CN113831562A - Flexible sensor film containing carbon nano cup base and preparation method and application thereof - Google Patents

Flexible sensor film containing carbon nano cup base and preparation method and application thereof Download PDF

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CN113831562A
CN113831562A CN202111144588.4A CN202111144588A CN113831562A CN 113831562 A CN113831562 A CN 113831562A CN 202111144588 A CN202111144588 A CN 202111144588A CN 113831562 A CN113831562 A CN 113831562A
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carbon
flexible sensor
carbon nano
sensor film
nanocup
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CN113831562B (en
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慕春红
郭新鹏
宁婧
朱涛
刘泽军
李雨哲
简贤
尹良君
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University of Electronic Science and Technology of China
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
    • G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
    • G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00—Measuring force or stress, in general
    • G01L1/20—Measuring 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
    • G01L1/22—Measuring 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2383/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients

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Abstract

The invention provides a flexible sensor film containing a carbon nano cup base and a preparation method and application thereof, wherein the preparation method comprises the following steps: placing the catalyst in an inert gas environment, introducing acetylene gas into the inert gas environment, and reacting for 20-50min at a high temperature environment to obtain a carbon-coated catalyst material; cleaning the carbon-coated catalyst material with an acid solution to obtain a carbon nano cup; carrying out plasma treatment on the carbon nano cup; placing the obtained carbon nanocup in an organic solvent, carrying out ultrasonic treatment to obtain a mixed solution, mixing the mixed solution with a film forming agent, and carrying out magnetic stirring for 4-6 hours to obtain a mixture; and (3) preparing a membrane from the mixture and curing to obtain the flexible sensor film containing the carbon nano cup base. The flexible membrane can effectively solve the problem of low sensitivity of the existing flexible membrane.

