CN115466427A - Preparation method of multi-dimensional flexible sensor based on PE material - Google Patents
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Abstract
The invention discloses a preparation method of a multi-dimensional flexible sensor based on a PE material, which comprises the following steps: dropping ITX acetone solution on the surface of LDPE Tape, clamping the LDPE Tape between two quartz plates, irradiating at room temperature under an ultraviolet mercury lamp, washing, and drying; to a PEDOT: adding chloroplatinic acid into the PSS solution, and uniformly stirring to obtain PEDOT: PSS modified solution; PEGDA, glycerol, deionized water, and PEDOT: and mixing the PSS modified solution, and mixing PEDOT: the PSS/PEGDA precursor solution is cast on LDPE Tape-ITXSP, placed between two quartz plates and fixed by a clamp, irradiated under visible light for polymerization, washed and dried. The flexible sensor prepared by the method disclosed by the invention has the advantages of high sensitivity, high transparency and quick response.
Description
Technical Field
The invention belongs to the technical field of flexible sensing material preparation, and particularly relates to a preparation method of a multi-dimensional flexible sensor based on a PE material.
Background
Polyethylene (PE) has been widely noticed from the world due to its excellent properties of low cost, low density, corrosion resistance, soft texture, easy processing, etc., and is the most widely used and most used polymer material at present. Polyethylene molecules do not contain polar groups, the material has rich C-H bonds and high crystallinity, so that the PE material has the characteristics of low surface energy and reaction inertia in practical use, and although the characteristics have the advantages of corrosion resistance, low temperature resistance, good chemical stability and the like in application, the problems of difficult printing, difficult bonding, easy generation of static electricity, poor biocompatibility, lack of reaction sites and the like on the surface of the PE material are caused. Therefore, on the basis of not changing the excellent characteristics of the PE material, the breakthrough of the use bottleneck of the PE material is very important.
The flexible sensor combining the flexible material and the electronic technology has great potential in the aspects of human health monitoring, biomedicine, flexible electronic skin, target deformation monitoring and the like. Compared with the traditional sensor prepared by metal and semiconductor materials, the flexible sensor has the advantages of good flexibility, stretchability, continuous monitoring and the like. It converts mechanical, chemical or other signals into detectable electrical signals for output. At present, most of materials for manufacturing the flexible sensor mainly comprise hydrogel, protein fiber and textile materials, and the materials are difficult to directly use for a long time. If the PE material is used for preparing the flexible sensor, the yield and the use scale of the flexible sensor are greatly improved, the cost of the flexible sensor is reduced, and the application of the flexible sensor is developed from the conventional electronic product, biomedicine and human health monitoring fields to the directions of large chemical industry, large materials, large machinery and the like, so that the flexible sensor is an ideal product which is very needed by new technology and integrated equipment.
Disclosure of Invention
The invention aims to provide a preparation method of a multi-dimensional flexible sensor based on a PE material, and the flexible sensor has high sensitivity, high transparency and quick response.
The technical scheme adopted by the invention is that the preparation method of the multi-dimensional flexible sensor based on the PE material is implemented according to the following steps:
step 1, dissolving ITX in acetone to form ITX acetone solution; uniformly dropwise adding an ITX acetone solution on the surface of an LDPE Tape, clamping the LDPE Tape between two quartz plates, and irradiating the LDPE Tape at room temperature under an ultraviolet mercury lamp to obtain LDPE Tape-ITXSP; then soaking the LDPE Tape-ITXSP in acetone, washing the surface for 3 times by using the acetone, and drying in vacuum;
and 2, performing PEDOT: and magnetically stirring the PSS solution, adding chloroplatinic acid, and uniformly stirring to obtain PEDOT: PSS modified solution and stored at 4 ℃; PEGDA, glycerol, deionized water, and PEDOT: and (3) mixing the PSS modified solution to obtain stably dispersed PEDOT: PSS/PEGDA precursor solution;
and 3, carrying out PEDOT: and casting the PSS/PEGDA precursor solution on LDPE Tape-ITXSP, then placing the LDPE Tape-ITXSP between two quartz plates, fixing the LDPE Tape-ITXSP by using a clamp, placing the LDPE Tape-ITXSP under visible light for irradiation polymerization, then placing the LDPE Tape-ITXSP in deionized water for soaking, washing the LDPE Tape-ITXSP for 3 times by using the deionized water, and drying the LDPE Tape-ITXSP in vacuum to obtain the multi-dimensional flexible sensor.
