CN117988094A - Sizing agent based on rigid-flexible combined nano particles, preparation method thereof and application thereof in CF/PEEK composite material - Google Patents
Sizing agent based on rigid-flexible combined nano particles, preparation method thereof and application thereof in CF/PEEK composite material Download PDFInfo
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- 239000004696 Poly ether ether ketone Substances 0.000 title claims abstract description 41
- 229920002530 polyetherether ketone Polymers 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 33
- 238000004513 sizing Methods 0.000 title claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 28
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 title claims abstract 8
- 238000002360 preparation method Methods 0.000 title abstract description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 67
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 57
- 239000004917 carbon fiber Substances 0.000 claims description 57
- 239000004744 fabric Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000004760 aramid Substances 0.000 claims description 14
- 229920003235 aromatic polyamide Polymers 0.000 claims description 14
- 239000002121 nanofiber Substances 0.000 claims description 13
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000009990 desizing Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- 235000011837 pasties Nutrition 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000000944 Soxhlet extraction Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000835 fiber Substances 0.000 abstract description 3
- 229910010413 TiO 2 Inorganic materials 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 230000006355 external stress Effects 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 230000003746 surface roughness Effects 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 230000007704 transition Effects 0.000 abstract description 2
- 239000004697 Polyetherimide Substances 0.000 description 11
- 229920001601 polyetherimide Polymers 0.000 description 11
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- 238000007796 conventional method Methods 0.000 description 1
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- NZZFYRREKKOMAT-UHFFFAOYSA-N diiodomethane Chemical compound ICI NZZFYRREKKOMAT-UHFFFAOYSA-N 0.000 description 1
- 229920003247 engineering thermoplastic Polymers 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229940101545 mi-acid Drugs 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
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- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
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- 229920000642 polymer Polymers 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Reinforced Plastic Materials (AREA)
Abstract
Sizing agent based on rigid-flexible combined nano particles, preparation method thereof and application thereof in CF/PEEK composite material. The invention belongs to the field of fiber sizing agents and preparation thereof. The invention aims to solve the technical problem that the overall mechanical properties of the conventional CF/PEEK interface and composite material are to be further optimized. The invention provides a sizing agent composed of hybrid nano particles of flexible ANF and rigid nano TiO 2 and a PEI transition layer. The modified CF/PEEK composite material has obviously improved active functional group content, surface roughness and wettability. Meanwhile, the synergistic effect of the rigid-flexible structure at the interface improves the external stress transmission, inhibits crack propagation, and improves the interface bonding strength and the overall mechanical property of the composite material so as to meet the requirements of the fields of automobiles, ships and aerospace.
Description
Technical Field
The invention belongs to the field of fiber sizing agents and preparation thereof, and particularly relates to a sizing agent based on rigid-flexible combined nano particles, a preparation method thereof and application thereof in CF/PEEK composite materials.
Background
Heretofore, carbon Fiber (CF) reinforced polymer composites have been widely used in the automotive, marine and aerospace industries due to their specific properties, including high specific strength and modulus, thermal stability and chemical durability.
Polyether ether ketone (PEEK) is used as engineering thermoplastic plastic, has excellent thermal stability and mechanical property, and can work for a long time at 250 ℃. The interface is the bridge for load transfer between the fibers and the resin, and its properties directly affect the overall properties of the composite. However, interfacial adhesion of the composite is limited not only by the smooth surface of the CF, low surface free energy, and inert chains of PEEK, but also by the presence of significant "modulus gaps" between the CF and PEEK, which also hamper the efficiency of stress transfer. Meanwhile, the weak interface can lead to stress concentration, and the performance advantage of the composite material is difficult to fully develop. Therefore, increasing the interfacial bond strength between CF and PEEK is a continuing problem to be solved in the art.
Disclosure of Invention
The invention aims to solve the technical problem that the overall mechanical properties of the traditional CF/PEEK interface and composite material are to be further optimized, and provides a sizing agent based on rigid-flexible combined nano particles, a preparation method thereof and application thereof in the CF/PEEK composite material.
It is an object of the present invention to provide a method for preparing rigid-flexible combined nanoparticles, the method comprising:
dispersing nano titanium dioxide and cerium chloride in ethanol by ultrasonic, adding aramid nanofiber dispersion liquid, continuing ultrasonic dispersion, stirring by magnetic force, filtering, washing, dispersing in deionized water again, and drying until the water content is 8-20wt.%, thus obtaining pasty rigid-flexible combined nano particles.
Further defined, the mass ratio of the nano titanium dioxide to the cerium chloride is (0.2-0.5): (0.1-1).
