CN110834444A - Preparation method of interlayer toughening composite material - Google Patents
Preparation method of interlayer toughening composite material Download PDFInfo
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- CN110834444A CN110834444A CN201911179151.7A CN201911179151A CN110834444A CN 110834444 A CN110834444 A CN 110834444A CN 201911179151 A CN201911179151 A CN 201911179151A CN 110834444 A CN110834444 A CN 110834444A
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Abstract
The invention discloses a preparation method of an interlayer toughening composite material, which comprises the following steps: the method comprises the following steps: selecting microcapsules with multiple capsule cores as a composite material interlayer toughening material, and performing the following steps: impregnating continuous fibers in a resin matrix to prepare a prepreg of the resin matrix and the fibers; step three: laying the prepreg obtained in the step two along a single direction, and transferring the prepreg to a hot press for heating and pressurizing for curing; step four: mixing the microcapsule, epoxy resin and curing agent, and manually stirring to prepare a resin glue solution with the microcapsule; step five: coating the resin glue solution with the microcapsules on the surface of the cured prepreg stacking object by using a brush; step six: and C, adhering the prepreg stacks which are coated and cured in the step V, and transferring to a hot press for heating and pressurizing to perform interlayer matrix curing treatment. The microcapsule preparation raw materials adopted in the preparation method are cheap, the preparation process is mature, the cost is lower, the operability is high, and the large-scale industrial popularization can be carried out.
Description
Technical Field
The invention belongs to a process preparation technology of a carbon fiber/resin matrix laminated composite material, in particular to a composite material modification method using agglomerated microcapsules as a toughening material, and belongs to the technical field of composite material science.
Background
The composite material has the unique advantages of high specific strength, large specific rigidity, heat resistance, corrosion resistance, good designability and the like, and is widely applied to the design and manufacture industries of high-speed motor cars, aerospace, wind turbine generators, automobiles and the like at present, for example, the dosage of the composite material on the large-scale passenger plane wave sound 787 is up to 50 percent, and the dosage of the composite material on the fan blade of the wind driven generator exceeds 90 percent.
As one of the common components, the composite material plate is a typical layered structure, and mainly depends on thermosetting matrix resin to perform a bonding effect, so that the composite material plate is prone to layering damage in a long-term service process, and along with the layering expansion, the bearing capacity of the composite material plate is rapidly reduced, so that the whole structure fails, huge economic loss and even casualties are caused, and the adverse effect on the surrounding environment is also caused.
In order to improve the delamination resistance of the composite material, a plurality of interlaminar toughening technologies are developed, mainly comprising matrix toughening and nanostructure toughening. Matrix toughening refers to the addition of rubber or thermoplastic to a resin to increase the fracture toughness of the composite, but this approach increases the weight of the structure and manufacturing costs, while the incorporation of the thermoplastic resin increases the viscosity of the matrix resin, resulting in poor in-plane properties of the composite. The nanostructure toughening method mainly comprises the step of inserting carbon nanotube gauze or a combined structure of structural fibers and carbon nanotubes between layers to achieve the effect of toughening the material, but the technical processes are relatively complex and are still in the basic research stage, so that the problems in the practical application process are more, and the method cannot be popularized and used on a large scale.
Disclosure of Invention
The invention mainly aims to solve the defects in the prior art and provides a method for enhancing the interlayer toughness of a composite material by adopting microcapsules. The method has simple implementation steps, low cost and high operability, and can be industrially popularized on a large scale; meanwhile, the nano-level microcapsule can not reduce the mechanical property of the composite material, and has wide application prospect in the fields of modification and toughening of resin matrix composite materials.
In order to achieve the purpose, the preparation method of the interlayer toughening composite material provided by the invention comprises the following specific preparation steps:
the method comprises the following steps: the microcapsule with multiple capsule cores is selected as a composite material interlayer toughening material, and the capsule core comprises the following components: bisphenol A diglycidyl ether, (3-mercaptopropionic acid) pentaerythritol ester, (dimethylaminomethyl) phenol, wherein the capsule wall material is urea formaldehyde, the mass fraction of the core material is more than 95wt%, and the average particle size of the microcapsule is 9.4 mu m;
step two: impregnating continuous fibers in a resin matrix to prepare a prepreg of the resin matrix and the fibers;
step three: laying the prepreg obtained in the step two along a single direction, transferring the prepreg to a hot press, heating and pressurizing the prepreg for curing treatment, wherein the curing temperature is 120 ℃, the pressure is 4Mpa, and the time is 1 h;
step four: mixing the microcapsule, epoxy resin and curing agent, and manually stirring to prepare a resin glue solution with the microcapsule;
step five: coating the resin glue solution with the microcapsules on the surface of the cured prepreg stacking object by using a brush;
step six: and (4) laminating the prepreg stacks which are coated and cured in the two fifth steps, transferring to a hot press, heating and pressurizing to perform interlayer matrix curing treatment, wherein the curing temperature is 120 ℃, the pressure is 4Mpa, and the time is 1h, and finally obtaining the composite material laminated plate with improved interlayer toughness.
