CN110256702A - Long-chain cured epoxy/graphene composite film and its preparation method, flexible strain transducer - Google Patents
Long-chain cured epoxy/graphene composite film and its preparation method, flexible strain transducer Download PDFInfo
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- CN110256702A CN110256702A CN201910475216.6A CN201910475216A CN110256702A CN 110256702 A CN110256702 A CN 110256702A CN 201910475216 A CN201910475216 A CN 201910475216A CN 110256702 A CN110256702 A CN 110256702A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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Abstract
A kind of long-chain cured epoxy/graphene composite film and its preparation method, flexible strain transducer, belong to transducer production method field.Preparation method are as follows: graphene suspension and epoxy resin acetone soln are mixed, J2000 long-chain curing agent is added, ultrasound removal acetone is stirred, pours into mold, solidified, obtain long-chain cured epoxy/graphene composite film.Using long-chain cured epoxy/graphene composite film as the sensing unit of flexible strain transducer, flexibility, electric conductivity and the sensing capabilities of flexible strain transducer can be effectively improved.
Description
Technical field
The present invention relates to the preparation method technical fields of graphene composite material flexible sensor, and in particular to a kind of long-chain
Cured epoxy/graphene composite film and its preparation method, flexible strain transducer.
Background technique
Conventional conductive filler for polymer is made of metal (such as stainless steel fibre) or noble metal (silver wire), reaches
Performance and contact tube ought to the limit.Metal is usually high density material, so that composite material has poor flexibility.It compares
Under, the electrical-conductive nanometer carbon developed recently has high conductivity and not only light-weight but also cost-effective.Therefore, it advocates and uses
Carbon nanomaterial develops conducting polymer composite material, because they have good flexibility, and has relatively low density and phase
To high electric conductivity.
Currently, more commonly used graphene is mostly graphene oxide GO (graphene oxide) or redox stone
Black alkene RGO (reduce graphene oxide), the property that they have many graphenes similar, but electric conductivity is poor, no
It can be used as sensor.
Summary of the invention
When preparing graphene/elastomer nanocomposites for conventional method, thin film flexible is poor, poorly conductive asks
Topic, the invention proposes a kind of long-chain cured epoxy/graphene composite film and its preparation methods, flexible strain transducer.Party's legal system
It is single as the sensitivity of flexible strain transducer for a kind of cured epoxy/graphene composite film of long chain curing agent
Member can effectively improve flexibility, electric conductivity and the sensing capabilities of flexible strain transducer.
A kind of preparation method of long-chain cured epoxy/graphene composite film of the invention, comprising the following steps:
Step 1: preparing material solution
(1) in acetone by graphene uniform dispersion, it is uniformly mixed, obtains evenly dispersed in 10~30 DEG C of sonic oscillations
Graphene suspension;Wherein, the dosage of acetone be can be fully dispersed by graphene amount;
(2) in acetone by epoxy resin dissolution, it stirs evenly, obtains epoxy resin acetone soln;Wherein, the use of acetone
Amount is the amount that can sufficiently dissolve epoxy resin;
Step 2: preparing reaction solution
Graphene suspension and epoxy resin acetone soln are mixed, ultrasonic mixing is uniform, obtains reaction solution;Wherein,
By volume, graphene: (graphene+epoxy resin)=1.25%~5%;
Step 3: removal solvent
Into reaction solution, J2000 long-chain curing agent is added, stirs ultrasound removal acetone, obtains mixture;Wherein, it presses
Mass ratio, J2000 long-chain curing agent: epoxy resin=3:1:
Step 4: solidification
Mixture is poured into mold, solidified, obtain long-chain cured epoxy/graphene composite film.
In the step 1 (1), the graphene is the graphene microchip (Graphene of high regularity
Platelets), carbon-to-oxygen ratio C/O is (12~13): 1, conductivity is 1300~1400S/cm.
Carbon-coating number >=10 layer of the graphene microchip, thickness are at 5~100 nanometers.
The graphene microchip of the high regularity is made using following graphene preparation method:
Step I: it is heated being put into 650~750 DEG C of Muffle furnace by the graphene intercalation compound (GIC) of intercalation
1min, the intercalated graphite alkene intercalation compound after being thermally expanded;
Step II: the intercalated graphite alkene intercalation compound after thermal expansion is put into acetone soln, carries out sonic oscillation 4-
8h obtains mixed solution;
Step III: mixed solution is dried, and the graphene microchip of high regularity can be obtained.
In the step 1, using thermal expansion+ultrasonic method preparation graphene microchip (graphene platelets)
With better electric conductivity, conductivity can achieve 1400S/cm, and high regularity makes it easier to be formed with polymer compound
Material, high carbon-oxygen ratio make it have higher conductivity, prepare simple, at low cost.
