CN113267276B - Flexible electronic material and preparation method and application thereof - Google Patents
Flexible electronic material and preparation method and application thereof Download PDFInfo
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- CN113267276B CN113267276B CN202110538473.7A CN202110538473A CN113267276B CN 113267276 B CN113267276 B CN 113267276B CN 202110538473 A CN202110538473 A CN 202110538473A CN 113267276 B CN113267276 B CN 113267276B
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- 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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/69—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with phosphorus; with halides or oxyhalides of phosphorus; with chlorophosphonic acid or its salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
Abstract
The invention discloses a flexible electronic material and a preparation method and application thereof. The method comprises the following steps: (1) mixing the gold nanoparticle solution with the two-dimensional sheet-shaped nano material solution, and stirring at room temperature for reaction to prepare a modified nano composite material; (2) adding the textile wire into the product obtained in the step (1), heating until the liquid is completely evaporated, taking out the textile wire and drying to obtain the nano composite material electrode; (3) printing conductive carbon paste on the flexible fabric to form an electrode, and then drying for 3-5 h at 40-50 ℃; (4) and (4) sewing the non-electrode areas of the products obtained in the steps (2) and (3) so as to enable the electrode contact areas to be naturally contacted. According to the invention, the flexible wearable electronic skin is manufactured by using the nano composite technology, the screen printing technology and the soft fabric, so that the wearing comfort and the sensitivity of the flexible wearable electronic skin are obviously improved, and the defects of the existing flexible wearable electronic skin are overcome.
Description
Technical Field
The invention belongs to the technical field of flexible electronic materials, and particularly relates to a flexible electronic material and a preparation method and application thereof.
Background
The flexible wearable electronic skin is a flexible sensor for realizing perception by replacing human skin, can convert pressure generated from the outside into a clear electric signal, and is a flexible electronic device with the function of imitating the human skin. The flexible wearable electronic skin relates to a plurality of fields such as electronic information technology, sensor technology, medical technology and nanotechnology, and functions such as human skin protection, perception and regulation are simulated by applying multidisciplinary knowledge, so that human skin functions are realized, and the flexible wearable electronic skin has a wide application scene in the aspects of human health detection, robot touch and the like.
The uk market analysis company IDTechEx forecasts that the global flexible electronic market is expected to reach $ 3010 billion by 2028. In addition, the wearable technology was studied by the idechex corporation over the last decade, and the results of the study showed that throughout this time, wearable technology has experienced a turbulent growth with a dramatic increase in topics, accompanied by billions of dollars of capital, thousands of new patent applications and new companies, and thousands of new products and billions of dollars of new revenues. To date, wearable technology products have had great success with a total market value of nearly $ 700 billion in 2019, which has doubled in size since 2014. In the emergency environment, wearable device can carry out remote monitoring to the patient, and medical personnel can monitor patient's vital sign in safe distance. Isolating and monitoring their health in real time during the most severe periods of COVID-19 has proven to be an effective self-protection measure, and thus the trend toward devices that can help people do this is positive. Meanwhile, the flexible wearable medical product brings comfortable wearing experience for the user due to the characteristics of softness and thinness. It is obvious that the flexible wearable device has great application value in the aspect of health management. With the continuous development of technologies such as 5G, AI and electronic skin, wearable medical equipment can overcome various difficulties, become wearable and intelligent medical equipment in a real sense, and provide firm and powerful guarantee for the healthy life of people in a wider range and in a deeper level.
Starting from two aspects of wearing comfort level and measurement accuracy of flexible wearable electronic skin, the material of current flexible electronic skin can't satisfy the demand of using, and sensitivity is not high, and life cycle is short, and is with high costs, has hindered electronic skin's development to it has very strong realistic meaning to develop a high sensitivity and wear comfortable flexible wearable electronic skin.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the flexible electronic material and the preparation method and the application thereof, and the flexible wearable electronic skin is manufactured by using the nano composite technology, the screen printing technology and the soft fabric, so that the wearing comfort and the sensitivity of the flexible wearable electronic skin are obviously improved, and the defects of the existing flexible wearable electronic skin are overcome.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a flexible electronic material is characterized by comprising the following steps:
(1) mixing the gold nanoparticle solution and the gold nanoparticles and the black phosphorus in the two-dimensional flaky nano material solution according to the mass ratio of 2: 5-10: 5, stirring at room temperature for reaction, and stopping stirring until the color is changed from black to wine red to prepare the modified nano composite material;
(2) adding a 5 cm textile thread into the product obtained in the step (1), heating until the liquid is completely evaporated, taking out the textile thread, and drying at 30-40 ℃ for 1-2 h to obtain a nano composite material electrode;
(3) printing conductive carbon paste on the flexible fabric to form an electrode, and then drying for 3-5 h at 40-50 ℃;
(4) and (4) sewing the non-electrode areas of the products obtained in the step (2) and the step (3) so as to enable the electrode contact areas to naturally contact.
