CN113503914A - Preparation method of flexible sensor - Google Patents
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- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims 3
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D21/00—Measuring or testing not otherwise provided for
- G01D21/02—Measuring two or more variables by means not covered by a single other subclass
Abstract
The invention provides a preparation method of a flexible sensor, which solves the defects that harmful reagents are used in the existing preparation of the flexible sensor, the environment is not friendly, and the liquid flows and permeates in the using process. The method comprises the following steps: 1) preparing a flexible viscous substrate, spraying a release agent on the rigid substrate, and preparing the flexible viscous substrate on the rigid substrate after the release agent is cured; 2) fixing a template, and pressing the template with the pre-processed pattern on the flexible viscous substrate prepared in the step 1) in a hot pressing mode; 3) filling a sensitive material, namely filling the sensitive material pretreated into a curable conductive solution into the template pattern fixed in the step 2); 4) and curing to prepare a flexible sensor, removing the template, curing the curable conductive solution, and peeling the flexible adhesive substrate from the rigid substrate to obtain the flexible sensor.
Description
Technical Field
The invention belongs to the technical field of flexible electronic devices, and particularly relates to a preparation method of a flexible sensor.
Background
With the continuous improvement of living standard of people, people pay more attention to their health condition, and effective monitoring of human health indexes is extremely important to human health. The traditional device for monitoring the human health is high in price and poor in comfort, the flexible sensor can be in close contact with the skin of a human body, the comfort is good, the response time is short, the human health signal can be detected in real time, the device can play an important role in disease diagnosis, surgical treatment and human rehabilitation, and the defects of the traditional device are expected to be overcome.
Document "A Temperature-Controlled Conductive PANI @ CNFs/MEO2The method of MA/PEGMA Hydrogel for Flexible Temperature Sensors' chemical synthesis prepares the Temperature sensor with excellent mechanical properties, but H is needed in the preparation process2SO4、HCl、(NH4)2SO4And aniline and other harmful reagents are not environment-friendly, and liquid flow and permeation can occur in the using process, so that the detection method is difficult to be used for detecting contact human health signals.
Disclosure of Invention
The invention aims to overcome the defects that harmful reagents are used when the existing flexible sensor is prepared, the environment is not friendly, and liquid flows and permeates in the using process, and provides a preparation method of the flexible sensor.
In order to achieve the purpose, the technical solution provided by the invention is as follows:
the preparation method of the flexible sensor is characterized by comprising the following steps:
1) preparation of Flexible adhesive substrates
Spraying a release agent on the rigid substrate, and preparing a flexible viscous substrate on the rigid substrate after the release agent is cured;
2) fixed template
Pressing a template with a pre-processed pattern on the flexible viscous substrate prepared in the step 1) in a hot pressing mode;
3) filled with sensitive material
Filling sensitive materials pretreated into a curable conductive solution into the template pattern fixed in the step 2);
4) curing preparation flexible sensor
And removing the template, curing the curable conductive solution, and peeling the flexible adhesive substrate from the rigid substrate to obtain the flexible sensor. The flexible sensor here should also be wired before use.
Further, the step 1) is specifically as follows:
spraying a release agent on the rigid substrate, uniformly spin-coating a flexible viscous substrate material on the rigid substrate after the release agent is cured, and heating and curing to prepare a flexible viscous substrate;
the flexible viscous substrate material is Eco-flex, PDMS (polydimethylsiloxane), PI (polyimide) or PU (polyurethane).
Further, in the step 2), the hot pressing refers to tightly combining the template and the flexible viscous substrate at a temperature of 60-100 ℃ by using a film coating machine, preferably 80 ℃.
Further, the preparation method of the curable conductive solution used in the step 3) is as follows:
the preparation method of the curable conductive solution used in the step 3) comprises the following steps:
s1, adding a sensitive material into a PDMS solution, and stirring to obtain a uniform solution; the PDMS solution is PDMS added with cyclohexane, the cyclohexane is used for diluting the PDMS and is easy to volatilize, other solvents with the function can be used, and in addition, the cyclohexane can be added before and after the sensitive material is added;
s2, crushing the uniform solution obtained in the step S1 by using an ultrasonic cell crusher, adding a PDMS curing agent, and stirring to obtain a curable conductive solution;
the viscosity of the curable conductive solution is higher along with the volatilization of the added cyclohexane, so that after the template is removed in the step 4), the curable conductive solution does not need to be worried about flowing to influence modeling;
wherein, the sensitive material refers to a material sensitive to temperature, pressure, humidity or gas;
the mass ratio of the specific sensitive material to PDMS can be adjusted according to the type of the sensitive material, but the prepared solution is ensured to be conductive; for example, the mass ratio of the temperature sensitive material to the PDMS can be 1: 2-1: 4;
the mass of the PDMS curing agent is one tenth of that of the PDMS solution; the curing agent is a curing agent matched with PDMS.
