CN115466427B - 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 PE materials, which comprises the following steps: dropwise adding ITX acetone solution on the surface of LDPE Tape, clamping the LDPE Tape between two quartz plates, placing under an ultraviolet mercury lamp, irradiating at room temperature, washing, and drying; to PEDOT: adding chloroplatinic acid into the PSS solution, and uniformly stirring to obtain PEDOT: PSS modifying solution, followed by PEGDA, glycerol, deionized water and PEDOT: PSS modifying solution was mixed, PEDOT: the PSS/PEGDA precursor solution is cast on LDPE Tape-ITXSP, placed between two quartz plates, fixed by clamps, polymerized by irradiation under visible light, washed and dried. The flexible sensor prepared by the method has 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) materials have been widely paid attention to since the advent of the present technology because of their excellent characteristics such as low cost, low density, corrosion resistance, soft texture, and easy processing, and are the most widely used and largest amount of polymer materials. The 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, inert reaction and the like in actual use, and the characteristics have the advantages of corrosion resistance, low temperature resistance, good chemical stability and the like in application, but also cause a plurality of problems of difficult printing, difficult adhesion, easy generation of static electricity, poor biocompatibility, lack of reaction sites and the like on the surface of the PE material. Therefore, on the basis of not changing the excellent characteristics of the PE material, it is important to break through the use bottleneck of the PE material.
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 sensors prepared from traditional 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 a detectable electrical signal output. At present, the materials for manufacturing the flexible sensor are mainly hydrogel, protein fiber and textile materials, and 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 flexible sensing is reduced, the application of the flexible sensor is developed from the traditional electronic product, biomedical and human health monitoring fields to the directions of large chemical industry, large materials, large machinery and the like, and the flexible sensor is an ideal product which is very required by the emerging technology and integrated equipment.
Disclosure of Invention
The invention aims to provide a preparation method of a multi-dimensional flexible sensor based on PE materials, 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 isopropylthioxanthone ITX in acetone to form ITX acetone solution; uniformly dripping ITX acetone solution on the surface of LDPE Tape, clamping the LDPE Tape between two quartz plates, and placing the quartz plates under an ultraviolet mercury lamp for irradiation at room temperature to obtain LDPE Tape-ITXSP; then, LDPE Tape-ITXSP is soaked in acetone, the surface is washed by the acetone for 3 times, and vacuum drying is carried out;
The present invention is also characterized in that,
in step 1, the concentration of ITX acetone solution was 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 The method comprises the steps of carrying out a first treatment on the surface of the The soaking time is 24 hours.
In step 2, PEDOT: the concentration of the PSS modification 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 as follows: the flexible sensor prepared by the method 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 glycerin 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 the advantages of low cost of raw materials, wide sources, environment-friendly reaction in the whole process, and simplicity and practicability.
Drawings
FIG. 1 is a plot of sheet resistance (KΩ/sq) versus conductivity (s/m) for Lt-3 (P) for various deionized water ((v/v)%);
FIG. 2 is a sensing graph of a human index finger movement monitored using the sensor of the present invention;
FIG. 3 is a sensing graph of monitoring human wrist motion 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 sensing graph of monitoring knee motion of a human using the sensor of the present invention;
