CN108613760A - A kind of preparation method and application based on graphene carbon nanotube composite membrane sensor - Google Patents

A kind of preparation method and application based on graphene carbon nanotube composite membrane sensor Download PDF

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Publication number
CN108613760A
CN108613760A CN201810268884.7A CN201810268884A CN108613760A CN 108613760 A CN108613760 A CN 108613760A CN 201810268884 A CN201810268884 A CN 201810268884A CN 108613760 A CN108613760 A CN 108613760A
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CN
China
Prior art keywords
film
composite membrane
carbon nanotube
silver electrode
polyimide film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810268884.7A
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Chinese (zh)
Inventor
吴幸
李乾昊
樊天意
田希悦
黄淳
张健
张金洁
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East China Normal University
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East China Normal University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by East China Normal University filed Critical East China Normal University
Priority to CN201810268884.7A priority Critical patent/CN108613760A/en
Publication of CN108613760A publication Critical patent/CN108613760A/en
Pending legal-status Critical Current

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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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B7/00Measuring arrangements characterised by the use of electric or magnetic techniques
    • G01B7/16Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
    • G01B7/18Measuring 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

Abstract

The invention discloses a kind of preparation method and application based on graphene carbon nanotube composite membrane sensor, compound film sensors are made using preparation graphene carbon nanotube composite membrane and with the bonding of silver electrode polyimide film in the present invention;The present invention is used selectes measurement point in the body surface to be measured, and prints resin glue holder, the compound film sensors of three pieces are pasted onto around measurement point on resin scaffold;When the object to be measured is wriggled, which is transferred to compound film sensors, monitors the variation of composite membrane sensor resistance, by calculating, you can obtains the ess-strain value of all directions of body surface to be measured, realizes the measurement to body surface ess-strain.Have the advantages that high sensitivity, measuring accuracy are high.

