CN110588015A - Inorganic nanoparticle/thermoplastic particle synergistic toughened resin-based composite material and preparation method thereof - Google Patents
Inorganic nanoparticle/thermoplastic particle synergistic toughened resin-based composite material and preparation method thereof Download PDFInfo
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- CN110588015A CN110588015A CN201910833410.7A CN201910833410A CN110588015A CN 110588015 A CN110588015 A CN 110588015A CN 201910833410 A CN201910833410 A CN 201910833410A CN 110588015 A CN110588015 A CN 110588015A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
- B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
- B29B15/10—Coating or impregnating independently of the moulding or shaping step
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
- B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
- B29B15/10—Coating or impregnating independently of the moulding or shaping step
- B29B15/105—Coating or impregnating independently of the moulding or shaping step of reinforcement of definite length with a matrix in solid form, e.g. powder, fibre or sheet form
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
- B29C70/34—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation
- B29C70/342—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation using isostatic pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
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Abstract
The invention discloses an inorganic nanoparticle/thermoplastic particle synergistic toughened resin-based composite material and a preparation method thereof, belonging to the technical field of high performance of composite materials. According to the invention, by a simple and easy method with low cost, the inorganic nanoparticles and the thermoplastic particles are simultaneously uniformly, effectively and stably introduced into the resin matrix composite material layer, so that the synergistic toughening of the composite material is realized, the toughening effect is far higher than that of the toughening effect of the inorganic nanoparticles or the thermoplastic particles which are singly used, the interlayer fracture toughness of the composite material is greatly improved, and the application field of the composite material is expanded.
Description
Technical Field
The invention relates to an inorganic nanoparticle/thermoplastic particle synergistic toughened resin-based composite material and a preparation method thereof, belonging to the technical field of high performance of composite materials.
Background
The fiber reinforced resin matrix composite material has excellent performances such as high specific strength, high specific modulus, strong designability and the like, and is widely applied to a plurality of fields such as aviation, aerospace, navigation, automobiles, industry and the like. However, the load is mainly transferred between the layers of the composite material by the matrix, and the high-crosslinked network structure of the resin matrix makes the composite material brittle, so that the fracture toughness between the layers of the composite material is low, the delamination damage is easy to occur, and the comprehensive performance of the resin matrix composite material is greatly reduced. With the improvement of the performance requirements of various fields on the composite material, particularly the requirement on high toughness, the toughening of the resin-based composite material becomes an important direction for the research of the advanced composite material. Common methods for toughening composite materials include Z-direction toughening, interface modification, matrix toughening, interlaminar toughening, and the like. The interlayer toughening method has the best combination property, and the prior composite material interlayer toughening method comprises interlayer film toughening, interlayer fiber toughening, interlayer particle toughening and the like. Although the methods have a certain interlayer toughening effect on the composite material, the toughening effect is limited, and sometimes special requirements on the operation process and the like are required, so that the methods cannot meet the higher toughening requirement on the advanced composite material. Therefore, it is necessary to develop a method for greatly improving the interlayer toughening effect of the composite material.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for synergistically toughening resin matrix composite material interlamination by simultaneously adopting inorganic nano particles and thermoplastic particles, so that the toughening effect of the composite material interlamination is obviously improved, and the related preparation method of the high-toughness composite material is simple to operate.
The invention provides a novel method for toughening a resin-based composite material by using inorganic nano particles/thermoplastic particles in a synergistic manner, aiming at the requirement that the interlayer toughening of an advanced composite material needs to be further improved, and the method has the characteristics of easiness in operation, low cost and the like and can greatly improve the interlayer toughening effect of the composite material.
The invention provides a method for toughening a resin-based composite material by the cooperation of inorganic nano particles/thermoplastic particles, which comprises the following steps:
1) dissolving inorganic nano particles in an ethanol solution, uniformly spraying the solution on one surface of the fiber reinforced resin based prepreg after ultrasonic oscillation, drying the coated prepreg after the spraying is finished, and cooling the coated prepreg to room temperature;
2) uniformly distributing thermoplastic particles on the surface of the fiber reinforced resin based prepreg sprayed with the inorganic nano particles in the step 1), heating the obtained fiber reinforced resin based prepreg to a certain temperature, and cooling to room temperature;
3) placing the mould into a clean room, laying the fiber reinforced resin matrix prepreg obtained in the step 2) into the mould layer by layer, curing and forming by adopting a vacuum bag-autoclave forming method, cooling the temperature in the autoclave to room temperature, and demoulding to obtain the product.