fig. 6 is a graph of a sensing signal for monitoring slight vibration of the human throat using the sensor of the present invention.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The invention discloses a preparation method of a multi-dimensional flexible sensor based on PE materials, which is implemented according to the following steps:
step 1, dissolving isopropylthioxanthone ITX in acetone to form ITX acetone solution; uniformly dripping ITX acetone solution on the surface of a low-density polyethylene Tape (LDPE Tape), sandwiching the LDPE Tape between two quartz plates to form a sandwich structure, and irradiating at room temperature under an ultraviolet mercury lamp to obtain the LDPE Tape (LDPE Tape-ITXSP) grafted with ITX semipinacol free radical dormant species; then, soaking LDPE Tape-ITXSP in acetone for 24 hours, washing the surface with acetone for 3 times to remove residual ITX, drying in vacuum, and preserving under the condition of constant temperature and constant humidity;
the ITX acetone solution had a concentration of 3mmolmL -1 ;
The irradiation time is 3-5min, the wavelength of ultraviolet mercury lamp is 254nm, and the light intensity is 9m W/cm 2 ;
The constant temperature and humidity conditions are as follows: the temperature is 23 ℃ and the relative humidity is 50%;
PEDOT: the concentration of the PSS modified solution is 0.035mol/L;
PEDOT: the optimal ratio of PSS/PEGDA precursor solution is: PEGDA, glycerol, deionized water and PEDOT: the volume fractions of the PSS modification solutions are 25%, 5% and 65%, respectively;
the irradiation polymerization time is 60-120 min;
the wavelength of visible light is 420nm, and the light intensity is 3mW/cm 2 ;
The constant temperature and humidity conditions are as follows: the temperature is 23 ℃ and the relative humidity is 50%;
the multifunctional multi-dimensional flexible sensor mainly adopts PEG as a three-dimensional 'molecular mesh fabric' to embed conductive polymer PEDOT-PSS, and when the sensor is acted by external force, a molecular mesh fabric layer embedded with the PEDOT-PSS deforms, so that the arrangement condition of the 'molecular mesh fabric' is changed, the combination state between PEDOT-PSS molecules is influenced, and an electronic channel is changed, so that the transmission of electric charges is changed. Therefore, the resistance of the sensor is changed, and different external force effects can give different resistance values to the sensor, so that the external force condition of the sensor can be monitored through resistance signals changing at any time.
Example 1
The invention discloses a preparation method of a multifunctional multi-dimensional flexible sensor based on PE materials, which comprises the following steps:
dissolving isopropylthioxanthone ITX in acetone to form ITX acetone solution; uniformly dripping ITX acetone solution on the surface of LDPE Tape, clamping the LDPE Tape between two quartz plates, and placing the quartz plates under an ultraviolet mercury lamp for irradiation at room temperature to obtain LDPE Tape-ITXSP; then, soaking LDPE Tape-ITXSP in acetone for 24 hours, washing the surface with acetone for 3 times, drying in vacuum, and preserving under the condition of constant temperature and constant humidity;
into a beaker was added dropwise 10ml of PEDOT: the PSS solution was magnetically stirred, 0.18g chloroplatinic acid was added and mixed at a stirring speed of 2000r/min for 2 hours to finally prepare PEDOT at a concentration of 0.035 mol/L: PSS modified solution and stored at 4 ℃; 25% (v/v%) PEGDA, 5% (v/v%) glycerol, 5% (v/v%) deionized water and 65% (v/v%) PEDOT at a concentration of 0.035mol/L were then added: the PSS modified solution is mixed, and the mixture is mixed for 2 hours at a stirring speed of 2000r/min, so that the stable dispersed PEDOT is obtained: PSS/PEGDA precursor solution, PEDOT prepared: the PSS/PEGDA precursor solution is directly used as a coating emulsion;
PEDOT: casting 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 in visible light for irradiation polymerization, then placing the LDPE Tape-ITXSP in deionized water for soaking, washing the LDPE Tape-ITXSP with the deionized water for 3 times, drying the LDPE Tape-ITXSP in vacuum, and preserving the LDPE Tape-ITXSP under the conditions of constant temperature and constant humidity to obtain the multi-dimensional flexible sensor; the finally prepared LT-3 (P) sheet resistance is 4.58kΩ/sq; and the obtained coating is uniform.