The present invention is also characterized in that,
in step 1, the concentration of ITX acetone solution is 3mmolmL -1 。
In step 1, the irradiation time is 3-5min, the wavelength of the ultraviolet mercury lamp is 254nm, and the light intensity is 9m W/cm 2 (ii) a The soaking time is 24h.
In step 2, PEDOT: the concentration of the PSS modified solution was 0.035mol/L.
In the step 3, the irradiation polymerization time is 60-120 min; the wavelength of visible light is 420nm, and the light intensity is 3mW/cm 2 。
The beneficial effects of the invention are: the flexible sensor prepared by the method disclosed by the invention has high sensitivity, high transparency and quick response, the sheet resistance of the PE-based flexible sensor can be adjusted by adding the proportion of glycerol and deionized water, and the obtained sensor has good conductivity and excellent self-adhesion and can be conveniently applied to a target unit with complex deformation. In addition, the method has low cost and wide source of raw materials, and the reaction in the whole process is green, environment-friendly, simple and feasible.
Drawings
FIG. 1 is a plot of sheet resistance (K Ω/sq) versus conductivity (s/m) for L T-3 (P) with different deionized water ((v/v)%);
FIG. 2 is a graph of a sensing curve for monitoring human index finger movement using the sensor of the present invention;
FIG. 3 is a graph of a sensing curve for monitoring human wrist movement using the sensor of the present invention;
FIG. 4 is a graph of a sensing curve for monitoring human elbow joint motion using the sensor of the present invention;
FIG. 5 is a graph of a sensing curve for monitoring human knee motion using the sensor of the present invention;
fig. 6 is a graph of the sensing signal for monitoring slight laryngeal vibrations of a human body using the sensor of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a multi-dimensional flexible sensor based on a PE material, which is implemented according to the following steps:
step 1, dissolving ITX in acetone to form ITX acetone solution; uniformly dropwise adding an ITX acetone solution on the surface of a low-density polyethylene adhesive Tape (LDPE Tape), clamping the LDPE Tape between two quartz plates to form a sandwich structure, and placing the sandwich structure under an ultraviolet mercury lamp for room-temperature irradiation to obtain the LDPE Tape (LDPE Tape-ITXSP) grafted with ITX semi-pinacol free radical dormant species; then soaking the LDPE Tape-ITXSP in acetone for 24h, washing the surface for 3 times by using the acetone to remove residual ITX, drying in vacuum, and storing under the conditions of constant temperature and constant humidity;
the concentration of ITX acetone solution is 3mmol mL -1 ；
The irradiation time is 3-5min, the wavelength of the ultraviolet mercury lamp is 254nm, and the light intensity is 9m W/cm 2 ；
The conditions of constant temperature and constant humidity are as follows: the temperature is 23 ℃ and the relative humidity is 50 percent;
and 2, performing PEDOT: and magnetically stirring the PSS solution, adding chloroplatinic acid, and uniformly stirring to obtain PEDOT: PSS modified solution and stored at 4 ℃; polyethylene glycol diacrylate (PEGDA), glycerol, deionized water, and PEDOT: and (3) mixing the PSS modified solution to obtain stably dispersed PEDOT: PSS/PEGDA precursor solution is coating emulsion;
PEDOT: the concentration of the PSS modified solution is 0.035mol/L;
PEDOT: the optimal mixture ratio of the PSS/PEGDA precursor solution is as follows: PEGDA, glycerol, deionized water, and PEDOT: the volume fractions of the PSS modified solution are respectively 25%, 5% and 65%;
and 3, carrying out PEDOT: the PSS/PEGDA precursor solution is cast on LDPE Tape-ITXSP, then placed between two quartz plates and fixed by a clamp, placed under visible light for irradiation polymerization, then placed in deionized water for soaking, washed for 3 times by the deionized water, and the non-immobilized substances are removed, finally, vacuum-dried and stored under the conditions of constant temperature and humidity, thus obtaining the multi-dimensional flexible sensor;
the irradiation polymerization time is 60-120 min;
the wavelength of visible light is 420nm, and the light intensity is 3mW/cm 2 ；
The conditions of constant temperature and constant humidity are as follows: the temperature is 23 ℃, and the relative humidity is 50%;
the multifunctional multidimensional flexible sensor has the sensing mechanism that PEG is mainly used as a three-dimensional molecular net cloth to embed conductive polymers PEDOT and PSS, when the sensor is subjected to external force, the molecular net cloth layer embedding the PEDOT and the PSS deforms, the arrangement condition of the molecular net cloth is changed accordingly, the combination state of the PEDOT and the PSS molecules is influenced, an electronic channel is changed, and the transmission of electric charges is changed accordingly. The resistance of the sensor is changed, different resistance values of the sensor can be given under different external force actions, and therefore the external force condition borne by the sensor can be monitored through the resistance signals which are changed at any time.
