CN114316512B - Bionic carbon fiber/epoxy composite material and preparation method thereof - Google Patents
Bionic carbon fiber/epoxy composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of a bionic carbon fiber/epoxy composite material, which uses H for carbon fiber cloth 2 O 2 Oxidizing the aqueous solution; preparation of CoCl 2 ·6H 2 O、NiCl 2 ·6H 2 A mixed solution of O and urea; and transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, immersing carbon fiber cloth in the mixed solution for reaction, taking out the carbon fiber cloth, immersing the carbon fiber cloth in thiourea aqueous solution for reaction, taking out and drying the carbon fiber cloth, and carrying out vacuum auxiliary resin transfer molding composite curing on the carbon fiber cloth and epoxy resin to obtain the carbon fiber/epoxy composite material. The invention prepares NiCo with structure surface modified with hedgehog-like back thorn 2 S 4 The microneedle structure enables the microneedle structure to interpenetrate when the carbon fiber fabric and the carbon fiber fabric are layered and compounded, so that transverse shearing stress is effectively borne, and the expansion of transverse microcracks between composite material layers can be prevented.
Description
Technical Field
The invention belongs to the field of preparation of fiber reinforced polymer matrix composite materials, and particularly relates to a bionic carbon fiber/epoxy composite material and a preparation method thereof.
Background
The carbon fiber/epoxy composite material has the unique advantages of high specific strength and specific rigidity, strong designability, good fatigue fracture resistance, corrosion resistance, good structural dimensional stability and convenience for large-area integral molding, and is widely applied to various fields of national economy such as aerospace, sports equipment, automobiles and the like. However, a considerable amount of carbon fiber composite materials are laminated plate structures, and because the bonding between carbon fiber layers is completely dependent on resin, the interlayer shearing performance of the carbon fiber composite materials is relatively poor, and the phenomenon of cracking between the layers occurs in the use process of the materials. The interlaminar shear performance of the composite material is mainly determined by the performance of the matrix resin and the interfacial bonding condition of the matrix resin and the carbon fiber.
To improve the interlaminar shear performance of the carbon fiber composite material, on one hand, the surface treatment is required to be carried out on the carbon fiber: han et al surface treat the carbon fiber with acid to have reactive groups on the surface to increase the interfacial bonding strength between the carbon fiber and the epoxy resin; liu Kui and the like treat the carbon fiber by supercritical carbon dioxide, so that the roughness of the surface of the carbon fiber is improved, the surface of the carbon fiber is easy to be soaked by epoxy resin, and the interface bonding effect between the epoxy resin and the epoxy resin is improved through a mechanical anchoring effect; liu Zhanqing and the like are coated on the surface of the carbon fiber, an intermediate layer with better performance is introduced on the interface between the carbon fiber and the epoxy resin, so that the interface stress is released, the stress concentration is reduced, and the aim of improving the interface performance is achieved. On the other hand, there is a need to improve the properties of the resin matrix itself (including its mechanical properties and wettability to carbon fibers): at present, polyimide, polycarbonate, polyether-ether-ketone, phenolic resin and the like are introduced into epoxy resin in a traditional way, so that the epoxy resin exists in a sea-island structure in a crosslinked network of the epoxy resin, and an interpenetrating or semi-interpenetrating network structure is formed to dissipate stress; active functional groups with flexible chain segments can also be introduced to react with the epoxy resin to improve the flexibility of the network chain molecules. In recent years, the use of nanomaterials to modify epoxy resins has attracted increasing attention from researchers. The surface active group and small size effect of the nano material can be used for being physically or chemically combined with the epoxy resin, so that the nano material forms penetrating entanglement in the interface area of the carbon fiber and the epoxy resin, and bridging effect is achieved between the carbon fiber and the epoxy matrix, thereby achieving the purposes of improving interface adhesion and interface performance. The nanometer materials which are commonly used at present are nanometer silicon dioxide, nanometer titanium dioxide, nanometer clay, carbon nanometer tube and the like.
