CN107036741A - A kind of graphene-based pressure sensor of selfreparing and preparation method thereof - Google Patents
A kind of graphene-based pressure sensor of selfreparing and preparation method thereof Download PDFInfo
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Abstract
The invention discloses graphene-based pressure sensor of a kind of selfreparing and preparation method thereof.The conductive elastomer with self-repair function is made by adding graphene@nano silver wire composite electric conductors in selfreparing macromolecule matrix in the present invention；Then the selfreparing conductive elastomer is packaged into pressure sensor.The electric conductivity and self-healing properties that the present invention solves traditional selfreparing conducting polymer composite are difficult to while the contradictory problems of optimization.The present invention has advantages below：1st, the hard aggregation problem of graphene@nano silver wires can be reduced without drying and processing in the post processing of graphene@nano silver wires composite electric conductor；2nd, graphene@nano silver wires composite electric conductor is more likely formed three-dimensional crosslinked network structure in selfreparing macromolecule matrix；3rd, the graphene-based pressure sensor of selfreparing has the advantages that long lifespan, electric conductivity height, sensitivity are high.
Description
Technical field
The present invention relates to intelligent macromolecule field, more particularly, to a kind of graphene-based pressure sensor of selfreparing and
Its preparation method.
Background technology
In recent years, developing rapidly with wearable electronic, flexible electronic device is in medicine equipment, the energy, information, industry
Huge application prospect is shown Deng field.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 service life and stability of serious reduction equipment.Therefore, develop
Go out a kind of pliable pressure sensor with self-repair function to have great importance.
In order to obtain selfreparing pliable pressure sensor, domestic and international researcher has carried out numerous studies in sensing unit.Example
Such as, Xiamen University Weng Wen osmanthus, Xia Haiping seminars devise two kinds of monomers with carbamate and carried 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 electrical conductivity up to 1 s/cm.Bao Zhe nanmus seminar of Stanford Univ USA is prepared for a kind of electricity with self-healing properties
Pole material.This material is that the polymer with self-healing properties and conductive particle are carried out into blending realization.Utilize hydrogen bond
Reversible dynamic, material is without can be achieved the multiple mechanics of room temperature and electricity selfreparing under conditions of outside agent.S. A. Odom
Deng then have studied a kind of electric conductivity microcapsules, this microcapsules are implanted into material matrix.After material is destroyed, conduction liquid
Body or solvent rupture from microcapsules, so as to realize reviewing one's lessons by oneself redoubling and keeping its electric property for material.
But, existing selfreparing conducting polymer composite, in order to realize high conduction performance, often by macromolecule
A large amount of conductive particles are filled in matrix.Under a large amount of introducings of these conductive particles necessarily cause high molecular self-healing properties significantly
Drop.These problems greatly limit follow-up preparation selfreparing pressure sensor.Therefore, a kind of low addition number, electric conductivity are studied
Can the good and high a kind of selfreparing pressure sensor of self-healing properties and preparation method thereof be necessary.
The content of the invention
It is an object of the invention to provide graphene-based pressure sensor of a kind of selfreparing and preparation method thereof.This method solution
The problem and selfreparing conducting polymer electric conductivity and self-healing properties that certainly existing pressure sensor is unable to selfreparing can not
The problem of improving simultaneously, and graphene-based pressure sensor of a kind of selfreparing and preparation method thereof is provided.With huge market
Application prospect and good economic and social benefits.