Description

Flexible sensor film containing carbon nano cup base and preparation method and application thereof
Technical Field
The invention belongs to the technical field of flexible materials, and particularly relates to a flexible sensor film containing a carbon nano cup base, and a preparation method and application thereof.
Background
With the advent of the big data era, wearable electronic equipment stands out in the field of collection of numerous data terminals, and becomes an indispensable part of life of people. In wearable electronic device technology, flexible sensor technology is a direction with great development potential, and with the continuous refinement and development of the fields of human-computer interaction, exercise health monitoring and the like, the related products urgently require that the flexible sensor has better flexibility, recoverability, biocompatibility and the like.
Flexible strain sensors have become an object of interest to researchers at home and abroad because of their great potential for development in the field of flexible sensors. At present, carbon-based materials are often used as sensitive materials for forming flexible strain sensors due to good electrical and mechanical properties of the carbon-based materials, and the interface bonding strength between the nano materials and polymers is weak, so that the sensitivity of the carbon-based materials is reduced, and the morphology and structure of the carbon-based materials need to be regulated and controlled, so that the development of the flexible strain sensors of the composite materials at present still faces challenges.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a flexible sensor film containing a carbon nano cup base, a preparation method and application thereof, and the flexible film can effectively solve the problem of low sensitivity of the existing flexible film.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a flexible sensor film containing a carbon nano cup base comprises the following steps:
(1) putting the catalyst in an inert gas environment, introducing a carbon source gas into the inert gas environment, and reacting for 20-50min in a high-temperature environment to obtain a carbon-coated catalyst material;
(2) cleaning the carbon-coated catalyst material obtained in the step (1) with an acid solution to obtain a carbon nanocup;
(3) carrying out plasma treatment on the carbon nano cup in the step (2);
(4) placing the carbon nanocup obtained in the step (3) in an organic solvent, performing ultrasonic treatment to obtain a mixed solution, mixing the mixed solution with a film forming agent, and magnetically stirring for 4-6 hours to obtain a mixture;
(5) and (3) preparing a membrane from the mixture and curing to obtain the flexible sensor film containing the carbon nano cup base.
Further, the inert gas in the step (1) is nitrogen.
Further, the carbon source gas in the step (1) is acetylene or methane.
Further, in the step (1), the catalyst is magnesium oxide or zinc oxide.
Further, the high temperature environment in the step (1) is 650-.
Further, the specific process of the plasma treatment in the step (3) is as follows: and (3) placing the carbon nano cup in an argon environment with the temperature of 180-220 ℃, introducing induction gas to the carbon nano cup, and then carrying out plasma treatment on the carbon nano cup by using a plasma excitation source.
Furthermore, the power of the plasma excitation light source is 300-400W, and the processing time is 20-40 min.
Further, the organic solvent in the step (4) is cyclohexane or acetone.
Further, the film forming agent in the step (4) is polydimethylsiloxane.
Further, before the film preparation in the step (5), the mixture is subjected to bubble removal treatment, specifically comprising the following steps: and standing the mixture in a vacuum environment for 0.5-2 h.
Further, the curing temperature in the step (5) is 70-80 ℃, and the curing time is 2-4 h.
Further, the mass ratio of the carbon nano cup in the polydimethylsiloxane is 4-5%.
Further, the thickness of the prepared flexible sensor film is 1-2 mm.
The beneficial effects produced by the invention are as follows:
the flexible sensor film can be applied to flexible strain sensors and flexible pressure sensors, and the carbon nano-cup in the film is of a spherical hollow structure with an opening, so that the flexibility and the tensile property of the sensor are increased; the carbon nano cup is subjected to plasma treatment, so that a small amount of active functional groups are grafted on the surface of the carbon nano cup, a richer and more stable branch point contact space conductive network structure is constructed, and the response sensitivity of tunneling effect to strain in the deformation process is enhanced, so that the film can reach 25675.8 ultrahigh strain sensitivity under the strain condition of 0-20%, and the carbon nano cup has the advantage of high sensitivity.
Drawings
FIG. 1 is an SEM cross-sectional view of a flexible sensor film of example 1;
FIG. 2 is a Raman diagram of the flexible sensor film of example 1;
FIG. 3 is a pressure sensitivity test chart of the flexible sensor film of example 1;
FIG. 4 is a graph showing repeated pressure response tests of the flexible sensor film of example 1;
FIG. 5 is a tensile strain sensitivity test chart of the flexible sensor film of example 1;
FIG. 6 is an I-V curve test chart of the flexible sensor film of example 1.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings.
Example 1
