CN113670488A - Preparation method of carbon black/porous PDMS and application of carbon black/porous PDMS in resistance-type flexible pressure sensor - Google Patents

Preparation method of carbon black/porous PDMS and application of carbon black/porous PDMS in resistance-type flexible pressure sensor Download PDF

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Publication number
CN113670488A
CN113670488A CN202110958162.6A CN202110958162A CN113670488A CN 113670488 A CN113670488 A CN 113670488A CN 202110958162 A CN202110958162 A CN 202110958162A CN 113670488 A CN113670488 A CN 113670488A
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carbon black
pdms
porous
porous pdms
powder
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季久玉
苑宁予
于佳群
周坤
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Liaoning Shihua University
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Liaoning Shihua University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00Measuring force or stress, in general
    • G01L1/20Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
    • G01L1/22Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges

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  • General Physics & Mathematics (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention discloses a preparation method of carbon black/porous PDMS and application of the carbon black/porous PDMS in a resistance-type flexible pressure sensor. And uniformly scattering the powder template on the uncured PDMS layer, and heating and curing. And then soaking the PDMS in deionized water to obtain a porous PDMS layer. And then uniformly coating with a carbon black conductive solution. The preparation method has simple operation and low cost. The resistance-type flexible pressure sensor prepared from the carbon black/porous PDMS prepared by the method disclosed by the invention is adjustable in shape and size, and can be used for detecting micro mechanical movement and human physiological signals, including weak air flow blowing, swallowing action, finger touch and pronunciation.