To achieve the above object of the invention, the technical solution adopted by the present invention is：A kind of graphene-based pressure sensing of selfreparing
Device and preparation method thereof, comprises the following steps：
1）Prepare one-dimensional nano silver wire material
a）Ethylene glycol is pre-processed：50~100 mL ethylene glycol is added in three-necked flask in 150~170 DEG C of fully heating 10
~30 minutes；
b）The NaCl aqueous solution for measuring 1~4 mL adds a）In solution, heat 10~15 minutes；NaCl concentration of aqueous solution is
0.002~0.004 mol/L；
c）A certain amount of silver nitrate is dissolved in ethylene glycol, 0.3~0.5 mol/L silver nitrate solution is formed；By a certain amount of poly- second
Alkene pyrrolones（PVP）It is dissolved in ethylene glycol, forms 0.4~0.6 mol/L PVP solution；10~15 mL silver nitrate solutiones are taken to add
Enter to mixed solution b）In, while taking 30~45mL PVP solution to be slowly dropped into by peristaltic pump, time control is at 50~90 points
In clock；
d）After completion of dropwise addition, above-mentioned reaction solution is taken out and stood to room temperature；Then above-mentioned reaction solution is centrifuged under 9000 rpm
10 minutes and it is cleaned multiple times with deionized water and absolute ethyl alcohol, finally obtains powdery product；
2）Prepare graphene@nano silver wire composite electric conductors
a）First a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in the solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, it is 0.1 ~ 0.9 mg/mL's to obtain expanded graphite concentration
Dispersion soln, ultrasonic disperse makes whole expanded graphite formation graphene dispersing solutions, above-mentioned dispersion soln is existed after 14 ~ 20 hours
30 min are centrifuged under 8000 rpm, it is stable graphene organic solution to take upper liquid（Labeled as solution 1）；It is above-mentioned to use
The mass ratio of cellulose and expanded graphite is 5:1~10:1；Solvent is one kind in acetone, ethanol, tetrahydrofuran, dichloromethane
Or several mixtures；
b）By 1）In obtained nano silver wire be added in above-mentioned solution 1, with 500 rpm/min mechanical agitation speed stirring 2 ~
6 hours, further ultrasound was after 3 hours, you can obtain graphene@nano silver wire composite electric conductors；The expanded graphite and silver used
The mass ratio of nano wire is 1:15~4:1；
3）Prepare graphene-based selfreparing high polymer material
a）Macromolecule prepolymer：A certain amount of dimeric dibasic acid and diethylenetriamine is taken to be put into three-necked flask, with nitrogen as protection gas
Body, is heated to 150 ~ 170 DEG C, mechanical agitation 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 in dichloromethane, both mass ratioes 1:1~1:5；Then by 2）In graphite
Alkene@nano silver wire composite electric conductors are added in above-mentioned dichloromethane mixed solution；Then a certain amount of methanol and distilled water are added,
It is sufficiently stirred for, then stands 12 hours；Subnatant is taken out and heated 48 hours in 50 DEG C of baking ovens；The gross mass of solid particle
It is 0 ~ 55 with macromolecule prepolymer mass ratio:100；Dichloromethane, methanol, the volume ratio of water are 3:1:2；
c）A certain amount of urea is weighed, the b added to after purifying）In mixture, it is crosslinked at 130 ~ 145 DEG C, the time 2 ~
12 hours, you can obtain the graphene-based high polymer material of selfreparing；The mass ratio of urea and prepolymer is 5:100~20:100；
d）The graphene-based pressure-sensitive high polymer material of selfreparing in step c is subjected to molded curing film forming with mould.Solidification temperature
160 DEG C, 2 hours hardening times, 5 ~ 200 microns of film thickness；
4）The graphene-based pressure sensor package of selfreparing
a）By step 3）In the obtained graphene-based pressure-sensitive macromolecule membrane upper and lower surface of selfreparing to plate conducting metal respectively thin
Film, and drawn with wire；Conductive metal film is the conducting metals such as gold, silver, platinum, copper, and metal layer thickness is 10 ~ 200 microns；Lead
Line is nano silver wire, nanowires of gold, copper foil etc., diameter of wire（Thickness）For 10 ~ 1000 microns；
b）The upper and lower surface of film after treatment carries out protection packaging with flexible cover sheet, and the thickness of protective layer is micro- for 10 ~ 2500
Rice；Flexible cover sheet may include dimethyl silicone polymer, polyethylene, polyethylene terephthalate.
A kind of described graphene-based pressure sensor of selfreparing and preparation method thereof, it is characterised in that ultrasonic power used
For 90 W.
The graphene-based pressure sensor of selfreparing of the present invention can be used for detection curved because of its excellent sensitivity and stability
The milli machine power such as Qu Li, twisting resistance, can be used for detecting pressure of the human pulse to vascular wall, can be used for detection sound wave shake
It is dynamic.