A flexible sensor film containing a carbon nano cup base is prepared by the following steps:
(1) placing the catalyst in a nitrogen environment, introducing acetylene gas into the nitrogen environment, and reacting for 40min at the high temperature of 700 ℃ to obtain a carbon-coated catalyst material;
(2) cleaning the carbon-coated catalyst material obtained in the step (1) with a 30% nitric acid solution to obtain a carbon nanocup;
(3) performing plasma treatment on the carbon nano cup in the step (2), wherein the specific operation process is as follows: placing the carbon nano cup in an argon environment at 200 ℃, introducing oxygen into the carbon nano cup, and then carrying out plasma treatment on the carbon nano cup by using a plasma excitation source, wherein the power of the plasma excitation source is 350W, and the treatment time is 30 min;
(4) placing the carbon nanocup obtained in the step (3) in cyclohexane, performing ultrasonic treatment to obtain a well-dispersed mixed solution, mixing the mixed solution with polydimethylsiloxane, and magnetically stirring for 5 hours at normal temperature to obtain a mixture;
(5) the mixture is subjected to bubble removal treatment, and the specific operation is as follows: and standing the mixture in a vacuum environment for 1h, then dropwise coating the mixture on a smooth template, blade-coating the thickness of a control film by a scraper, and then curing for 3h at 75 ℃ to prepare the flexible sensor film containing the carbon nanocup base with the thickness of 2mm, wherein the mass ratio of the carbon nanocup in the polydimethylsiloxane is 4%.
Example 2
A flexible sensor film containing a carbon nano cup base is prepared by the following steps:
(1) placing the catalyst in a nitrogen environment, introducing acetylene gas into the nitrogen environment, and reacting for 50min at the high temperature of 800 ℃ to obtain a carbon-coated catalyst material;
(2) cleaning the carbon-coated catalyst material obtained in the step (1) with a 30% nitric acid solution to obtain a carbon nanocup;
(3) performing plasma treatment on the carbon nano cup in the step (2), wherein the specific operation process is as follows: placing the carbon nano cup in an argon environment at 220 ℃, introducing oxygen into the carbon nano cup, and then carrying out plasma treatment on the carbon nano cup by using a plasma excitation source, wherein the power of the plasma excitation source is 400W, and the treatment time is 40 min;
(4) placing the carbon nanocup obtained in the step (3) in cyclohexane, performing ultrasonic treatment to obtain a well-dispersed mixed solution, mixing the mixed solution with polydimethylsiloxane, and magnetically stirring for 6 hours at normal temperature to obtain a mixture;
(5) the mixture is subjected to bubble removal treatment, and the specific operation is as follows: and standing the mixture in a vacuum environment for 2h, then dropwise coating the mixture on a smooth template, blade-coating the thickness of a control film by a scraper, and then curing at 80 ℃ for 4h to prepare the flexible sensor film containing the carbon nanocup base with the thickness of 2mm, wherein the mass ratio of the carbon nanocup in the polydimethylsiloxane is 4.5%.
Example 3
A flexible sensor film containing a carbon nano cup base is prepared by the following steps:
(1) placing the catalyst in a nitrogen environment, introducing acetylene gas into the nitrogen environment, and reacting for 40min at the high temperature of 700 ℃ to obtain a carbon-coated catalyst material;
(2) cleaning the carbon-coated catalyst material obtained in the step (1) with a 30% nitric acid solution to obtain a carbon nanocup;
(3) performing plasma treatment on the carbon nano cup in the step (2), wherein the specific operation process is as follows: placing the carbon nano cup in an argon environment at 200 ℃, introducing oxygen into the carbon nano cup, and then carrying out plasma treatment on the carbon nano cup by using a plasma excitation source, wherein the power of the plasma excitation source is 350W, and the treatment time is 30 min;
(4) placing the carbon nanocup obtained in the step (3) in cyclohexane, performing ultrasonic treatment to obtain a well-dispersed mixed solution, mixing the mixed solution with polydimethylsiloxane, and magnetically stirring for 5 hours at normal temperature to obtain a mixture;
(5) the mixture is subjected to bubble removal treatment, and the specific operation is as follows: and standing the mixture in a vacuum environment for 1h, then dropwise coating the mixture on a smooth template, blade-coating the thickness of a control film by a scraper, and then curing for 3h at 75 ℃ to prepare the flexible sensor film containing the carbon nanocup base with the thickness of 2mm, wherein the mass ratio of the carbon nanocup in the polydimethylsiloxane is 5%.
Comparative example 1
On the basis of example 1, the plasma treatment of the carbon nanocup was omitted.
Comparative example 2
A flexible sensor film containing a carbon nano cup base is prepared by the following steps:
(1) placing the catalyst in a nitrogen environment, introducing acetylene gas into the nitrogen environment, and reacting for 30min at a high temperature of 650 ℃ to obtain a carbon-coated catalyst material;
(2) cleaning the carbon-coated catalyst material obtained in the step (1) with a 30% nitric acid solution to obtain a carbon nanocup;