Example 2
The invention discloses a preparation method of a multifunctional multi-dimensional flexible sensor based on PE materials, which comprises the following steps:
dissolving isopropylthioxanthone ITX in acetone to form ITX acetone solution; uniformly dripping ITX acetone solution on the surface of LDPE Tape, clamping the LDPE Tape between two quartz plates, and placing the quartz plates under an ultraviolet mercury lamp for irradiation at room temperature to obtain LDPE Tape-ITXSP; then, soaking LDPE Tape-ITXSP in acetone for 24 hours, washing the surface with acetone for 3 times, drying in vacuum, and preserving under the condition of constant temperature and constant humidity;
into a beaker was added dropwise 10ml of PEDOT: the PSS solution was magnetically stirred, 0.18g chloroplatinic acid was added and mixed at a stirring speed of 2000r/min for 2 hours to finally prepare PEDOT at a concentration of 0.035 mol/L: PSS modified solution and stored at 4 ℃; 25% (v/v%) PEGDA, 5% (v/v%) glycerol, 10% (v/v%) deionized water and 60% (v/v%) PEDOT at a concentration of 0.035mol/L were then added: the PSS modified solution is mixed, and the mixture is mixed for 2 hours at a stirring speed of 2000r/min, so that the stable dispersed PEDOT is obtained: PSS/PEGDA precursor solution, PEDOT prepared: the PSS/PEGDA precursor solution is directly used as a coating emulsion;
PEDOT: casting 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 in visible light for irradiation polymerization, then placing the LDPE Tape-ITXSP in deionized water for soaking, washing the LDPE Tape-ITXSP with the deionized water for 3 times, drying the LDPE Tape-ITXSP in vacuum, and preserving the LDPE Tape-ITXSP under the conditions of constant temperature and constant humidity to obtain the multi-dimensional flexible sensor; the finally prepared LT-3 (P) sheet resistance is 30kΩ/sq;
example 3
The invention discloses a preparation method of a multifunctional multi-dimensional flexible sensor based on PE materials, which comprises the following steps:
dissolving isopropylthioxanthone ITX in acetone to form ITX acetone solution; uniformly dripping ITX acetone solution on the surface of LDPE Tape, clamping the LDPE Tape between two quartz plates, and placing the quartz plates under an ultraviolet mercury lamp for irradiation at room temperature to obtain LDPE Tape-ITXSP; then, soaking LDPE Tape-ITXSP in acetone for 24 hours, washing the surface with acetone for 3 times, drying in vacuum, and preserving under the condition of constant temperature and constant humidity;
into a beaker was added dropwise 10ml of PEDOT: the PSS solution was magnetically stirred, 0.18g chloroplatinic acid was added and mixed at a stirring speed of 2000r/min for 2 hours to finally prepare PEDOT at a concentration of 0.035 mol/L: PSS modified solution and stored at 4 ℃; 25% (v/v%) PEGDA, 5% (v/v%) glycerol, 15% (v/v%) deionized water and 55% (v/v%) PEDOT at a concentration of 0.035mol/L were then added: the PSS modified solution is mixed, and the mixture is mixed for 2 hours at a stirring speed of 2000r/min, so that the stable dispersed PEDOT is obtained: PSS/PEGDA precursor solution, PEDOT prepared: the PSS/PEGDA precursor solution is directly used as a coating emulsion;
PEDOT: casting 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 in visible light for irradiation polymerization, then placing the LDPE Tape-ITXSP in deionized water for soaking, washing the LDPE Tape-ITXSP with the deionized water for 3 times, drying the LDPE Tape-ITXSP in vacuum, and preserving the LDPE Tape-ITXSP under the conditions of constant temperature and constant humidity to obtain the multi-dimensional flexible sensor; the finally prepared LT-3 (P) sheet resistance is 80kΩ/sq;
example 4
The invention discloses a preparation method of a multifunctional multi-dimensional flexible sensor based on PE materials, which comprises the following steps:
dissolving isopropylthioxanthone ITX in acetone to form ITX acetone solution; uniformly dripping ITX acetone solution on the surface of LDPE Tape, clamping the LDPE Tape between two quartz plates, and placing the quartz plates under an ultraviolet mercury lamp for irradiation at room temperature to obtain LDPE Tape-ITXSP; then, soaking LDPE Tape-ITXSP in acetone for 24 hours, washing the surface with acetone for 3 times, drying in vacuum, and preserving under the condition of constant temperature and constant humidity;
into a beaker was added dropwise 10ml of PEDOT: the PSS solution was magnetically stirred, 0.18g chloroplatinic acid was added and mixed at a stirring speed of 2000r/min for 2 hours to finally prepare PEDOT at a concentration of 0.035 mol/L: PSS modified solution and stored at 4 ℃; 25% (v/v%) PEGDA, 5% (v/v%) glycerol, 20% (v/v%) deionized water and 50% (v/v%) PEDOT at a concentration of 0.035mol/L were then added: the PSS modified solution is mixed, and the mixture is mixed for 2 hours at a stirring speed of 2000r/min, so that the stable dispersed PEDOT is obtained: PSS/PEGDA precursor solution, PEDOT prepared: the PSS/PEGDA precursor solution is directly used as a coating emulsion;
PEDOT: casting 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 in visible light for irradiation polymerization, then placing the LDPE Tape-ITXSP in deionized water for soaking, washing the LDPE Tape-ITXSP with the deionized water for 3 times, drying the LDPE Tape-ITXSP in vacuum, and preserving the LDPE Tape-ITXSP under the conditions of constant temperature and constant humidity to obtain the multi-dimensional flexible sensor; the finally prepared LT-3 (P) sheet resistance is 138kΩ/sq;
comparative example
The invention discloses a preparation method of a multifunctional multi-dimensional flexible sensor based on PE materials, which comprises the following steps:
dissolving isopropylthioxanthone ITX in acetone to form ITX acetone solution; uniformly dripping ITX acetone solution on the surface of LDPE Tape, clamping the LDPE Tape between two quartz plates, and placing the quartz plates under an ultraviolet mercury lamp for irradiation at room temperature to obtain LDPE Tape-ITXSP; then, soaking LDPE Tape-ITXSP in acetone for 24 hours, washing the surface with acetone for 3 times, drying in vacuum, and preserving under the condition of constant temperature and constant humidity;
into a beaker was added dropwise 10ml of PEDOT: the PSS solution was magnetically stirred, 0.18g chloroplatinic acid was added and mixed at a stirring speed of 2000r/min for 2 hours to finally prepare PEDOT at a concentration of 0.035 mol/L: PSS modified solution and stored at 4 ℃; 25% (v/v%) of PEGDA, 5% (v/v%) of glycerol and 70% (v/v%) of PEDOT at a concentration of 0.035 mol/L: the PSS modified solution is mixed, and the mixture is mixed for 2 hours at a stirring speed of 2000r/min, so that the stable dispersed PEDOT is obtained: PSS/PEGDA precursor solution, PEDOT prepared: the PSS/PEGDA precursor solution is directly used as a coating emulsion;
PEDOT: casting 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 in visible light for irradiation polymerization, then placing the LDPE Tape-ITXSP in deionized water for soaking, washing the LDPE Tape-ITXSP with the deionized water for 3 times, drying the LDPE Tape-ITXSP in vacuum, and preserving the LDPE Tape-ITXSP under the conditions of constant temperature and constant humidity to obtain the multi-dimensional flexible sensor; the finally prepared LT-3 (P) sheet resistance is 3.06kΩ/sq; but the resulting coating was not uniform.
FIG. 1 is a plot of sheet resistance (KΩ/sq) versus conductivity (s/m) for L T-3 (P) under different deionized water ((v/v)%) and PEGDA/PEDOT was obtained by sheet resistance and conductivity testing L T-3 (P) using a dual electrical four probe resistance tester: the best ratio of PSS precursor solution: 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 case of adding 5% ((v/v)%) glycerin, the added amounts of water were 0% ((v/v)%) and 5% ((v/v)%) and the sheet resistances were 3.06kΩ and 4.58kΩ, respectively, but after adding 5% ((v/v)%) deionized water, P (PEGDA)/PEDOT: the PSS layer is more uniform and smooth.
