CN113491509A - Preparation method of flexible electronic sensor - Google Patents

Preparation method of flexible electronic sensor Download PDF

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Publication number
CN113491509A
CN113491509A CN202110673010.1A CN202110673010A CN113491509A CN 113491509 A CN113491509 A CN 113491509A CN 202110673010 A CN202110673010 A CN 202110673010A CN 113491509 A CN113491509 A CN 113491509A
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China
Prior art keywords
film
flexible
electronic sensor
silver
flexible electronic
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CN202110673010.1A
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Chinese (zh)
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周星
王咚
宋仁坊
方长青
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Xian University of Technology
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Xian University of Technology
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Priority to CN202110673010.1A priority Critical patent/CN113491509A/en
Publication of CN113491509A publication Critical patent/CN113491509A/en
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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
    • A61B5/02—Detecting, measuring or recording pulse, heart rate, blood pressure or blood flow; Combined pulse/heart-rate/blood pressure determination; Evaluating a cardiovascular condition not otherwise provided for, e.g. using combinations of techniques provided for in this group with electrocardiography or electroauscultation; Heart catheters for measuring blood pressure
    • A61B5/0205—Simultaneously evaluating both cardiovascular conditions and different types of body conditions, e.g. heart and respiratory condition
    • 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
    • A61B5/6801—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be attached to or worn on the body surface
    • 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
    • A61B5/6801—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be attached to or worn on the body surface
    • A61B5/6843—Monitoring or controlling sensor contact pressure
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
    • A61B2562/12—Manufacturing methods specially adapted for producing sensors for in-vivo measurements
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
    • A61B2562/12—Manufacturing methods specially adapted for producing sensors for in-vivo measurements
    • A61B2562/125—Manufacturing methods specially adapted for producing sensors for in-vivo measurements characterised by the manufacture of electrodes
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
    • A61B2562/16—Details of sensor housings or probes; Details of structural supports for sensors
    • A61B2562/164—Details of sensor housings or probes; Details of structural supports for sensors the sensor is mounted in or on a conformable substrate or carrier

Abstract

The invention discloses a preparation method of a flexible electronic sensor, which comprises the steps of constructing a patterned polydimethylsiloxane film by using a lotus leaf surface with a natural microstructure as a mold, forming a self-supporting polypyrrole/silver film on a gas-liquid interface by using an oxidation-reduction reaction of silver nitrate and pyrrole under the catalysis of ultraviolet illumination, and constructing the flexible sensor with the surface having the microstructure by using the patterned polydimethylsiloxane film as a flexible substrate and a packaging layer. The flexible sensor disclosed by the invention is simple in preparation process, can sense pressure, strain and micro vibration, such as throat vibration during speaking and breath and pulse vibration in different states, has high flexibility, high stability, high sensitivity and high response speed, and is expected to be applied to the fields of motion detection, health monitoring systems, information transmission and the like.