(3) performing plasma treatment on the carbon nano cup in the step (2), wherein the specific operation process is as follows: placing the carbon nano cup in an argon environment at 180 ℃, introducing oxygen into the carbon nano cup, and then carrying out plasma treatment on the carbon nano cup by using a plasma excitation source, wherein the power of the plasma excitation source is 300W, and the treatment time is 20 min;
(4) placing the carbon nanocup obtained in the step (3) in cyclohexane, performing ultrasonic treatment to obtain a well-dispersed mixed solution, mixing the mixed solution with polydimethylsiloxane, and magnetically stirring for 4 hours at normal temperature to obtain a mixture;
(5) the mixture is subjected to bubble removal treatment, and the specific operation is as follows: and (2) standing the mixture in a vacuum environment for 0.5h, then dropwise coating the mixture on a smooth template, blade-coating the thickness of a control film by a scraper, and then curing for 2h at 70 ℃ to obtain the flexible sensor film containing the carbon nano cup base with the thickness of 1mm, wherein the mass ratio of the carbon nano cup in the polydimethylsiloxane is 8%.
Test examples
The obtained flexible sensor films of example 3 and comparative example 1 were tested separately, and the specific test procedure was as follows: the detection process is as follows: the data of the resistance is obtained through a ZQ-990 tester of smart precision instruments Inc. of Dongguan city and a digital original table of KEITHLEY Jishili 2450 series. The membrane to be tested is placed on a testing machine in an initial state without stress and strain, the stretching speed is set to be 10mm/min by using testing software on a computer, the pressure sensitivity testing speed is set to be 2mm/min, the pressure cycle testing is set to be 10mm/min, then the testing is started, the testing software obtains data in the testing process, and the testing is finished. Test data are obtained through test software, and then the data are presented in a picture form through Origin drawing software. The specific test results are shown in the attached figure and table 1.
Table 1: comparison of tensile strain sensitivity before and after plasma treatment
Sample number Adding mass ratio (wt%) of carbon nano cup Sensitivity of the probe
Example 1 4 25675.8
Example 2 4.5 16005.2
Example 3 5 14013.1
Comparative example 1 4 14564.4
Comparative example 2 8 3.8
In the table above, the data in example 1 is compared with the data in comparative example 2, and after the addition amount of the carbon nanocups is changed, the sensitivity is greatly changed, which proves that the addition amount of the carbon nanocups has a large influence on the sensor, and when the addition amount is increased, clusters occur between the carbon nanocups, thereby affecting the sensitivity; comparing the data in example 1 with that in comparative example 1, it was found that the sensitivity of the resulting film was severely degraded after the plasma treatment of the carbon nanocapsuies was cancelled.
FIG. 1 is an SEM image of a flexible sensor film containing a carbon nanocup base obtained in example 1 of the present invention; the carbon nanocapsuies are well dispersed in the polydimethylsiloxane, and the hollow carbon nanocapsuies are in point contact due to the low length-diameter ratio of the carbon nanocapsuies.
FIG. 2 is a Raman characterization diagram of the flexible sensor film containing the carbon nanocup base obtained in example 1 of the present invention, and the curves show Raman characteristic peaks corresponding to polydimethylsiloxane, which are 500, 613, 697, 2683, and 2905cm respectively-1Characteristic peak at position, and at 1350cm-1、1580cm-1The nearby peaks correspond to the D peak and the G peak of the carbon material respectively, and the ID/IG ratio of the composite flexible film is 1.05.
Fig. 3 is a pressure sensitivity test chart of the flexible sensor thin film containing the carbon nanocup base obtained in example 1 of the present invention, and thus it is seen that the flexible film exhibits better sensitivity, the change of the resistance is mainly due to the deformation of the hollow nanocarbon spheres under the action of pressure, the hollow nanocarbon spheres exist in the form of clusters, more defect states occur, the electron transmission is affected due to the increase of the defect states, and the resistance of the thin film is increased.
Fig. 4 is a repeated pressure response test chart of the flexible sensor film containing the carbon nanocup base obtained in embodiment 1 of the present invention, and it can be seen that the resistance change of the flexible film is relatively stable through 500 times of loading and unloading pressure under the condition of 200kPa of applied pressure, i.e. there is good response repeatability.
Fig. 5 is a tensile strain sensitivity test chart of the flexible sensor film containing a carbon nanocup base obtained in example 1 of the present invention. For the flexible film with the low carbon nano cup mass fraction, because dense conductive paths are not formed, the contact mode among carbon nano cup clusters is point contact, so that the flexible film has high tensile strain sensitivity, and the flexible film with the 4 wt% of carbon nano cup conductive network has the strain range of 0-11.3%, the sensitivity of 3000.5, the strain range of 11.3-16% of 8645.2 and the strain range of 16-20% of 25675.8.
Fig. 6 is an I-V curve of the flexible sensor film containing carbon nanocup base obtained in example 1 of the present invention under different strains, which shows that the flexible film has good ohmic characteristics under different strains.