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：（1）With nano silver wire with
Graphene carries out compound obtained graphene@nano silver wire composite electric conductors, not only with higher electric conductivity, and finally
Electric conductor is without drying and processing, and contained reagent can be directly applied in follow-up macromolecule combination process, reduces graphene@silver and receives
The hard aggregation problem of rice noodles；（2）By that toward addition graphene@nano silver wire composite electric conductors in macromolecule performed polymer, can be formed
Three-dimensional crosslinked network structure, and the loading and three-dimensional net structure controllability of graphene@nano silver wires are more preferable；（3）Silver is received
Rice noodles intercalation enters after graphene synusia, the defect part of the low-level oxidation on nano silver wire surface layer and graphene will with it is polymer-based
Body forms new hydrogen bond, improves the high molecular mechanical property of selfreparing graphene conductive.
Embodiment
With reference to embodiment, the invention will be further described：
Embodiment one
A kind of graphene-based pressure sensor of selfreparing and preparation method thereof, comprises the following steps：
1）Prepare one-dimensional nano silver wire material
a）Ethylene glycol is pre-processed：50 mL ethylene glycol is added in three-necked flask and fully heated 10 minutes at 150 DEG C；
b）The NaCl aqueous solution for measuring 1 mL adds a）In solution, heat 10 minutes；NaCl concentration of aqueous solution is 0.002 mol/
L；
c）10 g silver nitrates are dissolved in ethylene glycol, 0.3 mol/L silver nitrate solution is formed；By 15 g polyvinyl pyrrolidones
（PVP）It is dissolved in ethylene glycol, forms 0.4 mol/L PVP solution；10 mL silver nitrate solutiones are taken to be added to mixed solution b）In,
30 mL PVP solution is taken to be slowly dropped into by peristaltic pump simultaneously, time control is in 50 minutes；
d）After completion of dropwise addition, above-mentioned reaction solution is taken out and stood to room temperature；Then above-mentioned reaction solution is centrifuged under 9000 rpm
10 minutes and it is cleaned multiple times with deionized water and absolute ethyl alcohol, finally obtains powdery product；
2）Prepare graphene@nano silver wire composite electric conductors
a）First a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in the solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, it is the scattered of 0.1 mg/mL to obtain expanded graphite concentration
Solution, ultrasonic disperse makes whole expanded graphite formation graphene dispersing solutions, by above-mentioned dispersion soln in 8000 rpm after 14 hours
30 min of lower centrifugation, it is stable graphene organic solution to take upper liquid（Labeled as solution 1）；The above-mentioned cellulose used with
The mass ratio of expanded graphite is 5:1；Solvent is acetone；
b）By 1）In obtained nano silver wire be added in above-mentioned solution 1, stir 2 with 500 rpm/min mechanical agitation speed
Hour, further ultrasound is after 3 hours, you can obtain graphene@nano silver wire composite electric conductors；The expanded graphite and Yin Na used
The mass ratio of rice noodles is 1:15；
3）Prepare graphene-based selfreparing high polymer material
a）Macromolecule prepolymer：10 g dimeric dibasic acids and 5 g diethylenetriamines are taken to be put into three-necked flask, with nitrogen as protection gas
Body, is heated to 150 DEG C, mechanical agitation is reacted 20 hours, forms macromolecule prepolymer；Wherein dimeric dibasic acid and diethylenetriamine
Mass ratio is 2:1；
b）Above-mentioned macromolecule prepolymer is added in dichloromethane, both mass ratioes 1:1；Then by 2）In graphene@silver
Nano wire composite electric conductor is added in above-mentioned dichloromethane mixed solution；Then a certain amount of methanol and distilled water are added, fully
Stirring, then stands 12 hours；Subnatant is taken out and heated 48 hours in 50 DEG C of baking ovens；The gross mass of solid particle and height
Molecule prepolymer mass ratio is 15:100；Dichloromethane, methanol, the volume ratio of water are 3:1:2；
c）Weigh 0.75 urea, add to purify after b）In mixture, it is crosslinked at 130 DEG C, time 2 h, i.e.,
It can obtain the graphene-based high polymer material of selfreparing；The mass ratio of urea and prepolymer is 5:100；
d）The graphene-based pressure-sensitive high polymer material of selfreparing in step c is subjected to molded curing film forming with mould.Solidification temperature
160 DEG C, 2 hours hardening times, 5 microns of film thickness；
4）The graphene-based pressure sensor package of selfreparing
a）By step 3）In the obtained graphene-based pressure-sensitive macromolecule membrane upper and lower surface of selfreparing to plate conducting metal respectively thin
Film, and drawn with wire；Conductive metal film is gold, and metal layer thickness is 10 microns；Wire is nano silver wire, diameter of wire
（Thickness）For 10 microns；
b）The upper and lower surface of film after treatment carries out protection packaging with flexible cover sheet, and the thickness of protective layer is 10 microns；It is soft
Property protective layer be polyethylene.