Description

Preparation method of carbon black/porous PDMS and application of carbon black/porous PDMS in resistance-type flexible pressure sensor
Technical Field
The invention relates to porous PDMS, in particular to a preparation method of carbon black/porous PDMS and application thereof in a resistance-type flexible pressure sensor.
Background
In recent years, polymer foams have attracted much attention because of their excellent elastic properties, and flexible piezoresistive pressure sensors made of conductive nanomaterials coated with porous polymers have attracted much attention. However, polymer foams are brittle, which results in devices that have poor stability during long-term cycling tests. Therefore, a simple template method has been developed to prepare porous thin films. Over the past few years, a variety of compressible and flexible PDMS sponges have been prepared using sacrificial powder templates (e.g., potassium chloride, sodium chloride, and sugar). The flexible conductive sponge can also adopt a sacrificial powder template method, and a conductive nano material is added in the sponge preparation process, or a conductive solution is dripped after the sponge preparation. The performance of the flexible pressure sensor based on the silver nanowire/porous PDMS and multi-wall CNTs/porous PDMS template methods is improved. However, at present, a carbon black/porous PDMS-based resistive flexible pressure sensor is not researched by a template method, and the influence of the pore size of template powder on the performance of the pressure sensor is not researched systematically.
Disclosure of Invention
The invention aims to provide a preparation method of carbon black/porous PDMS and application of the carbon black/porous PDMS in a resistance-type flexible pressure sensor. The method is simple to operate, and the resistance-type flexible pressure sensor prepared from the carbon black/porous PDMS prepared by the method can be used for detecting micro mechanical movement and human physiological signals.
In order to solve the problems in the prior art, the technical scheme adopted by the invention is as follows:
the preparation method of the carbon black/porous PDMS comprises the following steps:
fully and uniformly mixing a PDMS prepolymer and a curing agent according to the weight part ratio of 10:1 to form a PDMS precursor;
coating the PDMS precursor on the glass substrate;
thirdly, uniformly coating the powder template on the uncured PDMS layer,
placing the PDMS coated with the powder template in a forced air drying oven to be dried for 2 hours at the temperature of 80 ℃;
taking the PDMS permeated with the powder template out of the forced air drying box and putting the PDMS into deionized water for soaking;
drying after soaking to obtain porous PDMS;
seventhly, adding carbon black into the dimethylformamide to prepare a carbon black conductive solution, wherein the concentration of the carbon black is 1 g/L-2 g/L; eighthly, ultrasonically oscillating the carbon black conductive solution prepared in the step seven for 30 min;
ninthly, dropping the carbon black conductive solution after ultrasonic oscillation into the porous PDMS obtained in the step (C), and drying at 110 ℃ on a heating plate to obtain the carbon black/porous PDMS.
Further, the preparation method of the carbon black/porous PDMS further comprises the following steps: and ninthly, repeating the step.
Further, the volume ratio of the carbon black conductive solution in the step (nini) to the PDMS precursor in the step (②) is 8: 5.
further, in the step (i), the prepolymer of PDMS and the curing agent are mixed uniformly and then placed into a vacuum air extractor for degassing treatment.
Further, the powder is one of KCl, NaCl, or sugar powder.
Further, the powder was sieved through a 100 mesh sieve.
Further, changing water for 3-4 times in the soaking process.
The carbon black/porous PDMS prepared by the preparation method of the carbon black/porous PDMS is applied to a resistance-type flexible pressure sensor.
The invention has the advantages and beneficial effects that:
the preparation method of the carbon black/porous PDMS is to mix the PDMS prepolymer with the curing agent and then coat the mixture on the glass substrate. The powder template was sprinkled evenly onto the uncured PDMS layer. The PDMS coated with the powder template was then cured at elevated temperature. The PDMS was then soaked in deionized water to dissolve away the powder that penetrated the PDMS, resulting in a thin porous PDMS layer. And then uniformly coating with a carbon black conductive solution. The preparation method has simple operation and low cost. The resistance-type flexible pressure sensor prepared from the carbon black/porous PDMS prepared by the method disclosed by the invention is adjustable in shape and size, and the KCl, NaCl and powdered sugar are different in size, so that the function of adjusting the aperture size can be realized by selecting KCl, NaCl and powdered sugar templates. The resistance-type flexible pressure sensor made of the carbon black/porous PDMS prepared by the method can be used for detecting tiny mechanical movement and human physiological signals, including weak airflow blowing, swallowing action, finger touch and pronunciation. The resistance-type flexible pressure sensor prepared from the carbon black/porous PDMS prepared by the method has the advantages of simple and convenient operation, low cost and good performance.
Drawings
The invention is described in further detail below with reference to the accompanying drawings:
FIG. 1 is a scanning electron micrograph of carbon black/porous PDMS templated with KCl powder;
FIG. 2 is a scanning electron micrograph of carbon black/porous PDMS with NaCl powder as a template;
FIG. 3 is a scanning electron micrograph of carbon black/porous PDMS with sugar powder as a template;
FIG. 4 is an I-V curve of a carbon black/porous PDMS pressure sensor prepared with KCl powder as a template under different pressures;
FIG. 5 is the current response of a carbon black/porous PDMS pressure sensor prepared with KCl powder as a template under different applied pressures ranging from 35 Pa to 8500 Pa;
FIG. 6 is the current response of carbon black/porous PDMS pressure sensor prepared by using KCl powder as a template under different frequency applied pressures;
FIG. 7 is a fatigue test curve of a carbon black/porous PDMS pressure sensor prepared with KCl powder as a template;
FIG. 8 is a graph of current response versus applied voltage for a carbon black/porous PDMS pressure sensor prepared using KCl, NaCl and powdered sugar as templates, respectively;
FIG. 9 shows the response time and recovery time of a carbon black/porous PDMS pressure sensor prepared using KCl, NaCl and powdered sugar as templates, respectively;
FIG. 10 is a graph of the current response of a carbon black/porous PDMS pressure sensor prepared with KCl powder as a template when a small piece of succulent plant foliage was loaded/removed;
FIG. 11 is a graph of a carbon black/porous PDMS pressure sensor prepared using KCl powder as a template and tested for the current response of the air pressure blown from an aurilave;
FIG. 12 is a graph of the current response of a carbon black/porous PDMS pressure sensor prepared with KCl powder as a template mounted in the neck for testing swallowing;
FIG. 13 is a photograph of a test finger pressing a carbon black/porous PDMS pressure sensor prepared with NaCl powder as a template;
FIG. 14 is a graph of the current response of a test finger pressing a carbon black/porous PDMS pressure sensor prepared with NaCl powder as the template;
FIG. 15 is a graph of the current response of a carbon black/porous PDMS pressure sensor prepared with NaCl powder as the template, mounted on the back of the wrist for tracking the wrist bending;
FIG. 16 is a photograph of a carbon black/porous PDMS pressure sensor prepared using sugar powder as a template, applied to the throat for voice recognition;
FIG. 17 is a response curve generated when a carbon black/porous PDMS pressure sensor prepared using powdered sugar as a template was placed in the throat and "Press" was emitted;