Description

Preparation method of flexible electronic sensor
Technical Field
The invention belongs to the technical field of sensors, and relates to a preparation method of a flexible electronic sensor.
Background
With the popularization of intelligent terminals, wearable electronic equipment presents huge market prospects. The sensor, as one of the core components, will affect the functional design and future development of the wearable device. Sensors play a crucial role in human health monitoring. In recent years, significant progress has been made in the field of wearable implantable sensors, and a variety of sensors have been heavily adopted by many intelligent detection devices, and applications thereof have long penetrated aspects such as medical diagnosis, bioengineering, and industrial production. With the increasing application demand of the information age, the expected values and the ideal requirements for various performance parameters such as the range, the precision and the stability of the measured information are gradually increased.
New sensor technologies have evolved towards the following trends: developing new materials, new processes and new sensors; the sensitivity of the sensing device is realized. At the same time, it is desirable that the sensor also be flexible, extensible, freely bendable or even foldable, portable, wearable, etc. Along with the popularization of intelligent terminals, wearable flexible electronic devices show great market prospects. Significant progress has been made in the field of wearable implantable sensors, such as sensors that respond to pressure or deformation made of functional materials, such as carbon nanotubes, graphene or conductive polymers. The flexible wearable electronic sensor has the characteristics of being light, thin, portable, excellent in electrical performance, high in integration level and the like, so that the flexible wearable electronic sensor becomes one of the most concerned electrical sensors. However, it remains a great challenge to implement high resolution, high sensitivity, fast response and complex signal detection of flexible wearable electronic sensors, such as sensing a slight vibration of the throat when a person speaks to implement the sensing of fundamental tone signals and monitoring the breath and pulse micro-vibrations in different states.
With the development of flexible substrate materials, flexible sensors meeting the above-mentioned various trend characteristics have come to be developed. Among various novel sensing devices, the sensor based on the two-dimensional film has potential application prospects in the aspects of sensing, catalysis, biomedical monitoring and the like due to the diversity of preparation and performance, and has received wide attention. The conductive polymer/metal two-dimensional film composed of conductive polymer (polypyrrole, polyaniline, polythiophene, and the like) and metal nano material (gold, silver, copper, and the like) is considered as a method with a great application prospect for preparing an integrated device, and the silver nano particles can overcome the defects of poor conductive stability, poor toughness and the like of polypyrrole due to high conductivity, easy ductility and low cost. Polypyrrole films provide a uniform and large surface area to immobilize silver nanoparticles, while the conductivity of PPy doped with silver nanoparticles is further enhanced. A key problem in the development of sensors based on conductive polymer/metal two-dimensional thin films is how to effectively combine a two-dimensional conductive film with a flexible conductive film to maintain its efficient performance.
Disclosure of Invention
The invention aims to provide a preparation method of a flexible electronic sensor, which has the characteristics of high flexibility, high stability, high sensitivity and high response speed.
The technical scheme adopted by the invention is that the preparation method of the flexible electronic sensor is implemented according to the following steps:
step 1, constructing a patterned polydimethylsiloxane film;
step 2, mixing 10-600 mmol/L silver nitrate aqueous solution and 5-200 mul of pyrrole solution, and irradiating for 0.5-6 hours under ultraviolet light to form a self-supporting polypyrrole/silver composite film on the surface of the mixed solution;
and 3, taking the patterned polydimethylsiloxane film as a flexible substrate, transferring the self-supporting polypyrrole/silver composite film to the patterned surface of the flexible substrate, then solidifying the flexible lead at two ends of the polypyrrole/silver film by using conductive silver paste, finally packaging the polypyrrole/silver film by using another patterned polydimethylsiloxane film, and contacting the patterned surface of the packaged polydimethylsiloxane film with the polypyrrole/silver film to obtain the flexible electronic sensor.
The invention is also characterized in that:
step 1 specifically adopts the lotus leaf surface with a natural microstructure as a mold to construct a patterned polydimethylsiloxane film.
Step 1 specifically, cleaning the surface of fresh lotus leaves or dried lotus leaves completely soaked by ultrapure water by using ethanol and ultrapure water in sequence, wiping water drops on the surface of the lotus leaves, flatly sticking the water drops on the surface of a base material, spin-coating mixed liquid of dimethyl siloxane and a curing agent in a mass ratio of 9:1 on the surface of the lotus leaves, carrying out vacuum defoaming and curing, and tearing off the cured polydimethylsiloxane to obtain the patterned polydimethylsiloxane film.
In the step 1, the vacuum defoaming time is 20-30 minutes.
In the step 1, the curing temperature is 70-80 ℃ and the curing time is 2-3 hours.
The thickness of the self-supporting polypyrrole/silver composite film is 100-200 nm.
In the step 3, the curing temperature of the conductive silver paste is 60-70 ℃, and the curing time is 1-2 hours.
The flexible lead is a copper wire, and the diameter of the copper wire is 0.3-0.4 mm.
The invention has the beneficial effects that:
the flexible sensor utilizes the self-supporting polypyrrole and silver composite film as a conductive layer, the patterned polydimethylsiloxane film as a substrate and an encapsulation layer and the copper wire as a flexible electrode, can sense pressure, tensile and bending strain and micro vibration, such as throat vibration during speaking and breath and pulse vibration in different states, has high flexibility, high stability, high sensitivity and high response speed, and is expected to be applied to the fields of motion detection, health monitoring systems, information transmission and the like.
