CN107036741B - A kind of preparation method of the graphene-based pressure sensor of selfreparing - Google Patents
A kind of preparation method of the graphene-based pressure sensor of selfreparing Download PDFInfo
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- 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
- G01L1/18—Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/34—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids using polymerised unsaturated fatty acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
- G01L9/06—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning of piezo-resistive devices
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
- C08J2377/08—Polyamides derived from polyamines and polycarboxylic acids from polyamines and polymerised unsaturated fatty acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/0806—Silver
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
Abstract
The invention discloses a kind of preparation methods of the graphene-based pressure sensor of selfreparing.The conductive elastomer with self-repair function is made by the way that graphene@silver nanowires composite electric conductor is added in selfreparing macromolecule matrix in the present invention；Then the selfreparing conductive elastomer is packaged into pressure sensor.The present invention solves the electric conductivity of traditional selfreparing conductive polymer material and self-healing properties are difficult to the contradictory problems optimized simultaneously.The invention has the following advantages that being not necessarily to drying and processing in the post-processing of 1, graphene@silver nanowires composite electric conductor, the hard aggregation problem of graphene@silver nanowires can be reduced；2, graphene@silver nanowires composite electric conductor is more likely formed three-dimensional crosslinked network structure in selfreparing macromolecule matrix；3, the graphene-based pressure sensor of selfreparing has the advantages that the service life is long, electric conductivity is high, high sensitivity.
Description
Technical field
The present invention relates to intelligent macromolecule fields, more particularly, to a kind of graphene-based pressure sensor of selfreparing
Preparation method.
Background technique
In recent years, with the rapid development of wearable electronic, flexible electronic device is in medical instrument, the energy, information, industry
Equal fields show huge application prospect.Wherein, pliable pressure sensor is that extraneous force signal is changed into electric signal
A kind of electronic device, is widely applied.However, traditional pliable pressure sensor is by external world, itself fatigue, old
After change, pressure sensor loses its basic sensing function, the serious service life and stability for reducing equipment.Therefore, it develops
A kind of pliable pressure sensor with self-repair function has great importance out.
Selfreparing pliable pressure sensor, domestic and international researcher have conducted extensive research in sensing unit in order to obtain.Example
Such as, Xiamen University Weng Wengui, Xia Haiping seminar devises two kinds of monomers with carbamate and carries out free-radical polymerized
Obtain a kind of super molecular compound of selfreparing.Then superconductive carbon black is compounded with selfreparing macromolecule, obtains one kind
Semiconductor of the conductivity up to 1 s/cm.Bao Zhenan seminar, Stanford Univ USA is prepared for a kind of electricity with self-healing properties
Pole material.This material is that will there is the polymer of self-healing properties to carry out that realization is blended with conductive particle.Utilize hydrogen bond
Reversible dynamic, material are not necessarily to that the multiple mechanics of room temperature and electricity selfreparing can be achieved under conditions of outside agent.S. A. Odom
Deng then having studied a kind of electric conductivity microcapsules, this microcapsules are implanted into material matrix.After material is destroyed, conduction liquid
Body or solvent are ruptured from microcapsules, to realize that the redoubling of reviewing one's lessons by oneself of material is able to maintain its electric property.
But existing selfreparing conductive polymer material, in order to realize high conduction performance, often by macromolecule
A large amount of conductive particles are filled in matrix.These conductive particles it is a large amount of introducing necessarily cause high molecular self-healing properties substantially under
Drop.These problems greatly limit subsequent preparation selfreparing pressure sensor.Therefore, the low addition number of one kind, electric conductivity are studied
A kind of preparation method for selfreparing pressure sensor that energy is good and self-healing properties are high is necessary.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of the graphene-based pressure sensor of selfreparing.This method solves
Existing pressure sensor is unable to the problem of selfreparing and selfreparing conducting polymer electric conductivity and self-healing properties can not be same
The problem of Shi Tigao, and a kind of graphene-based pressure sensor preparation method of selfreparing is provided.Before the application of huge market
Scape and good economic and social benefits.
