CN110117408A - A method of using nano multilayer graphene toughening composition interlayer - Google Patents
A method of using nano multilayer graphene toughening composition interlayer Download PDFInfo
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- CN110117408A CN110117408A CN201910370572.1A CN201910370572A CN110117408A CN 110117408 A CN110117408 A CN 110117408A CN 201910370572 A CN201910370572 A CN 201910370572A CN 110117408 A CN110117408 A CN 110117408A
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- prepreg
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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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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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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
- C08K2201/011—Nanostructured additives
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention belongs to carbon fiber/base layer of resin to close composite material manufacture and mechanical property field, be related to a kind of method of nano multilayer graphene toughening composition interlayer.The present invention selects toughening material of the lower cost nano multilayer graphene as material prepreg interlayer, after prepreg cuts out completion, it is quantitatively put in proportion into acetone or alcohol liquid and abundant disperse is carried out by ultrasonic wave, again by the uniform spray attachment of pneumatic gun on prepreg surface, the paving for carrying out prepreg is evaporated completely to acetone or alcohol, it is re-fed into autoclave and carries out heat-pressure curing, it is finally cut into DCB and ENF standard sample carries out I type and II type fracture toughness test, test result shows that the material is spraying density as 1g/m2When GICWith GIICIt is obviously improved, improves the interlaminal toughness of composite laminated structures, compensate for the deficiency of laminated composite interlayer performance.
Description
Technical field
The invention belongs to thermosetting property carbon fiber/polymer matrix composites technique preparation field, in particular to a kind of nanometer is more
The method of layer graphene toughening composition interlayer.
Background technique
At present resin base continuous fibers composite material in aviation field using relatively broad, have specific stiffness and specific strength compared with
High, antifatigue, corrosion resistant advantage such as reaches 50% or more in 787 structure dosage of Boeing.Resin base continuous fibers prepreg is multiple
Material of the condensation material as aircraft surfaces structure, layering is easy to produce when being impacted, and greatly reduces holding for structure used
Loading capability, therefore resin base continuous fibers prepreg composite carries out interlayer toughened, improves its anti-vertical resolution.Nanometer multilayer
Graphene is a kind of new material, is used as conductive material according to the attribute of material itself at present.
Nano material being directly dissolved in resin, then the mixing and integral heat pressure that carry out with fiber solidify, technique is relative complex,
The nano material for needing to be added is more, will affect the non-interlayer performance of composite material.Chinese patent (CN107459820A) discloses
A kind of preparation method of micro-and nano-particles collaboration interlayer toughened span carbon fibre composite comprising following steps " multiphase
It is compound " the compound low viscosity resin system of method acquisition solid-liquid, it disperses thermoplasticity micro particles and core-shell nano in by alkene
In the liquid toughener of compound and epoxy composite, span micro mist is then added and premix uniformly, then is placed in three
Physical blending on roller mill makes micro-and nano-particles evenly dispersed, obtains toughening bismaleimide resin by shearing and diffusion
Above-mentioned bismaleimide resin system in film, is then presoaked with carbon fiber reinforcement hot pressing compound by system, is acted on the sieving of fiber
Prepreg is cut and is layed in mold by the prepreg that multiple dimensioned micro-and nano-particles are enriched between acquisition reinforcement surface and synnema,
The composite material of micro-and nano-particles collaboration interlayer toughened is obtained using compression molding.This method obtains preferable interlayer performance, but
It is that technique is still complex, while nano material is dissolved in resin to change stiffness and strength in prepreg；And this Shen
Please in only test GIC, other materials is not recorded, such as GIICDetection.
Chinese patent (CN104945852A) discloses a kind of micro-and nano-particles interlayer toughened technology, first by the micro-nano grain of rice
Son is the mixed solution even application of inorganic particulate on fiber, is subsequently placed in baking oven and is dried, is evaporated completely to solvent
Quan Houzai is compound with thermosetting resin, and the composite material of micro-and nano-particles interlayer toughened is made, although this method significantly improves
The interlaminar fracture toughness work of composite material, but moulding process is complex and at high cost, needs first to spray on fiber, can change
The interface bond strength of material itself, and the superpower carbon nano-tube material of performance in recent years is not used.
Summary of the invention
Technical problems to be solved:
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of use nano multilayer graphene toughening composite wood
Method between the bed of material using the method toughening sprayed in each interlayer of prepreg, simple process, and uses lower cost, surpasses
The nano multilayer graphene of strong mechanical performance, which carries out quantitatively controllable spray attachment to prepreg surface, will not change to composite material itself
Attribute.