Further, in the above technical scheme, the inorganic nanoparticles in step 1) include nano aluminum oxyhydroxide and nano Fe2O3Particles, nano montmorillonite and carboxylated multi-wall carbon nano tube.
Further, in the above technical scheme, the concentration of the inorganic nanoparticles in the fiber reinforced resin based prepreg in step 1) is 0.5 wt% to 2 wt%.
Further, in the above technical scheme, the time of the ultrasonic oscillation in the step 1) is 0.5-2 h; after the spraying is finished, drying for 0.5-1.5h at the temperature of 75-85 ℃.
Further, in the above technical scheme, the thermoplastic particles in step 2) are micrometer-scale thermoplastic particles, and specifically include polyaryletherketone, polyethersulfone, polyphenylene oxide, polysulfone, bismaleimide, polyetheretherketone, polycarbonate, and polyphenylene sulfide.
Further, in the above technical scheme, in the step 2), the thermoplastic particles are uniformly distributed on one surface of the fiber reinforced resin matrix prepreg obtained in the step 1) by adopting a sample separation sieve, and the concentration of the thermoplastic particles in the resin matrix is 10-30 wt%; the heating temperature in the step 2) is 75-85 ℃, and the heating time is 5 minutes.
Further, in the above technical scheme, before the mold is placed in the clean room in step 3), the mold needs to be wiped with ethanol, and after the ethanol is volatilized, a piece of release cloth is attached to the surface of the mold.
Further, in the above technical scheme, the temperature in the clean room in step 3) is 18 to 26 ℃, the relative humidity is 25 to 65%, and the laying mode of the fiber reinforced resin-based prepreg in step 3) in the mold is as follows: and in the purification room, the surface sprayed with the inorganic nano particles/thermoplastic particles is laid in the mould layer by layer, the first layer is prepreg which is not sprayed so as to obtain a layer without toughening particles on the surface, the layers of the toughening particles are uniformly distributed among the layers, and the number of the laid layers is set according to the requirement.
Further, in the above technical solution, the vacuum bag-autoclave forming method in step 3) specifically includes: and (2) putting the laid mould of the fiber reinforced resin-based prepreg into a vacuum bag, vacuumizing the vacuum bag, putting the mould into an autoclave after vacuumizing, pressurizing to 0.3MPa, curing and forming according to the curing process of 0.5h at 80 ℃, 2h at 120 ℃ and 4h at 180 ℃, and then demolding after the temperature in the autoclave is reduced to room temperature.
The invention also provides the inorganic nano particle/thermoplastic particle synergistic toughening resin matrix composite material prepared by the method.
Advantageous effects of the invention
According to the invention, by a simple and easy method with low cost, the inorganic nanoparticles and the thermoplastic particles are simultaneously uniformly, effectively and stably introduced into the resin matrix composite material layer, so that the synergistic toughening of the composite material is realized, the toughening effect is far higher than that of the toughening effect of the inorganic nanoparticles or the thermoplastic particles which are singly used, the interlayer fracture toughness of the composite material is greatly improved, and the application field of the composite material is expanded.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of the microstructure of the fracture surface of the polyaryletherketone thermoplastic particle toughened composite material of example 1.
FIG. 2 is a Scanning Electron Microscope (SEM) image of the micro-morphology of the fracture surface of the nano aluminum oxyhydroxide/polyaryletherketone thermoplastic particle toughened composite material of example 1.
FIG. 3(a) is a Scanning Electron Micrograph (SEM) of the interfacial microtopography of the non-toughened composite of example 1; (b) scanning Electron Microscope (SEM) images of the 1% nano aluminum oxyhydroxide toughened composite material interface microscopic morphology in example 1; FIG. 3(c) is a Scanning Electron Microscope (SEM) image of the interfacial micro-morphology of the nano aluminum oxyhydroxide/polyaryletherketone thermoplastic particle toughened composite material of example 1.