FIG. 18 is a response curve generated when a carbon black/porous PDMS pressure sensor prepared with powdered sugar as a template was attached to the throat and "Science" (Science) was issued;
FIG. 19 is a response curve generated when a carbon black/porous PDMS pressure sensor prepared with sugar powder as a template is applied to the throat and "Wave" (Wave) is emitted;
FIG. 20 is a response curve generated when a carbon black/porous PDMS pressure sensor prepared with sugar powder as a template was attached to the throat and "Paper" (Paper) was sent out.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the carbon black/porous PDMS comprises the following steps:
fully and uniformly mixing PDMS prepolymer and curing agent according to the weight ratio of 10:1, and then placing the mixture into a vacuum air extractor for degassing treatment to remove air bubbles in the mixture to form a PDMS precursor;
coating the PDMS precursor on the glass substrate to form a liquid PDMS layer;
thirdly, uniformly scattering a KCl, NaCl or powdered sugar template on the surface of the uncured PDMS by adopting a 100-mesh screen;
and fourthly, placing the PDMS coated with the KCl, NaCl or powdered sugar template in a blast drying oven for drying for 2 hours at the temperature of 80 ℃, and curing the PDMS.
Fifthly, after the curing is finished, taking the PDMS permeated with the powder template out of the air drying box and putting the PDMS into deionized water for soaking so as to dissolve the powder template. In order to accelerate the in-out speed, water is changed for 3-4 times in the middle, and the dissolution of filling particles is accelerated.
And sixthly, drying after the dissolution is finished to obtain the thin porous PDMS.
Seventhly, adding carbon black into the dimethylformamide to prepare a carbon black conductive solution, wherein the concentration of the carbon black is as follows: 1 g/L-2 g/L. The particle size of the carbon black is 30-45 nm.
And then ultrasonically oscillating the obtained carbon black conductive solution for 30 min.
Ninthly, dropping the carbon black conductive solution subjected to ultrasonic oscillation into the porous PDMS by using a liquid-moving gun, wherein the volume ratio of the carbon black conductive solution to the PDMS precursor in the step II is 8: 5. then dried on a hot plate at 110 ℃.
And ninthly, repeating the step.
The preparation method of the resistance-type flexible pressure sensor comprises the following steps:
and (3) sticking a section of aluminum foil wire to the edge of the carbon black/porous PDMS by using a small amount of silver paste, and sticking a double-sided insulating polyimide adhesive tape to the exposed area of the aluminum wire for packaging. The diameter of the aluminum foil wire is 0.5 mm.
Example 1:
the preparation method of the carbon black/porous PDMS using KCl powder as the template in the embodiment comprises the following steps:
first, 10g of the prepolymer of PDMS and 1g of the curing agent were mixed thoroughly and uniformly, and then placed in a vacuum pump for 3 minutes to perform degassing treatment, thereby removing air bubbles therein to form a PDMS precursor.
Secondly, 0.5ml of PDMS precursor is taken by a liquid transfer gun, evenly dripped on a glass substrate, kept stand for 10 minutes, and a liquid PDMS layer is formed through the automatic leveling process of liquid.
Thirdly, uniformly scattering a KCl powder template on the surface of the uncured PDMS by adopting a 100-mesh screen; a weight was then applied to the KCl powder at a pressure of 50kPa, the KCl powder was poured into PDMS, and then the excess KCl powder was shaken off.
And fourthly, placing the PDMS coated with the KCl powder template in a blast drying oven to be dried for 2 hours at the temperature of 80 ℃, and curing the PDMS.
Fifthly, after the solidification is finished, taking the PDMS permeated with the KCl powder template out of the air drying box, putting the PDMS into deionized water, soaking for 40 minutes, and leaching out the KCl powder template. Changing water 3-4 times in the midway.
Sixthly, after the dissolution is finished, the mixture is placed in a forced air drying oven for drying treatment at the temperature of 60 ℃ to obtain thin porous PDMS.
Seventhly, 0.2g of carbon black is added into 100ml of dimethylformamide to prepare a carbon black conductive solution, and the diameter of the nano-particles of the carbon black is 35 nm.
And in order to improve the dispersibility of the carbon black conductive solution, ultrasonically oscillating the obtained carbon black conductive solution for 30 min.
Ninthly, dropping 0.8 mL of the conductive solution of carbon black prepared in the step (b) into the porous PDMS by using a liquid-transferring gun, and drying the solution at 110 ℃ on a heating plate.
And ninthly, weighing.
The preparation method of the resistance-type flexible pressure sensor comprises the following steps:
and (3) sticking a section of aluminum foil wire to the edge of the carbon black/porous PDMS by using a small amount of silver paste, and sticking a double-sided insulating polyimide adhesive tape to the exposed area of the aluminum foil wire for packaging. The diameter of the aluminum foil wire is 0.5 mm. The silver paste plays a role in reducing contact resistance. The polyimide tape plays a role in packaging.
In this embodiment, a scanning electron microscope image of the porous PDMS coated with the carbon black conductive layer using KCl powder as a template is shown in fig. 1.
Example 2:
this example is different from example 1 only in the step of uniformly scattering a NaCl powder template on the surface of the uncured PDMS. The rest is the same as example 1. In this embodiment, a scanning electron microscope image of the porous PDMS coated with the carbon black conductive layer using NaCl powder as a template is shown in fig. 2.
Example 3:
this example differs from example 1 only in the step of spreading powdered template uniformly on the surface of the uncured PDMS. The rest is the same as example 1. In this embodiment, a scanning electron microscope image of the porous PDMS coated with the carbon black conductive layer using the sugar powder as the template is shown in fig. 3.
As can be seen from FIGS. 1-3, the KCl, NaCl and powdered sugar templates affect the pore size and thus the sensor sensitivity and recovery time. Wherein the apertures generated by the KCl template, the NaCl template and the powdered sugar template are respectively 70-110 μm, 200-260 μm and 350-430 μm. It can be seen that the KCl powder template produces the smallest size of pores, while the powdered powder template produces the largest size of pores. As can be seen from FIG. 8, the sensitivity of the pressure sensor made of carbon black/porous PDMS templated with KCl powder was 1.07 kPa in the range of pressure application of 0-2kPa−1The sensitivity of the pressure sensor using NaCl powder as the template was 0.86 kPa−1The sensitivity of the pressure sensor using sugar powder as a template was 0.4 kPa−1. Compared with the other two sensors, the sensor of the KCl template has smaller pores and larger specific volume ratio, when pressure is applied, the sensor with smaller pores can increase the contact area of carbon black on the surface of the pore layer, the conductivity is increased, and therefore the sensor has the highest sensitivity. As can be seen from fig. 9, the pressure sensor prepared from carbon black/porous PDMS using KCl powder as a template has the fastest fast response time, 16ms, compared to the pressure sensors of the other two templates. In addition, the recovery time of the KCl template sensor with the smallest aperture is 16ms at the fastest speed; the recovery time of the NaCl template sensor with moderate aperture is centered at 26 ms; the recovery time for the largest pore size sugar template sensor was 37ms at the slowest. As can be seen from fig. 10-20, the pressure sensor made of carbon black/porous PDMS can be used for detection of small mechanical movements and physiological signals of human body, including weak air flow blowing, swallowing, finger touch, voice, etc. Therefore, the novel pressure sensor with excellent comprehensive performance is healthyThe monitoring and wearable device has wide application prospect.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (8)