Further defined, the ratio of the mass of nano-titania to the volume of ethanol is (0.2-0.5) g: (10-80) mL.
Further defined, the ratio of nano titanium dioxide to aramid nanofiber dispersion is (0.2-0.5) g: (30-50) mL.
Further defined, the concentration of the aramid nanofiber dispersion is 3-6g/L.
Further defined, the power of the ultrasonic dispersion is 500-700W.
Further defined, the magnetic stirring is carried out for 1-3 hours.
It is a second object of the present invention to provide a rigid-flexible nanoparticle prepared as described above, wherein the rigid nano titanium dioxide and the flexible aramid nanofiber are cross-linked to each other into a hybrid nano-network.
It is a further object of the present invention to provide a sizing agent based on the above-described rigid-flexible nanoparticles, comprising the above-described rigid-flexible nanoparticles and PEI (polyetherimide).
The fourth object of the present invention is to provide a method for preparing a sizing agent based on the above-mentioned rigid-flexible combined nanoparticles, the method comprising:
the nano particles combined with rigid and flexible and PEI (polyetherimide) are added into DMF, and then ultrasonic and magnetic stirring are carried out to obtain the sizing agent.
Further defined, the solid content of the hard-soft combined nanoparticles in the sizing agent is 0.1-1.0wt.%, and the solid content of PEI (polyetherimide) is 0.5-1.0wt.%.
The invention aims at providing an application of the sizing agent in the interface modification of a CF/PEEK composite material, which comprises the following specific steps:
Firstly desizing and oxidizing the carbon fiber cloth, then soaking the carbon fiber cloth in the sizing agent, standing and drying the carbon fiber cloth to obtain the modified carbon fiber cloth, and then carrying out hot press molding on the modified carbon fiber cloth and PEEK resin powder according to a proportion.
Further defined, the desizing is performed in an acetone solution using a soxhlet extraction method.
Further defined, the oxidation is achieved by immersion in a mixed solution of Mi's acid/ethanol.
The sixth purpose of the invention is to provide the CF/PEEK composite material obtained by the application, wherein the bending strength of the composite material is more than or equal to 800MPa, and the interlayer shearing strength of the composite material is more than or equal to 80MPa.
The invention aims at providing an application of the CF/PEEK composite material in the fields of automobiles, ships and aerospace.
Compared with the prior art, the invention has the remarkable effects that:
(1) The invention provides a sizing agent based on mixed nano particles with a rigid-flexible structure in consideration of inertness of CF and PEEK and a modulus difference between the CF and PEEK so as to improve interfacial adhesion and mechanical properties of a CF/PEEK composite material. The sizing agent consists of hybrid nano particles of flexible Aramid Nanofibers (ANF) and rigid nano TiO 2 in cross-linking and a Polyetherimide (PEI) transition layer. The active functional group content, the surface roughness and the wettability of the modified CF/PEEK composite material are all obviously improved. Meanwhile, the synergistic effect of the rigid-flexible structure at the interface improves the external stress transmission, inhibits crack propagation, and improves the interface bonding strength and the overall mechanical property of the composite material so as to meet the requirements of the fields of automobiles, ships and aerospace.
(2) The invention provides a carbon fiber sizing modification method, which comprises the steps of firstly desizing and oxidizing the surface of commercial carbon fiber, then sizing the surface of the carbon fiber by utilizing aramid nanofiber-nano titanium dioxide 'rigid-flexible' hybrid nano particles and polyetherimide, and improving the wettability of the surface of the carbon fiber, thereby effectively improving the bonding strength between the carbon fiber and resin in a composite material, wherein the bending strength of the modified carbon fiber reinforced polyether-ether-ketone composite material is more than or equal to 800MPa, the interlaminar shearing strength is more than or equal to 80MPa, and the comprehensive performance is excellent.
Drawings
FIG. 1 is an SEM image of the surface morphology of a hard-soft bonded nanoparticle prepared in the first step of the present invention;
FIG. 2 is an infrared spectrum of a rigid-flexible nanoparticle prepared in the first step of the present invention;
FIG. 3 is an SEM image of the surface morphology of the modified carbon fiber obtained in the third step of the embodiment of the present invention;
FIG. 4 is a graph showing the apparent contact angles of deionized water and diiodomethane on the surface of a carbon fiber before and after the third step of modification in accordance with the present invention;
FIG. 5 is a graph showing the comparison of the surface energy of carbon fibers before and after the third step of modification according to the embodiment of the present invention;
FIG. 6 is a graph showing the comparison of flexural strength and interlaminar shear strength tests of carbon fiber reinforced polyether ether ketone composites prepared in examples of the present invention and comparative examples.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, methods and apparatus used, without any particular description, are those conventional in the art and are commercially available to those skilled in the art.