FIG. 4 shows the interlaminar fracture toughness of the layer II of the nano aluminum oxyhydroxide/polyaryletherketone thermoplastic particle toughened composite material of example 1.
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
Example 1
1) Cutting the carbon fiber reinforced epoxy resin-based prepreg into a size of 30cm multiplied by 30 cm;
2) dissolving nano-aluminum oxyhydroxide (AlOOH) in an ethanol solution according to the proportion of 1 wt% of a resin matrix, oscillating for 1.5 hours in ultrasound to uniformly disperse nanoparticles, uniformly spraying the nano-aluminum oxyhydroxide (AlOOH) on one surface of the surface of a fiber-reinforced resin-based prepreg by using a sprayer, placing the fiber-reinforced resin-based prepreg in an oven at 80 ℃ for drying for 1 hour to completely remove the ethanol solution, and cooling to room temperature to ensure that inorganic nanoparticles are stably and uniformly distributed in the fiber-reinforced resin-based prepreg;
3) uniformly distributing Polyaryletherketone (PAEK) thermoplastic particles on the surface of a fiber reinforced resin matrix prepreg on one surface of which AlOOH particles are dispersed by using a sample separation sieve, controlling the content to be about 10 wt%, heating the fiber reinforced resin matrix prepreg to 80 ℃ to uniformly embed the PAEK particles into a resin matrix, and cooling the temperature of the fiber reinforced resin matrix prepreg to room temperature for later use;
4) wiping the surface of the mould by using a wiping cloth soaked with ethanol, and sticking a demoulding cloth on the surface of the mould after the solvent is volatilized.
5) Placing a mould into a purification room, wherein the temperature of the purification room is set to be 25 ℃, the relative humidity is 50%, laying fiber reinforced resin-based prepreg with AlOOH particles and PAEK particles dispersed on one surface into the mould layer by layer, wherein the first layer is prepreg which is not sprayed to obtain a layer without toughening particles on the surface, and the layers with toughening particles uniformly distributed among the layers are laid for 12 layers;
6) putting the mould with the laid fiber reinforced resin matrix prepreg into a vacuum bag, vacuumizing the fiber reinforced resin matrix prepreg paving layer, putting the mould with the vacuum bag wrapped in the vacuum bag into an autoclave by adopting a vacuum bag-autoclave forming method, pressurizing to 0.3MPa, and curing and forming according to a curing process of 0.5h at 80 ℃, 2h at 120 ℃ and 4h at 180 ℃;
7) and (3) after the temperature in the autoclave is reduced to room temperature, carrying out demoulding treatment to finally obtain the 2mm AlOOH/PAEK toughened unidirectional composite material laminated plate.
According to the test standard of ASTM D7905/D7905M-14, the II-type fracture toughness research of the unidirectional composite material laminated plate shows that 1 wt% of AlOOH and 10 wt% of PAEK are simultaneously added into the carbon fiber/epoxy resin composite material, and the II-type fracture toughness reaches 1368.0J/m2Compared with the composite material without the addition, the toughening effect is improved by 90.1 percent and is far higher than that of the toughening effect of the composite material with one particle added separately.
The interlaminar fracture toughness of the toughened carbon fiber composite material obtained by the embodiment is as follows:
FIG. 1 is a Scanning Electron Microscope (SEM) image of the microscopic morphology of the fracture surface of the polyaryletherketone thermoplastic particle toughened composite material, and it can be seen from FIG. 1 that polyaryletherketone thermoplastic particles are distributed on the fracture surface of the composite material more uniformly, but the particle diameters of the particles are uneven, so that the toughness of the composite material toughened by a single thermoplastic particle is improved, but the improvement ratio is limited;
FIG. 2 is a Scanning Electron Microscope (SEM) image of the microscopic morphology of the fracture surface of the nano-sized hydroxy aluminum oxide/polyaryletherketone thermoplastic particle toughened composite material, and it can be seen from FIG. 2 that two types of toughening particles are mutually fused and uniformly distributed on the fracture surface of the composite material, so that the interlayer binding force of the composite material can be effectively improved, and a good synergistic toughening effect is achieved.