Description

A kind of preparation method and application based on graphene carbon nanotube composite membrane sensor
Technical field
The present invention relates to stress-strain measurement technical fields, especially a kind of to be sensed based on graphene carbon nanotube composite membrane The preparation method and application of device.
Background technology
With the development of measuring technique, the requirement to measuring technique is also higher and higher, and the range of measurement is more and more extensive, from The space of macroscopic view measures microcosmic nanometer measurement, and new material is such as emerged rapidly in large numbersBamboo shoots after a spring rain fast development in addition, is often needed in scientific experiment Relevant physical characteristic relationship between measuring environment and new material is wanted, the subtle variation of material need to be detected, for this purpose, small flexible Sensor gradually shows its unique superiority in fields of measurement.The problem is that existing conventional test measuring device is Through cannot be satisfied development in science and technology demand, using the measurement of sensor combination detecting instrument, and by computer or microcontroller into line number The favor of scientific and technological circle is obtained according to the measurement method of processing, for this purpose, going out to have for different detection environment and detection object designs Targetedly sensor will be the effective way for reducing measurement cost, improving measurement accuracy.
Invention content
One kind that the purpose of patent of the present invention is in view of the deficiencies of the prior art and provides is multiple based on graphene carbon nanotube The preparation method and application of film sensors is closed, the present invention is using preparation graphene carbon nanotube composite membrane and sub- with silver electrode polyamides Compound film sensors are made in the bonding of amine film;The present invention is used in the selected measurement dot of the body surface to be measured, and prints resin glue The compound film sensors of three pieces are pasted onto around dot is measured on resin scaffold by holder;It, should when the object to be measured is wriggled Wriggling is transferred to compound film sensors, monitors the variation of composite membrane sensor resistance, by calculating, you can obtains and is intended to measuring surface All directions ess-strain value, realize measurement to body surface ess-strain.With simple in structure, high sensitivity, survey Measure the high advantage of accuracy.
Realizing the specific technical solution of the object of the invention is:
A kind of preparation method based on graphene carbon nanotube composite membrane, feature include the following steps:
A) mixed solution, is matched
250~750 milli of 0.2~1 gram of graphene, 0.05~0.25 gram of carbon nanotube and absolute ethyl alcohol is added in beaker It rises, forms non-agitating solution;Non- agitating solution is placed in ultrasonic wave stirring instrument and is stirred, the duration 60 divides, and forms mixing Solution;
B), vacuum filtration method prepares initial film
Mixed solution is poured into above the filter paper of bottle,suction, open vacuum filtration machine, taken out in the lower section of bottle,suction filter paper true Sky, 0.098 megapascal of vacuum degree, pumpdown time 60-120 second, mixed solution form initial film in filter paper disposed thereon;
C) composite material film, is formed
The filter paper being attached in initial film is dissolved with acetone, forms composite material film;
D) silver electrode, is grown on polyimide film
Choose 0.8 × 0.4cm of polyimide film2;Acetone, absolute ethyl alcohol and deionized water is used to be cleaned by ultrasonic respectively, drying; Polyimide film is put into soak at room temperature in 4 moles of potassium hydroxide solution, the time 180 divides;It is cleaned with deionized water after taking-up, Remove the potassium ion of film surface, drying;
Polyimide film is put into 0.01~0.05 mole of silver ammino solution, soaking time 20 is divided;
It is cleaned using deionized water after taking-up, removes the silver ion of film surface;
Mask pattern is printed on polyimide film surface, and the surface of polyimide film is restored with hydrogen peroxide, it is molten with acetone Liquid memory dump ink powder forms silver electrode;The connecting wire in silver electrode, drying;Form silver electrode polyimide film;
E) graphene carbon nanotube composite membrane sensor, is formed
The composite material film that selecting step c) is formed, is cut into 0.8 × 0.4cm2Thin slice, be covered in silver electrode polyamides In imines film, composite material film and silver electrode polyimide film are bonded by high temperature resistance polyester film, form composite membrane sensing Device.
It is a kind of based on graphene carbon nanotube composite membrane sensor measure body surface strain application, specifically include as Lower step:
F), 3D printing resin material holder
Measurement point is selected in the body surface to be measured, with 3D printing resin glue, three are printed in radioactive ray along measurement point The resin glue holder that angle is 120 ° waits for resin glue holder spontaneous curing;
G) compound film sensors, are pasted
The compound film sensors of three pieces are pasted around measurement point, and the both ends of every compound film sensors is made to be pasted onto two On adjacent resin scaffold;
H), the measurement of compound film sensors
Strain detector is connected in the silver electrode of compound film sensors, applies external force, measurement point to the object to be measured And periphery is wriggled, and is wriggled and is transferred to compound film sensors through resin scaffold, compound film sensors deform and lead to resistance Value variation reads the variation of corresponding composite membrane sensor resistance by strain detector, by calculating, you can acquisition is intended to measure The ess-strain value of all directions of object measurement point.
Composite membrane is made using preparation graphene carbon nanotube composite membrane and with the bonding of silver electrode polyimide film in the present invention Sensor;The present invention is used in the selected measurement dot of the body surface to be measured, and prints resin glue holder, three pieces composite membrane is passed Sensor is pasted onto around dot is measured on resin scaffold;When the object to be measured is wriggled, which is transferred to composite membrane biography Sensor monitors the variation of composite membrane sensor resistance, by calculating, you can obtains the ess-strain for being intended to measuring surface all directions Value realizes the measurement to body surface ess-strain.Have the advantages that simple in structure, high sensitivity, measuring accuracy are high.
Description of the drawings
Fig. 1 is the measuring state schematic diagram of graphene carbon nanotube composite membrane sensor;
Fig. 2 is the front and back contrast schematic diagram of graphene carbon nanotube composite membrane sensor deformation.
Specific implementation mode
Embodiment
A kind of preparation method based on graphene carbon nanotube composite membrane, includes the following steps:
A) mixed solution, is matched
Be added in beaker 250 milliliters of 0.2 gram of graphene, 0.05 gram of carbon nanotube and absolute ethyl alcohol formed do not stir it is molten Liquid;Non- agitating solution is placed in ultrasonic wave stirring instrument and is stirred, the duration 60 divides, and forms mixed solution;
B), vacuum filtration method prepares initial film
Mixed solution is poured into above the filter paper of bottle,suction, open vacuum filtration machine, taken out in the lower section of bottle,suction filter paper true Sky, 0.098 megapascal of vacuum degree, 90 seconds pumpdown times, mixed solution form initial film in bottle,suction filter paper disposed thereon;
C) composite material film, is formed
The filter paper being attached in initial film is dissolved with acetone, forms composite material film;
D) silver electrode, is grown on polyimide film
Choose 0.8 × 0.4cm of polyimide film2;Acetone, absolute ethyl alcohol and deionized water is used to be cleaned by ultrasonic respectively, drying; Polyimide film is put into soak at room temperature in 4 moles of potassium hydroxide solution, the time 180 divides;It is cleaned with deionized water after taking-up, Remove the potassium ion of film surface, drying;
Polyimide film is put into 0.02 mole of silver ammino solution, soaking time 20 is divided;
It is cleaned using deionized water after taking-up, removes the silver ion of film surface;
Polyimide film is attached on printing paper, mask pattern is printed on polyimide film surface, is restored with hydrogen peroxide The surface of polyimide film forms silver electrode with acetone soln memory dump ink powder;The connecting wire in silver electrode, drying;Shape At silver electrode polyimide film;
E) graphene carbon nanotube composite membrane sensor, is formed
The composite material film that selecting step c) is formed, is cut into 0.8 × 0.4cm2Thin slice, be covered in silver electrode polyamides In imines film, composite material film 3 and silver electrode polyimide film 4 are bonded by high temperature resistance polyester film, composite membrane is formed and passes Sensor.
Refering to fig. 1-2, a kind of application based on graphene carbon nanotube composite membrane sensor, includes the following steps:
F), 3D printing resin material holder
In the selected measurement dot of the body surface to be measured three are printed in radioactive ray with 3D printing resin glue along dot The resin glue holder 6 that angle is 120 ° waits for 6 spontaneous curing of resin glue holder;
G) compound film sensors, are pasted
The compound film sensors 5 of three pieces are pasted around dot is measured, and the both ends of every compound film sensors is made to be pasted onto On two adjacent resin scaffolds 6;
H), the measurement of compound film sensors
Strain detector is connected in the silver electrode of compound film sensors 5, applies external force to the object to be measured, at this point, It measures dot periphery to wriggle, which is transferred to compound film sensors 5 through resin scaffold 6, and compound film sensors 5 become Shape leads to resistance change, the variation of corresponding compound 5 resistance value of film sensors is read by strain detector, by calculating, i.e., The ess-strain value that can get measuring surface circle all directions to be measured, is completed using the measurement process of compound film sensors.
Plane stress measures and Computing Principle:
Three deformation values ε that the compound film sensors of three pieces are measureda, εb, εcSubstitute into following equation group:
It solves
εxAnd εyTwo quadrature components of the stress on x/y plane, this three determine object on x/y plane by Final stress size and direction.

