CN105400119B - A kind of electro shape memory composite material and preparation method and application - Google Patents
A kind of electro shape memory composite material and preparation method and application Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L53/02—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/28—Treatment by wave energy or particle radiation
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
- F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
- F04B43/00—Machines, pumps, or pumping installations having flexible working members
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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
- C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2353/02—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers of vinyl aromatic monomers and conjugated dienes
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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
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
Abstract
A kind of electro shape memory composite material and preparation method and application, the composite material can be by styrene-isoprene-styrene block copolymer and low density polyethylene (LDPE) (SIS/LDPE) according to mass ratio 60：40~80：20 crosslinking by radiation obtain polymeric matrix, then add the graphite blending equivalent to polymeric matrix mass fraction 6%~30% and are made.Preparation method and application present invention additionally comprises electroluminescent graphite/SIS/LDPE composite materials.Electroluminescent graphite/SIS/LDPE composite materials of the present invention have electro-induced shape memory effect.It is demonstrated experimentally that when content of graphite is higher than 6%, graphite/SIS/LDPE composite materials have good electro-induced shape memory effect；Meanwhile under certain voltage effect, deformation-recovery rate is up to 100%, and the response time reduces with the increase of content of graphite, and with the increase of voltage, the response time of sample shortens；In addition, repeatedly electroluminescent circulation shape memory test shows that deformation-recovery rate is above 95%.
Description
Technical field
The present invention relates to a kind of shape-memory material and preparation method and application, and in particular to a kind of electro shape memory
Composite material and preparation method and application.
Background technology
Shape-memory polymer refers to polymer (such as heat, light, the electricity, PH) implementation under certain conditions to figuration
Deformation, this deformation can be saved, and when stimulating again it, polymer can return to original figuration state again
Material.Since the 1980s, shape-memory polymer obtains very big development, and with thermotropic shape memory polymers
The development of thing is the most ripe.Compared with marmem and shape memory ceramics, shape-memory polymer have weight it is small, into
The advantages that this is low, deformation is big, easy processing.Therefore, shape-memory polymer is shown in intelligent active deformation structural research field
Huge application potential, has started to be widely used in the fields such as aerospace, srnart biomaterials and insulated enclosure.
At present, shape-memory polymer strongly limit shape note due to itself relatively low mechanical property and recovery of shape power
Recall the application field of polymer, in order to overcome the drawbacks described above that shape-memory polymer occurs, numerous scholars have carried out largely
Experimental study.Wherein, most efficient method is to use organic or inorganic additive to improve the modulus of shape-memory polymer.Example
Such as, nano whisker is added in shape memory polyurethane by Luo et al., it is found that the modulus of material greatly increases, while shape
The shape fixed rate of shape memory polyurethane increases with the increase of Whisker Content.But after the content of whisker is more than 23%, shape
The shape fixed rate of shape memory polyurethane will drastically reduce.Lv of Harbin Institute of Technology et al. is fine using carbon black and chopped carbon
Dimension enhancing shape memory styrene resin, is made a kind of advanced composite material (ACM), in the composite, the content of carbon black is fixed on
5%, and the content of chopped carbon fiber progressively increases to 2% from 0.5%.Test result indicates that when content of carbon black is 5%, it is and short
When the content for cutting carbon fiber is 2%, 160% and 200% is respectively increased in the mechanical property and heat conductivity of composite material.In addition,
The glass transition temperature of composite material has also brought up to 57.28 DEG C from 46.38 DEG C, it is seen then that the carbon black of addition and chopped carbon are fine
Tie up and have a great influence to the glass transition temperature of composite material.
Therefore, a kind of electro shape memory composite material with excellent mechanical performances and recovery of shape power is developed,
It is the task of top priority of shape-memory polymer research.
The content of the invention
The technical problem to be solved by the invention is to provide a kind of electroluminescent with excellent mechanical performances and recovery of shape power
Composite material of shape memory and preparation method and application.