Drawings
FIG. 1 is a current-voltage plot of a flexible sensor prepared in example 1;
FIG. 2 is a graph of resistance cycle period for bending strain sensed by the flexible sensor prepared in example 1;
FIG. 3 is a graph of current versus time for tensile strain sensed by the flexible sensor prepared in example 1;
FIG. 4 is a graph of current versus time for pressure sensing in the flexible sensor prepared in example 1;
FIG. 5 is a graph of current versus time for the flexible sensor prepared in example 1 to sense the vibration of the throat of a subject when the subject speaks a different word;
FIG. 6 is a graph of the current time of the breath of the flexible sensor prepared in example 1 in different states;
FIG. 7 is a graph of the current time curve of the pulse vibration in different states of the flexible sensor induction examiner prepared in example 1.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
Dried lotus leaf Dimethylsiloxane Curing agent Silver nitrate
2×5cm 10 to 90 parts by weight of 0.5 to 10 parts by weight 0.1 to 1 part by weight
Azole compounds Ethanol Ultrapure water Conductive silver paste
1 to 10 parts by weight 10 to 200 parts by weight of 50-500 parts by weight 2 to 10 parts by weight of
The invention relates to a preparation method of a flexible electronic sensor, which is implemented according to the following steps:
step 1, soaking dry lotus leaves in ultrapure water for about 5 hours to completely soak the lotus leaves, then sequentially cleaning the surfaces of the lotus leaves for 3 times by using ethanol and ultrapure water respectively, wiping water drops on the surfaces of the lotus leaves, and flatly pasting the lotus leaves on glass slides with the sizes of 50mm multiplied by 20 mm; mixing dimethyl siloxane and a curing agent in the Dow Corning 184 according to a mass ratio of 9:1, spin-coating on the surface of lotus leaves, defoaming the lotus leaves in a vacuum drying oven for about 30 minutes, curing the lotus leaves in an oven at 80 ℃ for 2 hours, and carefully tearing off the cured dimethyl siloxane to obtain a patterned polydimethylsiloxane film with the thickness of about 0.3 mm;
step 2, adding 0.3 part by weight of silver nitrate into ultrapure water to prepare a silver nitrate aqueous solution with the mass fraction of 12%, placing 2.5mL of the silver nitrate aqueous solution with the mass fraction of 12% into a 20mL culture dish, dropwise adding 20 mul of pyrrole, fixing the volume to 10mL by using the ultrapure water to obtain a mixed solution of the silver nitrate and the pyrrole with the mass fraction of 3%, irradiating for 3 hours under ultraviolet light, and forming a layer of self-supporting polypyrrole/silver film on the surface of the mixed solution;
step 3, taking the patterned polydimethylsiloxane film as a flexible substrate, transferring the self-supporting polypyrrole/silver film to the patterned surface of the flexible substrate, airing at room temperature, and then curing flexible copper wires with the diameter of 0.4mm at the two ends of the silver film by using conductive silver paste, wherein the curing temperature is 80 ℃ and the curing time is 2 hours; and finally, encapsulating the silver film by using another patterned polydimethylsiloxane film, and contacting the patterned surface of the encapsulated polydimethylsiloxane film with the silver film to obtain the flexible electronic sensor.
The electrochemical workstation of Shanghai Chenghua CHI660E is adopted to represent the electrical property, the induced bending property, the tensile strain property and the induced pressure property of the sensor, and the result is shown in figures 1-4. As can be seen from FIGS. 1-4, the sensor has excellent conductivity, and the ability to sense tensile, bending strain and pressure.
The performance of the strain in the sensing surface of the sensor is characterized by using the Shanghai Chenghua CHI660E electrochemical workstation and a tensile machine, the sensor is fixed in a clamp of the tensile machine and is bent 1000 times and stretched 2000 times by 20%, the obtained resistance cycle number curve is shown in figure 3, the current cycle number is shown in figure 4, and the sensor is proved to have excellent stretchability.
The performance of the sensor for sensing the micro-vibration of the throat when a person speaks is characterized by adopting the Shanghai Chenghua CHI660E electrochemical workstation, the sensor is attached to the laryngeal node of a detected person (male), words (a) Hi, (b) No and (c) Yes are read respectively at normal volume and speed, and the obtained current-time curve is shown in figure 5, which shows that the sensor has the capability of sensing the micro-vibration of the laryngeal node.
The method is characterized in that a Shanghai Hua CHI660E electrochemical workstation is adopted to represent the micro vibration of a sensor by the gas absorbed and exhaled when the sensor senses the shallow breathing and the deep breathing of a person, the sensor is attached to an exhalation hole of a mask and performs the shallow breathing and the deep breathing with two kinds of exhalation intensities, and the obtained current-time curve is shown in figure 6, so that the sensor has the capability of sensing the respiratory vibration with different intensities.
The sensor is attached to the wrist at the pulse position, the pulse vibrations of the sensor under the conditions of (a) movement and (b) normal condition are measured respectively, the shock wave (P) and the diastolic wave (D) after the movement and the shock wave (P), the tidal wave (T) and the diastolic wave (D) under the normal condition are detected respectively, the disappearance of the tidal wave (T) after the movement is caused by vasodilation, muscular artery expansion and chamber-blood vessel coupling, and the obtained current-time curve is shown in fig. 7, which illustrates that the sensor has the capability of sensing the pulse vibrations under different conditions.
The sensor prepared by the method can sense pressure, tensile and bending strain and micro vibration, such as throat vibration during speaking and breath and pulse vibration in different states, has high flexibility, stability, sensitivity and response speed, and is expected to be applied to the fields of motion detection, health monitoring systems, information transmission and the like.