In recent years, transition metal sulfides, particularly ternary transition metal sulfides, have been attracting attention due to their excellent properties over single metal sulfides and their potential applications in electronic, optical and optoelectronic devices. NiCo 2 S 4 Electrode materials commonly used as supercapacitors and other energy storage devices, having conductivities very close to that of metals, compared to NiCo 2 O 4 100 times higher.
But NiCo is modified on the surface of the carbon fiber 2 S 4 Microneedle structures (resembling a thorn on the back of a hedgehog) have not been publicly reported by related work.
Disclosure of Invention
The invention aims to provide a bionic carbon fiber/epoxy composite material, wherein NiCo is modified on the surface of the bionic carbon fiber 2 S 4 The micro-needle structure can enable the micro-needle structure to be mutually inserted when the carbon fiber fabric and the carbon fiber fabric are layered and compounded, so that transverse shearing stress is effectively borne, the expansion of transverse microcracks between layers of the composite material is prevented, and the interlayer shearing performance of the carbon fiber/epoxy composite material is improved.
The invention is realized by the following technical proposal
One) scheme one
A preparation method of a bionic carbon fiber/epoxy composite material comprises the following steps:
1) The desized carbon fiber cloth is used with H 2 O 2 Oxidation treatment with aqueous solution 0.52h, and then drying;
2) CoCl is to be processed 2 ·6H 2 O、NiCl 2 ·6H 2 O and urea are dissolved in deionized water to obtain CoCl 2 ·6H 2 O、NiCl 2 ·6H 2 A mixed solution of O and urea, wherein the CoCl 2 ·6H 2 The concentration of O is 1-100 mmol/L, niCl 2 ·6H 2 The concentration of O is 1-50 mmol/L, and the concentration of urea is 1-50 mmol/L;
3) Transferring the mixed solution obtained in the step 2) into a reaction kettle with a polytetrafluoroethylene lining, immersing the carbon fiber cloth treated in the step 1) into the mixed solution obtained in the step 2), reacting for 2-20 h at 90-120 ℃, and naturally cooling the reaction kettle to room temperature;
4) Taking out the carbon fiber cloth obtained in the step 3), and then washing and drying;
5) Immersing the carbon fiber cloth obtained in the step 4) into thiourea aqueous solution with the concentration of 1-200 mmol/L, reacting for 2-20 h at 80-180 ℃, and naturally cooling the reaction kettle to room temperature;
6) Taking out the carbon fiber cloth in the step 5), washing and drying;
7) And (3) carrying out vacuum auxiliary resin transfer molding composite curing on the carbon fiber cloth obtained in the step (6) and the epoxy resin to obtain the carbon fiber/epoxy composite material.
Further, H is described in step 1) 2 O 2 H in aqueous solution 2 O 2 The mass percentage of the (C) is more than or equal to 10 percent.
Further, in the step 4), ethanol and deionized water are alternately used for washing for more than 3 times.
Further, the drying temperature in the step 4) is 60-120 ℃, and the drying time is 6-24 hours.
Further, in the step 6), the washing is performed by using ethanol and deionized water alternately for more than 3 times.
Further, in the step 7), the carbon fiber cloth obtained in the step 6) is laid in a mould in advance, then a mould cavity is closed, the mould cavity is vacuumized, the vacuum degree is set to be 0.01-0.1pa, and then heated and melted epoxy resin is injected into the mould cavity to obtain the bionic carbon fiber/epoxy composite material, wherein the volume ratio of the carbon fiber cloth to the epoxy resin is 40-50:50-60.
Scheme II
The preparation method of the bionic carbon fiber/epoxy composite material is prepared by any of the methods.
Compared with the prior art, the invention has the following beneficial effects: the surface of the bionic carbon fiber prepared by the preparation method of the bionic carbon fiber/epoxy composite material is modified with NiCo 2 S 4 The microneedle structure is similar to thorns on the back of hedgehog, so that when the carbon fiber fabric and the carbon fiber fabric are layered and compounded, the microneedle structure is mutually inserted, so that transverse shearing stress is effectively borne, the expansion of transverse microcracks between layers of the composite material is prevented, and the interlayer shearing performance of the carbon fiber/epoxy composite material is improved.
The invention provides a new method for solving the interface problem of the carbon fiber/epoxy composite material and the defect of poor transverse shear stress bearing between carbon fiber fabric layers in the composite material, and has great significance in practical application.