FIG. 3(a) is a Scanning Electron Microscope (SEM) image of the micro-morphology of the interface of the non-toughened composite material, and it can be seen that the interface of the non-toughened composite material is smoother, which indicates that the interlayer bonding of the non-toughened composite material is weaker and the toughness is lower; FIG. 3(b) is a Scanning Electron Microscope (SEM) image of the microscopic morphology of the interface of the 1% nano aluminum oxyhydroxide toughened composite material, and it can be seen that the interface of the composite material toughened by the nano aluminum oxyhydroxide particles becomes rough, and the fractured interface has feather-shaped resin, which indicates that more energy needs to be consumed and the toughness is improved when the interface of the composite material toughened by the inorganic nano particles is damaged; fig. 3(c) is a Scanning Electron Microscope (SEM) image of the microscopic interface morphology of the nano aluminum oxyhydroxide/polyaryletherketone thermoplastic particle toughened composite material, and it can be seen that the composite material interface toughened by the nano aluminum oxyhydroxide particles and the polyaryletherketone thermoplastic particles is rougher, and the feather-like resin at the fracture interface is more obvious, which indicates that the two toughened composite material interfaces have higher bonding strength and higher toughness.
Fig. 4 shows that the nano-hydroxy-alumina/polyaryletherketone thermoplastic particle toughened composite material II type layer has discontinuous fracture toughness, and it can be seen that the nano-hydroxy-alumina particles and the polyaryletherketone thermoplastic particles have a certain toughening effect on the composite material independently, the toughening effect of the two particles on the composite material is more obvious simultaneously, and the toughening effect is greater than the sum of the toughening effects of the two particles independently, which indicates that the two particles have a synergistic effect on the toughening of the material.
Example 2
1) Cutting the carbon fiber reinforced epoxy resin-based prepreg into a size of 30cm multiplied by 30 cm;
2) according to the proportion of 1.5 wt% of resin matrix, nano Fe2O3Dissolving the particles in ethanol solution, oscillating for 2h in ultrasound to disperse the nanoparticles uniformly, spraying the particles on one surface of the fiber reinforced resin based prepreg uniformly by using a sprayer, and placing the fiber reinforced resin based prepregDrying in an oven at 80 ℃ for 1h to completely remove the ethanol solution, and cooling to room temperature to ensure that the inorganic nanoparticles are stably and uniformly distributed in the fiber reinforced resin matrix prepreg;
3) polyether sulfone (PES) thermoplastic particles are uniformly distributed on the dispersed nano Fe by using a sample separation sieve2O3Controlling the content of the surface of the fiber reinforced resin-based prepreg on one surface of the particle to be about 20 wt%, heating the fiber reinforced resin-based prepreg to 80 ℃ so that PES particles are uniformly embedded into the resin matrix, and cooling the temperature of the fiber reinforced resin-based prepreg to room temperature for later use;
4) wiping the surface of the mould by using a wiping cloth soaked with ethanol, and sticking a demoulding cloth on the surface of the mould after the solvent is volatilized.
5) Placing the mold in a clean room with a temperature of 25 deg.C and a relative humidity of 50%, dispersing nanometer Fe on one surface2O3Laying fiber reinforced resin-based prepregs of particles and PES particles into a mould layer by layer, wherein the first layer is a prepreg which is not sprayed so as to obtain a layer with no toughening particles on the surface, and the layers of the toughening particles are uniformly distributed among the layers, and 24 layers are laid;
6) putting the mould with the laid fiber reinforced resin matrix prepreg into a vacuum bag, vacuumizing the fiber reinforced resin matrix prepreg paving layer, putting the mould with the vacuum bag wrapped in the vacuum bag into an autoclave by adopting a vacuum bag-autoclave forming method, pressurizing to 0.3MPa, and curing and forming according to a curing process of 0.5h at 80 ℃, 2h at 120 ℃ and 4h at 180 ℃;
7) after the temperature in the autoclave is reduced to room temperature, demoulding treatment is carried out to finally prepare 4mm Fe2O3PES toughened unidirectional composite laminates.