1. The preparation method of the carbon black/porous PDMS is characterized by comprising the following steps:
fully and uniformly mixing a PDMS prepolymer and a curing agent according to the weight part ratio of 10:1 to form a PDMS precursor;
coating the PDMS precursor on the glass substrate;
thirdly, uniformly coating the powder template on the uncured PDMS layer,
placing the PDMS coated with the powder template in a forced air drying oven to be dried for 2 hours at the temperature of 80 ℃;
taking the PDMS permeated with the powder template out of the forced air drying box and putting the PDMS into deionized water for soaking;
drying after soaking to obtain porous PDMS;
seventhly, adding carbon black into the dimethylformamide to prepare a carbon black conductive solution, wherein the concentration of the carbon black is 1 g/L-2 g/L; eighthly, ultrasonically oscillating the carbon black conductive solution prepared in the step seven for 30 min;
ninthly, dropping the carbon black conductive solution after ultrasonic oscillation into the porous PDMS obtained in the step (C), and drying at 110 ℃ on a heating plate to obtain the carbon black/porous PDMS.
2. The method of preparing carbon black/porous PDMS according to claim 1, further comprising the steps of: and ninthly, repeating the step.
3. The method of preparing carbon black/porous PDMS according to claim 1, characterized in that: the volume ratio of the carbon black conductive solution in the step (ninthly) to the PDMS precursor in the step (②) is 8: 5.
4. the method of preparing carbon black/porous PDMS according to claim 1, characterized in that: in the step I, the prepolymer of PDMS and the curing agent are fully and uniformly mixed and then are placed into a vacuum air extractor for degassing treatment.
5. The method of preparing carbon black/porous PDMS according to claim 1, characterized in that: the powder is one of KCl, NaCl or sugar powder.
6. The method of preparing carbon black/porous PDMS according to claim 5, characterized in that: the powder was sieved through a 100 mesh sieve.
7. The method of preparing carbon black/porous PDMS according to claim 1, characterized in that: and fifthly, changing water for 3-4 times in the soaking process.
8. Use of the carbon black/porous PDMS prepared by the method of preparation of carbon black/porous PDMS according to any one of claims 1-7 in a resistive flexible pressure sensor.
CN202110958162.6A 2021-08-20 2021-08-20 Preparation method of carbon black/porous PDMS and application of carbon black/porous PDMS in resistance-type flexible pressure sensor Pending CN113670488A (en)