Drawings
FIG. 1 is a surface modified NiCo of example 1 2 S 4 Scanning electron microscope image of the carbon fiber surface of the microneedle structure.
Detailed Description
Example 1
A preparation method of a bionic carbon fiber/epoxy composite material comprises the following steps:
1) The desized carbon fiber cloth is treated with 10 percent of H 2 O 2 Oxidizing the aqueous solution for 0.5h, and then drying;
2) CoCl is to be processed 2 ·6H 2 O、NiCl 2 ·6H 2 O and urea are dissolved in deionized water to obtain CoCl 2 ·6H 2 O、NiCl 2 ·6H 2 A mixed solution of O and urea, wherein the CoCl 2 ·6H 2 The concentration of O is 1mmol/L, niCl 2 ·6H 2 The concentration of O is 2mmol/L, and the concentration of urea is 1mmol/L;
3) Transferring the mixed solution obtained in the step 2) into a reaction kettle with a polytetrafluoroethylene lining, immersing the carbon fiber cloth treated in the step 1) into the mixed solution obtained in the step 2), reacting for 2 hours at 90 ℃, and naturally cooling the reaction kettle to room temperature;
4) Taking out the carbon fiber cloth obtained in the step 3), alternately flushing with ethanol and deionized water for more than 3 times, and drying at 60 ℃ for 24 hours;
5) Immersing the carbon fiber cloth obtained in the step 4) in thiourea aqueous solution with the concentration of 4mmol/L, reacting for 2 hours at 80 ℃, and naturally cooling the reaction kettle to room temperature;
6) Taking out the carbon fiber cloth in the step 5), alternately flushing with ethanol and deionized water for more than 3 times, and drying;
7) And (3) carrying out vacuum auxiliary resin transfer molding composite curing on the carbon fiber cloth obtained in the step (6) and the epoxy resin to obtain the carbon fiber/epoxy composite material.
And 7) in the step 7), laying the carbon fiber cloth obtained in the step 6) in a mould in advance, closing a mould cavity, vacuumizing the mould cavity, setting the vacuum degree to be 0.1pa, and then injecting heated and melted epoxy resin into the mould cavity to obtain the bionic carbon fiber/epoxy composite material, wherein the volume ratio of the carbon fiber cloth to the epoxy resin is 40:60. the interlaminar shear strength of the obtained carbon fiber/epoxy composite material is 52MPa.
Example 2
A preparation method of a bionic carbon fiber/epoxy composite material comprises the following steps:
1) The desized carbon fiber cloth is treated with 10 percent of H 2 O 2 Oxidizing the aqueous solution for 1h, and then drying;
2) CoCl is to be processed 2 ·6H 2 O、NiCl 2 ·6H 2 O and urea are dissolved in deionized water to obtain CoCl 2 ·6H 2 O、NiCl 2 ·6H 2 A mixed solution of O and urea, wherein the CoCl 2 ·6H 2 The concentration of O is 10mmol/L, niCl 2 ·6H 2 The concentration of O is 5mmol/L, and the concentration of urea is 30mmol/L;
3) Transferring the mixed solution obtained in the step 2) into a reaction kettle with a polytetrafluoroethylene lining, immersing the carbon fiber cloth treated in the step 1) into the mixed solution obtained in the step 2), reacting for 12 hours at 90 ℃, and naturally cooling the reaction kettle to room temperature;
4) Taking out the carbon fiber cloth obtained in the step 3), alternately flushing with ethanol and deionized water for more than 3 times, and drying at 90 ℃ for 15 hours;
5) Immersing the carbon fiber cloth obtained in the step 4) in a thiourea aqueous solution with the concentration of 20mmol/L, reacting for 12 hours at 180 ℃, and naturally cooling the reaction kettle to room temperature;
6) Taking out the carbon fiber cloth in the step 5), alternately flushing with ethanol and deionized water for more than 3 times, and drying;
7) And (3) carrying out vacuum auxiliary resin transfer molding composite curing on the carbon fiber cloth obtained in the step (6) and the epoxy resin to obtain the carbon fiber/epoxy composite material.
