CN110421920A - A kind of preparation method of graphene modified carbon fiber composite material - Google Patents
A kind of preparation method of graphene modified carbon fiber composite material Download PDFInfo
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- CN110421920A CN110421920A CN201910730250.3A CN201910730250A CN110421920A CN 110421920 A CN110421920 A CN 110421920A CN 201910730250 A CN201910730250 A CN 201910730250A CN 110421920 A CN110421920 A CN 110421920A
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/55—Epoxy resins
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2255/00—Coating on the layer surface
- B32B2255/02—Coating on the layer surface on fibrous or filamentary layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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Abstract
The invention discloses a kind of preparation methods of graphene modified carbon fiber composite material, the binding force solved between existing carbon fiber layer and graphene inter-layer bonding force and carbon fiber monomer is poor, so as to cause the problem that the inter-layer bonding force of entire carbon fibre composite is poor.The present invention includes the following steps: that performing etching processing to carbon fiber obtains surface pore；Dip-coating is carried out to carbon fiber respectively using graphene aqueous solution, promotes graphene aqueous solution to enter in the gap between surface pore and carbon fiber by the way of taking out negative pressure in dip-coating；The carbon fiber of dip-coating is dried；Epoxy resin layer is coated on the carbon fiber that step 3 obtains obtains composite material unit；Multiple composite material units are laminated to obtain composite material, two neighboring composite material unit vertical arrangement obtains orthogonal composite material.The present invention has many advantages, such as that carbon fibre composite inter-layer bonding force is good, and puncture-resistant ability is strong.
Description
Technical field
The present invention relates to carbon fibre composite preparation technical fields, and in particular to a kind of graphene modified carbon fiber is compound
The preparation method of material.
Background technique
Carbon fiber is to be transformed by organic fiber by a series of heat treatments, and phosphorus content is higher than 90% inorganic high property
Energy fiber, is a kind of new material of excellent in mechanical performance, the intrinsic person's character feature with carbon material, and has both the soft of textile fabric
Soft processable type is reinforcing fiber of new generation.
Being mainly used for for carbon fiber is compound with matrixes such as resin, metal, ceramics, and structural material is made.Fibre reinforced
Epoxy resin composite material, specific strength, specific modulus overall target are highest in existing structure material.In density, just
Degree, weight, fatigue properties etc. have the field of strict demand, in the occasion for requiring high temperature, chemical stability high, carbon fiber composite
Material all has much advantage.
But the further exploration with people to technology, the application conditions of material are more and more harsher, and this requires carbon fibers
The performance of dimension composite material is further improved.
Graphene (Graphene) be one kind by carbon atom with sp2Hybridized orbit forms the two dimension that hexangle type is in honeycomb lattice
Carbon nanomaterial.Graphene has excellent optics, electricity, mechanical characteristic, specific manifestation are as follows: thermal coefficient 5300W/mK,
Carrier mobility 15000cm2/ (V.s) at room temperature, theoretical Young's modulus 1.0TPa, materialogy, micro-nano technology, the energy,
Biomedical and drug delivery etc. is with important application prospects, it is considered to be a kind of future revolutionary material.
Just because of the considerable performance of graphene, applies it in carbon fibre material, carbon fibre composite can be improved
Performance, also there are a large amount of relation technological researchings, there is that graphene is improved entire carbon fiber directly as middle layer is compound
The performance of material, but inter-layer bonding force is poor, is easy to happen layer in use and splits, in addition, therefore, it is necessary to graphite
The combination of alkene and carbon fiber improves, and is desirably to obtain that performance is more preferable, and the graphene modified carbon fiber that can persistently use is multiple
Condensation material.
Summary of the invention
The technical problems to be solved by the present invention are: existing carbon fiber layer and graphene inter-layer bonding force and carbon fiber
Binding force between monomer is poor, and the inter-layer bonding force so as to cause entire carbon fibre composite is poor.
The present invention provides a kind of preparation methods of the graphene modified carbon fiber composite material to solve the above problems.
The present invention is achieved through the following technical solutions:
Include the following steps:
Step 1: processing being performed etching to carbon fiber and obtains surface pore；
Step 2: dip-coating being carried out to carbon fiber respectively using graphene aqueous solution, is promoted by the way of taking out negative pressure in dip-coating
Enter in the gap between surface pore and carbon fiber into graphene aqueous solution；
Step 3: the carbon fiber of dip-coating is dried；
Step 4: coating epoxy resin layer on the carbon fiber that step 3 obtains and obtain composite material unit；
Step 5: multiple composite material units being laminated to obtain composite material, two neighboring composite material unit is vertical
It arranges and obtains orthogonal composite material.