To achieve the above object of the invention, the technical solution adopted by the present invention is that: a kind of graphene-based pressure sensing of selfreparing
The preparation method of device, comprising the following steps:
1) one-dimensional silver nanowires material is prepared
A) ethylene glycol pre-processes: the ethylene glycol of 50~100 mL being added in three-necked flask and is sufficiently added at 150~170 DEG C
Heat 10~30 minutes；
B) the NaCl aqueous solution for measuring 1~4 mL is added in the solution that step a) is formed, and heats 10~15 minutes；NaCl water
Solution concentration is 0.002~0.004 mol/L；
C) a certain amount of silver nitrate is dissolved in ethylene glycol, forms the silver nitrate solution of 0.3~0.5 mol/L；It will be a certain amount of
Polyvinyl pyrrolidone (PVP) is dissolved in ethylene glycol, forms the PVP solution of 0.4~0.6 mol/L；Take 10~15 mL silver nitrates molten
Liquid is added in the mixed solution of step b) formation, while the PVP solution of 30~45mL being taken to be slowly dropped by peristaltic pump, the time
Control is in 50~90 minutes；
D) after completion of dropwise addition, the reaction solution that step c) is obtained, which takes out, to be stood to room temperature；Then by reaction solution 9000
It is centrifuged 10 minutes under rpm and is cleaned multiple times with deionized water and dehydrated alcohol, finally obtain powdery product；
2) graphene@silver nanowires composite electric conductor is prepared
A) first a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, obtaining expanded graphite concentration is 0.1 ~ 0.9 mg/mL's
Disperse solution, after ultrasonic disperse 14 ~ 20 hours, so that whole expanded graphites is formed graphene dispersing solution, by above-mentioned graphene dispersion
Liquid is centrifuged 30 min at 8000 rpm, and taking upper liquid is stable graphene organic solution；The above-mentioned carboxymethyl used is fine
The mass ratio of dimension element or hydroxyethyl cellulose and expanded graphite is 5:1 ~ 10:1；Solvent is acetone, ethyl alcohol, tetrahydrofuran, two
One or more of chloromethanes mixture；
B) 1) silver nanowires obtained in is added in stable graphene organic solution, with the machine of 500 rpm/min
Tool mixing speed stirs 2 ~ 6 hours, and further graphene@silver nanowires composite electric conductor can be obtained after 3 hours in ultrasound；Make
Expanded graphite and the mass ratio of silver nanowires are 1:15 ~ 4:1；
3) the graphene-based high molecular material of selfreparing is prepared
A) macromolecule prepolymer: a certain amount of dimeric dibasic acid and diethylenetriamine is taken to be put into three-necked flask, with nitrogen as guarantor
Gas is protected, is heated to 150 ~ 170 DEG C, mechanical stirring is reacted 20 ~ 26 hours, and macromolecule prepolymer is formed；Wherein dimeric dibasic acid and two
The mass ratio of ethylene triamine is 2:1 ~ 3:1；
B) above-mentioned macromolecule prepolymer is added to formation methylene chloride mixed solution in methylene chloride, the two mass ratio 1:
1~1:5；Then the graphene@silver nanowires composite electric conductor in 2) is added in above-mentioned methylene chloride mixed solution；Then
A certain amount of methanol and distilled water is added, is sufficiently stirred, is then allowed to stand 12 hours；Subnatant is taken out and is heated in 50 DEG C of baking ovens
Obtain final mixture within 48 hours；The gross mass and macromolecule prepolymer mass ratio of graphene@silver nanowires composite electric conductor are 0
~55:100；Methylene chloride, methanol, water volume ratio be 3:1:2；
C) a certain amount of urea is weighed, in the final mixture that the step b) being added to after purifying is obtained, at 130 ~ 145 DEG C
Under be crosslinked, the time 2 ~ 12 hours, the graphene-based high molecular material of selfreparing can be obtained；Urea and macromolecule prepolymer
Mass ratio is 5:100 ~ 20:100；
D) the graphene-based high molecular material of selfreparing in step c) is subjected to molded curing film forming with mold；Solidification temperature
160 DEG C, curing time 2 hours, 5 ~ 200 microns of film thickness；
4) the graphene-based pressure sensor package of selfreparing
A) the graphene-based macromolecule membrane upper and lower surface of selfreparing obtained in step 3) d) is plated into conductive metal respectively
Film, and drawn with conducting wire；Conductive metal film is gold, silver, platinum or copper, and metal layer thickness is 10 ~ 200 microns；Conducting wire is silver
Nano wire, nanowires of gold or copper nano-wire, diameter of wire are 10 ~ 1000 microns；
B) protection packaging is carried out with flexible cover sheet in the product upper and lower surfaces that step 4) a) is obtained, flexible cover sheet's
With a thickness of 10 ~ 2500 microns；Flexible cover sheet is dimethyl silicone polymer, polyethylene or polyethylene terephthalate.
A kind of preparation method of the graphene-based pressure sensor of selfreparing, it is characterised in that in step 2 a) used in surpass
The power of sound is 90 W.
The graphene-based pressure sensor of selfreparing of the invention can be used for detecting curved because of its excellent sensitivity and stability
The milli machines power such as Qu Li, twisting resistance can be used for detecting human pulse to the pressure of vascular wall, can be used for detecting sound wave shake
It is dynamic.