And 7) in the step 7), laying the carbon fiber cloth obtained in the step 6) in a mould in advance, closing a mould cavity, vacuumizing the mould cavity, setting the vacuum degree to be 0.1pa, and then injecting heated and melted epoxy resin into the mould cavity to obtain the bionic carbon fiber/epoxy composite material, wherein the volume ratio of the carbon fiber cloth to the epoxy resin is 50:50. the interlaminar shear strength of the obtained carbon fiber/epoxy composite material is 55MPa.
Example 3
A preparation method of a bionic carbon fiber/epoxy composite material comprises the following steps:
1) The desized carbon fiber cloth is treated with 10 percent of H 2 O 2 Oxidizing the aqueous solution for 2 hours, and then drying;
2) CoCl is to be processed 2 ·6H 2 O、NiCl 2 ·6H 2 O and urea are dissolved in deionized water to obtain CoCl 2 ·6H 2 O、NiCl 2 ·6H 2 A mixed solution of O and urea, wherein the CoCl 2 ·6H 2 The concentration of O is 100mmol/L, niCl 2 ·6H 2 The concentration of O is 50mmol/L, and the concentration of urea is 50mmol/L;
3) Transferring the mixed solution obtained in the step 2) into a reaction kettle with a polytetrafluoroethylene lining, immersing the carbon fiber cloth treated in the step 1) into the mixed solution obtained in the step 2), reacting for 20 hours at 120 ℃, and naturally cooling the reaction kettle to room temperature;
4) Taking out the carbon fiber cloth obtained in the step 3), alternately flushing with ethanol and deionized water for more than 3 times, and drying at 120 ℃ for 6 hours;
5) Immersing the carbon fiber cloth obtained in the step 4) in a thiourea aqueous solution with the concentration of 200mmol/L, reacting for 20 hours at 180 ℃, and naturally cooling the reaction kettle to room temperature;
6) Taking out the carbon fiber cloth in the step 5), alternately flushing with ethanol and deionized water for more than 3 times, and drying;
7) And (3) carrying out vacuum auxiliary resin transfer molding composite curing on the carbon fiber cloth obtained in the step (6) and the epoxy resin to obtain the carbon fiber/epoxy composite material.
And 7) in the step 7), laying the carbon fiber cloth obtained in the step 6) in a mould in advance, closing a mould cavity, vacuumizing the mould cavity, setting the vacuum degree to be 0.1pa, and then injecting heated and melted epoxy resin into the mould cavity to obtain the bionic carbon fiber/epoxy composite material, wherein the volume ratio of the carbon fiber cloth to the epoxy resin is 45:55. the interlaminar shear strength of the obtained carbon fiber/epoxy composite material is 58MPa.
Example 4
A preparation method of a bionic carbon fiber/epoxy composite material comprises the following steps:
1) The desized carbon fiber cloth is treated with 10 percent of H 2 O 2 Oxidizing the aqueous solution for 1h, and then drying;
2) CoCl is to be processed 2 ·6H 2 O、NiCl 2 ·6H 2 O and urea are dissolved in deionized water to obtain CoCl 2 ·6H 2 O、NiCl 2 ·6H 2 A mixed solution of O and urea, wherein the CoCl 2 ·6H 2 The concentration of O is 20mmol/L, niCl 2 ·6H 2 The concentration of O is 50mmol/L, and the concentration of urea is 30mmol/L;
3) Transferring the mixed solution obtained in the step 2) into a reaction kettle with a polytetrafluoroethylene lining, immersing the carbon fiber cloth treated in the step 1) into the mixed solution obtained in the step 2), reacting for 10 hours at 100 ℃, and naturally cooling the reaction kettle to room temperature;
4) Taking out the carbon fiber cloth obtained in the step 3), alternately flushing with ethanol and deionized water for more than 3 times, and drying at 120 ℃ for 6.5 hours;
5) Immersing the carbon fiber cloth obtained in the step 4) in 100mmol/L thiourea aqueous solution, reacting for 20 hours at 150 ℃, and naturally cooling the reaction kettle to room temperature;
6) Taking out the carbon fiber cloth in the step 5), alternately flushing with ethanol and deionized water for more than 3 times, and drying;
7) And (3) carrying out vacuum auxiliary resin transfer molding composite curing on the carbon fiber cloth obtained in the step (6) and the epoxy resin to obtain the carbon fiber/epoxy composite material.