In the step 1 (1), preferably, in mass ratio, graphene: acetone=1:(1~2).
In the step 1 (1), the sonic oscillation time is 1~2h.
In the step 1 (2), the epoxy resin is WSR618 (E-51), epoxide equivalent 184-200g/eq.
In the step 1 (2), in epoxy resin acetone soln, by volume, epoxy resin: acetone=1:(1~2).
In the step 2, the sonic oscillation time is 1~2h.
In the step 3, the stirring ultrasound removal acetone method particularly includes: it is anti-to be heated to 50~70 DEG C of stirrings
Answer 20~50min.
In the step 3, the J2000 long-chain curing agent is Jeffamine D2000, has longer molecule
Chain, average molecular weight 2000g/mol, total amine value are 0.98~1.05meq/g.
The structural formula of the J2000 long-chain curing agent are as follows:
Wherein, x is the degree of polymerization, chooses 32~34.
The effect of the curing agent is chemically reacted with epoxy resin, and netted space polymers are formed, the present invention
The epoxy resin of middle use is to belong to most common bisphenol A type epoxy resin, and the epoxy resin brittleness is stronger, and passes through addition
Cured long-chain cured epoxy/graphene composite film toughness and flexibility at the same time it can also enhance preparation of J2000 curing agent,
This is because the molecular chain length for the J2000 curing agent being added is able to achieve better flexibility, together in cured epoxy resin molecule
When, avoid molecular weight too long, thus strength reduction.
In the step 4, the solidification, condition of cure is to be determined according to epoxy resin, preferably solidification temperature
It is 110~130 DEG C, curing time is 10~12h.
A kind of long-chain cured epoxy/graphene composite film of the invention is made using the above method.
Long-chain cured epoxy/the graphene composite film, Young's modulus 5-20MPa, elongation at break 10%-
15%, percolation threshold 0.97vol%.
A kind of flexible strain transducer of the invention, including above-mentioned long-chain cured epoxy/graphene composite film.
The flexible strain transducer, conductivity >=10-6S/cm, ga(u)ge factor are 3~15.
Long-chain cured epoxy/graphene composite film of the invention and its preparation method, flexible strain transducer, its advantages exist
In:
1, the graphene raw material that the present invention uses is prepared using combining ultrasonic methods of thermal expansion, obtained graphene microchip
(Graphene platelets) has high regularity and good electric conductivity, and preparation cost is low, with organic polymer
Compatibility preferably.
2, by the present invention in that with the cured epoxy/graphene composite film of curing agent J2000 of long chain, preparation
Epoxy/graphene composite film combines the flexibility of the good electric conductivity of graphene and the cured epoxy resin of J2000, can
As flexible strain transducer, it to be used for health monitoring.
Detailed description of the invention
Fig. 1 is long-chain cured epoxy/graphene composite film preparation method process flow chart of the invention;
Fig. 2 is the Young's modulus curve for the flexible sensor 1~5 that comparative example and Examples 1 to 4 obtain;
Fig. 3 is the tensile strength curve for the flexible sensor 1~5 that comparative example and Examples 1 to 4 obtain;
Fig. 4 is the conductive linearity curve for the flexible sensor 1~5 that comparative example and Examples 1 to 4 obtain;
Fig. 5 is the sensitivity curve for the flexible sensor 2~5 that Examples 1 to 4 obtains;
Fig. 6 is the result of the XPS analysis carbon-to-oxygen ratio for the graphene microchip that the present invention uses.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
In following embodiment, specified otherwise is removed, the reagent of use is commercially available.
In following embodiment, the graphene of use is prepared using following methods:
Step I: 1min is heated by being put into 700 DEG C of Muffle furnace by the graphene intercalation compound (GIC) of intercalation, is obtained
Intercalated graphite alkene intercalation compound after to thermal expansion;
Step II: the intercalated graphite alkene intercalation compound after thermal expansion is put into acetone soln, carries out sonic oscillation 6h,
Obtain mixed solution;
Step III: mixed solution is dried, and the graphene microchip of high regularity can be obtained.
The graphene microchip of preparation, conductivity 1400S/cm.
The graphene microchip of preparation, the result of XPS analysis carbon-to-oxygen ratio are shown in Fig. 6, carbon-to-oxygen ratio 12:1;Its carbon-coating number is
12 layers, with a thickness of 50nm.
In following embodiment, J2000 long-chain curing agent is Jeffamine D2000, has longer strand, is averaged
Molecular weight is 2000g/mol, and total amine value is 0.98~1.05meq/g.