Due to the above technical solutions, the present invention has the following advantages over the prior art: (1) with silver nanowires with
Graphene carries out compound obtained graphene@silver nanowires composite electric conductor, not only electric conductivity with higher, but also final
Electric conductor is not necessarily to drying and processing, and contained reagent can be directly applied in subsequent macromolecule combination process, reduce graphene@silver and receive
The hard aggregation problem of rice noodles；(2) it by the way that graphene@silver nanowires composite electric conductor is added into macromolecule performed polymer, can be formed
Three-dimensional crosslinked network structure, and the loading of graphene@silver nanowires and three-dimensional net structure controllability are more preferable；(3) silver is received
After rice noodles intercalation enters graphene synusia, the defect part of the low-level oxidation layer on silver nanowires surface and graphene will with it is polymer-based
Body forms new hydrogen bond, improves the high molecular mechanical property of selfreparing graphene conductive.
Specific embodiment
The present invention will be further described below with reference to examples:
Embodiment one
A kind of preparation method of the graphene-based pressure sensor of selfreparing, comprising the following steps:
1) one-dimensional silver nanowires material is prepared
A) ethylene glycol pre-processes: the ethylene glycol of 50 mL being added in three-necked flask and is sufficiently heated 10 minutes at 150 DEG C；
B) the NaCl aqueous solution for measuring 1 mL is added in the solution that step a) is formed, and heats 10 minutes；NaCl aqueous solution is dense
Degree is 0.002 mol/L；
C) 10 g silver nitrates are dissolved in ethylene glycol, form the silver nitrate solution of 0.3 mol/L；By 15 g polyvinyl pyrroles
Ketone (PVP) is dissolved in ethylene glycol, forms the PVP solution of 0.4 mol/L；It takes 10 mL silver nitrate solutions to be added to step b) to be formed
Mixed solution in, while the PVP solution of 30 mL being taken to be slowly dropped by peristaltic pump, the time controlled in 50 minutes；
D) after completion of dropwise addition, the reaction solution that step c) is obtained, which takes out, to be stood to room temperature；Then by reaction solution 9000
It is centrifuged 10 minutes under rpm and is cleaned multiple times with deionized water and dehydrated alcohol, finally obtain powdery product；
2) graphene@silver nanowires composite electric conductor is prepared
A) first a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, obtains the dispersion that expanded graphite concentration is 0.1 mg/mL
Solution after ultrasonic disperse 14 hours, makes whole expanded graphites form graphene dispersing solution, by above-mentioned graphene dispersing solution 8000
30 min are centrifuged under rpm, taking upper liquid is stable graphene organic solution；The above-mentioned carboxymethyl cellulose or hydroxyl used
The mass ratio of ethyl cellulose and expanded graphite is 5:1；Solvent is acetone；
B) 1) silver nanowires obtained in is added in stable graphene organic solution, with the machine of 500 rpm/min
Tool mixing speed stirs 2 hours, and further graphene@silver nanowires composite electric conductor can be obtained after 3 hours in ultrasound；It uses
Expanded graphite and silver nanowires mass ratio be 1:15；
3) the graphene-based high molecular material of selfreparing is prepared
A) macromolecule prepolymer: 10 g dimeric dibasic acids and 5 g diethylenetriamines are taken to be put into three-necked flask, with nitrogen as guarantor
Gas is protected, is heated to 150 DEG C, mechanical stirring is reacted 20 hours, and macromolecule prepolymer is formed；Wherein dimeric dibasic acid and divinyl three
The mass ratio of amine is 2:1；
B) above-mentioned macromolecule prepolymer is added to formation methylene chloride mixed solution in methylene chloride, the two mass ratio 1:
1；Then the graphene@silver nanowires composite electric conductor in 2) is added in above-mentioned methylene chloride mixed solution；Then it is added
A certain amount of methanol and distilled water, are sufficiently stirred, and are then allowed to stand 12 hours；Subnatant is taken out and in 50 DEG C of baking ovens heating it is 48 small
When；The gross mass and macromolecule prepolymer mass ratio of graphene@silver nanowires composite electric conductor are 15:100；Methylene chloride, first
Alcohol, water volume ratio be 3:1:2；
C) 0.75 urea is weighed, the final mixture that the step b) being added to after purifying is obtained is handed at 130 DEG C
The graphene-based high molecular material of selfreparing can be obtained in connection, time 2 h；The mass ratio of urea and macromolecule prepolymer is 5:
100；
D) the graphene-based high molecular material of selfreparing in step c) is subjected to molded curing film forming with mold.Solidification temperature
160 DEG C, curing time 2 hours, 5 microns of film thickness；
4) the graphene-based pressure sensor package of selfreparing
A) the graphene-based macromolecule membrane upper and lower surface of selfreparing obtained in step 3) d) is plated into conductive metal respectively
Film, and drawn with conducting wire；Conductive metal film is gold, and metal layer thickness is 10 microns；Conducting wire is silver nanowires, diameter of wire
It is 10 microns；
B) protection packaging is carried out with flexible cover sheet in the product upper and lower surfaces that step 4) a) is obtained, flexible cover sheet's
With a thickness of 10 microns；Flexible cover sheet is polyethylene.