It is a kind of electro shape memory composite material that the present invention, which solves the technical solution that its technical problem uses, can be by benzene
Ethene-isoprene-styrene block copolymer is with low density polyethylene (LDPE) (SIS/LDPE) according to mass ratio 60：40~80：20
Crosslinking by radiation obtains polymeric matrix, then add equivalent to polymeric matrix mass fraction 6%~30% graphite (preferably
12%~24%, more preferably 18%~24%, most preferably 24%) blending is made.
Further, the crosslinking with radiation is crosslinked for gamma-ray irradiation.
Further, the gamma-ray irradiation dosage be respectively 50~250KGy (preferably 50~150KGy, more preferably
100KGy)。
The technical solution that the present invention further solves the use of its technical problem is a kind of electro shape memory composite material,
First by styrene-isoprene-styrene block copolymer and low density polyethylene (LDPE) (SIS/LDPE) according to mass ratio 60：40~
80：20 crosslinking by radiation obtain polymeric matrix, then add the graphite equivalent to polymeric matrix mass fraction 6%~30%
Blending,.
The technical solution that the present invention further solves the use of its technical problem is that a kind of electro shape memory composite material exists
The application in Micropump in MEMS.
The present invention obtains the polymeric matrix with shape memory characteristic with cross-linking radiation SIS/LDPE, and graphite is filled out for conduction
Material is successfully prepared a kind of new conducing composite material with electro-induced shape memory effect.It is demonstrated experimentally that in SIS/LDPE
The modulus and tensile strength of composite material can be significantly improved after adding graphite in matrix, and conductive network can be formed in the base,
Composite material is set to possess conductive characteristic.When content of graphite is higher than 6%, graphite/SIS/LDPE composite materials have good electricity
Cause shape memory characteristic；Meanwhile under certain voltage effect, deformation-recovery rate is up to 100%, and the response time is with content of graphite
Increase and reduce, with the increase of voltage, the response time of sample shortens；In addition, repeatedly electroluminescent circulation shape memory tests table
Bright deformation-recovery rate is above 95%.
Brief description of the drawings
Fig. 1 is the shape memory model of composite material of the present invention.
Fig. 2 is the gel content of cross-linking radiation SIS/LDPE blends.
The SEM that Fig. 3 is graphite/SIS/LDPE schemes.
Fig. 4 is the DMA curves of graphite/SIS/LDPE composite materials.
Fig. 5 is the Mechanics Performance Testing of graphite/SIS/LDPE composite materials at room temperature.
Fig. 6 is influence of the cycle-index to graphite/SIS/LDPE composite shapes response rates.
Embodiment
The invention will be further described with attached drawing with reference to embodiments.
1st, primary raw material
SIS, 1209, S/I=29/71, yueyang, hunan Ba Ling petrochemical industry Co., Ltd；LDPE, the limited public affairs of Beijing Yanshan Petrochemical
Department；Graphite, Qingdao Xing Yuan Graphite Companies；Toluene, Tianjin Jin Dong Tian Zheng fine chemistries chemical reagent work；Acetone, Jin Dong days, Tianjin
Positive fine chemistry chemical reagent work.
2nd, instrument and equipment
Opening rubber mixing machine：X (S) K-400, Qingdao Xincheng Yiming Rubber Machinery Co., Ltd；Vulcanizing press：XLZ-
25T types, No.3 Rubber Machinery Factory, Qingdao；Tensile testing machine：AI-7000M types, high ferro Science and Technology Co., Ltd.；Differential scanning
Calorimeter, DSC-200F3, German Nai Chi companies；DMA dynamic mechanical analysis instrument：Q800, TA companies of the U.S.；Scanning electron microscope：S-
4800, Hitachi, Japan.
Embodiment 1
1st, the preparation of electro shape memory composite material：The sample of SIS/LDPE=30/70 is encapsulated in polybag,
Limitation air under conditions of use irradiation bomb for60The gamma-ray irradiation of Co, irradiation dose is respectively 50,100,150,200,
250KGy, it is 12% graphite then to add content, after mixing, is kneaded in X (S) K-400 rubber mixing machines, at a temperature of 180 DEG C, makes
Become and be kneaded uniform material.