The structural formula of the J2000 long-chain curing agent are as follows:
Wherein, x is the degree of polymerization, chooses 33.
In following embodiment, epoxy resin is WSR618 (E-51).
Embodiment 1
A kind of preparation method of long-chain cured epoxy/graphene composite film, process flow chart are shown in Fig. 1, including following step
It is rapid:
Step 1: preparing material solution
1. first in acetone by graphene uniform dispersion, and at 30 DEG C bathing ultrasonic treatment 1h in ultrasonic cleaning, obtain
To evenly dispersed graphene suspension;Wherein, in mass ratio, graphene: acetone=1:1
2. epoxy resin is added in acetone, stirring obtains uniform epoxy resin acetone soln in 30 minutes, by volume,
Epoxy resin: acetone=1:1.5;
Step 2: preparing reaction solution
Graphene suspension and epoxy resin acetone soln are mixed, 1h is ultrasonically treated, obtains reaction solution;Wherein, it presses
Volume ratio, graphene: (graphene+epoxy resin)=1.25%;
Step 3: removal solvent
Into reaction solution, J2000 long-chain curing agent is added, in mass ratio, J2000 long-chain curing agent and epoxy resin
Ratio is 3:1, carries out heating electromagnetic stirring and ultrasound to remove acetone, obtains mixture.
Step 4: solidification
Then it will solidify 12 hours at mixture at high temperature 120 DEG C, obtain long-chain cured epoxy/graphene composite film
1。
Embodiment 2
A kind of preparation method of long-chain cured epoxy/graphene composite film, with embodiment 1, difference is:
In step 2, by volume, graphene: (graphene+epoxy resin)=2.5%.
The present embodiment obtains long-chain cured epoxy/graphene composite film 2.
Embodiment 3
A kind of preparation method of long-chain cured epoxy/graphene composite film, with embodiment 1, difference is:
In step 2, by volume, graphene: (graphene+epoxy resin)=3.75%.
The present embodiment obtains long-chain cured epoxy/graphene composite film 3.
Embodiment 4
A kind of preparation method of long-chain cured epoxy/graphene composite film, with embodiment 1, difference is:
In step 2, by volume, graphene: (graphene+epoxy resin)=5%.
The present embodiment obtains long-chain cured epoxy/graphene composite film 4.
Comparative example
A kind of preparation method of long-chain cured epoxy resin film, comprising the following steps:
Step 1: preparing material solution
Epoxy resin is added in acetone, stirring obtains uniform epoxy resin acetone soln, by volume, ring in 30 minutes
Oxygen resin: acetone=1:1.5;
Step 2: removal solvent
Into epoxy resin acetone soln, J2000 long-chain curing agent, in mass ratio, J2000 long-chain curing agent and ring is added
The ratio of oxygen resin is 3:1, carries out heating electromagnetic stirring and ultrasound to remove acetone, obtains mixture.
Step 4: solidification
Then it will solidify 12 hours at mixture at high temperature 120 DEG C, obtain long-chain cured epoxy resin film 1.
Experimental example
Long-chain cured epoxy/graphene composite film 1~4 prepared by Examples 1 to 4, according to long-chain cured epoxy/graphite
Alkene composite membrane flexible sensor shape is cut, and the first conductive silver paste and the second conductive silver is respectively coated in its opposite two sides
First conductive silver paste is drawn the first conducting wire by slurry, and the second conductive silver paste draws the second conducting wire, obtains long-chain cured epoxy/graphite
Alkene composite membrane flexible sensor 1~4;
The long-chain cured epoxy resin film that will be prepared in comparative example, it is flexible according to long-chain cured epoxy/graphene composite film
Sensor shape is cut, and the first conductive silver paste and the second conductive silver paste is respectively coated in its opposite two sides, first is led
Electric silver paste draws the first conducting wire, and the second conductive silver paste draws the second conducting wire, obtains long-chain cured epoxy resin film flexible sensor
5;
The flexible sensor 1~5 of above-mentioned preparation is tested, Young's modulus is obtained, with graphene volume content
Difference, Young's modulus curve is shown in Fig. 2, as can be drawn from Figure 2 with the raising of graphene content, the flexible sensor poplar of preparation
Family name's modulus improves.
The flexible sensor 1~5 of above-mentioned preparation is tested, tensile strength is obtained, with graphene volume content
Difference, tensile strength curve is shown in Fig. 3, as can be drawn from Figure 3 with the raising of graphene content, the flexible sensor of preparation
Tensile strength improves.