Embodiment two
A kind of preparation method of the graphene-based pressure sensor of selfreparing, comprising the following steps:
1) one-dimensional silver nanowires material is prepared
A) ethylene glycol pre-processes: the ethylene glycol of 60 mL being added in three-necked flask and is sufficiently heated 16 minutes at 155 DEG C；
B) the NaCl aqueous solution for measuring 1.8 mL is added in the solution that step a) is formed, and heats 10 minutes；NaCl aqueous solution
Concentration is 0.0025 mol/L；
C) 15 g silver nitrates are dissolved in ethylene glycol, form the silver nitrate solution of 0.35 mol/L；By 14 g polyethylene pyrroles
It coughs up ketone (PVP) to be dissolved in ethylene glycol, forms the PVP solution of 0.48 mol/L；13 mL silver nitrate solutions are taken to be added to step b) shape
At mixed solution in, while the PVP solution of 35 mL being taken to be slowly dropped by peristaltic pump, the time controlled in 65 minutes；
D) after completion of dropwise addition, the reaction solution that step c) is obtained, which takes out, to be stood to room temperature；Then by reaction solution 9000
It is centrifuged 10 minutes under rpm and is cleaned multiple times with deionized water and dehydrated alcohol, finally obtain powdery product；
2) graphene@silver nanowires composite electric conductor is prepared
A) first a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, obtains the dispersion that expanded graphite concentration is 0.3 mg/mL
Solution after ultrasonic disperse 16 hours, makes whole expanded graphites form graphene dispersing solution, by above-mentioned graphene dispersing solution 8000
30 min are centrifuged under rpm, taking upper liquid is stable graphene organic solution；The above-mentioned carboxymethyl cellulose or hydroxyl used
The mass ratio of ethyl cellulose and expanded graphite is 6:1；Solvent is ethyl alcohol；
B) 1) silver nanowires obtained in is added in stable graphene organic solution, with the machine of 500 rpm/min
Tool mixing speed stirs 3 hours, and further graphene@silver nanowires composite electric conductor can be obtained after 3 hours in ultrasound；It uses
Expanded graphite and silver nanowires mass ratio be 1:1；
3) the graphene-based high molecular material of selfreparing is prepared
A) macromolecule prepolymer: 12 g dimeric dibasic acids and 6 g diethylenetriamines are taken to be put into three-necked flask, with nitrogen as guarantor
Gas is protected, is heated to 155 DEG C, mechanical stirring is reacted 24 hours, and macromolecule prepolymer is formed；Wherein dimeric dibasic acid and divinyl three
The mass ratio of amine is 2:1；
B) above-mentioned macromolecule prepolymer is added to formation methylene chloride mixed solution in methylene chloride, the two mass ratio 1:
1.5；Then the graphene@silver nanowires composite electric conductor in 2) is added in above-mentioned methylene chloride mixed solution；Then plus
Enter a certain amount of methanol and distilled water, be sufficiently stirred, is then allowed to stand 12 hours；Subnatant is taken out and heats 48 in 50 DEG C of baking ovens
Hour；The gross mass and macromolecule prepolymer mass ratio of graphene@silver nanowires composite electric conductor are 20:100；Methylene chloride,
Methanol, water volume ratio be 3:1:2；
C) urea of 1.44 g is weighed, the final mixture that the step b) being added to after purifying is obtained carries out at 135 DEG C
Crosslinking, the time 4 hours, can be obtained the graphene-based high molecular material of selfreparing；The mass ratio of urea and macromolecule prepolymer is
8:100；
D) the graphene-based high molecular material of selfreparing in step c) is subjected to molded curing film forming with mold.Solidification temperature
160 DEG C, curing time 2 hours, 25 microns of film thickness；
4) the graphene-based pressure sensor package of selfreparing
A) the graphene-based macromolecule membrane upper and lower surface of selfreparing obtained in step 3) d) is plated into conductive metal respectively
Film, and drawn with conducting wire；Conductive metal film is silver, and metal layer thickness is 25 microns；Conducting wire is nanowires of gold, diameter of wire
It is 100 microns；
B) protection packaging is carried out with flexible cover sheet in the product upper and lower surfaces that step 4) a) is obtained, flexible cover sheet's
With a thickness of 800 microns；Flexible cover sheet is dimethyl silicone polymer.