The terms "comprising," "including," "having," "containing," or any other variation thereof, as used in the following embodiments, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
Reference in the following examples to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic may be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when ranges of "1 to 5" are disclosed, the described ranges should be construed to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range. In the description and claims of the application, the range limitations may be combined and/or interchanged, if not otherwise specified, including all the sub-ranges subsumed therein.
The indefinite articles "a" and "an" preceding an element or component of the invention are not limited to the requirement (i.e. the number of occurrences) of the element or component. Thus, the use of "a" or "an" should be interpreted as including one or at least one, and the singular reference of an element or component includes the plural reference unless the amount clearly dictates otherwise.
Examples:
The application of the sizing agent based on the rigid-flexible combined nano particles in the preparation of the CF/PEEK composite material is specifically carried out according to the following steps:
First, preparing rigid-flexible combined nano particles:
Firstly, adding 0.3g of nano titanium dioxide and 0.5g of cerium chloride into 50mL of ethanol, and then performing ultrasonic dispersion for 2 hours at 600W to obtain a mixed solution;
Then adding 50mL of aramid nanofiber dispersion liquid with the concentration of 6g/L into the treated mixed solution, continuing to carry out ultrasonic treatment for 1h at 600W, magnetically stirring for 2h, carrying out suction filtration, washing with deionized water, carrying out suction filtration, and re-dispersing to 100mL of deionized water to obtain a suspension;
Next, the suspension was dried at 60 ℃ for 12 hours to obtain pasty rigid-flexible combined nanoparticles having a water content of 15 wt.%.
The morphology analysis is carried out on the surface of the obtained pasty rigid-flexible combined nano particle, and the result is shown in figure 1, and as can be seen from figure 1, the rigid nano titanium dioxide and the flexible aramid nanofiber are crosslinked with each other, so that a hybrid nano network with a rigid-flexible structure is formed.
The obtained pasty rigid-flexible combined nano particles are subjected to infrared analysis, and the result is shown in figure 2, and as can be seen from figure 2, the rare earth ions are bonded between N atoms in the aramid nanofibers and O atoms in the nano titanium dioxide through the effect of the bridge connection, so that a nano network formed by mixing and interweaving the rigid nano titanium dioxide and the flexible aramid nanofibers is constructed.
Secondly, preparing sizing agent:
The pasty rigid-flexible combined nano particles and polyetherimide are added into DMF solution, ultrasonic treatment is carried out for 1h under 600W, and magnetic stirring is carried out for 1h, so as to obtain the sizing agent with the pasty rigid-flexible combined nano particles solid content of 0.7wt.% and the polyetherimide solid content of 1.0 wt.%.
Thirdly, preparing a carbon fiber reinforced polyether-ether-ketone composite material CF/PEEK composite material:
Firstly, adopting a Soxhlet extraction method to reflux T300 carbon fiber cloth in an acetone solution at 80 ℃ for 24 hours for desizing, washing with deionized water for 2 times, and then placing the washed cloth in an oven at 80 ℃ for drying for 48 hours to obtain desized carbon fiber cloth; immersing the desized carbon fiber cloth in a mixed solution of 30 ℃ Mirabilitic acid (6 g)/ethanol (400 mL), standing for 2 hours, and drying to obtain the oxidized carbon fiber cloth.
Then, immersing the carbon fiber cloth into the sizing agent obtained in the second step for 2 hours, and then drying at 100 ℃ for 8 hours to obtain the modified carbon fiber cloth. The surface of the modified carbon fiber cloth was subjected to morphological analysis, and the result is shown in fig. 3. As can be seen from fig. 3, the sizing agent is effectively attached to the surface of the carbon fiber, and the introduction of the "rigid-flexible" particles effectively improves the roughness of the surface of the carbon fiber. Subsequently, contact angle tests were performed on the carbon fiber surfaces before and after modification, the results are shown in fig. 4, and the carbon fiber surface energy was calculated from the contact angle results, and the results are shown in fig. 5. The sizing agent improves the wetting property of the resin on the surface of the carbon fiber.
Finally, modified carbon fiber cloth and PEEK resin powder are mixed according to a ratio of 6:4, through hot press molding after 9 layers of PEEK resin and 8 layers of T300 carbon fiber cloth are alternately paved, the hot press process is as follows: heating to 390 ℃ at a speed of 10 ℃/min from room temperature, preserving heat for 30min, then cooling to room temperature, keeping the speed of the cooling process at 1 ℃/min all the time, and keeping the whole pressure at 5MPa to obtain the carbon fiber reinforced polyether-ether-ketone CF/PEEK composite material with the thickness of 1.6 mm.