Claims (10)
1. A method for synergistically toughening a resin-based composite material by using inorganic nanoparticles/thermoplastic particles is characterized by comprising the following steps:
1) dissolving inorganic nano particles in an ethanol solution, uniformly spraying the solution on one surface of the fiber reinforced resin based prepreg after ultrasonic oscillation, drying the coated prepreg after the spraying is finished, and cooling the coated prepreg to room temperature;
2) uniformly distributing thermoplastic particles on the surface of the fiber reinforced resin based prepreg sprayed with the inorganic nano particles in the step 1), heating the obtained fiber reinforced resin based prepreg to a certain temperature, and cooling to room temperature;
3) placing the mould into a clean room, laying the fiber reinforced resin matrix prepreg obtained in the step 2) into the mould layer by layer, curing and forming by adopting a vacuum bag-autoclave forming method, cooling the temperature in the autoclave to room temperature, and demoulding to obtain the product.
2. The method as claimed in claim 1, wherein the inorganic nanoparticles in step 1) comprise nano aluminum hydroxide and nano Fe2O3Particles, nano montmorillonite and carboxylated multi-wall carbon nano tube.
3. The method according to claim 1, wherein the concentration of the inorganic nanoparticles in the fiber reinforced resin based prepreg in the step 1) is 0.5-2 wt%.
4. The method as claimed in claim 1, wherein the time of the ultrasonic oscillation in the step 1) is 0.5-2 h; after the spraying is finished, drying for 0.5-1.5h at the temperature of 75-85 ℃.
5. The method as claimed in claim 1, wherein the thermoplastic particles in step 2) are micron-sized thermoplastic particles, specifically comprising polyaryletherketone, polyethersulfone, polyphenylene oxide, polysulfone, bismaleimide, polyetheretherketone, polycarbonate, polyphenylene sulfide.
6. The method according to claim 1, wherein in the step 2), the thermoplastic particles are uniformly distributed on one surface of the fiber reinforced resin-based prepreg obtained in the step 1) by using a sample separation sieve, and the concentration of the thermoplastic particles in the resin matrix is 10-30 wt%; the heating temperature in the step 2) is 75-85 ℃, and the heating time is 5 minutes.
7. The method as claimed in claim 1, wherein the step 3) is carried out by wiping the mold with ethanol before the mold is placed in the clean room, and attaching a release cloth on the surface of the mold after the ethanol is volatilized.
8. The method as claimed in claim 1, wherein the temperature in the clean room in step 3) is 18-26 ℃ and the relative humidity is 25-65%; the laying mode of the fiber reinforced resin-based prepreg in the step 3) in the mould is as follows: and in the purification room, paving the surface sprayed with the inorganic nano particles/thermoplastic particles in a mold layer by layer, wherein the first layer is a non-sprayed fiber reinforced resin-based prepreg so as to obtain a layer with no toughening particles on the surface and toughening particles uniformly distributed among layers.
9. The method according to claim 1, wherein the vacuum bag-autoclave forming method in step 3) is specifically: putting the mould paved with the fiber reinforced resin matrix prepreg into a vacuum bag, vacuumizing the vacuum bag, putting the mould into an autoclave after vacuumizing, pressurizing to 0.3MPa, curing and forming according to the curing process of 0.5h at 80 ℃, 2h at 120 ℃ and 4h at 180 ℃, and then demoulding after the temperature in the autoclave is reduced to room temperature.
10. The inorganic nanoparticle/thermoplastic particle synergistic toughened resin-based composite material prepared by the method according to any one of claims 1 to 9.
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Cited By (5)
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| CN113246564A (en) * | 2020-02-13 | 2021-08-13 | 中国科学院化学研究所 | High-strength high-toughness phthalonitrile-based composite material and preparation method and application thereof |
| 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 |
| CN115109389A (en) * | 2022-08-12 | 2022-09-27 | 中复神鹰(上海)科技有限公司 | Epoxy resin for micron particle interlayer toughened prepreg and preparation method thereof |
| WO2022242162A1 (en) * | 2021-05-21 | 2022-11-24 | 大连理工大学 | Preparation method for composite vaccine adjuvant based on aluminum oxyhydroxide nano carboxyl modification |
| WO2024050806A1 (en) * | 2022-09-05 | 2024-03-14 | 中国科学院宁波材料技术与工程研究所 | Preparation method for high-toughness fiber-reinforced composite material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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