Claims (8)

1. A preparation method of a flexible electronic sensor is characterized by comprising the following steps:
step 1, constructing a patterned polydimethylsiloxane film;
step 2, mixing 10-600 mmol/L silver nitrate aqueous solution and 5-200 mul of pyrrole solution, and irradiating for 0.5-6 hours under ultraviolet light to form a self-supporting polypyrrole/silver composite film on the surface of the mixed solution;
and 3, taking the patterned polydimethylsiloxane film as a flexible substrate, transferring the self-supporting polypyrrole/silver composite film to the patterned surface of the flexible substrate, then solidifying the flexible lead at two ends of the polypyrrole/silver film by using conductive silver paste, finally packaging the polypyrrole/silver film by using another patterned polydimethylsiloxane film, and contacting the patterned surfaces of the two polydimethylsiloxane films for packaging with the polypyrrole/silver film to obtain the flexible electronic sensor.
2. The method as claimed in claim 1, wherein step 1 is to construct the patterned polydimethylsiloxane film by using a lotus leaf surface with a natural microstructure as a mold.
3. The method for preparing a flexible electronic sensor according to claim 1, wherein the step 1 is specifically that after the surface of a fresh lotus leaf or a dried lotus leaf completely soaked with ultrapure water is sequentially cleaned with ethanol and ultrapure water, water drops on the surface of the lotus leaf are wiped and flatly attached to the surface of a substrate, then a mixed solution of dimethyl siloxane and a curing agent in a mass ratio of 9:1 is spin-coated on the surface of the lotus leaf, vacuum defoaming and curing are performed, and the cured polydimethylsiloxane is torn off to obtain the patterned polydimethylsiloxane film.
4. The method for preparing a flexible electronic sensor according to claim 3, wherein the vacuum defoaming time in the step 1 is 20-30 minutes.
5. The method for preparing a flexible electronic sensor according to claim 3, wherein the curing temperature in step 1 is 70-80 ℃ for 2-3 hours.
6. The method for preparing a flexible electronic sensor according to claim 1, wherein the thickness of the self-supporting polypyrrole/silver composite film is 100 to 200 nm.
7. The method for preparing a flexible electronic sensor according to claim 1, wherein the temperature for curing the conductive silver paste in the step 3 is 60-70 ℃ and the curing time is 1-2 hours.
8. The method for manufacturing the flexible electronic sensor according to claim 1, wherein the flexible conducting wire is a copper wire, and the diameter of the copper wire is 0.3-0.4 mm.
CN202110673010.1A 2021-06-17 2021-06-17 Preparation method of flexible electronic sensor Pending CN113491509A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114543654A (en) * 2022-03-01 2022-05-27 吉林大学 Preparation method of flexible stretching sensor

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102140249A (en) * 2010-12-23 2011-08-03 华东理工大学 Method for quickly preparing silver/polypyrrole composite sol by adopting microwave method
US20130056068A1 (en) * 2011-09-06 2013-03-07 Korea Institute Of Science And Technology Preparation method of flexible electrodes and flexible dye-sensitized solar cells using the same
CN108318162A (en) * 2018-01-10 2018-07-24 中山大学 A kind of flexible sensor and preparation method thereof
CN108680190A (en) * 2018-05-14 2018-10-19 陕西师范大学 The flexible electronic sensor and preparation method prepared using the self-supporting Ag films of lysozyme welding
KR20200097479A (en) * 2019-02-08 2020-08-19 충남대학교산학협력단 Method of manufacturing crack-based strain sensor using electroless silver plating
CN112254630A (en) * 2020-09-24 2021-01-22 浙江工业大学 Flexible wearable sensor with high sensitivity and high deformation range and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102140249A (en) * 2010-12-23 2011-08-03 华东理工大学 Method for quickly preparing silver/polypyrrole composite sol by adopting microwave method
US20130056068A1 (en) * 2011-09-06 2013-03-07 Korea Institute Of Science And Technology Preparation method of flexible electrodes and flexible dye-sensitized solar cells using the same
CN108318162A (en) * 2018-01-10 2018-07-24 中山大学 A kind of flexible sensor and preparation method thereof
CN108680190A (en) * 2018-05-14 2018-10-19 陕西师范大学 The flexible electronic sensor and preparation method prepared using the self-supporting Ag films of lysozyme welding
KR20200097479A (en) * 2019-02-08 2020-08-19 충남대학교산학협력단 Method of manufacturing crack-based strain sensor using electroless silver plating
CN112254630A (en) * 2020-09-24 2021-01-22 浙江工业大学 Flexible wearable sensor with high sensitivity and high deformation range and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114543654A (en) * 2022-03-01 2022-05-27 吉林大学 Preparation method of flexible stretching sensor

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