The flexible sensor 1~5 of above-mentioned preparation is tested, obtains conductivity, and be to the volume content of graphene
0.7%, the flexible sensor of 0.5%, 0.3% preparation is tested, and with the difference of graphene volume content, conductivity is bent
Line is shown in Fig. 4, and graphene volume content presented and acutely increases before 1% as can be drawn from Figure 4, after reaching 1%, conductivity
Steady growth.
The flexible sensor 1~5 of above-mentioned preparation is tested, sensitivity is obtained, with graphene volume content
Difference, sensitivity curve are shown in Fig. 5, are as can be drawn from Figure 5 1.25% in graphene volume content, with the raising of strain,
It is fluctuated acutely, and is 2.5%, 3.75%, 5% in graphene volume content, relatively stable.
Claims (10)
1. a kind of preparation method of long-chain cured epoxy/graphene composite film, which comprises the following steps:
Step 1: preparing material solution
(1) in acetone by graphene uniform dispersion, it is uniformly mixed in 10~30 DEG C of sonic oscillations, obtains evenly dispersed graphite
Alkene suspension;Wherein, the dosage of acetone be can be fully dispersed by graphene amount;
(2) in acetone by epoxy resin dissolution, it stirs evenly, obtains epoxy resin acetone soln;Wherein, the dosage of acetone is
The amount that epoxy resin can be sufficiently dissolved;
Step 2: preparing reaction solution
Graphene suspension and epoxy resin acetone soln are mixed, ultrasonic mixing is uniform, obtains reaction solution;Wherein, by body
Product ratio, graphene: (graphene+epoxy resin)=1.25%~5%;
Step 3: removal solvent
Into reaction solution, J2000 long-chain curing agent is added, stirs ultrasound removal acetone, obtains mixture;Wherein, by quality
Than J2000 long-chain curing agent: epoxy resin=3:1:
Step 4: solidification
Mixture is poured into mold, solidified, obtain long-chain cured epoxy/graphene composite film.
2. the preparation method of long-chain cured epoxy/graphene composite film as described in claim 1, which is characterized in that described
In step 1 (1), the graphene is the graphene microchip of high regularity, and carbon-to-oxygen ratio C/O is (12~13): 1, conductance
Rate is 1300~1400S/cm;Carbon-coating number >=10 layer of the graphene microchip, thickness are at 5~100 nanometers.
3. the preparation method of long-chain cured epoxy/graphene composite film as claimed in claim 2, which is characterized in that described
The graphene microchip of high regularity is made using following graphene preparation method:
Step I: 1min is heated by being put into 650~750 DEG C of Muffle furnace by the graphene intercalation compound of intercalation, obtains heat
Intercalated graphite alkene intercalation compound after expansion;
Step II: the intercalated graphite alkene intercalation compound after thermal expansion is put into acetone soln, is carried out sonic oscillation 4-8h, is obtained
To mixed solution;
Step III: mixed solution is dried, and the graphene microchip of high regularity can be obtained.
4. the preparation method of long-chain cured epoxy/graphene composite film as described in claim 1, which is characterized in that described
In step 1 (2), the epoxy resin is WSR618 (E-51), epoxide equivalent 184-200g/eq.
5. the preparation method of long-chain cured epoxy/graphene composite film as described in claim 1, which is characterized in that described
In step 3, the stirring ultrasound removal acetone method particularly includes: be heated to 50~70 DEG C and be stirred to react 20~50min.
6. the preparation method of long-chain cured epoxy/graphene composite film as described in claim 1, which is characterized in that described
In step 3, the J2000 long-chain curing agent is Jeffamine D2000, average molecular weight 2000g/mol, total amine value
For 0.98~1.05meq/g;
The structural formula of the J2000 long-chain curing agent are as follows:
Wherein, x is the degree of polymerization, chooses 32~34.
7. the preparation method of long-chain cured epoxy/graphene composite film as described in claim 1, which is characterized in that described
In step 4, the solidification, condition of cure is to be determined according to epoxy resin, and solidification temperature is 110~130 DEG C, curing time
For 10~12h.
8. a kind of long-chain cured epoxy/graphene composite film, which is characterized in that the long-chain cured epoxy/graphene composite film is adopted
The method described in claim 1~7 any one is made.
9. long-chain cured epoxy/graphene composite film as claimed in claim 8, which is characterized in that the long-chain solidifies ring
Oxygen/graphene composite film, Young's modulus 5-20MPa, elongation at break 10%-15%, percolation threshold are
0.97vol%.
10. a kind of flexibility strain transducer, which is characterized in that including claim long-chain cured epoxy/graphene composite film;Institute
The flexible strain transducer stated, conductivity >=10-6S/cm, ga(u)ge factor are 3~15.
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