CN113024855B - High-toughness carbon fiber/epoxy resin composite material based on RFI process and preparation method thereof - Google Patents
High-toughness carbon fiber/epoxy resin composite material based on RFI process and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-toughness carbon fiber/epoxy resin composite material based on an RFI (radio frequency interference) process and a preparation method thereof, belonging to the technical field of carbon fiber reinforced epoxy resin composite materials. The method comprises the following steps: preparing a casting solution by using high-toughness thermoplastic resin, epoxy resin and a curing agent thereof to be matched with an organic solvent, coating the casting solution on the surface of a carbon fiber fabric by using a film scraping rod, immersing the carbon fiber fabric into deionized water to obtain a prefabricated body, and preparing the high-toughness carbon fiber/epoxy resin composite material by an RFI (radio frequency interference) process. The invention has the advantages that: the fabric surface adhesive film has higher viscosity at normal temperature and is not easy to flow, the viscosity is lower at the resin curing temperature and above, the carbon fiber fabric can be quickly infiltrated from top to bottom, the sizing of the carbon fiber fabric can be realized due to the surface tension of the adhesive film after the adhesive film is formed, and in addition, the accurate control of the volume content of the composite material fiber can be realized by regulating and controlling the interval width of the film scraping rod.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a high-toughness carbon fiber/epoxy resin composite material based on an RFI (radio frequency interference) process and a preparation method thereof, and particularly relates to a method for preparing the high-toughness carbon fiber/epoxy resin composite material by directly coating a high-toughness resin film on the surface of a carbon fiber fabric and forming a preform through RFI.
Background
Epoxy resins (EP) have excellent properties such as ease of handling, low shrinkage on crosslinking, and low creep, and are one of the most commonly used resins in liquid molding processes. However, due to the high brittleness of the epoxy resin, the toughness of the composite material prepared by using the epoxy resin as a matrix is low, and impact damage, delamination failure and other phenomena are easy to occur in the using process, so that the further application of the epoxy resin is limited.
Three of the most typical processes for liquid forming: compared with the latter two processes, RFI, VARI and RTM, the RFI process avoids the step of resin infusion/injection, but has strict requirements on the adhesive film prepared by the RFI process, and the ideal resin film for the RFI process requires that the used resin substrate has good film-forming property at room temperature, and the formed film can be bent at will without breaking and is not sticky; a low viscosity at the working temperature for a period of time, then a faster viscosity increase with increasing temperature; the solidification temperature is higher than the melting temperature, and the fiber preform has good wettability and adhesiveness during melting.
Therefore, how to increase the toughness of epoxy resin and satisfy the requirement of RFI on the manufacturability of resin adhesive films is an important research topic in the field of composite materials.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a high-toughness carbon fiber/epoxy resin composite material based on an RFI process and a preparation method thereof. The carbon fiber/epoxy resin composite material prepared by the RFI process is toughened, and the epoxy resin/curing agent/thermoplastic resin adhesive film is directly coated on the surface of the carbon fiber fabric by a phase inversion film scraping method.
The method for preparing the high-toughness carbon fiber/epoxy resin composite material comprises the following steps: dissolving high-performance thermoplastic resin, epoxy resin and a curing agent thereof in an organic solvent, coating the film casting solution on the surface of the carbon fiber fabric through a winding type film scraping rod, forming a high-toughness resin film on the surface of the carbon fiber fabric after a coagulating bath, and preparing the dried preform into the composite material by using an RFI process.
The designed resin system aims at the RFI process, the principle that the RFI process is not sticky at low temperature and has certain fluidity at high temperature is required to be met, a simple and practical high-toughness prepreg preparation method with accurately controllable resin content is provided in detail, and the resin content is tested in detail by preparing a composite material by a vacuum bag pressing method.
The purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of a high-toughness carbon fiber/epoxy resin composite material based on an RFI (radio frequency interference) process, which comprises the following steps of:
a1, preparing a casting solution: preparing a casting solution from the following components in percentage by mass: 22.5 to 40 percent of organic solvent, 10 to 15 percent of high-performance thermoplastic resin, 40 to 50 percent of epoxy resin and 10 to 12.5 percent of curing agent;
a2, coating the casting solution prepared in the step A1 on the surface of a carbon fiber fabric, then immersing the carbon fiber fabric in deionized water, taking out the carbon fiber fabric after the casting solution is cured and molded, and drying to obtain a prefabricated body;
and A3, preparing the prefabricated body obtained in the step A2 by an RFI process to obtain the high-toughness carbon fiber/epoxy resin composite material.
Preferably, in step A1, the organic solvent is at least one of dimethyl sulfoxide, dimethylformamide, dimethylacetamide and methylpyrrolidone.