Embodiment two
A kind of graphene-based pressure sensor of selfreparing and preparation method thereof, comprises the following steps：
1）Prepare one-dimensional nano silver wire material
a）Ethylene glycol is pre-processed：60 mL ethylene glycol is added in three-necked flask and fully heated 16 minutes at 155 DEG C；
b）The NaCl aqueous solution for measuring 1.8 mL adds a）In solution, heat 10 minutes；NaCl concentration of aqueous solution is 0.0025
mol/L；
c）15 g silver nitrates are dissolved in ethylene glycol, 0.35 mol/L silver nitrate solution is formed；By 14 g polyvinyl pyrrolidones
（PVP）It is dissolved in ethylene glycol, forms 0.48 mol/L PVP solution；13 mL silver nitrate solutiones are taken to be added to mixed solution b）
In, while taking 35 mL PVP solution to be slowly dropped into by peristaltic pump, time control is in 65 minutes；
d）After completion of dropwise addition, above-mentioned reaction solution is taken out and stood to room temperature；Then above-mentioned reaction solution is centrifuged under 9000 rpm
10 minutes and it is cleaned multiple times with deionized water and absolute ethyl alcohol, finally obtains powdery product；
2）Prepare graphene@nano silver wire composite electric conductors
a）First a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in the solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, it is the scattered of 0.3 mg/mL to obtain expanded graphite concentration
Solution, ultrasonic disperse makes whole expanded graphite formation graphene dispersing solutions, by above-mentioned dispersion soln in 8000 rpm after 16 hours
30 min of lower centrifugation, it is stable graphene organic solution to take upper liquid（Labeled as solution 1）；The above-mentioned cellulose used with
The mass ratio of expanded graphite is 6:1；Solvent is ethanol；
b）By 1）In obtained nano silver wire be added in above-mentioned solution 1, stir 3 with 500 rpm/min mechanical agitation speed
Hour, further ultrasound is after 3 hours, you can obtain graphene@nano silver wire composite electric conductors；The expanded graphite and Yin Na used
The mass ratio of rice noodles is 1:1；
3）Prepare graphene-based selfreparing high polymer material
a）Macromolecule prepolymer：12 g dimeric dibasic acids and 6 g diethylenetriamines are taken to be put into three-necked flask, with nitrogen as protection gas
Body, is heated to 155 DEG C, mechanical agitation is reacted 24 hours, forms macromolecule prepolymer；Wherein dimeric dibasic acid and diethylenetriamine
Mass ratio is 2:1；
b）Above-mentioned macromolecule prepolymer is added in dichloromethane, both mass ratioes 1:1.5；Then by 2）In graphene@
Nano silver wire composite electric conductor is added in above-mentioned dichloromethane mixed solution；Then a certain amount of methanol and distilled water are added, is filled
Divide stirring, then stand 12 hours；Subnatant is taken out and heated 48 hours in 50 DEG C of baking ovens；The gross mass of solid particle with
Macromolecule prepolymer mass ratio is 20:100；Dichloromethane, methanol, the volume ratio of water are 3:1:2；
c）1.44 g urea is weighed, the b added to after purifying）In mixture, it is crosslinked at 135 DEG C, 4 hours time,
It can obtain the graphene-based high polymer material of selfreparing；The mass ratio of urea and prepolymer is 8:100；
d）The graphene-based pressure-sensitive high polymer material of selfreparing in step c is subjected to molded curing film forming with mould.Solidification temperature
160 DEG C, 2 hours hardening times, 25 microns of film thickness；
4）The graphene-based pressure sensor package of selfreparing
a）By step 3）In the obtained graphene-based pressure-sensitive macromolecule membrane upper and lower surface of selfreparing to plate conducting metal respectively thin
Film, and drawn with wire；Conductive metal film is silver, and metal layer thickness is 25 microns；Wire is nanowires of gold, diameter of wire
（Thickness）For 100 microns；
b）The upper and lower surface of film after treatment carries out protection packaging with flexible cover sheet, and the thickness of protective layer is 800 microns；
Flexible cover sheet is dimethyl silicone polymer.