Further, in the step 4), the curing is performed on a hot plate at 75-80 ℃ for 30-50 minutes, preferably on a hot plate at 80 ℃ for 30 minutes.
Further, in step 2), before the template is used, a template pattern is designed according to requirements, and the template is prepared by a laser-assisted processing method, a chemical etching method or a mold processing method, preferably, the template is prepared by a laser-assisted processing method.
Further, the temperature sensitive material is one or more of PANI (polyaniline), carbon material (CB, multi-wall carbon nano-tube, single-wall carbon nano-tube, etc.), Ag, Pt, Ni and PEDOT;
the pressure-sensitive material adopts one or more of PVDF (polyvinylidene fluoride), graphene and carbon nano tubes;
the moisture and gas sensitive material employs one or more of a carbon material and a semiconducting metal oxide.
The invention also provides a flexible sensor prepared by the preparation method.
The invention has the advantages that:
1. according to the invention, the template and the flexible viscous base are tightly combined by using a hot pressing method to prepare the flexible sensor, the flowability of the solution can be overcome by using the template method, and the permeation of the solution between the substrate and the template can be effectively solved by using the flexible viscous base, so that the shape of the flexible sensor can be controlled; meanwhile, the template method can produce the sensing devices with the same shape and controllable shape in batch and at low cost; the template method can effectively reduce the consumption of materials, save the cost, has simple preparation process, low requirement on the production and preparation environment, does not need harsh clean environment (such as harsh experimental environment of ultra-clean dust-free and the like), and can realize high-efficiency and batch production.
2. The preparation method of the flexible sensor has universality, and flexible devices with different shapes and different functions can be prepared on different flexible viscous substrates by selecting different sensitive materials and flexible viscous substrates and based on templates with different shapes.
3. H is not used in the preparation process of the flexible sensor2SO4、HCl、(NH4)2SO4And aniline and other harmful reagents, and the preparation process is not only environment-friendly, but also can be directly contacted with a human body for use.
Drawings
FIG. 1 is a flow chart of the preparation process of the method of the present invention;
FIG. 2 is a schematic diagram of the structure during the preparation of the method of the present invention;
the reference numerals in fig. 2 are:
1-sensitive material, 2-template, 3-flexible viscous substrate, 4-release agent and 5-rigid substrate;
FIG. 3 is a template pattern designed according to embodiment 1 of the method of the present invention;
FIG. 4 is a graph of the change of electrical signal with temperature in example 1 of the method of the present invention.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
in order to make the method of the invention more suitable for industrial production, the steps of the invention are optimized to form a streamlined process flow of sensitive material preparation, template pattern design and processing, flexible viscous substrate preparation, template and viscous substrate combination and flexible sensing device preparation, so as to improve the production efficiency, and the specific flow chart is shown in figure 1; the sequence of the two steps of "sensitive material preparation" and "template pattern design and processing" may not be strictly specified.
Example 1
1) Preparation of temperature-sensitive materials
PANI and CB are selected as temperature sensitive materials and are sequentially added into the PDMS solution, and the total mass ratio of the PANI to the CB (wherein PANI CB is 1:1) is 20% in the embodiment, and the mass ratio of the PDMS is 80%.
