim 3, characterized in that the drying time in step S2 is 15 to 20min and the annealing time is 10 to 15min.
6. A flexible electronic skin sensor is characterized by comprising a plurality of sensor units, wherein the sensor units are abbreviated as PET/Cu-ITO/ZnO/PEDOT: PSS/ITO-Cu/PET/PDMS, and the flexible electronic skin sensor is formed by combining a ZnO/PEDOT: PSS composite film on an ITO/PET flexible substrate and a PDMS film on the ITO/PET flexible substrate according to claim 1 or 2 and then connecting the ITO with copper wires.
7. The flexible electronic skin sensor of claim 6, wherein the PDMS film on the ITO/PET flexible substrate is prepared by coating PDMS on a PET substrate of the ITO/PET flexible substrate and annealing at 90-100 ℃.
8. Use of a flexible electronic skin sensor according to claim 6 or 7 for monitoring the pulse of the radial artery of a human.
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| CN101798105A (en) * | 2009-11-13 | 2010-08-11 | 襄樊学院 | Preparation technology for growing ZnO nanorod arrays on ITO PET film |
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