Embodiment three
A kind of graphene-based pressure sensor of selfreparing and preparation method thereof, comprises the following steps：
1）Prepare one-dimensional nano silver wire material
a）Ethylene glycol is pre-processed：70 mL ethylene glycol is added in three-necked flask and fully heated 25 minutes at 160 DEG C；
b）The NaCl aqueous solution for measuring 2 mL adds a）In solution, heat 12 minutes；NaCl concentration of aqueous solution is 0.003 mol/
L；
c）8 g silver nitrates are dissolved in ethylene glycol, 0.4 mol/L silver nitrate solution is formed；By 20 g polyvinyl pyrrolidones
（PVP）It is dissolved in ethylene glycol, forms 0.5 mol/L PVP solution；15 mL silver nitrate solutiones are taken to be added to mixed solution b）In,
30 mL PVP solution is taken to be slowly dropped into by peristaltic pump simultaneously, time control is in 70 minutes；
d）After completion of dropwise addition, above-mentioned reaction solution is taken out and stood to room temperature；Then above-mentioned reaction solution is centrifuged under 9000 rpm
10 minutes and it is cleaned multiple times with deionized water and absolute ethyl alcohol, finally obtains powdery product；
2）Prepare graphene@nano silver wire composite electric conductors
a）First a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in the solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, it is the scattered of 0.5 mg/mL to obtain expanded graphite concentration
Solution, ultrasonic disperse makes whole expanded graphite formation graphene dispersing solutions, by above-mentioned dispersion soln in 8000 rpm after 18 hours
30 min of lower centrifugation, it is stable graphene organic solution to take upper liquid（Labeled as solution 1）；The above-mentioned cellulose used with
The mass ratio of expanded graphite is 7:1；Solvent is tetrahydrofuran；
b）By 1）In obtained nano silver wire be added in above-mentioned solution 1, stir 4 with 500 rpm/min mechanical agitation speed
Hour, further ultrasound is after 3 hours, you can obtain graphene@nano silver wire composite electric conductors；The expanded graphite and Yin Na used
The mass ratio of rice noodles is 2:1；
3）Prepare graphene-based selfreparing high polymer material
a）Macromolecule prepolymer：15 g dimeric dibasic acids and 5 g diethylenetriamines are taken to be put into three-necked flask, with nitrogen as protection gas
Body, is heated to 165 DEG C, mechanical agitation is reacted 22 hours, forms macromolecule prepolymer；Wherein dimeric dibasic acid and diethylenetriamine
Mass ratio is 3:1；
b）Above-mentioned macromolecule prepolymer is added in dichloromethane, both mass ratioes 1:2；Then by 2）In graphene@silver
Nano wire composite electric conductor is added in above-mentioned dichloromethane mixed solution；Then a certain amount of methanol and distilled water are added, fully
Stirring, then stands 12 hours；Subnatant is taken out and heated 48 hours in 50 DEG C of baking ovens；The gross mass of solid particle and height
Molecule prepolymer mass ratio is 25:100；Dichloromethane, methanol, the volume ratio of water are 3:1:2；
c）2 g urea is weighed, the b added to after purifying）In mixture, it is crosslinked at 140 DEG C, 6 hours time, you can
Obtain the graphene-based high polymer material of selfreparing；The mass ratio of urea and prepolymer is 10:100；
d）The graphene-based pressure-sensitive high polymer material of selfreparing in step c is subjected to molded curing film forming with mould.Solidification temperature
160 DEG C, 2 hours hardening times, 50 microns of film thickness；
4）The graphene-based pressure sensor package of selfreparing
a）By step 3）In the obtained graphene-based pressure-sensitive macromolecule membrane upper and lower surface of selfreparing to plate conducting metal respectively thin
Film, and drawn with wire；Conductive metal film is platinum, and metal layer thickness is 50 microns；Wire is copper nano-wire, diameter of wire
（Thickness）For 350 microns；
b）The upper and lower surface of film after treatment carries out protection packaging with flexible cover sheet, and the thickness of protective layer is 1000 microns；
Flexible cover sheet is polyethylene terephthalate.