The flexible electronic material prepared by the invention can be used for preparing flexible wearable electronic skin and consists of a wire-based nano composite material electrode and a screen printing electrode of a fabric substrate, the adopted wire-based nano composite material electrode and the adopted fabric substrate have good flexibility and strong deformability under the action of pressure, and the wire-based nano composite material and the fabric substrate only need to be simply cleaned in the preparation process, so that the flexible electronic material has the advantages of low cost, simplicity in manufacturing and use and the like. Therefore, the flexible wearable electronic skin has good flexibility and is comfortable to wear.
According to the invention, the gold nanoparticles are used for modifying the two-dimensional flaky nano material, the gold nanoparticles fill the edge defect of the two-dimensional flaky nano material, the two-dimensional flaky nano material is protected, and the obtained nano composite material has good conductivity and air acceptability, so that the sensitivity of the flexible wearable electronic skin is improved. The two-dimensional flaky nano material adopted by the invention comprises but is not limited to graphene, black phosphorus and molybdenum disulfide nanosheets. Then, the nanocomposite is transferred to the textile thread by evaporation of water in the nanocomposite dispersion, forming an electrode that encapsulates the nanocomposite.
Further, the concentration of the gold nanoparticle solution is 1 mg/mL; the concentration of the two-dimensional flaky nano material solution is 1 mg/mL.
Further, the gold nanoparticle solution is a chloroauric acid solution.
Further, the two-dimensional sheet-like nanomaterial includes, but is not limited to, graphene, black scale, or molybdenum disulfide nanoplatelets.
Further, the preparation method of the two-dimensional sheet-like nano material comprises the following steps:
grinding the blocky black phosphorus to prepare a black phosphorus dispersion liquid with the concentration of 1mg/mL, placing the black phosphorus dispersion liquid in a 500W ultrasonic ice water bath to strip for 20-25 h, finally, carrying out centrifugal treatment on the stripped mixed liquid to remove the un-stripped black phosphorus particles, and collecting the upper-layer black phosphorus nanosheets.
Further, the specific process of printing the conductive carbon paste on the flexible fabric in the step (3) is as follows:
pouring the conductive carbon paste onto a screen printing template, and forming an electrode on the flexible cotton cloth by using a scraper through the screen printing template; the screen printing template is in an interdigital circuit shape.
Further, the textile thread is nylon thread, cotton thread or silk thread.
Further, the conductive carbon paste is a mixed ink composed of carbon and graphite.
The template for silk-screen printing is in a customized shape, adopts an interdigital circuit shape, has the advantages of reducing impedance, quickly establishing a steady-state signal, having high signal-to-noise ratio and the like, is widely applied to the research of sensors, and is convenient for developing sensitive, quick and specific sensing equipment. The conductive carbon paste is the key in the printed electrode, and the conductivity and stability of the conductive carbon paste influence the whole flexible wearable electronic skin, so that the conductive carbon paste is selected from mixed printing ink consisting of carbon and graphite, and has excellent adhesive force, excellent flexibility, kneading resistance, acid and alkali resistance and good stability. According to the invention, cotton cloth is selected as a substrate material, and as the cotton cloth is good in hydrophilicity and wettability, the conductive carbon paste can be well attached to the cotton cloth, so that the formed electrode has very small resistance, and meanwhile, the cotton cloth is good in air permeability, soft and comfortable, and the wearing comfort level is greatly improved.
Further, in the step (3), the drying temperature is 40 ℃, the drying time is at least 3h, and the conductive carbon paste is drier, the lower the resistance is, the smaller the influence on the whole electronic skin is.
Further, the step (4) further comprises: sewing the nanocomposite electrode and the non-contact area of the electrode prepared in the step (3) through a needle and a thread, and naturally contacting the electrode contact areas of the nanocomposite electrode and the electrode.
The prepared flexible electronic material comprises a nano composite material electrode and a screen printing electrode; the nanocomposite electrode is in natural contact with the electrode contact area of the screen printed electrode.