Comparative example:
The preparation method of the carbon fiber reinforced polyether-ether-ketone CF/PEEK composite material of the comparative example comprises the following steps:
Firstly, adopting a Soxhlet extraction method to reflux T300 carbon fiber cloth in an acetone solution at 80 ℃ for 24 hours for desizing, washing with deionized water for 2 times, and then placing the washed cloth in an oven at 80 ℃ for drying for 48 hours to obtain desized carbon fiber cloth; immersing the desized carbon fiber cloth in a mixed solution of 30 ℃ Mirabilitic acid (6 g)/ethanol (400 mL), standing for 2 hours, and drying to obtain the oxidized carbon fiber cloth.
Then, the carbon fiber cloth and PEEK resin powder after desizing and oxidizing treatment are mixed according to the following ratio of 6:4, through hot briquetting after 9 layers PEEK resin and 8 layers T300 carbon fiber cloth are layered alternately, the hot briquetting process is as follows: heating to 390 ℃ at a speed of 10 ℃/min from room temperature, preserving heat for 30min, then cooling to room temperature, keeping the speed of the cooling process at 1 ℃/min all the time, and keeping the whole pressure at 5MPa to obtain the carbon fiber reinforced polyether-ether-ketone CF/PEEK composite material with the thickness of 1.6 mm.
The CF/PEEK composites prepared in the examples and comparative examples of the present invention were tested for mechanical properties and flexural strength and interlaminar shear strength according to ASTM D7264 and ASTM D2344, respectively. The test results are shown in fig. 6, and it can be seen from fig. 6 that the bending strength of the CF/PEEK composite material obtained in the embodiment of the invention is as high as 810.2MPa, the interlayer shear strength is as high as 82.6MPa, and the bending strength and the interlayer shear strength are respectively improved by 91.4% and 58.2% compared with the CF/PEEK composite material of the comparative example.
In the foregoing, the present invention is merely preferred embodiments, which are based on different implementations of the overall concept of the invention, and the protection scope of the invention is not limited thereto, and any changes or substitutions easily come within the technical scope of the present invention as those skilled in the art should not fall within the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (10)
1. A method of preparing a rigid-flexible nanoparticle, the method comprising:
dispersing nano titanium dioxide and cerium chloride in ethanol by ultrasonic, adding aramid nanofiber dispersion liquid, continuing ultrasonic dispersion, stirring by magnetic force, filtering, washing, dispersing in deionized water again, and drying until the water content is 8-20wt.%, thus obtaining pasty rigid-flexible combined nano particles.
2. The method according to claim 1, wherein the mass ratio of the nano titanium dioxide to the cerium chloride is (0.2-0.5): (0.1-1), the ratio of the nano titanium dioxide to the aramid nanofiber dispersion is (0.2-0.5) g: (30-50) mL, the concentration of the aramid nanofiber dispersion liquid is 3-6g/L.
3. The rigid-flexible nanoparticle prepared by the method of claim 1 or 2, wherein the rigid nano-titania and the flexible aramid nanofiber are cross-linked to each other to form a hybrid nano-network.
4. A sizing agent based on rigid-flexible bound nanoparticles according to claim 3, characterized by comprising rigid-flexible bound nanoparticles and PEI.
5. A method of preparing the sizing agent of claim 4, wherein the method comprises:
And adding the nano particles combined with the rigidity and the flexibility and PEI into DMF, and performing ultrasonic and magnetic stirring to obtain the sizing agent.
6. The method according to claim 5, characterized in that the solid content of the hard-soft bound nanoparticles in the sizing agent is 0.1-1.0wt.%, and the solid content of PEI is 0.5-1.0wt.%.
7. The use of the sizing agent according to claim 4 for the interfacial modification of CF/PEEK composites,
Firstly desizing and oxidizing the carbon fiber cloth, then soaking the carbon fiber cloth in a sizing agent, standing and drying the carbon fiber cloth to obtain the modified carbon fiber cloth, and then carrying out hot press molding on the modified carbon fiber cloth and PEEK resin powder according to a proportion.
8. Use according to claim 7, characterized in that the desizing is carried out by soxhlet extraction in acetone solution and the oxidation is carried out by immersion in a mixed solution of milbeic acid/ethanol.
9. The CF/PEEK composite material obtainable by the use according to claim 7 or 8, wherein the flexural strength is not less than 800MPa and the interlaminar shear strength is not less than 80MPa.
10. Use of the CF/PEEK composite of claim 9 in automotive, marine and aerospace applications.
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