The present invention in carbon fiber surface by performing etching to form hole, in this way when graphene aqueous solution carries out dip-coating,
It can enter in hole, the case where being difficult to enter small for hole, the present invention below carbon fiber by the way of vacuumizing, In
Under the action of the air pressure of top, graphene aqueous solution can preferably enter in hole, and for the gap between carbon fiber monomer
Due to there is also hole, graphene aqueous solution is not only incorporated between carbon fiber surface can also enter between carbon fiber monomer
, in the form of sheets due to graphene, can be interspersed wherein with different shape in gap and hole, on the one hand, improve carbon fiber layer and
Binding force between graphene layer effectively reduces layer and splits, and on the other hand, the binding force between carbon fiber monomer can be improved.
Preferably a kind of preparation method of graphene modified carbon fiber composite material of the present invention, the etching processing of the step 1
Method are as follows: using concentrated nitric acid in 100-120 DEG C of processing 120-150min.
Preferably a kind of preparation method of graphene modified carbon fiber composite material of the present invention, the diameter of the carbon fiber are 10
μm。
The present invention obtains the larger deeper carbon of hole by selecting the carbon fiber being relatively large in diameter to carry out the etching processing of depth
Fiber, convenient for the dip-coating of later period graphene.
Preferably a kind of preparation method of graphene modified carbon fiber composite material of the present invention, the carbon fiber is in etching processing
It is first pre-processed before using acetone, acetone is to remove the colloid of carbon fiber surface preferably to carry out subsequent quarter
Erosion processing.
Preferably a kind of preparation method of graphene modified carbon fiber composite material of the present invention, in step 2, the carbon fiber
It is first laid in dip-coating on the support web plate of container, then graphene aqueous solution is poured on the carbon fiber and makes graphene
Carbon fiber is completely covered in aqueous solution, opens vacuum, and lower section vacuumizes, and graphene aqueous solution can be made preferably to enter carbon fiber list
In the gap of body, play a significant role for improving bending strength, and under the pressure effect of air pressure above, graphene is water-soluble
Liquid can more closely dip-coating in carbon fiber upper surface, inter-layer bonding force is more secured.
Preferably a kind of preparation method of graphene modified carbon fiber composite material of the present invention, before carrying out step 3, dip-coating
After the completion, it first opens leakage fluid dram the remaining graphene aqueous solution in the bottom of container is discharged, in order to guarantee graphene aqueous solution energy
Completely between carbon fiber monomer gap and hole in, need graphene aqueous solution to penetrate carbon under vacuum-pumping conditions
Fiber, and the part graphene aqueous solution can be collected by leakage fluid dram.
Preferably a kind of preparation method of graphene modified carbon fiber composite material of the present invention, the drying process of the step 3
Mode are as follows: container is placed in drier using 80-100 DEG C of progress drying in 12-24 hours, forms interlayer knot in carbon fiber surface
Strong graphene layer with joint efforts.
Preferably a kind of preparation method of graphene modified carbon fiber composite material of the present invention, the graphene aqueous solution are oxygen
Graphite aqueous solution.
Preferably a kind of preparation method of graphene modified carbon fiber composite material of the present invention, the container includes cavity and lid
Body is provided with feed opening on the lid, and the bottom of the cavity is provided with leakage fluid dram, be provided in the cavity offer it is more
The support web plate of a through-hole, the exhaust outlet are located at the bottom side of the wall of the cavity, and the exhaust outlet is located at the support web plate
Lower section, the exhaust outlet connects vacuum evacuation device.
The present invention have it is following the utility model has the advantages that
1, the present invention first passes through the etching processing for selecting the carbon fiber being relatively large in diameter to carry out depth, and it is larger relatively deep to obtain hole
Carbon fiber, then by way of dip-coating by graphene aqueous solution be coated in carbon fiber on formed firm binding force graphene
Layer, and can also intert the graphene aqueous solution of different orientation between carbon fiber to enhance its carbon fiber layer and graphene layer
And the binding force between carbon fiber monomer.
2, the present invention is in dip-coating graphene aqueous solution, in such a way that lower section vacuumizes, enables graphene aqueous solution
More fully enter in the gap between carbon fiber monomer and the longitudinal hole of carbon fiber, improve inter-layer bonding force and
Binding force between carbon fiber monomer.
3, the present invention between carbon fiber by being arranged one layer of firm graphene layer, and the roughness of graphene layer is big,
The strong graphene modified carbon fiber composite material of whole inter-layer bonding force can be formed preferably in conjunction with epoxy resin layer.