Example 1
The invention relates to a preparation method of a multifunctional multi-dimensional flexible sensor based on a PE material, which comprises the following steps:
dissolving isopropyl thioxanthone ITX in acetone to form an ITX acetone solution; uniformly dropwise adding an ITX acetone solution on the surface of the LDPE Tape, clamping the LDPE Tape between two quartz plates, and irradiating the LDPE Tape at room temperature under an ultraviolet mercury lamp to obtain LDPE Tape-ITXSP; then soaking the LDPE Tape-ITXSP in acetone for 24h, washing the surface with acetone for 3 times, drying in vacuum, and storing under the conditions of constant temperature and humidity;
10ml of PEDOT: the PSS solution was magnetically stirred, 0.18g of chloroplatinic acid was added and mixed at a stirring speed of 2000r/min for 2h to finally prepare PEDOT having a concentration of 0.035 mol/L: PSS modified solution and stored at 4 ℃; subsequently 25% (v/v%) PEGDA, 5% (v/v%) glycerol, 5% (v/v%) deionized water and 65% (v/v%) PEDOT at a concentration of 0.035 mol/L: and mixing the PSS modified solution, and mixing for 2 hours at a stirring speed of 2000r/min to obtain the stably dispersed PEDOT: PSS/PEGDA precursor solution, PEDOT prepared: the PSS/PEGDA precursor solution is directly used as a coating emulsion;
and (3) mixing PEDOT: the PSS/PEGDA precursor solution is cast on LDPE Tape-ITXSP, then placed between two quartz plates and fixed by a clamp, placed under visible light for irradiation polymerization, then placed in deionized water for soaking, washed for 3 times by the deionized water, dried in vacuum, and stored under the conditions of constant temperature and constant humidity, so that the multi-dimensional flexible sensor can be obtained; the finally prepared LT-3 (P) sheet resistance is 4.58k omega/sq; and the obtained coating is uniform.
Example 2
The invention relates to a preparation method of a multifunctional multi-dimensional flexible sensor based on a PE material, which comprises the following steps:
dissolving isopropyl thioxanthone ITX in acetone to form an ITX acetone solution; uniformly dropwise adding an ITX acetone solution on the surface of the LDPE Tape, clamping the LDPE Tape between two quartz plates, and irradiating the LDPE Tape at room temperature under an ultraviolet mercury lamp to obtain LDPE Tape-ITXSP; then soaking the LDPE Tape-ITXSP in acetone for 24h, washing the surface with acetone for 3 times, drying in vacuum, and storing under the conditions of constant temperature and humidity;
10ml of PEDOT: the PSS solution was magnetically stirred, 0.18g of chloroplatinic acid was added and mixed at a stirring speed of 2000r/min for 2h to finally prepare PEDOT having a concentration of 0.035 mol/L: PSS modified solution and stored at 4 ℃; subsequently 25% (v/v%) PEGDA, 5% (v/v%) glycerol, 10% (v/v%) deionised water and 60% (v/v%) PEDOT at a concentration of 0.035 mol/L: and (3) mixing the PSS modified solution, and mixing for 2h at a stirring speed of 2000r/min to obtain the stably dispersed PEDOT: PSS/PEGDA precursor solution, PEDOT prepared: the PSS/PEGDA precursor solution is directly used as a coating emulsion;
and (3) mixing PEDOT: the PSS/PEGDA precursor solution is cast on LDPE Tape-ITXSP, then placed between two quartz plates and fixed by a clamp, placed under visible light for irradiation polymerization, then placed in deionized water for soaking, washed for 3 times by the deionized water, dried in vacuum, and stored under the conditions of constant temperature and constant humidity, so that the multi-dimensional flexible sensor can be obtained; the finally prepared LT-3 (P) sheet resistance is 30k omega/sq;
example 3
The invention relates to a preparation method of a multifunctional multi-dimensional flexible sensor based on a PE material, which comprises the following steps:
dissolving isopropyl thioxanthone ITX in acetone to form an ITX acetone solution; uniformly dropwise adding an ITX acetone solution on the surface of an LDPE Tape, clamping the LDPE Tape between two quartz plates, and irradiating the LDPE Tape at room temperature under an ultraviolet mercury lamp to obtain LDPE Tape-ITXSP; then soaking the LDPE Tape-ITXSP in acetone for 24h, washing the surface with acetone for 3 times, drying in vacuum, and storing under the conditions of constant temperature and humidity;
10ml of PEDOT: the PSS solution was magnetically stirred, 0.18g chloroplatinic acid was added and mixed at 2000r/min stirring speed for 2h to finally prepare PEDOT at a concentration of 0.035 mol/L: PSS modified solution, and storing at 4 ℃; subsequently 25% (v/v%) PEGDA, 5% (v/v%) glycerol, 15% (v/v%) deionised water and 55% (v/v%) PEDOT at a concentration of 0.035 mol/L: and mixing the PSS modified solution, and mixing for 2 hours at a stirring speed of 2000r/min to obtain the stably dispersed PEDOT: PSS/PEGDA precursor solution, PEDOT prepared: the PSS/PEGDA precursor solution is directly used as a coating emulsion;
and (3) mixing PEDOT: the PSS/PEGDA precursor solution is cast on LDPE Tape-ITXSP, then placed between two quartz plates and fixed by a clamp, placed under visible light for irradiation polymerization, then placed in deionized water for soaking, washed for 3 times by the deionized water, dried in vacuum, and stored under the conditions of constant temperature and constant humidity, so that the multi-dimensional flexible sensor can be obtained; the finally prepared LT-3 (P) sheet resistance is 80k omega/sq;
example 4
The invention relates to a preparation method of a multifunctional multi-dimensional flexible sensor based on a PE material, which comprises the following steps:
dissolving isopropyl thioxanthone ITX in acetone to form an ITX acetone solution; uniformly dropwise adding an ITX acetone solution on the surface of an LDPE Tape, clamping the LDPE Tape between two quartz plates, and irradiating the LDPE Tape at room temperature under an ultraviolet mercury lamp to obtain LDPE Tape-ITXSP; then soaking the LDPE Tape-ITXSP in acetone for 24h, washing the surface with acetone for 3 times, drying in vacuum, and storing under the conditions of constant temperature and humidity;
10ml of PEDOT: the PSS solution was magnetically stirred, 0.18g of chloroplatinic acid was added and mixed at a stirring speed of 2000r/min for 2h to finally prepare PEDOT having a concentration of 0.035 mol/L: PSS modified solution and stored at 4 ℃; subsequently 25% (v/v%) PEGDA, 5% (v/v%) glycerol, 20% (v/v%) deionised water and 50% (v/v%) PEDOT at a concentration of 0.035 mol/L: and mixing the PSS modified solution, and mixing for 2 hours at a stirring speed of 2000r/min to obtain the stably dispersed PEDOT: PSS/PEGDA precursor solution, PEDOT prepared: the PSS/PEGDA precursor solution is directly used as a coating emulsion;
and (3) mixing PEDOT: the PSS/PEGDA precursor solution is cast on LDPE Tape-ITXSP, then placed between two quartz plates and fixed by a clamp, placed under visible light for irradiation polymerization, then placed in deionized water for soaking, washed for 3 times by the deionized water, dried in vacuum, and stored under the conditions of constant temperature and constant humidity, so that the multi-dimensional flexible sensor can be obtained; the finally prepared LT-3 (P) sheet resistance is 138k omega/sq;
comparative example
The invention relates to a preparation method of a multifunctional multi-dimensional flexible sensor based on a PE material, which comprises the following steps:
dissolving isopropyl thioxanthone ITX in acetone to form an ITX acetone solution; uniformly dropwise adding an ITX acetone solution on the surface of an LDPE Tape, clamping the LDPE Tape between two quartz plates, and irradiating the LDPE Tape at room temperature under an ultraviolet mercury lamp to obtain LDPE Tape-ITXSP; then soaking the LDPE Tape-ITXSP in acetone for 24h, washing the surface with acetone for 3 times, drying in vacuum, and storing under the conditions of constant temperature and humidity;
10ml of PEDOT: the PSS solution was magnetically stirred, 0.18g of chloroplatinic acid was added and mixed at a stirring speed of 2000r/min for 2h to finally prepare PEDOT having a concentration of 0.035 mol/L: PSS modified solution and stored at 4 ℃; subsequently 25% (v/v%) PEGDA, 5% (v/v%) glycerol and 70% (v/v%) PEDOT at a concentration of 0.035 mol/L: and (3) mixing the PSS modified solution, and mixing for 2h at a stirring speed of 2000r/min to obtain the stably dispersed PEDOT: PSS/PEGDA precursor solution, PEDOT prepared: the PSS/PEGDA precursor solution is directly used as a coating emulsion;
and (3) mixing PEDOT: the PSS/PEGDA precursor solution is cast on LDPE Tape-ITXSP, then placed between two quartz plates and fixed by a clamp, placed under visible light for irradiation polymerization, then placed in deionized water for soaking, washed for 3 times by the deionized water, dried in vacuum, and stored under the conditions of constant temperature and constant humidity, so that the multi-dimensional flexible sensor can be obtained; the final LT-3 (P) sheet resistance is 3.06k omega/sq; but the resulting coating was not uniform.
FIG. 1 is a plot of sheet resistance (K Ω/sq) and conductivity (s/m) of L T-3 (P) in different deionized water ((v/v)%), and the sheet resistance and conductivity of L T-3 (P) were tested by a dual electrical four-probe resistance tester to obtain PEGDA/PEDOT: the PSS precursor solution has the optimal proportion: 25% pegda, 5% glycerol, 5% deionized water and 65% PEDOT at a concentration of 0.035 mol/L: as shown in FIG. 1, in the PSS-modified solution, when 5% ((v/v)%) glycerol was added, the sheet resistances were 3.06 K.OMEGA.and 4.58 K.OMEGA.for 0% ((v/v)%) and 5% ((v/v)%), respectively, but when 5% ((v/v)%) deionized water was added, P (PEGDA)/PEDOT: the PSS layer is more uniform and smooth.
Fig. 2 is a sensing graph for monitoring the movement of the index finger of the human body by using the sensor of the present invention, in which the relative resistance changes at different bending angles (15 °, 45 ° and 90 °) over a period of time and the relative resistance changes at different bending angles over time, so that it can be seen that the sensor can be used as an "electronic skin" that can be efficiently, conveniently and directly attached to the index finger of the human body, and at the same time, the sensor can be proved to have good repeatability, and excellent reliability, cycle stability, fast responsiveness and response accuracy.
Fig. 3 shows the relative resistance change at different bending angles (15 °, 30 ° and 90 °) and the relative resistance change with time at different bending angles in a period of time, which are monitored by using the sensor of the present invention, so that the sensor can be used as an "electronic skin" to be attached to the wrist efficiently, conveniently and directly, and the sensor can be proved to have good repeatability, excellent reliability, cycle stability, fast response and response accuracy.
Fig. 4 shows the relative resistance change at different bending angles (15 °, 45 ° and 90 °) and the relative resistance change with time at different bending angles in a period of time, which are monitored by using the sensor of the present invention, so that it can be seen that the sensor can be efficiently, conveniently and directly attached to the elbow joint of a human body as an "electronic skin", and at the same time, the sensor can be proved to have good repeatability and excellent reliability, cycle stability, fast response and response accuracy.