And 7) in the step 7), laying the carbon fiber cloth obtained in the step 6) in a mould in advance, closing a mould cavity, vacuumizing the mould cavity, setting the vacuum degree to be 0.1pa, and then injecting heated and melted epoxy resin into the mould cavity to obtain the bionic carbon fiber/epoxy composite material, wherein the volume ratio of the carbon fiber cloth to the epoxy resin is 40:60. the interlaminar shear strength of the obtained carbon fiber/epoxy composite material is 65MPa.
Example 5
A preparation method of a bionic carbon fiber/epoxy composite material comprises the following steps:
1) The desized carbon fiber cloth is treated with 10 percent of H 2 O 2 Oxidizing the aqueous solution for 1.5h, and then drying;
2) CoCl is to be processed 2 ·6H 2 O、NiCl 2 ·6H 2 O and urea are dissolved in deionized water to obtain CoCl 2 ·6H 2 O、NiCl 2 ·6H 2 A mixed solution of O and urea, wherein the CoCl 2 ·6H 2 The concentration of O is 50mmol/L, niCl 2 ·6H 2 The concentration of O is 20mmol/L, and the concentration of urea is 40mmol/L;
3) Transferring the mixed solution obtained in the step 2) into a reaction kettle with a polytetrafluoroethylene lining, immersing the carbon fiber cloth treated in the step 1) into the mixed solution obtained in the step 2), reacting for 2-20 h at 90-120 ℃, and naturally cooling the reaction kettle to room temperature;
4) Taking out the carbon fiber cloth obtained in the step 3), alternately flushing with ethanol and deionized water for more than 3 times, and drying at 70 ℃ for 20 hours;
5) Immersing the carbon fiber cloth obtained in the step 4) in a thiourea aqueous solution with the concentration of 120mmol/L, reacting for 15 hours at 120 ℃, and naturally cooling the reaction kettle to room temperature;
6) Taking out the carbon fiber cloth in the step 5), alternately flushing with ethanol and deionized water for more than 3 times, and drying;
7) And (3) carrying out vacuum auxiliary resin transfer molding composite curing on the carbon fiber cloth obtained in the step (6) and the epoxy resin to obtain the carbon fiber/epoxy composite material.
And 7) in the step 7), laying the carbon fiber cloth obtained in the step 6) in a mould in advance, closing a mould cavity, vacuumizing the mould cavity, setting the vacuum degree to be 0.1pa, and then injecting heated and melted epoxy resin into the mould cavity to obtain the bionic carbon fiber/epoxy composite material, wherein the volume ratio of the carbon fiber cloth to the epoxy resin is 42:58. the interlaminar shear strength of the obtained carbon fiber/epoxy composite material is 56MPa.
Example 6
A preparation method of a bionic carbon fiber/epoxy composite material comprises the following steps:
1) The desized carbon fiber cloth is treated with 10 percent of H 2 O 2 Oxidizing the aqueous solution for 2 hours, and then drying;
2) CoCl is to be processed 2 ·6H 2 O、NiCl 2 ·6H 2 O and urea are dissolved in deionized water to obtain CoCl 2 ·6H 2 O、NiCl 2 ·6H 2 A mixed solution of O and urea, wherein the CoCl 2 ·6H 2 The concentration of O is 30mmol/L, niCl 2 ·6H 2 The concentration of O is 10mmol/L, and the concentration of urea is 30mmol/L;
3) Transferring the mixed solution obtained in the step 2) into a reaction kettle with a polytetrafluoroethylene lining, immersing the carbon fiber cloth treated in the step 1) into the mixed solution obtained in the step 2), reacting for 10 hours at 90 ℃, and naturally cooling the reaction kettle to room temperature;
4) Taking out the carbon fiber cloth obtained in the step 3), alternately flushing with ethanol and deionized water for more than 3 times, and drying at 150 ℃ for 12 hours;
5) Immersing the carbon fiber cloth obtained in the step 4) in a thiourea aqueous solution with the concentration of 60mmol/L, reacting for 12 hours at 150 ℃, and naturally cooling the reaction kettle to room temperature;
6) Taking out the carbon fiber cloth in the step 5), alternately flushing with ethanol and deionized water for more than 3 times, and drying;
7) And (3) carrying out vacuum auxiliary resin transfer molding composite curing on the carbon fiber cloth obtained in the step (6) and the epoxy resin to obtain the carbon fiber/epoxy composite material.