2nd, performance test
Tensile strength is measured with reference to GB1039-1992, draw speed 100mm/min.
Gel content determining：Sample is shredded and weighs 0.5g or so, is wrapped in 300 mesh copper mesh, using toluene as solvent,
Ebuillition of heated reflux 72h in Soxhlet extractor.Sample bag is then taken out, is washed twice with acetone, 6h is dried in vacuo at 60 DEG C, takes
Go out to weigh quality, gel content is can be calculated through formula (1).
Gel content=(m2-m1)/m0× 100% (1)
In formula：m0Sample mass (g) before being tested for gel；m1For the quality (g) of copper mesh；m2For the quality of gel and copper mesh
(g)。
Resistivity：With the resistance value of UT61E type digital multimeter test samples, and calculate with formula (2) resistance of sample
Rate.
In formula：R is the resistance value of sample, and b is the width of sample, and d is the thickness of sample, and l is the length of sample.
Dsc analysis：From room temperature to 130 DEG C, 10 DEG C/min of heating rate.
Dynamic mechanical (DMA)：Specimen size is 2 × 12 × 30mm3, test frequency 1Hz, heating rate for 3 DEG C/
Min, amplitude 10um.
Shape memory is tested：Using the electro shape memory process of U-bend model evaluation composite material, as shown in Figure 1.
Sample is heated to more than melting temperature Tm first, by rectangle sample (100 × 10 × 2mm3) bend to U-shaped, holding stress
And cool down rapidly to fix deformation.Then apply certain voltage to sample, record sample replys angle (θi-θf) with the change of time
Change (t).Then recovery of shape speed is θi/ t, deformation-recovery rate are (θi-θf)/θi。
3rd, the results and discussion of the gel content of composite material, electrical property, DMA, electro shape memory
(1) gel content
The Shape memory behavior of composite material is studied, performance shadow of the irradiation dose to SIS/LDPE blends should be studied first
Ring to select to be adapted to the matrix of composite material.Therefore, the present invention first analyzes the degree of cross linking of SIS/LDPE blends,
The gel content of cross-linking radiation SIS/LDPE blends, as shown in Figure 2.
As shown in Figure 2, SIS/LDPE blends increase with the increase degree of cross linking of absorbed dose of radiation, when absorbed dose of radiation reaches
During 200KGy, the gel content of blend tends to balance, and the degree of cross linking reaches about 85%.This is because cobalt -60 can be sent out in decay
Two gamma-rays are projected, energy is 1.173MeV and 1.332MeV respectively, and the gamma-rays of this high energy is enough to open macromolecular chain
Chemical bond in section, generates free radicals it, and then triggers radical crosslinking reaction.But when irradiation dose is smaller, SBS/
The free radical produced in LDPE blends is few, and the cross-linking reaction that free radical triggers is also few.Therefore, the degree of cross linking is relatively low, on the contrary then hand over
Connection degree increases.
After tested, when irradiation dose is 50-150kGy, the degree of cross linking of blend is 44%-77%, and SIS/ at this time
LDPE blends have preferable thermal shape memory behavior.Therefore, the present invention select irradiation dose for 100kGy as graphite/
The irradiation dose of SIS/LDPE composite materials, tests through gel and finds that influence of the graphite to the degree of cross linking of matrix is smaller, therefore graphite/
The degree of cross linking of SIS/LDPE composite materials be SIS/LDPE blends the degree of cross linking, i.e., 61.59%.