Example IV
A kind of graphene-based pressure sensor of selfreparing and preparation method thereof, comprises the following steps：
1）Prepare one-dimensional nano silver wire material
a）Ethylene glycol is pre-processed：85 mL ethylene glycol is added in three-necked flask and fully heated 25 minutes at 165 DEG C；
b）The NaCl aqueous solution for measuring 3 mL adds a）In solution, heat 13 minutes；NaCl concentration of aqueous solution is 0.0035 mol/
L；
c）6 g silver nitrates are dissolved in ethylene glycol, 0.45 mol/L silver nitrate solution is formed；By 20 g polyvinyl pyrrolidones
（PVP）It is dissolved in ethylene glycol, forms 0.55 mol/L PVP solution；15 mL silver nitrate solutiones are taken to be added to mixed solution b）
In, while taking 40 mL PVP solution to be slowly dropped into by peristaltic pump, time control is in 80 minutes；
d）After completion of dropwise addition, above-mentioned reaction solution is taken out and stood to room temperature；Then above-mentioned reaction solution is centrifuged under 9000 rpm
10 minutes and it is cleaned multiple times with deionized water and absolute ethyl alcohol, finally obtains powdery product；
2）Prepare graphene@nano silver wire composite electric conductors
a）First a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in the solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, it is the scattered of 0.7 mg/mL to obtain expanded graphite concentration
Solution, ultrasonic disperse makes whole expanded graphite formation graphene dispersing solutions, by above-mentioned dispersion soln in 8000 rpm after 19 hours
30 min of lower centrifugation, it is stable graphene organic solution to take upper liquid（Labeled as solution 1）；The above-mentioned cellulose used with
The mass ratio of expanded graphite is 8:1；Solvent is dichloromethane；
b）By 1）In obtained nano silver wire be added in above-mentioned solution 1, stir 5 with 500 rpm/min mechanical agitation speed
Hour, further ultrasound is after 3 hours, you can obtain graphene@nano silver wire composite electric conductors；The expanded graphite and Yin Na used
The mass ratio of rice noodles is 3:1；
3）Prepare graphene-based selfreparing high polymer material
a）Macromolecule prepolymer：25 g dimeric dibasic acids and 10 g diethylenetriamines are taken to be put into three-necked flask, with nitrogen as protection
Gas, is heated to 165 DEG C, mechanical agitation is reacted 24 hours, forms macromolecule prepolymer；Wherein dimeric dibasic acid and diethylenetriamine
Mass ratio be 3:1；
b）Above-mentioned macromolecule prepolymer is added in dichloromethane, both mass ratioes 1:3；Then by 2）In graphene@silver
Nano wire composite electric conductor is added in above-mentioned dichloromethane mixed solution；Then a certain amount of methanol and distilled water are added, fully
Stirring, then stands 12 hours；Subnatant is taken out and heated 48 hours in 50 DEG C of baking ovens；The gross mass of solid particle and height
Molecule prepolymer mass ratio is 30:100；Dichloromethane, methanol, the volume ratio of water are 3:1:2；
c）5.25 g urea is weighed, the b added to after purifying）In mixture, it is crosslinked at 145 DEG C, 8 hours time,
It can obtain the graphene-based high polymer material of selfreparing；The mass ratio of urea and prepolymer is 15:100；
d）The graphene-based pressure-sensitive high polymer material of selfreparing in step c is subjected to molded curing film forming with mould.Solidification temperature
160 DEG C, 2 hours hardening times, 100 microns of film thickness；
4）The graphene-based pressure sensor package of selfreparing
a）By step 3）In the obtained graphene-based pressure-sensitive macromolecule membrane upper and lower surface of selfreparing to plate conducting metal respectively thin
Film, and drawn with wire；Conductive metal film is copper, and metal layer thickness is 100 microns；Wire is nano silver wire, diameter of wire
（Thickness）For 700 microns；
b）The upper and lower surface of film after treatment carries out protection packaging with flexible cover sheet, and the thickness of protective layer is 2000 microns；
Flexible cover sheet is dimethyl silicone polymer.