1.1) weighing 1.6g of PDMS, adding 0.3g of cyclohexane, and stirring with a magnetic stirrer at 1000rpm for 10 minutes to obtain a uniform solution A;
1.2) adding 0.2gCB into the uniform solution A, and stirring for 30 minutes at 1500rpm by using a magnetic stirrer to obtain a uniform solution B;
1.3) adding 0.2g of PANI into the uniform solution B, and stirring for 30 minutes at 1500rpm by using a magnetic stirrer to obtain a uniform solution C;
1.4) working the uniform solution C for 15 minutes at 270W by using an ultrasonic cell crusher to obtain a uniform solution D;
1.5) adding 0.16g of PDMS curing agent into the homogeneous solution D, and stirring with a magnetic stirrer at 1000rpm for 10 minutes to obtain a curable conductive solution;
2) design and processing of template patterns
Designing an electrode pattern (as shown in figure 3), and preparing a template by using a laser-assisted processing method;
3) preparation of Flexible adhesive substrates
Spraying a release agent on a rigid substrate, after the release agent is cured, uniformly coating Eco-flex on the rigid substrate, working for 30s at the rotating speed of 500rpm by using a spin coater, and then placing the rigid substrate on a hot plate at 80 ℃ for heating and curing for 2 min;
4) template bonding to flexible adhesive substrate
Tightly combining the template obtained in the step 2) with the flexible viscous substrate obtained in the step 3) through hot pressing, and then tightly combining the template and the substrate through a laminating machine heated to 80 ℃ by utilizing hot pressing and the viscosity of Eco-flex so as to effectively prevent the permeation phenomenon of a solution;
5) preparation and curing of flexible temperature sensor
Filling the curable conductive solution obtained in the step 1) into the pattern of the template in the step 4), removing the template, placing the template on a hot plate at 80 ℃ for curing for 30 minutes, and peeling the flexible adhesive substrate from the rigid substrate to obtain the flexible temperature sensor.
In order to facilitate performance testing, the obtained flexible temperature sensor is connected, then the flexible temperature sensor is placed on a constant temperature liquid nitrogen thermostat to be heated, a resistance-temperature-variation curve (as shown in fig. 4) is recorded, and calculation is performed according to a resistance temperature coefficient formula (1), wherein a resistance Temperature Coefficient (TCR) represents the relative variation of the resistance value of the resistance when the temperature is changed by 1 ℃, and the unit is ppm/DEG C:
wherein, R0 and T0 are the initial resistance value and the initial temperature, R, T is the resistance value and the temperature at a certain temperature, and Δ R and Δ T are the resistance variation value and the temperature difference.
Example 2:
1) preparation of pressure-sensitive materials
CNT is selected as a pressure sensitive material to be added into the PDMS solution, and the mass ratio of the CNT to the PDMS is 1:9 in the embodiment.
1.1) weighing 1.8g of PDMS, adding 0.2g of cyclohexane, and stirring with a magnetic stirrer at 1000rpm for 10 minutes to obtain a uniform solution A;
1.2) adding 0.2g of CNT into the uniform solution A, and stirring the mixture for 30 minutes at 1500rpm by using a magnetic stirrer to obtain a uniform solution B;
1.4) working the uniform solution B for 20 minutes at 200W by using an ultrasonic cell crusher to obtain a uniform solution C;
1.5) adding 0.18g of PDMS curing agent into the homogeneous solution C, and stirring with a magnetic stirrer at 1000rpm for 10 minutes to obtain a curable solution;
2) design and processing of template patterns
Designing an electrode pattern, and preparing a template by using a laser auxiliary processing method;
3) preparation of Flexible adhesive substrates
Spraying a release agent on a rigid substrate, after curing, uniformly coating Eco-flex on the rigid substrate, working for 30s at the rotating speed of 500rpm by using a spin coater, and then placing the rigid substrate on a hot plate at 80 ℃ for heating and curing for 2 minutes;
4) template bonding to flexible adhesive substrate
Tightly combining the template obtained in the step 2) with the flexible viscous substrate obtained in the step 3) through hot pressing, and then tightly combining the template and the substrate through a laminating machine heated to 80 ℃ by utilizing hot pressing and the viscosity of Eco-flex so as to effectively prevent the permeation phenomenon of a solution;
5) preparation and curing of flexible pressure sensor
Filling the curable solution obtained in the step 1) into the pattern of the template obtained in the step 4), removing the template, placing the template on a hot plate at 80 ℃ for curing for 35 minutes, peeling the flexible adhesive substrate from the rigid substrate to obtain the pressure sensor, and connecting wires to measure the pressure performance of the pressure sensor.
Example 3:
1) preparing a humidity sensitive material:
PANI is selected as a humidity sensitive material to be added into the PDMS solution, and the mass ratio of PANI to PDMS is 2:8 in the embodiment.