The flexible electronic material is applied to the preparation of flexible electronic skins, flexible sensors, wearable medical equipment and equipment for sensing pressure changes.
The invention converts the force into the electric signal by the principle that the contact area and the number between the nano composite material electrode and the screen printing electrode present different states under different pressures, and the contact area is small and the contact number is small when no pressure exists; when pressure is applied, the contact area is large and the contact number is large. Therefore, the flexible wearable electronic skin prepared by the invention can be suitable for all scenes for sensing pressure changes.
The invention has the beneficial effects that:
the flexible wearable electronic skin prepared by the invention has the advantages of simple manufacturing principle and process, good wearing comfort due to the adoption of soft textile threads and cotton cloth materials, improvement of the sensitivity of the electronic skin prepared by the invention due to the unique structure and the nano composite material, strong practicability, high reliability, very high practical value and commercial value, and effective promotion of the development of the electronic skin.
Drawings
Fig. 1 is a schematic structural diagram of a flexible wearable electronic skin prepared by the present invention;
FIG. 2 is a process for constructing a nanocomposite electrode according to the present invention;
FIG. 3 is a schematic diagram of the detection of the flexible wearable electronic skin prepared by the present invention;
FIG. 4 shows the conductivity of the nanocomposite electrode prepared with different proportions of gold and two-dimensional sheet nanomaterial of the present invention;
FIG. 5 is a scanning electron microscope photograph of the flexible wearable electronic skin nanocomposite electrode prepared in example 3 of the present invention;
fig. 6 is a graph of the sensitivity test result of the flexible wearable electronic skin prepared in embodiment 3 of the invention;
fig. 7 is a graph of response speed test results of the flexible wearable electronic skin prepared in embodiment 3 of the present invention:
fig. 8 is a graph showing the fatigue test results of the flexible wearable electronic skin prepared in example 3 of the present invention.
Detailed Description
The following description of the embodiments of the present invention is provided to facilitate the understanding of the present invention by those skilled in the art, but it should be understood that the present invention is not limited to the scope of the embodiments, and it will be apparent to those skilled in the art that various changes may be made without departing from the spirit and scope of the invention as defined and defined in the appended claims, and all matters produced by the invention using the inventive concept are protected.
Example 1
A preparation method of flexible wearable electronic skin comprises the following steps:
(1) adding 2mL of chloroauric acid solution (1 mg/mL) into 5mL of two-dimensional flaky nano-material suspension (1 mg/mL) at room temperature, and stirring to fully perform the reaction, wherein the mass ratio of gold to black phosphorus is 2:5, and the stirring conditions are as follows: stopping stirring when the color is changed from black to wine red, and finishing the preparation of the nano composite material;
the preparation method of the two-dimensional flaky nano material comprises the following steps:
grinding the blocky black phosphorus to be secreted, mixing the blocky black phosphorus with deionized water to prepare 1mg/mL black phosphorus dispersion liquid, placing the black phosphorus dispersion liquid in ultrasonic ice water bath (500W) to strip for 20 hours, finally, carrying out centrifugal treatment on the stripped mixed liquid to remove un-stripped black phosphorus particles, and collecting the upper-layer black phosphorus nanosheets for later use.
(2) Soaking nylon thread into the prepared nano composite material turbid liquid, heating by using an alcohol lamp to accelerate the evaporation of the liquid, wherein the heating stop conditions are as follows: stopping heating after the liquid is completely evaporated, taking out the nylon thread, and drying for 1 hour at the temperature of 30 ℃ to obtain a nano composite material electrode;
(3) pouring the conductive carbon paste onto a screen printing template, using a scraper to enable the conductive carbon paste to penetrate through the template to form an electrode on flexible cotton cloth, and after the conductive carbon paste is printed, drying conditions are as follows: the temperature is 40 ℃, and the drying time is 3 h;
(4) the nanometer composite material electrode and the screen printing electrode are sewn through needles and threads, the sewing area of the needles and the threads is a non-contact area of the screen printing electrode, the contact area of the electrode is a core area for generating a sensing effect, and the nanometer composite material electrode and the screen printing electrode naturally contact after sewing is completed, so that the flexible wearable electronic skin is manufactured.