Preferably, in step A1, the high performance thermoplastic resin is at least one of polyethersulfone, polyarylsulfone, polyetherimide, phenolphthalein based polyetherketone.
Preferably, in step A1, the epoxy resin is one of bisphenol a type epoxy resins E51 and E44.
Preferably, the high-performance thermoplastic resin is 20% by mass or more of the epoxy resin.
Preferably, in the step A1, the curing agent is at least one of diethyltoluenediamine and diaminodiphenylmethane.
Preferably, in step A2, the carbon fiber fabric structure is one of plain, twill and satin.
Preferably, in step A2, the coating bar is a wire-wound coating bar (north-south tide, japanese style OSP), and the wire gap is 100 to 200 μm, and may be one of 100 μm, 150 μm, and 200 μm.
Preferably, in the step A2, the drying temperature is 40-50 ℃ and the drying time is 20-24 hours.
Preferably, in step A3, the specific steps of the RFI process are:
laying layers on the prefabricated body, sealing the prefabricated body by adopting a vacuum bag, and heating, curing and forming to obtain the composite material;
the curing temperature of the heating curing molding is 120 ℃, and the curing time is 4 hours.
The invention also provides a high-toughness carbon fiber/epoxy resin composite material prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
(1) When the high-performance thermoplastic resin reaches 20% or more of the mass of the epoxy resin, the formed adhesive film (formed by curing the casting film liquid) has higher viscosity at normal temperature and is not easy to flow, and the adhesive film has lower viscosity at the resin curing temperature or above and can rapidly infiltrate the carbon fiber fabric from top to bottom, so that the compression strength after impact is improved.
(2) The high-toughness resin film casting solution is directly coated on the surface of the carbon fiber fabric, and the film casting solution has a shaping effect on a reinforced fabric due to the surface tension of the film casting solution after being formed by a coagulating bath, and does not influence the flatness of the fiber fabric.
(3) The invention can regulate the thickness of the adhesive film on the surface of the fabric by changing the winding width of the steel wires of the film scraping rod, thereby realizing the accurate control of the volume content of the reinforced fibers of the formed composite material.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 shows the microstructure of 200 μm (thickness of wire-wound coating rod) coating film on the surface of the carbon fiber fabric in example 3.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the invention.
Example 1
The embodiment provides a preparation method of a high-toughness carbon fiber/epoxy resin composite material based on an RFI process, which comprises the following steps:
(1) Preparing a casting solution by 37 percent of dimethylformamide, 13 percent of polyether sulfone, 40 percent of E44 epoxy resin and 10 percent of diethyl toluene diamine.
(2) Coating the casting solution on a wire-wound coating rod with a pitch of 150 μm to a grammage of 200g/m 2 The warps and the wefts are all the surfaces of plain woven fabrics made of 3K carbon fiber tows, the plain woven fabrics are immersed in deionized water for 2min, and the coated plain woven fabrics are dried for 24 hours in an oven at 40 ℃ for later use.
(3) Laying 20 preforms with high-toughness resin films on the surfaces, wherein the surfaces of the preforms are not sticky at normal temperature, and the laying design adopts [ (0/90)/(+ 45/-45)] 10 Vacuum bag sealing, heating, curing and forming (curing temperature is 120 ℃ and curing time is 4 h) preparingAnd (3) obtaining a carbon fiber/epoxy resin composite material with the carbon fiber volume content of 58%, and cutting the composite material to obtain a standard size sample bar with the size of 150mm x 100mm for the compression strength test after impact.
(4) According to ASTM D7316, the impact standard test uses a constant impact energy, normalized by the test thickness. The thickness of each laminate was measured and the required impact energy was calculated according to the following formula.
E＝C E ·h
Wherein E represents impact energy (J); c E 6.7J/mm, which is the ratio of the standard impact energy to the sample thickness; h is the specimen thickness (mm).
The falling height of the drop hammer is adjusted to reach the size of the calibrated impact energy. The drop weight height was calculated according to the following formula
H＝E/(m d ·g)
Wherein H is the drop height (m) m d The weight (kg) of the falling weight, g is the acceleration of gravity, and is generally 9.8m/s 2 。
After impact, the test specimens were compressed at a loading rate of 1.25mm/mim according to ASTM D7137, and calculated according to the following formula, to obtain the residual compressive strength of the laminate.
F CAI ＝P max /A
In the formula, F CAI Represents ultimate compressive residual strength (MPa), P max Represents the maximum force before failure (N), A represents the cross-sectional area of compression (mm) 2 ) The results are shown in table 1.