Detailed description of the invention
Attached drawing described herein is used to provide to further understand the embodiment of the present invention, constitutes one of the application
Point, do not constitute the restriction to the embodiment of the present invention.In the accompanying drawings:
Fig. 1 is the SEM photograph after carbon fiber etching processing of the present invention.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below with reference to embodiment, the present invention is made
Further to be described in detail, exemplary embodiment of the invention and its explanation for explaining only the invention, are not intended as to this
The restriction of invention.
Embodiment 1
A kind of preparation method of graphene modified carbon fiber composite material, the specific steps are as follows:
1, pre-treatment of carbon fiber: choosing the carbon fiber that diameter is 10 μm, and carbon fiber is placed on to the PP appearance for being loaded with acetone
In device, it is placed in ultrasonic device sonic oscillation 4-8 hours, mainly removes the glue of carbon fiber surface.
2, the surface etch of carbon fiber: 68% concentrated nitric acid and carbon fiber is placed in a reservoir, extremely by heating mantle heats
110 DEG C, 130min is kept the temperature, then the concentrated nitric acid on surface is cleaned up wash with distilled water, then drying and processing, obtains etching
Carbon fiber, pattern photo is as shown in Figure 1.
3, negative pressure dip-coating: weighing graphene oxide, and distilled water or ionized water is added to be made into the graphene oxide that concentration is 1g/l
Aqueous solution, then ultrasonic disperse 30min；The carbon fiber etched is laid on support web plate, is configured from feed opening addition
Graphene aqueous solution, when graphene aqueous solution all covering carbon fibers after open vacuum, graphene aqueous solution is in suction function
Lower carry out dip-coating closes vacuum, and stand 15min after the bottom deposit of cavity has graphene aqueous solution.
4, it is dried the carbon fiber after dip-coating: container is placed in drier using 80 DEG C of progress drying in 24 hours, In
Carbon fiber surface forms the strong graphene layer of inter-layer bonding force.
5, coat epoxy resin: one layer of epoxy resin of coating obtains composite wood material list on the carbon fiber of graphene processing
Member.
6, the preparation of carbon fibre composite: the combination that multiple composite material units are carried out by way of hot pressing is answered
Condensation material.
Carbon fibre composite performance test:
1, Push out test is carried out to carbon fibre composite, tests puncture-resistant intensity.
2, layer is carried out to the section of puncturing hole and splits degree observation.
Above-mentioned Push out test with reference to counter-bending test experiments carry out, be carried out on fatigue tester, and by reequip into
Row test, specific method is: the size of pressure head being reduced to 1mm, passes through formula: η=3PL/ (2bh2),
Wherein, η be being folded without breaking intensity, MPa, P be sample from be depressed into be pierced between maximum load value, N；L be across
Away from nm；B is specimen width, mm；H is sample thickness, mm.
Wherein, sample prepare it is as follows:
1, the carbon fiber of dip-coating graphene the preparation of carbon fibre composite sample: is cut into 60mm, specimen width
20mm, length of span 40mm, sample thickness 2mm.
Specific test parameter are as follows: loading velocity 3mm/min, using etc. method of additions load, using 1N as initial load, points ten grades
Load.
2, layer splits the preparation of observation experiment sample after puncturing: cutting open along puncturing hole, the layer for visually observing section splits situation.
Comparative example 1
By not vacuumizing when dip-coating in comparative example 1, other preparation conditions are same as Example 1, and verifying vacuumizes pair
The influence of binding force between inter-layer bonding force and carbon fiber monomer is labeled as sample 2#.
Comparative example 2
To the comparative experiments for carving etching temperature, 3 groups of experiments are carried out altogether, etching temperature is respectively 80 DEG C, 120 DEG C and 150 DEG C,
Etch period is 130min, is successively labeled as sample 3#, sample 4# and sample 5#.
Sample prepared by the above comparative example and embodiment 1 obtains puncture-resistant intensity and compares to the section after puncture as follows
Shown in table 1:
Table 1
As can be seen from Table 1, obviously excellent by vacuumizing the final punctured resistance of the carbon fibre composite of preparation
In what is do not vacuumized, this illustrates the hole for taking out the gap and etching that really graphene are better distributed between carbon fiber monomer
In gap, improve the binding force between inter-layer bonding force and carbon fiber monomer, in addition, using major diameter carbon fiber and with compared with
The etching temperature of high-temperature help to obtain more porous, and the binder course of graphene and carbon fiber is stronger, between carbon fiber monomer
Combination it is also stronger, be conducive to improve puncture-resistant intensity.