Example 2
A preparation method of flexible wearable electronic skin comprises the following steps:
(1) adding 4mL of chloroauric acid solution (1 mg/mL) into 5mL of two-dimensional flaky nano-material suspension (1 mg/mL) at room temperature, and stirring to fully perform the reaction, wherein the mass ratio of gold to black phosphorus is 4:5, and the stirring conditions are as follows: stopping stirring when the color is changed from black to wine red, and finishing the preparation of the nano composite material;
the preparation method of the two-dimensional flaky nano material comprises the following steps:
grinding the blocky black phosphorus to secrete, mixing the blocky black phosphorus with deionized water to prepare 1mg/mL black phosphorus dispersion liquid, placing the black phosphorus dispersion liquid in an ultrasonic ice-water bath (500W) to strip for 20 hours, finally, carrying out centrifugal treatment on the stripped mixed liquid to remove the un-stripped black phosphorus particles, and collecting the upper-layer black phosphorus nanosheet for later use.
(2) Soaking nylon thread into the prepared nano composite material turbid liquid, heating by using an alcohol lamp to accelerate the evaporation of liquid, wherein the heating stop conditions are as follows: stopping heating after the liquid is completely evaporated, taking out the nylon wire, and drying for 1 hour at 40 ℃ to obtain the nano composite material electrode;
(3) pouring the conductive carbon paste onto a screen printing template, using a scraper to enable the conductive carbon paste to penetrate through the template to form an electrode on flexible cotton cloth, and after the conductive carbon paste is printed, drying conditions are as follows: the temperature is 44 ℃, and the drying time is 3 h;
(4) the nanometer composite material electrode and the screen printing electrode are sewn through needles and threads, the sewing area of the needles and the threads is a non-contact area of the screen printing electrode, the contact area of the electrode is a core area for generating a sensing effect, and the nanometer composite material electrode and the screen printing electrode naturally contact after sewing is completed, so that the flexible wearable electronic skin is manufactured.
Example 3
A preparation method of flexible wearable electronic skin comprises the following steps:
(1) adding 6mL of chloroauric acid solution (1 mg/mL) into 15mL of two-dimensional flaky nano-material suspension (1 mg/mL) at room temperature, and stirring to fully perform the reaction, wherein the mass ratio of gold to black phosphorus is 6:5, and the stirring conditions are as follows: stopping stirring when the color is changed from black to wine red, and finishing the preparation of the nano composite material;
the preparation method of the two-dimensional flaky nano material comprises the following steps:
grinding the blocky black phosphorus to secrete, mixing the blocky black phosphorus with deionized water to prepare 1mg/mL black phosphorus dispersion liquid, placing the black phosphorus dispersion liquid in an ultrasonic ice-water bath (500W) to strip for 20 hours, finally, carrying out centrifugal treatment on the stripped mixed liquid to remove the un-stripped black phosphorus particles, and collecting the upper-layer black phosphorus nanosheet for later use.
(2) Soaking nylon thread into the prepared nano composite material turbid liquid, heating by using an alcohol lamp to accelerate the evaporation of liquid, wherein the heating stop conditions are as follows: stopping heating after the liquid is completely evaporated, taking out the nylon wire, and drying for 1 hour at the temperature of 30 ℃ to obtain a nano composite material electrode;
(3) pouring the conductive carbon paste onto a screen printing template, forming an electrode on the flexible cotton cloth by using a scraper to enable the conductive carbon paste to penetrate through the template, and drying the conductive carbon paste under the following conditions: the temperature is 40 ℃, and the drying time is 3 h;
(4) the nanometer composite material electrode and the screen printing electrode are sewn through needles and threads, the sewing area of the needles and the threads is a non-contact area of the screen printing electrode, the contact area of the electrode is a core area for generating a sensing effect, and the nanometer composite material electrode and the screen printing electrode naturally contact after sewing is completed, so that the flexible wearable electronic skin is manufactured.
Example 4
A preparation method of flexible wearable electronic skin comprises the following steps:
(1) adding 8mL of chloroauric acid solution (1 mg/mL) into 5mL of two-dimensional flaky nano-material suspension (1 mg/mL) at room temperature, and stirring to fully perform the reaction, wherein the mass ratio of gold to black phosphorus is 8:5, and the stirring condition is as follows: stopping stirring when the color is changed from black to wine red, and finishing the preparation of the nano composite material;
the preparation method of the two-dimensional flaky nano material comprises the following steps:
grinding the blocky black phosphorus to secrete, mixing the blocky black phosphorus with deionized water to prepare 1mg/mL black phosphorus dispersion liquid, placing the black phosphorus dispersion liquid in an ultrasonic ice-water bath (500W) to strip for 20 hours, finally, carrying out centrifugal treatment on the stripped mixed liquid to remove the un-stripped black phosphorus particles, and collecting the upper-layer black phosphorus nanosheet for later use.