FIG. 5 is a graph showing the relative resistance change over time at different bending angles (15, 30 and 90) and the relative resistance change over time at different bending angles using the sensor of the present invention to monitor knee movement in a human. It can be seen that the sensor can be attached to the knee of a human body as an "electronic skin" efficiently, conveniently and directly, and at the same time, the sensor can be proved to have good repeatability and excellent reliability, cycle stability, fast response and response accuracy.
FIG. 6 shows that the sensor of the present invention is used to monitor the slight vibration of the human throat, and the responding sounds are "Shanxi university of science and technology", "Shanxi university of science and technology" in sequence. Therefore, the sensor can be used as an 'electronic skin' to be attached to the throat of a human body efficiently, conveniently and directly, and meanwhile, the sensor can be proved to have good sensitivity and real-time response performance to slight vibration of the throat of the human body and the like.
Claims (5)
1. A preparation method of a multi-dimensional flexible sensor based on a PE material is characterized by comprising the following steps:
step 1, dissolving ITX in acetone to form ITX acetone solution; uniformly dropwise adding an ITX acetone solution on the surface of an LDPE Tape, clamping the LDPE Tape between two quartz plates, and irradiating the LDPE Tape at room temperature under an ultraviolet mercury lamp to obtain LDPE Tape-ITXSP; then soaking the LDPE Tape-ITXSP in acetone, washing the surface for 3 times by using the acetone, and drying in vacuum;
step 2, mixing PEDOT: and magnetically stirring the PSS solution, adding chloroplatinic acid, and uniformly stirring to obtain PEDOT: PSS modified solution and stored at 4 ℃; PEGDA, glycerol, deionized water, and PEDOT: and (3) mixing the PSS modified solution to obtain stably dispersed PEDOT: PSS/PEGDA precursor solution;
and step 3, mixing PEDOT: and casting the PSS/PEGDA precursor solution on LDPE Tape-ITXSP, then placing the LDPE Tape-ITXSP between two quartz plates, fixing the LDPE Tape-ITXSP by using a clamp, placing the LDPE Tape-ITXSP under visible light for irradiation polymerization, then placing the LDPE Tape-ITXSP in deionized water for soaking, washing the LDPE Tape-ITXSP for 3 times by using the deionized water, and drying the LDPE Tape-ITXSP in vacuum to obtain the multi-dimensional flexible sensor.
2. The method for preparing a PE-based multi-dimensional flexible sensor according to claim 1, wherein in the step 1, the concentration of ITX acetone solution is 3mmol mL -1 。
3. The method for preparing the PE-based multi-dimensional flexible sensor according to claim 1, wherein in the step 1, the irradiation time is 3-5min, the wavelength of an ultraviolet mercury lamp is 254nm, and the light intensity is 9m W/cm 2 (ii) a The soaking time is 24h.
4. The method for preparing a multi-dimensional flexible sensor based on PE material according to claim 1, wherein in the step 2, the ratio of PEDOT: the concentration of the PSS modified solution was 0.035mol/L.
5. The method for preparing the multi-dimensional flexible sensor based on the PE material as claimed in claim 1, wherein in the step 3, the irradiation polymerization time is 60-120 min; the wavelength of visible light is 420nm, and the light intensity is 3mW/cm 2 。
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| CN111961421A (en) * | 2020-09-09 | 2020-11-20 | 深圳大学 | Water-based conductive adhesive and preparation method thereof |
| US20200401042A1 (en) * | 2019-05-09 | 2020-12-24 | The Board Of Trustees Of The Leland Stanford Junior University | Directly photo-patternable, stretchable, electrically conductive polymer |
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| CN113611437A (en) * | 2021-07-30 | 2021-11-05 | 南京邮电大学 | Fully flexible transparent film electrode and preparation method and application thereof |
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| US20200401042A1 (en) * | 2019-05-09 | 2020-12-24 | The Board Of Trustees Of The Leland Stanford Junior University | Directly photo-patternable, stretchable, electrically conductive polymer |
| CN111961421A (en) * | 2020-09-09 | 2020-11-20 | 深圳大学 | Water-based conductive adhesive and preparation method thereof |
| CN112679776A (en) * | 2020-12-23 | 2021-04-20 | 苏州缔因安生物科技有限公司 | Functional flexible electronic device based on hydrogel and preparation method thereof |
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