Claims (3)

1. a kind of preparation method based on graphene carbon nanotube composite membrane sensor, which is characterized in that this method includes as follows Step:
a), prepare mixed solution
250~750 milliliters of 0.2~1 gram of graphene, 0.05~0.25 gram of carbon nanotube and absolute ethyl alcohol, shape are added in beaker At non-agitating solution;Non- agitating solution is placed in ultrasonic wave stirring instrument and is stirred, the duration 60 divides, and forms mixed solution;
b), vacuum filtration method prepare initial film
Mixed solution is poured into above the filter paper of bottle,suction, opens vacuum filtration machine, vacuumized below bottle,suction filter paper, very 0.098 megapascal of reciprocal of duty cycle, pumpdown time 60-120 second, mixed solution form initial film in filter paper disposed thereon;
c), formed composite material film
The filter paper being attached in initial film is dissolved with acetone, forms composite material film;
d), silver electrode is grown on polyimide film
A piece of polyimide film is chosen, uses acetone, absolute ethyl alcohol and deionized water to be cleaned by ultrasonic respectively, drying;By polyimides Film is put into soak at room temperature in 4 moles of potassium hydroxide solution, and the time 180 divides;It is cleaned with deionized water after taking-up, removes film surface Potassium ion, drying;
Polyimide film is put into 0.01~0.05 mole of silver ammino solution, soaking time 20 is divided;
It is cleaned using deionized water after taking-up, removes the silver ion of film surface;
Mask pattern is printed on polyimide film surface, and the surface of polyimide film is restored with hydrogen peroxide, it is clear with acetone soln Except printing ink powder forms silver electrode;The connecting wire in silver electrode, drying;Form silver electrode polyimide film;
e), formed graphene carbon nanotube composite membrane sensor
Selecting step c)The composite material film of formation is cut into identical as silver electrode polyimide film size;It is covered in silver-colored electricity On the polyimide film of pole, composite material film and silver electrode polyimide film are bonded by high temperature resistance polyester film, described in formation Compound film sensors.
2. a kind of application strained in measurement body surface based on graphene carbon nanotube composite membrane sensor.
3. application according to claim 2, which is characterized in that the application includes step in detail below:
a), 3D printing resin material holder
Measurement point is selected in the body surface to be measured, with 3D printing resin glue, three resins are printed in radioactive ray along measurement point Glue holder waits for resin glue holder spontaneous curing;
b), paste compound film sensors
By the compound film sensors of three pieces around measurement point paste, and make the both ends of every compound film sensors be pasted onto two it is adjacent Resin scaffold on;
c), compound film sensors measurement
Strain detector is connected in the silver electrode of compound film sensors, applies external force, measurement point and week to the object to be measured Side is wriggled, and is wriggled and is transferred to compound film sensors through resin scaffold, compound film sensors deform and resistance value is caused to become Change, the variation of corresponding composite membrane sensor resistance is read by strain detector, by calculating, you can obtain the object to be measured The ess-strain value of all directions of body surface planar survey point.
CN201810268884.7A 2018-03-29 2018-03-29 A kind of preparation method and application based on graphene carbon nanotube composite membrane sensor Pending CN108613760A (en)