Embodiment 2
Preferably a kind of preparation method of graphene modified carbon fiber composite material of the present invention, the container includes cavity and lid
Body is provided with feed opening on the lid, and the bottom of the cavity is provided with leakage fluid dram, be provided in the cavity offer it is more
The support web plate of a through-hole, the exhaust outlet are located at the bottom side of the wall of the cavity, and the exhaust outlet is located at the support web plate
Lower section, the exhaust outlet connects vacuum evacuation device.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not intended to limit the present invention the foregoing is merely a specific embodiment of the invention
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of graphene modified carbon fiber composite material, which comprises the steps of:
Step 1: processing being performed etching to carbon fiber and obtains surface pore；
Step 2: dip-coating being carried out to carbon fiber respectively using graphene aqueous solution, promotes stone by the way of taking out negative pressure in dip-coating
Black aqueous solution enters in the gap between surface pore and carbon fiber；
Step 3: the carbon fiber of dip-coating is dried；
Step 4: coating epoxy resin layer on the carbon fiber that the step 3 obtains and obtain composite material unit；
Step 5: multiple composite materials being laminated to obtain composite material, two neighboring composite material unit is arranged vertically and obtains
To orthogonal composite material.
2. according to a kind of preparation method of graphene modified carbon fiber composite material according to claim 1, feature exists
In the etching processing method of the step 1 are as follows: using concentrated nitric acid in 100-120 DEG C of processing 120-150min.
3. according to a kind of preparation method of graphene modified carbon fiber composite material according to claim 1 or 2, feature
It is, the diameter of the carbon fiber is 10 μm.
4. a kind of preparation method of graphene modified carbon fiber composite material according to claim 1 or 2, feature exist
In the carbon fiber is first pre-processed using acetone before etching processing.
5. a kind of preparation method of graphene modified carbon fiber composite material according to claim 1 or 2, feature exist
In in step 2, the carbon fiber is first laid on the support web plate of container in dip-coating, then graphene aqueous solution is poured on
On the carbon fiber and make graphene aqueous solution that carbon fiber be completely covered, opens vacuum.
6. a kind of preparation method of graphene modified carbon fiber composite material according to claim 1 or 2, feature exist
In before carrying out step 3, after the completion of dip-coating, first the remaining graphene aqueous solution in the bottom of container is discharged opening leakage fluid dram.
7. a kind of preparation method of graphene modified carbon fiber composite material according to claim 1 or 2, feature exist
In the drying process mode of the step 3 are as follows: container to be placed in drier using 80-100 DEG C of progress drying in 12-24 hours.
8. a kind of preparation method of graphene modified carbon fiber composite material according to claim 1 or 2, feature exist
In the graphene aqueous solution is graphene oxide water solution.
9. a kind of preparation method of graphene modified carbon fiber composite material according to claim 5, which is characterized in that institute
Stating container includes cavity and lid, and feed opening is provided on the lid, and the bottom of the cavity is provided with leakage fluid dram, the chamber
The support web plate for offering multiple through-holes is provided in body, the bottom side of the wall of the cavity is provided with exhaust outlet, the exhaust outlet
Positioned at the lower section of the support web plate, the exhaust outlet connects vacuum evacuation device.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116041798A (en) * | 2022-12-23 | 2023-05-02 | 海南中之林仿生科技有限公司 | Fiber reinforced thermoplastic starch plate and preparation method thereof |
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|---|---|---|---|---|
| CN103243544A (en) * | 2013-05-07 | 2013-08-14 | 中国科学院山西煤炭化学研究所 | Method for modifying carbon fiber surface |
| CN106367952A (en) * | 2015-07-23 | 2017-02-01 | 徐海波 | Surface treatment method for carbon fibers using oxidized graphene quantum dots as coating, and composite material |
| CN106867199A (en) * | 2017-02-16 | 2017-06-20 | 嘉兴学院 | One kind orientation graphene oxide modified carbon fiber composite and preparation method thereof |
| CN107673773A (en) * | 2017-11-02 | 2018-02-09 | 重庆交通大学 | The preparation method of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon |
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2019
- 2019-08-08 CN CN201910730250.3A patent/CN110421920A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103243544A (en) * | 2013-05-07 | 2013-08-14 | 中国科学院山西煤炭化学研究所 | Method for modifying carbon fiber surface |
| CN106367952A (en) * | 2015-07-23 | 2017-02-01 | 徐海波 | Surface treatment method for carbon fibers using oxidized graphene quantum dots as coating, and composite material |
| CN106867199A (en) * | 2017-02-16 | 2017-06-20 | 嘉兴学院 | One kind orientation graphene oxide modified carbon fiber composite and preparation method thereof |
| CN107673773A (en) * | 2017-11-02 | 2018-02-09 | 重庆交通大学 | The preparation method of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116041798A (en) * | 2022-12-23 | 2023-05-02 | 海南中之林仿生科技有限公司 | Fiber reinforced thermoplastic starch plate and preparation method thereof |
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Application publication date: 20191108 |