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Publication number Priority date Publication date Assignee Title
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CN105708425A (en) * 2016-04-06 2016-06-29 姜凯 Development of flexible resistance type pressure transducer capable of being applied to human body pulse detection
CN107101754A (en) * 2017-03-16 2017-08-29 清华大学 Pressure sensor with porous graphene foaming structure and preparation method thereof
CN109785995A (en) * 2018-12-07 2019-05-21 深圳大学 A kind of porous, electrically conductive slurry and its preparation method and application being used to prepare flexible piezoresistive transducer
CN111256888A (en) * 2020-03-02 2020-06-09 吉林大学 Bionic multilevel structure flexible stress and strain combined sensor and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140088397A1 (en) * 2012-09-18 2014-03-27 Ki Chon Fabrication and Use of Epidermal Electrodes
CN105708425A (en) * 2016-04-06 2016-06-29 姜凯 Development of flexible resistance type pressure transducer capable of being applied to human body pulse detection
CN107101754A (en) * 2017-03-16 2017-08-29 清华大学 Pressure sensor with porous graphene foaming structure and preparation method thereof
CN109785995A (en) * 2018-12-07 2019-05-21 深圳大学 A kind of porous, electrically conductive slurry and its preparation method and application being used to prepare flexible piezoresistive transducer
CN111256888A (en) * 2020-03-02 2020-06-09 吉林大学 Bionic multilevel structure flexible stress and strain combined sensor and preparation method thereof

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段田田: "基于多孔PDMS的柔性压力传感器设计及制备" *

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