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Application Number Priority Date Filing Date Title
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010017409A1 (en) * 2008-08-07 2010-02-11 The Trustees Of Columbia University In The City Of New York Force, pressure, or stiffness measurement or calibration using graphene or other sheet membrane
CN103219066A (en) * 2012-01-19 2013-07-24 中国科学院上海硅酸盐研究所 Flexible conductive thin film compositing two-dimensional graphene and one-dimensional nanowire and preparation method thereof
CN105021329A (en) * 2015-07-22 2015-11-04 上海交通大学 Resistor-type pressure sensor and making method thereof
CN105869719A (en) * 2016-05-24 2016-08-17 重庆大学 PET-graphene-AgNW (polyethylene terephthalate-graphene-Ag nanowire) composite transparent conducting film and preparation method thereof
CN106045515A (en) * 2016-06-01 2016-10-26 斯迪克新型材料(江苏)有限公司 Preparation method of graphene-polyimide composite heat conducting film
CN106531733A (en) * 2016-12-21 2017-03-22 清华大学 Flexible pressure sensor and preparation method therefor
CN107219028A (en) * 2017-05-05 2017-09-29 华东师范大学 A kind of preparation method of the flexible wireless pressure detecting system based on inkjet technology
CN107655598A (en) * 2017-09-12 2018-02-02 电子科技大学 Flexibility stress sensor based on CNT and nano silver wire composite conductive thin film

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010017409A1 (en) * 2008-08-07 2010-02-11 The Trustees Of Columbia University In The City Of New York Force, pressure, or stiffness measurement or calibration using graphene or other sheet membrane
CN103219066A (en) * 2012-01-19 2013-07-24 中国科学院上海硅酸盐研究所 Flexible conductive thin film compositing two-dimensional graphene and one-dimensional nanowire and preparation method thereof
CN105021329A (en) * 2015-07-22 2015-11-04 上海交通大学 Resistor-type pressure sensor and making method thereof
CN105869719A (en) * 2016-05-24 2016-08-17 重庆大学 PET-graphene-AgNW (polyethylene terephthalate-graphene-Ag nanowire) composite transparent conducting film and preparation method thereof
CN106045515A (en) * 2016-06-01 2016-10-26 斯迪克新型材料(江苏)有限公司 Preparation method of graphene-polyimide composite heat conducting film
CN106531733A (en) * 2016-12-21 2017-03-22 清华大学 Flexible pressure sensor and preparation method therefor
CN107219028A (en) * 2017-05-05 2017-09-29 华东师范大学 A kind of preparation method of the flexible wireless pressure detecting system based on inkjet technology
CN107655598A (en) * 2017-09-12 2018-02-02 电子科技大学 Flexibility stress sensor based on CNT and nano silver wire composite conductive thin film

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Application publication date: 20181002