(2) Soaking nylon thread into the prepared nano composite material turbid liquid, heating by using an alcohol lamp to accelerate the evaporation of the liquid, wherein the heating stop conditions are as follows: stopping heating after the liquid is completely evaporated, taking out the nylon wire, and drying for 1 hour at 35 ℃ to obtain a nano composite material electrode;
(3) pouring the conductive carbon paste onto a screen printing template, using a scraper to enable the conductive carbon paste to penetrate through the template to form an electrode on flexible cotton cloth, and after the conductive carbon paste is printed, drying conditions are as follows: the temperature is 50 ℃, and the drying time is 3 h;
(4) the nanometer composite material electrode and the screen printing electrode are sewn through needles and threads, the sewing area of the needles and the threads is a non-contact area of the screen printing electrode, the contact area of the electrode is a core area for generating a sensing effect, and the nanometer composite material electrode and the screen printing electrode naturally contact after sewing is completed, so that the flexible wearable electronic skin is manufactured.
Example 5
A preparation method of flexible wearable electronic skin comprises the following steps:
(1) adding 10mL of chloroauric acid solution (1 mg/mL) into 5mL of two-dimensional flaky nano-material suspension (1 mg/mL) at room temperature, and stirring to fully perform the reaction, wherein the mass ratio of gold to black phosphorus is 10:5, and the stirring conditions are as follows: stopping stirring when the color is changed from black to wine red, and finishing the preparation of the nano composite material;
the preparation method of the two-dimensional flaky nano material comprises the following steps:
grinding the blocky black phosphorus to secrete, mixing the blocky black phosphorus with deionized water to prepare 1mg/mL black phosphorus dispersion liquid, placing the black phosphorus dispersion liquid in an ultrasonic ice-water bath (500W) to strip for 20 hours, finally, carrying out centrifugal treatment on the stripped mixed liquid to remove the un-stripped black phosphorus particles, and collecting the upper-layer black phosphorus nanosheet for later use.
(2) Soaking nylon thread into the prepared nano composite material turbid liquid, heating by using an alcohol lamp to accelerate the evaporation of the liquid, wherein the heating stop conditions are as follows: stopping heating after the liquid is completely evaporated, taking out the nylon wire, and drying for 1 hour at the temperature of 30 ℃ to obtain a nano composite material electrode;
(3) pouring the conductive carbon paste onto a screen printing template, using a scraper to enable the conductive carbon paste to penetrate through the template to form an electrode on flexible cotton cloth, and after the conductive carbon paste is printed, drying conditions are as follows: the temperature is 40 ℃, and the drying time is 3 h;
(4) the nanometer composite material electrode and the screen printing electrode are sewn through needles and threads, the sewing area of the needles and the threads is a non-contact area of the screen printing electrode, the contact area of the electrode is a core area for generating a sensing effect, and the nanometer composite material electrode and the screen printing electrode naturally contact after sewing is completed, so that the flexible wearable electronic skin is manufactured.
Examples of the experiments
1. Nano composite material electrode and conductivity of screen printing electrode
The experiment verifies the correctness of the method and the optimal proportion of the mixture ratio by respectively detecting resistance signals of the nano flexible electrode and the silk-screen printing which are prepared by different mass ratios of gold and black phosphorus. Whereas the resistance value of the screen printed electrode was 30 Ω (much less than that of the nanocomposite electrode, the screen printed resistance was negligible).
As shown in fig. 4, at a ratio of 6:5 hours is the optimal selection, and simultaneously, the purposes of good conductivity and resource saving are achieved.
2. Synthesis of nano composite material and verification of electrode modification result
The microscopic morphology of the synthesized nanocomposite electrode was observed with a scanning electron microscope, and the results are shown in fig. 5, which shows that the black phosphorus nanosheets have gold nanoparticles, and that both black phosphorus and gold are nanoscale and densely stacked on the textile threads to form electrodes, demonstrating that the black phosphorus gold nanomaterials with special structures were synthesized and successfully decorated on the flexible textile threads.