Fig. 2 is a graph of sensing for monitoring movement of an index finger of a human body using the sensor of the present invention, in which the relative resistance changes under different bending angles (15 °, 45 ° and 90 °) and the relative resistance changes with time under different bending angles over a period of time, so that it can be seen that the sensor can be effectively, conveniently and directly attached to an index finger of a human body as an "electronic skin", and at the same time, it can be demonstrated that the sensor has good repeatability and excellent reliability, cycling stability, rapid responsiveness and response accuracy.
Fig. 3 shows the sensor of the present invention for monitoring human wrist motion, relative resistance changes under different bending angles (15 °, 30 ° and 90 °) and relative resistance changes over time under different bending angles over a period of time, so that it can be seen that the sensor can be used as an "electronic skin" and can be efficiently, conveniently and directly attached to the human wrist, and at the same time, the sensor can be demonstrated to have good repeatability and excellent reliability, cycling stability, rapid response and response accuracy.
Fig. 4 shows the sensor of the present invention for monitoring human elbow joint motion, relative resistance change under different bending angles (15 °, 45 ° and 90 °) and relative resistance change with time under different bending angles over a period of time, so that it can be seen that the sensor can be used as an "electronic skin" and can be effectively, conveniently and directly attached to human elbow joint, and at the same time, the sensor can be proved to have good repeatability and excellent reliability, cycling stability, rapid response and response accuracy.
Fig. 5 is a graph of the monitoring of knee motion of a human using the sensor of the present invention, relative resistance changes over time at different bending angles (15 °, 30 ° and 90 °) and relative resistance changes over time at different bending angles. It can be seen that the sensor can be used as an 'electronic skin' and can be efficiently, conveniently and directly attached to a human knee, and meanwhile, the sensor can be proved to have good repeatability and excellent reliability, circulation stability, quick response and response accuracy.
Fig. 6 shows the sensor of the present invention for monitoring the slight vibration of human throat, and the response sounds are "university of science and technology of Shaanxi", "university of Shaanxi", and "science and technology", in this order. Therefore, the sensor can be used as an 'electronic skin' which can be efficiently, conveniently and directly attached to the throat of a human body, and can prove that the sensor has good sensitivity and real-time response performance to slight vibration of the throat of the human body.
Claims (5)
1. The preparation method of the multi-dimensional flexible sensor based on the PE material is characterized by comprising the following steps of:
step 1, dissolving isopropylthioxanthone ITX in acetone to form ITX acetone solution; uniformly dripping ITX acetone solution on the surface of LDPE Tape, clamping the LDPE Tape between two quartz plates, and placing the quartz plates under an ultraviolet mercury lamp for irradiation at room temperature to obtain LDPE Tape-ITXSP; then, LDPE Tape-ITXSP is soaked in acetone, the surface is washed by the acetone for 3 times, and vacuum drying is carried out;
step 2, PEDOT: magnetically stirring the PSS solution, then adding chloroplatinic acid, and uniformly stirring to obtain PEDOT: PSS modified solution and stored at 4 ℃; PEGDA, glycerol, deionized water and PEDOT were then added: the PSS modified solution is mixed to obtain the stable dispersed PEDOT: PSS/PEGDA precursor solution;
step 3, PEDOT: the PSS/PEGDA precursor solution is cast on LDPE Tape-ITXSP, then is placed between two quartz plates, is fixed by clamps, is placed under visible light for irradiation polymerization, is then placed in deionized water for soaking, is washed for 3 times by the deionized water, and is dried in vacuum, so that the multi-dimensional flexible sensor can be obtained.
2. The method for preparing a multi-dimensional flexible sensor based on PE material according to claim 1, wherein in the step 1, the concentration of ITX acetone solution is 3mmolmL -1 。
3. The method for preparing a multi-dimensional flexible sensor based on PE material according to claim 1, wherein in the 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 The method comprises the steps of carrying out a first treatment on the surface of the The soaking time is 24 hours.
4. The method for preparing the multi-dimensional flexible sensor based on the PE material according to claim 1, wherein in the step 2, the PEDOT: the concentration of the PSS modification solution was 0.035mol/L.
5. The method for preparing the multi-dimensional flexible sensor based on the PE material according to 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 |
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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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 |
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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