(2) electrical property of sample
The volume resistance and volume resistivity of table 1- composite materials
| Samples | R/Ω | ρ/Ω·cm |
| 6%Graphite/SIS/LDPE | 27.5×103 | 549.2 |
| 12%Graphite/SIS/LDPE | 965.7 | 19.314 |
| 18%Graphite/SIS/LDPE | 316.4 | 6.328 |
| 24%Graphite/SIS/LDPE | 66.48 | 1.3296 |
| 30%Graphite/SIS/LDPE | 32.05 | 0.641 |
As shown in Table 1, as the increase of content of graphite, the volume resistivity of sample are gradually reduced.When content of graphite reaches
When 12%, the volume resistivity of sample is down to 19.314 Ω cm, this shows that sample has been conductor at this time, and SIS/LDPE is blended
Thing is insulator, thus illustrates that composite material realizes the transformation from insulator to conductor.At this time, in composite system,
Conductive network has been formed, and with the increase of content of graphite, the conductive network of composite material can more crypto set, therefore composite bodies
The electric conductivity of system improves.
The SEM figures of graphite/SIS/LDPE, as shown in Figure 3.From the figure 3, it may be seen that when content of graphite is 6%, graphite is in SIS/
Scattered laxer in LDPE blends, gap is larger between graphite.And when content reaches 24%, the dispersed phase pair of graphite
Compare concentration and quantity showed increased, the gap between graphite is obviously reduced, this is conducive to composite material and forms conductive network.By
This understands that the resistivity of composite material is gradually reduced with the increase of content of graphite.
(3) dynamic mechanical (DMA)
The DMA curves of graphite/SIS/LDPE composite materials, as shown in Figure 4.As shown in Figure 4, with the increasing of content of graphite
Add, the storage modulus increase of composite material.When content of graphite is 24%, the storage modulus of composite material increased dramatically, reachable
The addition of this explanation graphite of 250MPa. can effectively improve the modulus of composite material.In addition, according to pertinent literature, work as temperature
When degree is less than shape memory transition temperature, the high 2-3 quantity of storage modulus when its storage modulus is than more than transfer of shapes temperature
Level.Meanwhile analyzed from Fig. 4, when temperature is -40 DEG C, the storage modulus of 24% graphite/SIS/LDPE composite materials is
253.7MPa, and when temperature is 120 DEG C, its storage modulus is only 1.211MPa.Thus graphite/SIS/LDPE composite woods are illustrated
Material meets that above-mentioned condition can become a kind of more satisfactory composite material of shape memory.
(4) mechanical property
The Mechanics Performance Testing of graphite/SIS/LDPE composite materials at room temperature, as shown in Figure 5.As shown in Figure 5, graphite/
The tensile strength of SIS/LDPE composite materials gradually increases with the increase of content of graphite, and when content of graphite is higher than 24%,
The tensile strength of composite material tends to balance substantially, illustrates that graphite can significantly improve the mechanical property of composite material.And work as stone
When black content is higher than 24%, graphite realizes dispersed more difficulty, easily produces agglomeration since content is more.Therefore,
When content of graphite is 32%, the tensile strength of composite material does not obtain raising significantly.In addition, also known by Fig. 5,
With the increase of content of graphite, the elongation at break of composite material gradually reduces.When content of graphite reaches 24%, composite material
Elongation at break is restrained, this is because after adding graphite in SIS/LDPE matrixes, graphite hinders molecule segment in matrix
Free movement, caused by causing the toughness of material to reduce.
(5) electro shape memory is analyzed
The turnaround time of graphite/SIS/LDPE composite materials under table 2- different voltages
| Samples | 20V | 40V | 60V | 80V | 100V | 120V |
| 6%Graphite/SIS/LDPE | — | — | — | — | — | — |
| 12%Graphite/SIS/LDPE | — | — | — | 267s | 62.7 | 28s |
| 18%Graphite/SIS/LDPE | — | 90s | 42s | 18s | 11s | 2s |
| 24%Graphite/SIS/LDPE | 285s | 23s | 13s | 5.3s | 2.1s | >2s |
| 30%Graphite/SIS/LDPE | 206s | 14s | 3s | >2s | >1s | >1s |
The graphite of different content/turnaround time of the SIS/LDPE composite materials under different voltage, is shown in Table 2.Can by table 2
Know, when content of graphite is 6%, the shape of composite material cannot reply；When content of graphite is 12%, composite material is in 80V
Voltage under can return back to original shape and be gradually reduced with its turnaround time of the increase of voltage；When content of graphite increases to 18%
When, composite material only can be replied easily completely with 90s under the voltage of 40V；And when content of graphite reaches 24%, it is only necessary to
The low pressure of 20V can cause composite material to be replied completely.In addition, when content of graphite is identical, with alive enhancing is applied, again
The recovery rate of condensation material is gradually accelerated, this is related with the resistivity of composite material, and the resistivity of composite material is smaller, then its time
Complex velocity is faster.It follows that content of graphite and apply voltage be determine composite material electro shape memory performance it is crucial because
Element.When content of graphite is higher than 6%, composite material can return back to original shape under voltage stimulation.And with the increasing of content of graphite
Add, composite material can realize recovery of shape and the response of the increase sample with voltage rapidly in the case where the voltage of smaller stimulates
Time shortens.