Embodiment five
A kind of graphene-based pressure sensor of selfreparing and preparation method thereof, comprises the following steps：
1）Prepare one-dimensional nano silver wire material
a）Ethylene glycol is pre-processed：100 mL ethylene glycol is added in three-necked flask and fully heated 30 minutes at 170 DEG C；
b）The NaCl aqueous solution for measuring 4 mL adds a）In solution, heat 15 minutes；NaCl concentration of aqueous solution is 0.004 mol/
L；
c）13 g silver nitrates are dissolved in ethylene glycol, 0.5 mol/L silver nitrate solution is formed；By 25 g polyvinyl pyrrolidones
（PVP）It is dissolved in ethylene glycol, forms 0.6 mol/L PVP solution；14 mL silver nitrate solutiones are taken to be added to mixed solution b）In,
45 mL PVP solution is taken to be slowly dropped into by peristaltic pump simultaneously, time control is in 90 minutes；
d）After completion of dropwise addition, above-mentioned reaction solution is taken out and stood to room temperature；Then above-mentioned reaction solution is centrifuged under 9000 rpm
10 minutes and it is cleaned multiple times with deionized water and absolute ethyl alcohol, finally obtains powdery product；
2）Prepare graphene@nano silver wire composite electric conductors
a）First a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in the solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, it is the scattered of 0.9 mg/mL to obtain expanded graphite concentration
Solution, ultrasonic disperse makes whole expanded graphite formation graphene dispersing solutions, by above-mentioned dispersion soln in 8000 rpm after 20 hours
30 min of lower centrifugation, it is stable graphene organic solution to take upper liquid（Labeled as solution 1）；The above-mentioned cellulose used with
The mass ratio of expanded graphite is 10:1；Solvent is dichloromethane and ethanol according to volume ratio 2:1 obtained mixed solution；
b）By 1）In obtained nano silver wire be added in above-mentioned solution 1, stir 6 with 500 rpm/min mechanical agitation speed
Hour, further ultrasound is after 3 hours, you can obtain graphene@nano silver wire composite electric conductors；The expanded graphite and Yin Na used
The mass ratio of rice noodles is 4:1；
3）Prepare graphene-based selfreparing high polymer material
a）Macromolecule prepolymer：30 g dimeric dibasic acids and 10 g diethylenetriamines are taken to be put into three-necked flask, with nitrogen as protection
Gas, is heated to 170 DEG C, mechanical agitation is reacted 26 hours, forms macromolecule prepolymer；Wherein dimeric dibasic acid and diethylenetriamine
Mass ratio be 3:1；
b）Above-mentioned macromolecule prepolymer is added in dichloromethane, both mass ratioes 1:5；Then by 2）In graphene@silver
Nano wire composite electric conductor is added in above-mentioned dichloromethane mixed solution；Then a certain amount of methanol and distilled water are added, fully
Stirring, then stands 12 hours；Subnatant is taken out and heated 48 hours in 50 DEG C of baking ovens；The gross mass of solid particle and height
Molecule prepolymer mass ratio is 55:100；Dichloromethane, methanol, the volume ratio of water are 3:1:2；
c）8 g urea is weighed, the b added to after purifying）In mixture, it is crosslinked at 145 DEG C, 12 hours time, i.e.,
It can obtain the graphene-based high polymer material of selfreparing；The mass ratio of urea and prepolymer is 20:100；
d）The graphene-based pressure-sensitive high polymer material of selfreparing in step c is subjected to molded curing film forming with mould.Solidification temperature
160 DEG C, 2 hours hardening times, 200 microns of film thickness；
4）The graphene-based pressure sensor package of selfreparing
a）By step 3）In the obtained graphene-based pressure-sensitive macromolecule membrane upper and lower surface of selfreparing to plate conducting metal respectively thin
Film, and drawn with wire；Conductive metal film is gold, and metal layer thickness is 200 microns；Wire is nanowires of gold, diameter of wire
（Thickness）For 1000 microns；
b）The upper and lower surface of film after treatment carries out protection packaging with flexible cover sheet, and the thickness of protective layer is 2500 microns；
Flexible cover sheet is polyethylene terephthalate.
A kind of selfreparing graphene pressure sensor excellent performance that above example is obtained.Embodiment one to five, product
Specific insulation 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 is obtained, the product that the present invention is obtained has more low volume
Resistivity.