1.1) weighing 1.6g of PDMS, adding 0.4g of cyclohexane, and stirring with a magnetic stirrer at 1000rpm for 10 minutes to obtain a uniform solution A;
1.2) adding 0.4g of PANI into the uniform solution A, and stirring for 45 minutes at 1500rpm by using a magnetic stirrer to obtain a uniform solution B;
1.4) working the uniform solution B for 15 minutes at the power of 300W by using an ultrasonic cell crusher to obtain a uniform solution C;
1.5) adding 0.16g of PDMS curing agent into the homogeneous solution C, and stirring with a magnetic stirrer at 1000rpm for 15 minutes to obtain a curable solution;
2) design and processing of template patterns
Designing an electrode pattern, and preparing a template by using a laser auxiliary processing method;
3) preparation of Flexible adhesive substrates
Spraying a release agent on a rigid substrate, after curing, uniformly coating Eco-flex on the rigid substrate, working for 30s at the rotating speed of 500rpm by using a spin coater, and then placing the rigid substrate on a hot plate at 80 ℃ for heating and curing for 2 minutes;
4) template bonding to flexible adhesive substrate
Tightly combining the template obtained in the step 2) with the flexible viscous substrate obtained in the step 3) through hot pressing, and then tightly combining the template and the substrate through a laminating machine heated to 80 ℃ by utilizing hot pressing and the viscosity of Eco-flex so as to effectively prevent the permeation phenomenon of a solution;
5) preparation and curing of flexible humidity sensor
Filling the curable solution obtained in the step 1) into the pattern of the template obtained in the step 4), removing the template, placing the template on a hot plate at 80 ℃ for curing for 45 minutes, peeling the flexible adhesive substrate from the rigid substrate to obtain a humidity sensor, and connecting wires to measure the humidity performance of the humidity sensor.
While the invention has been described with reference to specific embodiments, the invention is not limited thereto, and various equivalent modifications or substitutions can be easily made by those skilled in the art within the technical scope of the present disclosure.
Claims (8)
1. A method for preparing a flexible sensor is characterized by comprising the following steps:
1) preparation of Flexible adhesive substrates
Spraying a release agent on the rigid substrate, and preparing a flexible viscous substrate on the rigid substrate after the release agent is cured;
2) fixed template
Pressing a template with a pre-processed pattern on the flexible viscous substrate prepared in the step 1) in a hot pressing mode;
3) filled with sensitive material
Filling sensitive materials pretreated into a curable conductive solution into the template pattern fixed in the step 2);
4) curing preparation flexible sensor
And removing the template, curing the curable conductive solution, and peeling the flexible adhesive substrate from the rigid substrate to obtain the flexible sensor.
2. The method for preparing the flexible sensor according to claim 1, wherein the step 1) is specifically as follows:
spraying a release agent on the rigid substrate, uniformly spin-coating a flexible viscous substrate material on the rigid substrate after the release agent is cured, and heating and curing to prepare a flexible viscous substrate;
the flexible viscous substrate material is Eco-flex, PDMS, PI or PU.
3. The method for manufacturing a flexible sensor according to claim 2, wherein:
in the step 2), the hot pressing refers to tightly combining the template and the flexible viscous substrate at the temperature of 60-100 ℃ by using a film laminating machine.
4. A method of manufacturing a flexible sensor according to claim 3, wherein:
the preparation method of the curable conductive solution used in the step 3) comprises the following steps:
s1, adding a sensitive material into a PDMS solution, and stirring to obtain a uniform solution;
s2, crushing the uniform solution obtained in the step S1 by using an ultrasonic cell crusher, adding a PDMS curing agent, and stirring to obtain a curable conductive solution;
wherein the sensitive material refers to a material sensitive to temperature, pressure, humidity or gas.
5. The method for manufacturing a flexible sensor according to claim 4, wherein:
in the step 4), the curing is carried out on a hot plate at the temperature of 75-80 ℃ for 30-50 minutes.
6. The method for manufacturing a flexible sensor according to claim 1, wherein:
the template which is used in the step 2) and is processed with patterns in advance is prepared by adopting a laser auxiliary processing method, a chemical etching method or a mould processing method.
7. A method of manufacturing a flexible sensor according to claim 3, wherein:
the temperature sensitive material is one or more of PANI, carbon material, Ag, Pt, Ni and PEDOT, PSS;
the pressure-sensitive material adopts one or more of PVDF, graphene and carbon nanotubes;
the moisture and gas sensitive material employs one or more of a carbon material and a semiconducting metal oxide.
8. A flexible sensor, characterized by: prepared by the preparation method of any one of claims 1 to 7.
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