The technical scheme is that a kind of method using nano multilayer graphene toughening composition interlayer, special
Sign is that specific step is as follows:
Step 1: material of the nano multilayer graphene as composite material interlayer toughening, the nanometer multilayer graphite are selected
The lamella diameter of alkene is 15-50 μm, and purity is 95wt% or more；
Step 2: the nano multilayer graphene is shaken more in ethyl alcohol or acetone using ultrasonic dispersion method
It dissipates, shaking the time at room temperature is 10-15 minutes；
Step 3: after the completion of resin base continuous fibers material prepreg is cut out, disperse is had using spraying apparatus
The uniform spray attachment of acetone or alcohol solution of nano multilayer graphene is in the surface of each interlayer of the prepreg, until the prepreg
Until disperse needed for each layer surface has the acetone or alcohol solution of nano multilayer graphene to spray；The every layer surface of prepreg
Spray attachment surface density is 1g/m2；
Step 4: will be sprayed in step 3 completion the prepreg carry out paving and and solidification of hot-press tank, the preimpregnation
Temperature is 80-130 DEG C when material solidification, pressure 0.4MPa.
A further technical solution of the present invention is: the resin base continuous fibers material prepreg is multiple for epoxy resin
Condensation material prepreg.
A further technical solution of the present invention is: the spraying apparatus is the air gun with gas source.
Beneficial effect
The beneficial effects of the present invention are: the present invention carries out interlayer increasing using the nano multilayer graphene of superelevation mechanical property
It is tough, and the surface spray treatment of each interlayer is directly carried out by simple spray attachment technique to the prepreg of semi-finished product, it greatly simplifies
Technique, and spray attachment density is precisely controllable.
Disperse is had the uniform spray attachment of acetone or alcohol solution of nano multilayer graphene in tree by the present invention using spraying apparatus
It the surface of each interlayer of aliphatic radical continuous fiber composite material prepreg can by being sprayed to each layer of prepreg of surface
Enhance the fracture toughness of composite material interlayer, and the attribute of composite material itself will not be changed；Simultaneously in resin base continuous fibers
The spray attachment surface density of the every layer surface of material prepreg is 1g/m2, Resisting fractre toughness effect is enabled to reach best.
Using the method for the present invention prepare toughening after composite laminated structures be machined into double cantilever beam DCB and
Two kinds of samples of end cut ENF, for testing the variation of one, two type fracture toughnesses, the spray attachment technique of nano multilayer graphene
I type fracture toughness G of the prepared DCB sample compared with the former DCB sample of non-tougheningICImprove 103.2%.；Nanometer multilayer graphite
II type fracture toughness G of the ENF sample prepared by the spray attachment technique of alkene compared with the former ENF sample of non-tougheningIICImprove 67.8%.
Specific effect is described in detail by attached drawing and following instance comparison.
Detailed description of the invention
Fig. 1 is nano multilayer graphene toughening composition interlayer toughened schematic diagram；
Fig. 2 is the explanatory diagram of composite sample preparation process in example 1 and example 2；
Fig. 3 is DCB composite sample sizing specification figure in example 1；
Fig. 4 is that ENF composite sample loads explanatory diagram in example 2.
Specific embodiment
The embodiments described below with reference to the accompanying drawings are exemplary, it is intended to be used to explain the present invention, and cannot understand
For limitation of the present invention.
Embodiment 1:
Nano multilayer graphene toughening T700 (production of toray company) epoxy resin composite material, specifically includes following
The nano multilayer graphene that step: (1) selecting lower cost and is easier to obtain is as composite laminated structures interlayer toughened
Material, the lamella diameter range of nano multilayer graphene are 15-50 μm, and purity is 95wt% or more, and in high-precision quality
The good 0.5g of scale on scale；(2) nano multilayer graphene is sufficiently shaken in ethyl alcohol or acetone using " ultrasonic dispersion method "
Disperse, vibration time are 10-15 minutes, and temperature is 20 DEG C；(3) after the completion of cutting out epoxy resin composite material prepreg, in advance
Leaching material surface area is 0.5m2, have the acetone or alcohol solution of nano multilayer graphene uniform disperse using the air gun with gas source
Spray attachment has the third of nanometer multilayer graphite in the surface of each interlayer of the prepreg, the disperse needed for each layer surface of the prepreg
Until ketone or ethanol solution have sprayed；The spray attachment surface density of the every layer surface of prepreg is 1g/m2；(4) by production in step (3)
Good prepreg carries out paving and solidification of hot-press tank, and prepreg solidification carries out autoclave using 120 DEG C of temperature and 0.4MPa pressure
Solidification, curing time 10 hours；(5) whole composite material plank is cut into DCB standard sample, and is stained with metal plate anchorage.