Claims (2)
1. a kind of graphene-based pressure sensor of selfreparing and preparation method thereof, it is characterised in that comprise the following steps：
1）Prepare one-dimensional nano silver wire material
A) ethylene glycol is pre-processed：50~100 mL ethylene glycol is added in three-necked flask in 150~170 DEG C of fully heating 10
~30 minutes；
b）The NaCl aqueous solution for measuring 1~4 mL adds a）In solution, heat 10~15 minutes；NaCl concentration of aqueous solution is
0.002~0.004 mol/L；
c）A certain amount of silver nitrate is dissolved in ethylene glycol, 0.3~0.5 mol/L silver nitrate solution is formed；By a certain amount of poly- second
Alkene pyrrolones（PVP）It is dissolved in ethylene glycol, forms 0.4~0.6 mol/L PVP solution；10~15 mL silver nitrate solutiones are taken to add
Enter to mixed solution b）In, while taking 30~45mL PVP solution to be slowly dropped into by peristaltic pump, time control is at 50~90 points
In clock；
D) after completion of dropwise addition, above-mentioned reaction solution is taken out and stood to room temperature；Then above-mentioned reaction solution is centrifuged under 9000 rpm
10 minutes and it is cleaned multiple times with deionized water and absolute ethyl alcohol, finally obtains powdery product；
2）Prepare graphene@nano silver wire composite electric conductors
a）First a certain amount of carboxymethyl cellulose or hydroxyethyl cellulose are added in the solvent and are configured to homogeneous phase solution,
The expanded graphite of certain mass is added in above-mentioned homogeneous phase solution again, it is 0.1 ~ 0.9 mg/mL's to obtain expanded graphite concentration
Dispersion soln, ultrasonic disperse makes whole expanded graphite formation graphene dispersing solutions, above-mentioned dispersion soln is existed after 14 ~ 20 hours
30 min are centrifuged under 8000 rpm, it is stable graphene organic solution to take upper liquid（Labeled as solution 1）；It is above-mentioned to use
The mass ratio of cellulose and expanded graphite is 5:1~10:1；Solvent is one kind in acetone, ethanol, tetrahydrofuran, dichloromethane
Or several mixtures；
b）By 1）In obtained nano silver wire be added in above-mentioned solution 1, with 500 rpm/min mechanical agitation speed stirring 2 ~
6 hours, further ultrasound was after 3 hours, you can obtain graphene@nano silver wire composite electric conductors；The expanded graphite and silver used
The mass ratio of nano wire is 1:15~4:1；
3）Prepare graphene-based selfreparing high polymer material
a）Macromolecule prepolymer：A certain amount of dimeric dibasic acid and diethylenetriamine is taken to be put into three-necked flask, with nitrogen as protection gas
Body, is heated to 150 ~ 170 DEG C, mechanical agitation 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 in dichloromethane, both mass ratioes 1:1~1:5；Then by 2）In graphite
Alkene@nano silver wire composite electric conductors are added in above-mentioned dichloromethane mixed solution；Then a certain amount of methanol and distilled water are added,
It is sufficiently stirred for, then stands 12 hours；Subnatant is taken out and heated 48 hours in 50 DEG C of baking ovens；The gross mass of solid particle
It is 0 ~ 55 with macromolecule prepolymer mass ratio:100；Dichloromethane, methanol, the volume ratio of water are 3:1:2；
c）A certain amount of urea is weighed, the b added to after purifying）In mixture, it is crosslinked at 130 ~ 145 DEG C, the time 2 ~
12 hours, you can obtain the graphene-based high polymer material of selfreparing；The mass ratio of urea and prepolymer is 5:100~20:100；
d）The graphene-based pressure-sensitive high polymer material of selfreparing in step c is subjected to molded curing film forming with mould；Solidification temperature
160 DEG C, 2 hours hardening times, 5 ~ 200 microns of film thickness；
4）The graphene-based pressure sensor package of selfreparing
a）By step 3）In the obtained graphene-based pressure-sensitive macromolecule membrane upper and lower surface of selfreparing to plate conducting metal respectively thin
Film, and drawn with wire；Conductive metal film is the conducting metals such as gold, silver, platinum, copper, and metal layer thickness is 10 ~ 200 microns；Lead
Line is nano silver wire, nanowires of gold, copper foil etc., diameter of wire（Thickness）For 10 ~ 1000 microns；
b）The upper and lower surface of film after treatment carries out protection packaging with flexible cover sheet, and the thickness of protective layer is micro- for 10 ~ 2500
Rice；Flexible cover sheet may include dimethyl silicone polymer, polyethylene, polyethylene terephthalate.
2. a kind of graphene-based pressure sensor of selfreparing and preparation method thereof according to claim 1, it is characterised in that institute
It is 90 W with ultrasonic power.
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