3. Sensitivity measurement
The sensitivity is one of the core parameters of the sensor, and the pressure P-resistance change R/R is measured by adopting a tension press machine and a digital multimeter which are provided with a force sensor with the measuring range of 5N0The linear relation of (1), namely the sensitivity of the flexible wearable electronic skin, wherein P = F/S, F is the stress applied by the tension and compression machine, S is the contact area of the clamp and the flexible wearable electronic skin, R is the resistance in the process of force application0Resistance when unstressed. The obtained curve was fitted to obtain sensitivity G of the electronic skin, and the detection result is shown in FIG. 6Sensitivity G when the detected pressure is 0-1.5kPa1＝0.372kPa-1Sensitivity G when the detected pressure is greater than 1.5kPa2＝0.061kPa-1。
4. Response speed measurement
The response speed is one of the core parameters of the sensor, a pressure pulling machine with a force sensor with the measuring range of 5N and a digital multimeter are adopted to match a computer to measure the response speed, the pressure pulling machine achieves a set force value, a stepping motor controlled by the computer and the flexible wearable electronic skin manufactured by the invention form a testing system, force is applied to the surface of the flexible wearable electronic skin, meanwhile, the current passing through the flexible wearable electronic skin is monitored, the response time is obtained according to the signal time difference acquired by calculation, the detection result is shown in figure 7, and the response time is 24ms at the moment of pressure application and 32ms at the moment of pressure release.
5. Fatigue test
The fatigue test of the product is one of the core parameters of the sensor, the repeatability (more than 4000 times) is measured by adopting a pulling and pressing machine and a digital multimeter which are provided with a force sensor with the measuring range of 5N, the force is applied to the flexible wearable electronic skin by the pulling and pressing machine in a circulating manner, the digital multimeter reads an electric signal, the error degree of the electric signal is judged, the durability of the flexible wearable electronic skin is measured, the detection result is shown in figure 8, and the sensor can stably work after the pressure is applied and released for 4000 times.
Claims (8)
1. A preparation method of a flexible electronic material is characterized by comprising the following steps:
(1) mixing the gold nanoparticle solution with the two-dimensional sheet-shaped nano material solution, and stirring at room temperature for reaction to prepare a modified nano composite material; the mass ratio of the gold nanoparticles to the two-dimensional flaky nano material in the gold nanoparticle solution is 2: 5-10: 5; the preparation method of the two-dimensional flaky nano material comprises the following steps:
grinding the blocky black phosphorus to prepare black phosphorus dispersion liquid with the concentration of 1mg/mL, placing the black phosphorus dispersion liquid in 500W ultrasonic ice water bath to strip for 20-25 h, finally, carrying out centrifugal treatment on the stripped mixed liquid to remove un-stripped black phosphorus particles, and collecting upper-layer black phosphorus nanosheets;
(2) adding the textile wire into the product obtained in the step (1), heating until the liquid is completely evaporated, taking out the textile wire, and drying at 30-40 ℃ for 1-2 h to obtain a nano composite material electrode;
(3) printing conductive carbon paste on the flexible fabric to form an electrode, and then drying for 3-5 h at 40-50 ℃;
(4) and (4) naturally contacting the electrode contact area of the products obtained in the step (2) and the step (3).
2. The method of preparing a flexible electronic material according to claim 1, wherein the concentration of the gold nanoparticle solution is 1 mg/mL; the concentration of the two-dimensional flaky nano material solution is 1 mg/mL.
3. The method of claim 1 or 2, wherein the gold nanoparticle solution is a chloroauric acid solution.
4. The method for preparing the flexible electronic material according to claim 1, wherein the step (3) of printing the conductive carbon paste on the flexible fabric comprises the following specific steps:
pouring the conductive carbon paste onto a screen printing template, and forming an electrode on the flexible cotton cloth by using a scraper to enable the conductive carbon paste to penetrate through the screen printing template; the silk-screen printing template is in an interdigital circuit shape.
5. The method for preparing a flexible electronic material according to claim 1, wherein the drying temperature in the step (3) is 40 ℃ and the drying time is 3 hours.
6. The method of preparing a flexible electronic material according to claim 1, wherein the step (4) further comprises: sewing the nanocomposite electrode and the non-contact area of the electrode prepared in the step (3) through a needle and a thread, and naturally contacting the electrode contact areas of the nanocomposite electrode and the electrode.
7. The flexible electronic material prepared by the method for preparing the flexible electronic material according to any one of claims 1 to 6, which is characterized by comprising a nano composite material electrode and a screen printing electrode; the electrode contact area of the nanocomposite electrode and the screen printed electrode naturally contacts.
8. Use of the flexible electronic material of claim 7 in the manufacture of flexible electronic skin, wearable medical devices, pressure change sensing devices.
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