Embodiment 2:
Nano multilayer graphene toughening T700 (production of toray company) epoxy resin composite material, specifically include with
The nano multilayer graphene that lower step: (1) selecting lower cost and is easier to obtain is as composite laminated structures interlayer toughened
Material, the lamella diameter range of nano multilayer graphene is 15-50 μm, and purity is 95wt% or more, and in high-precision matter
Measure the good 0.6g of scale on scale；(2) nano multilayer graphene is sufficiently shaken in ethyl alcohol or acetone using " ultrasonic dispersion method "
Dynamic disperse, vibration time are 10-15 minutes, and temperature is 20 DEG C；(3) after the completion of epoxy resin composite material prepreg being cut out,
Prepreg surface area is 0.6m2,There is the acetone or alcohol solution of nano multilayer graphene uniform disperse using the air gun with gas source
Spray attachment has nano multilayer graphene in the surface of each interlayer of the prepreg, the disperse needed for each layer surface of the prepreg
Until acetone or alcohol solution has sprayed；The spray attachment surface density of the every layer surface of prepreg is 1g/m2；(4) by system in step (3)
The prepreg performed carries out paving and solidification of hot-press tank, and prepreg solidification should use 120 DEG C of temperature and 0.4MPa pressure to carry out heat
Tank is pressed to solidify, curing time 10 hours；(5) whole composite material plank is cut into ENF standard sample.
Fracture toughness between table 1T700/ epoxide resin nano multiple graphene layers
| Toughening material | 1 G of embodimentIC(J/m2) | 2 G of embodimentIIC(J/m2) |
| Nothing | 265.3 | 871.2 |
| Nano multilayer graphene | 539.1 | 1462.0 |
1 data of table explanation:
Former DCB sample of the DCB sample prepared by spray attachment technique by 1 nano multilayer graphene of embodiment compared with non-toughening
I type fracture toughness GICImprove 103.2%.The examination of ENF prepared by spray attachment technique by 2 nano multilayer graphene of embodiment
II type fracture toughness G of the sample compared with the former ENF sample of non-tougheningIICImprove 67.8%.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (3)
1. a kind of method using nano multilayer graphene toughening composition interlayer, it is characterised in that specific step is as follows:
Step 1: selecting material of the nano multilayer graphene as composite material interlayer toughening, the nano multilayer graphene
Lamella diameter is 15-50 μm, and purity is 95wt% or more；
Step 2: carrying out vibration disperse for the nano multilayer graphene using ultrasonic dispersion method in ethyl alcohol or acetone,
The vibration time is 10-15 minutes at room temperature；
Step 3: after the completion of resin base continuous fibers material prepreg is cut out, disperse there is into nanometer using spraying apparatus
The uniform spray attachment of acetone or alcohol solution of multi-layer graphene is in the surface of each interlayer of the prepreg, until each layer of the prepreg
Until disperse needed for surface has the acetone or alcohol solution of nano multilayer graphene to spray；The spray attachment of the every layer surface of prepreg
Surface density is 1g/m2；
Step 4: the prepreg for spraying completion in step 3 is subjected to paving and is consolidated with solidification of hot-press tank, the prepreg
Temperature is 80-130 DEG C when change, pressure 0.4MPa.
2. using the method for nano multilayer graphene toughening composition interlayer according to claim 1, it is characterised in that: institute
Stating resin base continuous fibers material prepreg is epoxy resin composite material prepreg.
3. using the method for nano multilayer graphene toughening composition interlayer according to claim 1, it is characterised in that: institute
Stating spraying apparatus is the air gun with gas source.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910370572.1A CN110117408A (en) | 2019-05-06 | 2019-05-06 | A method of using nano multilayer graphene toughening composition interlayer |
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| CN201910370572.1A CN110117408A (en) | 2019-05-06 | 2019-05-06 | A method of using nano multilayer graphene toughening composition interlayer |
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| CN201910370572.1A Pending CN110117408A (en) | 2019-05-06 | 2019-05-06 | A method of using nano multilayer graphene toughening composition interlayer |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021092788A1 (en) * | 2019-11-13 | 2021-05-20 | 远景能源有限公司 | Method and apparatus for use in manufacturing graphene-modified fiber reinforced material |
| CN113402755A (en) * | 2021-06-04 | 2021-09-17 | 西北工业大学 | Interlayer toughening method for multi-walled carbon nanotube of military aircraft composite material hot patch |
| GB2596293A (en) * | 2020-06-22 | 2021-12-29 | Univ Cranfield | A method and system for forming a fibre composite and a composite |
-
2019
- 2019-05-06 CN CN201910370572.1A patent/CN110117408A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| FAUSTINO MUJIKA, ET AL.: ""Influence of the modification with MWCNT on the interlaminar fracture properties of long carbon fiber composites"", 《COMPOSITES: PART B》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021092788A1 (en) * | 2019-11-13 | 2021-05-20 | 远景能源有限公司 | Method and apparatus for use in manufacturing graphene-modified fiber reinforced material |
| GB2596293A (en) * | 2020-06-22 | 2021-12-29 | Univ Cranfield | A method and system for forming a fibre composite and a composite |
| WO2021260355A1 (en) * | 2020-06-22 | 2021-12-30 | Cranfield University | A method and system for forming a fibre composite and a composite |
| CN113402755A (en) * | 2021-06-04 | 2021-09-17 | 西北工业大学 | Interlayer toughening method for multi-walled carbon nanotube of military aircraft composite material hot patch |
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Application publication date: 20190813 |