Under 80V voltages, after circulation electro shape memory test is carried out to graphite/SIS/LDPE composite materials, composite wood
The shape recovery rate of material, as shown in Figure 6.It will be appreciated from fig. 6 that preceding 2 circulations influence less the electro shape memory performance of sample,
But as the shape recovery rate of the increase composite material of cycle-index slightly reduces.This be probably due in bending repeatedly and
The distribution of graphite in the sample receives influence in Recovery Process, and conductive network can be subject to caused by a degree of destruction.In addition, by
Fig. 6 is also known, although cycle-index has a certain impact shape recovery rate, its shape recovery rate is still more than 95%,
This fully shows that graphite/SIS/LDPE composite materials are a kind of electro shape memory materials well.
Embodiment 2：The preparation of electroluminescent graphite/SIS/LDPE composite materials
By SIS:The sample of LDPE=30/70 is encapsulated in polybag, used under conditions of air of limiting the quantity irradiation bomb for60The gamma-ray irradiation of Co, irradiation dose are respectively 100KGy, and it is 24% graphite then to add content, after mixing, in XLZ-25T
It is molded on type vulcanizing press, controls 180 DEG C of mold temperature, pressure 10MPa, then cools down 10min, and thickness is made about
The blend thin slice of 2mm.
Embodiment 3：Using
By electroluminescent graphite/SIS/LDPE composite sheets in embodiment 2, in the Micropump in MEMS,
In the case where applying 20-120v voltages, there is the ability that deformation can recover completely, and be suitable for large deformation.
Claims (8)
1. a kind of electro shape memory composite material, it is characterised in that can be by styrene-isoprene-phenylethene block copolymerization
Thing is with low density polyethylene (LDPE) according to mass ratio 60：40~80：20 crosslinking by radiation obtain polymeric matrix, then add equivalent to
The graphite blending of polymeric matrix mass fraction 6%~30% is made；
The crosslinking with radiation is crosslinked for gamma-ray irradiation；
The gamma-ray irradiation dosage is respectively 50~250KGy.
2. electro shape memory composite material according to claim 1, it is characterised in that the mass fraction of the graphite is
Polymeric matrix mass fraction 12%~24%.
3. electro shape memory composite material according to claim 2, it is characterised in that the mass fraction of the graphite is
Polymeric matrix mass fraction 18%~24%.
4. electro shape memory composite material according to claim 3, it is characterised in that the mass fraction of the graphite is
Polymeric matrix mass fraction 24%.
5. electro shape memory composite material according to claim 1, it is characterised in that the gamma-ray irradiation dosage point
Wei not 50~150KGy.
6. electro shape memory composite material according to claim 1, it is characterised in that the gamma-ray irradiation dosage point
Wei not 100KGy.
A kind of 7. preparation method of electro shape memory composite material as described in one of claim 1~6, it is characterised in that
First by styrene-isoprene-styrene block copolymer and low density polyethylene (LDPE) according to mass ratio 60：40~80：20 through spoke
Penetrate crosslinking and obtain polymeric matrix, then add the graphite blending equivalent to polymeric matrix mass fraction 6%~30%, i.e.,
Into.
8. in Micropump of the electro shape memory composite material in MEMS according to one of claim 1~6
Using.
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