And 7) in the step 7), laying the carbon fiber cloth obtained in the step 6) in a mould in advance, closing a mould cavity, vacuumizing the mould cavity, setting the vacuum degree to be 0.1pa, and then injecting heated and melted epoxy resin into the mould cavity to obtain the bionic carbon fiber/epoxy composite material, wherein the volume ratio of the carbon fiber cloth to the epoxy resin is 46:54. the interlaminar shear strength of the obtained carbon fiber/epoxy composite material is 60MPa.
Claims (7)
1. The preparation method of the bionic carbon fiber/epoxy composite material is characterized by comprising the following steps of:
1) The desized carbon fiber cloth is used with H 2 O 2 Oxidizing the aqueous solution for 0.5 to 2 hours, and then drying;
2) CoCl is to be processed 2 ·6H 2 O、NiCl 2 ·6H 2 O and urea are dissolved in deionized water to obtain CoCl 2 ·6H 2 O、NiCl 2 ·6H 2 A mixed solution of O and urea, wherein the CoCl 2 ·6H 2 The concentration of O is 1-100 mmol/L, niCl 2 ·6H 2 The concentration of O is 1-50 mmol/L, and the concentration of urea is 1-50 mmol/L;
3) Transferring the mixed solution obtained in the step 2) into a reaction kettle with a polytetrafluoroethylene lining, immersing the carbon fiber cloth treated in the step 1) into the mixed solution transferred into the reaction kettle, reacting for 2-20 h at 90-120 ℃, and naturally cooling the reaction kettle to room temperature;
4) Taking out the carbon fiber cloth treated in the step 3), and then washing and drying;
5) Immersing the carbon fiber cloth obtained in the step 4) into thiourea aqueous solution with the concentration of 1-200 mmol/L, reacting for 2-20 h at 80-180 ℃, and naturally cooling the reaction kettle to room temperature;
6) Taking out the carbon fiber cloth in the step 5), washing and drying;
7) And (3) carrying out vacuum auxiliary resin transfer molding composite curing on the carbon fiber cloth obtained in the step (6) and the epoxy resin to obtain the carbon fiber/epoxy composite material.
2. The method for preparing the bionic carbon fiber/epoxy composite material according to claim 1, which is characterized in that: h as described in step 1) 2 O 2 H in aqueous solution 2 O 2 The mass percentage of (2) is more than or equal to 10 percent.
3. The method for preparing the bionic carbon fiber/epoxy composite material according to claim 1, which is characterized in that: and 4) during the flushing, ethanol and deionized water are used for alternately flushing for more than 3 times.
4. The method for preparing the bionic carbon fiber/epoxy composite material according to claim 1, which is characterized in that: and 4) the drying temperature is 60-120 ℃ and the drying time is 6-24h.
5. The method for preparing the bionic carbon fiber/epoxy composite material according to claim 1, which is characterized in that: and 6) during the flushing, ethanol and deionized water are used for alternately flushing for more than 3 times.
6. The method for preparing the bionic carbon fiber/epoxy composite material according to claim 1, which is characterized in that: in the step 7), the carbon fiber cloth obtained in the step 6) is laid in a mould in advance, then a mould cavity is closed, the mould cavity is vacuumized, the vacuum degree is set to be 0.01-0.1pa, and then heated and melted epoxy resin is injected into the mould cavity to obtain the bionic carbon fiber/epoxy composite material, wherein the volume ratio of the carbon fiber cloth to the epoxy resin is 40-50:50-60.
7. A bionic carbon fiber/epoxy composite material is characterized in that: prepared by the method of any one of claims 1-6.
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