Embodiment three
A kind of preparation method of the graphene-based pressure sensor of selfreparing, comprising the following steps:
1) one-dimensional silver nanowires material is prepared
A) ethylene glycol pre-processes: the ethylene glycol of 70 mL being added in three-necked flask and is sufficiently heated 25 minutes at 160 DEG C；
B) the NaCl aqueous solution for measuring 2 mL is added in the solution that step a) is formed, and heats 12 minutes；NaCl aqueous solution is dense
Degree is 0.003 mol/L；
C) 8 g silver nitrates are dissolved in ethylene glycol, form the silver nitrate solution of 0.4 mol/L；By 20 g polyvinyl pyrroles
Ketone (PVP) is dissolved in ethylene glycol, forms the PVP solution of 0.5 mol/L；It takes 15 mL silver nitrate solutions to be added to step b) to be formed
Mixed solution in, while the PVP solution of 30 mL being taken to be slowly dropped by peristaltic pump, the time controlled in 70 minutes；
D) after completion of dropwise addition, the reaction solution that step c) is obtained, which takes out, to be stood to room temperature；Then by reaction solution 9000
It is centrifuged 10 minutes under rpm and is cleaned multiple times with deionized water and dehydrated alcohol, finally obtain powdery product；
2) graphene@silver nanowires composite electric conductor is prepared
A) first a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, obtains the dispersion that expanded graphite concentration is 0.5 mg/mL
Solution after ultrasonic disperse 18 hours, makes whole expanded graphites form graphene dispersing solution, by above-mentioned graphene dispersing solution 8000
30 min are centrifuged under rpm, taking upper liquid is stable graphene organic solution；The above-mentioned carboxymethyl cellulose or hydroxyl used
The mass ratio of ethyl cellulose and expanded graphite is 7:1；Solvent is tetrahydrofuran；
B) 1) silver nanowires obtained in is added in stable graphene organic solution, with the machine of 500 rpm/min
Tool mixing speed stirs 4 hours, and further graphene@silver nanowires composite electric conductor can be obtained after 3 hours in ultrasound；It uses
Expanded graphite and silver nanowires mass ratio be 2:1；
3) the graphene-based high molecular material of selfreparing is prepared
A) macromolecule prepolymer: 15 g dimeric dibasic acids and 5 g diethylenetriamines are taken to be put into three-necked flask, with nitrogen as guarantor
Gas is protected, is heated to 165 DEG C, mechanical stirring is reacted 22 hours, and macromolecule prepolymer is formed；Wherein dimeric dibasic acid and divinyl three
The mass ratio of amine is 3:1；
B) above-mentioned macromolecule prepolymer is added to formation methylene chloride mixed solution in methylene chloride, the two mass ratio 1:
2；Then the graphene@silver nanowires composite electric conductor in 2) is added in above-mentioned methylene chloride mixed solution；Then it is added
A certain amount of methanol and distilled water, are sufficiently stirred, and are then allowed to stand 12 hours；Subnatant is taken out and in 50 DEG C of baking ovens heating it is 48 small
When；The gross mass and macromolecule prepolymer mass ratio of graphene@silver nanowires composite electric conductor are 25:100；Methylene chloride, first
Alcohol, water volume ratio be 3:1:2；
C) urea of 2 g is weighed, the final mixture that the step b) being added to after purifying is obtained is handed at 140 DEG C
Connection, the time 6 hours, can be obtained the graphene-based high molecular material of selfreparing；The mass ratio of urea and macromolecule prepolymer is 10:
100；
D) the graphene-based high molecular material of selfreparing in step c) is subjected to molded curing film forming with mold.Solidification temperature
160 DEG C, curing time 2 hours, 50 microns of film thickness；
4) the graphene-based pressure sensor package of selfreparing
A) the graphene-based macromolecule membrane upper and lower surface of selfreparing obtained in step 3) d) is plated into conductive metal respectively
Film, and drawn with conducting wire；Conductive metal film is platinum, and metal layer thickness is 50 microns；Conducting wire is copper nano-wire, diameter of wire
It is 350 microns；
B) protection packaging is carried out with flexible cover sheet in the product upper and lower surfaces that step 4) a) is obtained, flexible cover sheet's
With a thickness of 1000 microns；Flexible cover sheet is polyethylene terephthalate.