Claims (10)

1. A preparation method of a flexible sensor film containing a carbon nano cup base is characterized by comprising the following steps:
(1) putting the catalyst in an inert gas environment, introducing a carbon source gas into the inert gas environment, and reacting for 20-50min in a high-temperature environment to obtain a carbon-coated catalyst material;
(2) cleaning the carbon-coated catalyst material obtained in the step (1) with an acid solution to obtain a carbon nanocup;
(3) carrying out plasma treatment on the carbon nano cup in the step (2);
(4) placing the carbon nanocup obtained in the step (3) in an organic solvent, performing ultrasonic treatment to obtain a mixed solution, mixing the mixed solution with a film forming agent, and magnetically stirring for 4-6 hours to obtain a mixture;
(5) and (3) preparing a membrane from the mixture and curing to obtain the flexible sensor film containing the carbon nano cup base.
2. The method for preparing a flexible sensor film containing a carbon nanocup according to claim 1, wherein the catalyst in the step (1) is magnesium oxide or zinc oxide.
3. The method for preparing the carbon nanocup-based flexible sensor film as claimed in claim 1, wherein the high temperature environment in the step (1) is 650-800 ℃.
4. The method for preparing a flexible sensor film containing a carbon nanocup base according to claim 1, wherein the plasma treatment in the step (3) is performed by the following steps: and (3) placing the carbon nano cup in an argon environment with the temperature of 180-220 ℃, introducing induction gas to the carbon nano cup, and then carrying out plasma treatment on the carbon nano cup by using a plasma excitation source.
5. The method as claimed in claim 4, wherein the power of the plasma excitation light source is 300-400W, and the processing time is 20-40 min.
6. The method for preparing a flexible sensor film containing a carbon nanocup according to claim 1, wherein the organic solvent in the step (4) is cyclohexane or acetone.
7. The method for preparing a flexible sensor film containing a carbon nanocup base according to claim 1, wherein the film forming agent in the step (4) is polydimethylsiloxane.
8. The method of claim 1, wherein the carbon nanocup is present in an amount of 4 to 5% by weight of the polydimethylsiloxane.
9. A flexible sensor film comprising a carbon nanocup base, characterized in that it is produced by the method according to any one of claims 1 to 9.
10. Use of the flexible sensor film comprising a carbon nanocup base as claimed in claim 9 in flexible strain sensors and flexible pressure sensors.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2012125245A (en) * 2012-06-19 2013-12-27 Федеральное государственное бюджетное учреждение науки Институт нанотехнологий микроэлектроники Российской академии наук METHOD FOR PRODUCING A PRESSURE SENSOR CONTAINING CARBON NANOTUBES
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RU2012125245A (en) * 2012-06-19 2013-12-27 Федеральное государственное бюджетное учреждение науки Институт нанотехнологий микроэлектроники Российской академии наук METHOD FOR PRODUCING A PRESSURE SENSOR CONTAINING CARBON NANOTUBES
CN110511569A (en) * 2019-07-25 2019-11-29 复旦大学 One kind is based on barbed hollow carbosphere ultra-sensitivity pressure sensing film and preparation method thereof
CN111750975A (en) * 2020-06-19 2020-10-09 电子科技大学 Flexible vibration sensor with piezoresistive effect and preparation method thereof
CN112980022A (en) * 2021-04-25 2021-06-18 电子科技大学 Porous carbon capsule base/polydimethylsiloxane composite flexible membrane and preparation method and application thereof

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