Example 2
The embodiment provides a preparation method of a high-toughness carbon fiber/epoxy resin composite material based on an RFI process, which comprises the following steps:
(1) Preparing a casting solution by using 22.5 percent of dimethylacetamide, 15 percent of polyarylsulfone, 50 percent of E51 epoxy resin and 12.5 percent of diethyltoluenediamine.
(2) Coating the casting solution on a wire-wound coating rod with a gap width of 100 μm to obtain a coating film with a gram weight of 200g/m 2 The warps and the wefts are all the surfaces of plain woven fabrics of 3K carbon fiber tows, and are immersed in deionized water,after 2min, the coated fabric was dried in an oven at 50 ℃ for 20 hours for use.
(3) Laying 20 preforms with high-toughness resin films on the surfaces at 0/90 degrees, wherein the surfaces of the preforms are not sticky at normal temperature, and the laying design adopts [ (0/90)/(+ 45/-45)] 10 And sealing the vacuum bag, and heating, curing and forming (the curing temperature is 120 ℃ and the curing time is 4 hours) to prepare the carbon fiber/epoxy resin composite material with the carbon fiber volume content of 64 percent. The composite was cut to obtain standard size bars with dimensions 150mm x 100mm for post impact compression strength testing.
(4) The impact standard test uses a constant impact energy, normalized by the test thickness, according to ASTM D7316. The thickness of each laminate was measured and the required impact energy was calculated according to the following formula.
E＝C E ·h
Wherein E represents impact energy (J); c E Is the ratio of standard impact energy to sample thickness, 6.7J/mm; h is the specimen thickness (mm).
The size of the calibrated impact energy is achieved by adjusting the falling height of the drop hammer. The drop weight height was calculated according to the following formula
H＝E/(m d ·g)
Wherein H is the drop height (m) m d The weight (kg) of the falling weight, g is the acceleration of gravity, and is generally 9.8m/s 2 。
After impact, the test specimens were compressed at a loading rate of 1.25mm/mim according to ASTM D7137, and calculated according to the following formula, to obtain the residual compressive strength of the laminate.
F CAI ＝P max /A
In the formula, F CAI Representing ultimate compressive residual strength (Mpa), P max Represents the maximum force before failure (N), A represents the cross-sectional area of compression (mm) 2 ) The results are shown in table 1.
Example 3
The embodiment provides a preparation method of a high-toughness carbon fiber/epoxy resin composite material based on an RFI process, which comprises the following steps:
(1) Preparing a casting solution according to 37 percent of dimethylformamide, 13 percent of polyetherimide, 40 percent of E51 epoxy resin and 10 percent of diaminodiphenylmethane.
(2) Coating the casting solution on a wire-wound coating rod with a gap width of 200 μm to obtain a coating film with a gram weight of 200g/m 2 The warp yarns and the weft yarns are all the surfaces of plain woven fabrics made of 3K carbon fiber tows (as shown in figure 1), the plain woven fabrics are immersed in deionized water for 2min, and the coated fabrics are dried in an oven at 40 ℃ for 24 hours for standby.
(3) Laying 20 preforms with high-toughness resin films on the surfaces, wherein the surfaces of the preforms are not sticky at normal temperature, and the laying design adopts [ (0/90)/(+ 45/-45)] 10 And sealing the vacuum bag, and heating, curing and forming (the curing temperature is 120 ℃ and the curing time is 4 hours) to prepare the carbon fiber/epoxy resin composite material with the carbon fiber volume content of 50 percent. The composite was cut to obtain standard size bars with dimensions 150mm x 100mm for post impact compression strength testing.
(4) According to ASTM D7316, the impact standard test uses a constant impact energy, normalized by the test thickness. The thickness of each laminate was measured and the required impact energy was calculated according to the following formula.
E＝C E ·h
Wherein E represents impact energy (J); c E 6.7J/mm, which is the ratio of the standard impact energy to the sample thickness; h is the specimen thickness (mm).
The size of the calibrated impact energy is achieved by adjusting the falling height of the drop hammer. The drop weight height was calculated according to the following formula
H＝E/(m d ·g)
Wherein H is the drop height (m) m d The weight (kg) of the falling weight, g is the acceleration of gravity, and is generally 9.8m/s 2 。
After impact, the test specimens were compressed at a loading rate of 1.25mm/mim according to ASTM D7137, and calculated according to the following formula, to obtain the residual compressive strength of the laminate.
F CAI ＝P max /A
In the formula, F CAI Representing extreme compression residualsResidual Strength (MPa), P max Represents the maximum force before failure (N), A represents the cross-sectional area of compression (mm) 2 ) The results are shown in table 1.