Example IV
A kind of preparation method of the graphene-based pressure sensor of selfreparing, comprising the following steps:
1) one-dimensional silver nanowires material is prepared
A) ethylene glycol pre-processes: the ethylene glycol of 85 mL being added in three-necked flask and is sufficiently heated 25 minutes at 165 DEG C；
B) the NaCl aqueous solution for measuring 3 mL is added in the solution that step a) is formed, and heats 13 minutes；NaCl aqueous solution is dense
Degree is 0.0035 mol/L；
C) 6 g silver nitrates are dissolved in ethylene glycol, form the silver nitrate solution of 0.45 mol/L；By 20 g polyvinyl pyrroles
Ketone (PVP) is dissolved in ethylene glycol, forms the PVP solution of 0.55 mol/L；It takes 15 mL silver nitrate solutions to be added to step b) to be formed
Mixed solution in, while the PVP solution of 40 mL being taken to be slowly dropped by peristaltic pump, the time controlled in 80 minutes；
D) after completion of dropwise addition, the reaction solution that step c) is obtained, which takes out, to be stood to room temperature；Then by reaction solution 9000
It is centrifuged 10 minutes under rpm and is cleaned multiple times with deionized water and dehydrated alcohol, finally obtain powdery product；
2) graphene@silver nanowires composite electric conductor is prepared
A) first a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, obtains the dispersion that expanded graphite concentration is 0.7 mg/mL
Solution after ultrasonic disperse 19 hours, makes whole expanded graphites form graphene dispersing solution, by above-mentioned graphene dispersing solution 8000
30 min are centrifuged under rpm, taking upper liquid is stable graphene organic solution；The above-mentioned carboxymethyl cellulose or hydroxyl used
The mass ratio of ethyl cellulose and expanded graphite is 8:1；Solvent is methylene chloride；
B) 1) silver nanowires obtained in is added in stable graphene organic solution, with the machine of 500 rpm/min
Tool mixing speed stirs 5 hours, and further graphene@silver nanowires composite electric conductor can be obtained after 3 hours in ultrasound；It uses
Expanded graphite and silver nanowires mass ratio be 3:1；
3) the graphene-based high molecular material of selfreparing is prepared
A) macromolecule prepolymer: taking 25 g dimeric dibasic acids and 10 g diethylenetriamines to be put into three-necked flask, with nitrogen as
Protective gas is heated to 165 DEG C, and mechanical stirring is reacted 24 hours, forms macromolecule prepolymer；Wherein dimeric dibasic acid and divinyl
The mass ratio of triamine is 3:1；
B) above-mentioned macromolecule prepolymer is added to formation methylene chloride mixed solution in methylene chloride, the two mass ratio 1:
3；Then the graphene@silver nanowires composite electric conductor in 2) is added in above-mentioned methylene chloride mixed solution；Then it is added
A certain amount of methanol and distilled water, are sufficiently stirred, and are then allowed to stand 12 hours；Subnatant is taken out and in 50 DEG C of baking ovens heating it is 48 small
When；The gross mass and macromolecule prepolymer mass ratio of graphene@silver nanowires composite electric conductor are 30:100；Methylene chloride, first
Alcohol, water volume ratio be 3:1:2；
C) urea of 5.25 g is weighed, the final mixture that the step b) being added to after purifying is obtained carries out at 145 DEG C
Crosslinking, the time 8 hours, can be obtained the graphene-based high molecular material of selfreparing；The mass ratio of urea and macromolecule prepolymer is
15:100；
D) the graphene-based high molecular material of selfreparing in step c) is subjected to molded curing film forming with mold.Solidification temperature
160 DEG C, curing time 2 hours, 100 microns of film thickness；
4) the graphene-based pressure sensor package of selfreparing
A) the graphene-based macromolecule membrane upper and lower surface of selfreparing obtained in step 3) d) is plated into conductive metal respectively
Film, and drawn with conducting wire；Conductive metal film is copper, and metal layer thickness is 100 microns；Conducting wire is silver nanowires, and conducting wire is straight
Diameter is 700 microns；
B) protection packaging is carried out with flexible cover sheet in the product upper and lower surfaces that step 4) a) is obtained, flexible cover sheet's
With a thickness of 2000 microns；Flexible cover sheet is dimethyl silicone polymer.
Embodiment five
A kind of preparation method of the graphene-based pressure sensor of selfreparing, comprising the following steps:
1) one-dimensional silver nanowires material is prepared
A) ethylene glycol pre-processes: the ethylene glycol of 100 mL being added in three-necked flask and is sufficiently heated 30 minutes at 170 DEG C；
B) the NaCl aqueous solution for measuring 4 mL is added in the solution that step a) is formed, and heats 15 minutes；NaCl aqueous solution is dense
Degree is 0.004 mol/L；
C) 13 g silver nitrates are dissolved in ethylene glycol, form the silver nitrate solution of 0.5 mol/L；By 25 g polyvinyl pyrroles
Ketone (PVP) is dissolved in ethylene glycol, forms the PVP solution of 0.6 mol/L；It takes 14 mL silver nitrate solutions to be added to step b) to be formed
Mixed solution in, while the PVP solution of 45 mL being taken to be slowly dropped by peristaltic pump, the time controlled in 90 minutes；
D) after completion of dropwise addition, the reaction solution that step c) is obtained, which takes out, to be stood to room temperature；Then by reaction solution 9000
It is centrifuged 10 minutes under rpm and is cleaned multiple times with deionized water and dehydrated alcohol, finally obtain powdery product；
2) graphene@silver nanowires composite electric conductor is prepared
A) first a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, obtains the dispersion that expanded graphite concentration is 0.9 mg/mL
Solution after ultrasonic disperse 20 hours, makes whole expanded graphites form graphene dispersing solution, by above-mentioned graphene dispersing solution 8000
30 min are centrifuged under rpm, taking upper liquid is stable graphene organic solution；The above-mentioned carboxymethyl cellulose or hydroxyl used
The mass ratio of ethyl cellulose and expanded graphite is 10:1；Solvent is that methylene chloride and ethyl alcohol are mixed according to what volume ratio 2:1 was obtained
Close solution；
B) 1) silver nanowires obtained in is added in stable graphene organic solution, with the machine of 500 rpm/min
Tool mixing speed stirs 6 hours, and further graphene@silver nanowires composite electric conductor can be obtained after 3 hours in ultrasound；It uses
Expanded graphite and silver nanowires mass ratio be 4:1；
3) the graphene-based high molecular material of selfreparing is prepared
A) macromolecule prepolymer: taking 30 g dimeric dibasic acids and 10 g diethylenetriamines to be put into three-necked flask, with nitrogen as
Protective gas is heated to 170 DEG C, and mechanical stirring is reacted 26 hours, forms macromolecule prepolymer；Wherein dimeric dibasic acid and divinyl
The mass ratio of triamine is 3:1；
B) above-mentioned macromolecule prepolymer is added to formation methylene chloride mixed solution in methylene chloride, the two mass ratio 1:
5；Then the graphene@silver nanowires composite electric conductor in 2) is added to and above-mentioned macromolecule prepolymer is added to methylene chloride
Middle formation methylene chloride mixed solution；Then a certain amount of methanol and distilled water is added, is sufficiently stirred, is then allowed to stand 12 hours；It will
Subnatant takes out and heats 48 hours in 50 DEG C of baking ovens；The gross mass and macromolecule of graphene@silver nanowires composite electric conductor
Prepolymer mass ratio is 55:100；Methylene chloride, methanol, water volume ratio be 3:1:2；
C) urea of 8 g is weighed, the final mixture that the step b) being added to after purifying is obtained is handed at 145 DEG C
Connection, the time 12 hours, can be obtained the graphene-based high molecular material of selfreparing；The mass ratio of urea and macromolecule prepolymer is
20:100；
D) the graphene-based high molecular material of selfreparing in step c) is subjected to molded curing film forming with mold.Solidification temperature
160 DEG C, curing time 2 hours, 200 microns of film thickness；
4) the graphene-based pressure sensor package of selfreparing
A) the graphene-based macromolecule membrane upper and lower surface of selfreparing obtained in step 3) d) is plated into conductive metal respectively
Film, and drawn with conducting wire；Conductive metal film is gold, and metal layer thickness is 200 microns；Conducting wire is nanowires of gold, and conducting wire is straight
Diameter is 1000 microns；
B) protection packaging is carried out with flexible cover sheet in the product upper and lower surfaces that step 4) a) is obtained, flexible cover sheet's
With a thickness of 2500 microns；Flexible cover sheet is polyethylene terephthalate.
A kind of selfreparing graphene pressure sensor performance that above embodiments obtain is excellent.Embodiment one to five, product
Volume resistivity be respectively 462,311,306,143 and 66 Ω .cm；Selfreparing rate is respectively 76%, 72%, 81%, 84% and
73%.Compared with the pressure sensor that addition equal parts conductive black obtains, present invention product obtained has more low volume
Resistivity.
Claims (2)
1. a kind of preparation method of the graphene-based pressure sensor of selfreparing, which comprises the following steps:
1) one-dimensional silver nanowires material is prepared
A) ethylene glycol pre-processes: the ethylene glycol of 50~100 mL is added in three-necked flask in 150~170 DEG C of sufficiently heating 10
~30 minutes；
B) the NaCl aqueous solution for measuring 1~4 mL is added in the solution that step a) is formed, and heats 10~15 minutes；NaCl aqueous solution
Concentration is 0.002~0.004 mol/L；
C) a certain amount of silver nitrate is dissolved in ethylene glycol, forms the silver nitrate solution of 0.3~0.5 mol/L；By a certain amount of poly- second
Alkene pyrrolones (PVP) is dissolved in ethylene glycol, forms the PVP solution of 0.4~0.6 mol/L；10~15 mL silver nitrate solutions are taken to add
Enter in the mixed solution formed to step b), while the PVP solution of 30~45mL being taken to be slowly dropped by peristaltic pump, time control
In 50~90 minutes；