Comparative example 1
(1) The gram weight of 20 pieces is 200g/m 2 The warp yarns and the weft yarns are all laid by plain weave fabrics of 3K carbon fiber tows, and the laid design adopts [ (0/90)/(+ 45/-45)] 10 And installing an exhaust pipe and a rubber inlet pipe on two sides, injecting E51 and diaminodiphenylmethane (in a weight ratio of 4: 1) at 60 ℃, and curing the laminated plate at 120 ℃ for 4 hours to prepare the carbon fiber/epoxy resin composite material. The composite was cut to obtain standard size bars with dimensions 150mm x 100mm for post impact compression strength testing.
(2) According to ASTM D7316, the impact standard test uses a constant impact energy, normalized by the test thickness. The thickness of each laminate was measured and the required impact energy was calculated according to the following formula.
E＝C E ·h
Wherein E represents impact energy (J); c E 6.7J/mm, which is the ratio of the standard impact energy to the sample thickness; h is the specimen thickness (mm).
The falling height of the drop hammer is adjusted to reach the size of the calibrated impact energy. The drop weight height was calculated according to the following formula
H＝E/(m d ·g)
Wherein H is the drop height (m) m d The weight (kg) of the falling weight, g is the acceleration of gravity, and is generally 9.8m/s 2 。
After impact, the test specimens were compressed at a loading rate of 1.25mm/mim according to ASTM D7137, and calculated according to the following formula, to obtain the residual compressive strength of the laminate.
F CAI ＝P max /A
In the formula, F CAI Representing ultimate compressive residual strength (Mpa), P max Represents the maximum force before failure (N), A represents the cross-sectional area of compression (mm) 2 ) The results are shown in table 1.
Comparative example 2
This comparative example provides a method of making a high tenacity carbon fiber/epoxy composite based on RFI processing, the procedure being essentially the same as in example 3, except that: in the step (1), a casting solution is prepared according to 37% of dimethylformamide, 8% of polyetherimide, 45% of E51 epoxy resin and 10% of diaminodiphenylmethane.
The standard size bars obtained in this comparative example were tested for post-impact compressive strength in the same manner as in example 3 and the results are shown in Table 1.
TABLE 1
| Sample (I) | Compressive strength after impact (MPa) |
| Example 1 | 211 |
| Example 2 | 199 |
| Example 3 | 203 |
| Comparative example 1 | 158 |
| Comparative example 2 | 167 |
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (6)
1. A preparation method of a high-toughness carbon fiber/epoxy resin composite material based on an RFI process is characterized by comprising the following steps:
a1, preparing a casting solution: preparing a casting solution from the following components in percentage by mass: 22.5 to 40 percent of organic solvent, 10 to 15 percent of high-performance thermoplastic resin, 40 to 50 percent of epoxy resin and 10 to 12.5 percent of curing agent;
a2, coating the casting solution prepared in the step A1 on the surface of a carbon fiber fabric, then immersing the carbon fiber fabric in deionized water, taking out the carbon fiber fabric after the casting solution is cured and molded, and drying to obtain a prefabricated body;
a3, preparing the prefabricated body obtained in the step A2 into a high-toughness carbon fiber/epoxy resin composite material through an RFI (radio frequency interference) process;
in the step A1, the organic solvent is at least one of dimethyl sulfoxide, dimethylformamide, dimethylacetamide and methylpyrrolidone;
in the step A2, the drying temperature is 40-50 ℃, and the drying time is 20-24 hours;
in the step A1, the high-performance thermoplastic resin is at least one of polyarylsulfone, polyetherimide and phenolphthalein polyether ketone; the curing agent is at least one of diethyltoluenediamine and diaminodiphenylmethane.
2. The method for preparing a high-toughness carbon fiber/epoxy resin composite material based on an RFI process as claimed in claim 1, wherein in the step A1, the epoxy resin is one of bisphenol A epoxy resins E51 and E44.
3. The method for preparing a high-tenacity carbon fiber/epoxy resin composite material based on an RFI process according to claim 1, wherein in the step A2, the carbon fiber fabric structure is one of plain weave, twill weave and satin weave.
4. A method for preparing a high toughness carbon fiber/epoxy resin composite material based on RFI process as claimed in claim 1, wherein in step A2, the film scraping bar used for coating is a wire wound coating bar, and the steel wire gap is 100-200 μm.
5. The method for preparing the high-toughness carbon fiber/epoxy resin composite material based on the RFI process according to claim 1, wherein in the step A3, the RFI process comprises the following specific steps:
laying layers on the prefabricated body, sealing the prefabricated body by adopting a vacuum bag, and heating, curing and forming to obtain the composite material;
the curing temperature of the heating curing molding is 120 ℃, and the curing time is 4 hours.
6. A high tenacity carbon fiber/epoxy composite prepared according to the process of any one of claims 1 to 5.
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