D) after completion of dropwise addition, the reaction solution that step c) is obtained, which takes out, to be stood to room temperature；Then by reaction solution at 9000 rpm
It is centrifuged 10 minutes and is cleaned multiple times with deionized water and dehydrated alcohol, finally obtain powdery product；
2) graphene@silver nanowires composite electric conductor is prepared
A) first a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in solvent and are configured to homogeneous phase solution, then will
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution, obtains the dispersion that expanded graphite concentration is 0.1 ~ 0.9 mg/mL
Solution after ultrasonic disperse 14 ~ 20 hours, makes whole expanded graphites form graphene dispersing solution, above-mentioned graphene dispersing solution is existed
30 min are centrifuged under 8000 rpm, taking upper liquid is stable graphene organic solution；The above-mentioned carboxymethyl cellulose used
Or the mass ratio of hydroxyethyl cellulose and expanded graphite is 5:1 ~ 10:1；Solvent is acetone, ethyl alcohol, tetrahydrofuran, dichloromethane
One or more of alkane mixture；
B) 1) silver nanowires obtained in is added in stable graphene organic solution, is stirred with the machinery of 500 rpm/min
It mixes speed to stir 2 ~ 6 hours, further graphene@silver nanowires composite electric conductor can be obtained after 3 hours in ultrasound；It uses
Expanded graphite and the mass ratio of silver nanowires are 1:15 ~ 4:1；
3) the graphene-based high molecular material of selfreparing is prepared
A) macromolecule prepolymer: taking a certain amount of dimeric dibasic acid and diethylenetriamine to be put into three-necked flask, with nitrogen as protection gas
Body is heated to 150 ~ 170 DEG C, and mechanical stirring is reacted 20 ~ 26 hours, forms macromolecule prepolymer；Wherein dimeric dibasic acid and divinyl
The mass ratio of triamine is 2:1 ~ 3:1；
B) above-mentioned macromolecule prepolymer is added to formation methylene chloride mixed solution in methylene chloride, the two mass ratio 1:1 ~ 1:
5；Then the graphene@silver nanowires composite electric conductor in 2) is added in above-mentioned methylene chloride mixed solution；Then it is added
A certain amount of methanol and distilled water, are sufficiently stirred, and are then allowed to stand 12 hours；Subnatant is taken out and in 50 DEG C of baking ovens heating it is 48 small
When obtain final mixture；The gross mass and macromolecule prepolymer mass ratio of graphene@silver nanowires composite electric conductor are 0 ~ 55:
100；Methylene chloride, methanol, water volume ratio be 3:1:2；
C) weigh a certain amount of urea, in the final mixture that the step b) being added to after purifying is obtained, at 130 ~ 145 DEG C into
Row crosslinking, the time 2 ~ 12 hours, can be obtained the graphene-based high molecular material of selfreparing；The quality of urea and macromolecule prepolymer
Than for 5:100 ~ 20:100；
D) the graphene-based high molecular material of selfreparing in step c) is subjected to molded curing film forming with mold；Solidification temperature 160
DEG C, curing time 2 hours, 5 ~ 200 microns of film thickness；
4) the graphene-based pressure sensor package of selfreparing
A) the graphene-based macromolecule membrane upper and lower surface of selfreparing obtained in step 3) d) is plated into conductive metal film respectively,
And it is drawn with conducting wire；Conductive metal film is gold, silver, platinum or copper, and metal layer thickness is 10 ~ 200 microns；Conducting wire is silver nanoparticle
Line, nanowires of gold or copper nano-wire, diameter of wire are 10 ~ 1000 microns；
B) protection packaging, the thickness of flexible cover sheet are carried out with flexible cover sheet in the product upper and lower surfaces that step 4) a) is obtained
It is 10 ~ 2500 microns；Flexible cover sheet is dimethyl silicone polymer, polyethylene or polyethylene terephthalate.
2. the preparation method of the graphene-based pressure sensor of a kind of selfreparing according to claim 1, it is characterised in that step
2) in a) used in ultrasonic power be 90 W.
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| CN108611695A (en) * | 2018-03-21 | 2018-10-02 | 浙江理工大学 | A kind of preparation method of the flexible photoreceptor conductive fiber of azo-based benzene/graphene oxide/nano silver wire |
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| CN108548480A (en) * | 2018-05-09 | 2018-09-18 | 电子科技大学 | Three layers of selfreparing flexibility strain transducer of one kind and preparation method thereof |
| CN108997750A (en) * | 2018-09-28 | 2018-12-14 | 东北林业大学 | A kind of preparation method of graphene oxide self-healing polymers |
| CN109682509B (en) * | 2019-02-19 | 2020-09-01 | 浙江理工大学 | Preparation method of large-size flexible pressure sensor |
| CN112442253A (en) * | 2019-08-29 | 2021-03-05 | 邵武市万家美家居用品制造有限公司 | Filter net bag and preparation method thereof |
| CN111564237B (en) * | 2020-05-21 | 2021-02-02 | 电子科技大学中山学院 | Preparation method of near-infrared thermal-repair flexible conductive film |
| CN113150547A (en) * | 2021-05-25 | 2021-07-23 | 松山湖材料实验室 | Polyimide composite film with electromagnetic shielding function and preparation method and application thereof |
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