Preferably, in the first step, the capsule core is made of bisphenol a diglycidyl ether, (3-mercaptopropionic acid) pentaerythritol ester, (dimethylaminomethyl) phenol, and the capsule wall is made of urea formaldehyde.
Optionally, in the second step, the carbon fiber is selected from commercial T300.
Optionally, in the third step, the laying direction of the prepreg is a single direction.
Preferably, in the third step and the sixth step, the curing temperature is 120 ℃, the pressure is 4Mpa, and the time is 1 h;
preferably, in the sixth step, the two laminated prepreg stacks are coated with the resin glue solution of the capsule.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
the toughening substance microcapsules utilized in the invention are distributed in an interlayer matrix in an agglomerated form, and are broken in the curing process of high temperature and high pressure to induce the core material to carry out polymerization reaction, which is equivalent to forming a plurality of special pins in the resin matrix, thereby effectively improving the interlayer toughness of the composite material. In the process of capsule core polymerization, bisphenol A diglycidyl ether is used as a main body, pentaerythritol ester (3-mercaptopropionic acid) is used as a curing agent, and dimethyl aminomethyl phenol is used as a catalyst.
Compared with the prior toughening technology, the method has the following advantages:
1) after the microcapsule adopted in the method is broken, the capsule core is induced to generate polymerization reaction to form a plurality of special pins, and the interlayer toughening effect of the product is effectively improved.
2) In the method, microcapsules with the average grain diameter of only 9.4 mu m are used as toughening materials, and the microcapsules do not have negative influence on the self-attribute of the structure in the process of filling the microcapsules into an interlayer resin matrix.
3) In the process of curing the composite material, the method adopts the high temperature of 120 ℃ and the high pressure of 4Mpa, which is not only beneficial to enhancing the interlaminar toughness of the structure, but also beneficial to the polymerization reaction of the capsule, thereby improving the toughening effect.
4) The microcapsule preparation raw materials adopted in the method are cheap, and the preparation process is mature, so the toughening technology has simple implementation steps, lower cost and high operability, and can be industrially popularized on a large scale.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments will be briefly described below, which are intended to illustrate the present invention and should not be construed as limiting the present invention.
FIG. 1 is a flow chart of a composite sheet fabrication process according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the distribution of microcapsules in a resin matrix according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a preparation method of an interlayer toughening composite material, which has the advantages of low cost, simple implementation steps, high operability and good toughening effect.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example (b):
the interlayer toughening composite material plate containing the agglomerated microcapsules comprises a fiber prepreg stacking object and an epoxy resin glue solution, wherein the microcapsules are arranged in the epoxy resin glue solution, and the resin glue solution is filled and coated on the surface of the cured prepreg stacking object. In this embodiment, 10 layers of fiber prepregs with a thickness of 0.15mm are unidirectionally paved into a stack with a thickness of 1.5mm, and the finally formed interlaminar toughened sample is a composite plate-shaped structure with a thickness of 3 mm.
Fig. 2 is a schematic diagram of the distribution of microcapsules in a resin matrix. As can be seen from FIG. 2, the capsules are distributed in the interlaminar resin matrix in an agglomerated form, and in the process of placing a sample on a hot press and curing at a high temperature of 120 ℃ and a high pressure of 4MPa, the capsules are extruded to be broken, the capsule cores are induced to generate polymerization reaction, and a plurality of special pins are formed in the matrix, so that the interlaminar fracture toughness is improved, and the toughening effect is achieved, wherein the high temperature of 120 ℃ is more beneficial to the polymerization reaction. The microcapsules in this example were produced by Hangzhou Tuomeles technologies, Inc.
The specific steps of this example are as follows:
1) the microcapsule with lower cost and mature production process is selected as a composite material laminated structure interlayer toughening material, the average grain diameter of the microcapsule is 9.4 mu m, the capsule wall material is urea formaldehyde, and the capsule core comprises the following components: bisphenol A diglycidyl ether, (3-mercaptopropionic acid) pentaerythritol ester, (dimethylaminomethyl) phenol, the mass fraction of core materials is more than 95wt%, and 5g of core materials are weighed on a high-precision mass balance;
2) and (2) weighing 10g of epoxy resin and 10g of curing agent on a high-precision mass scale, putting the epoxy resin and the curing agent into a beaker, uniformly stirring, putting the microcapsule obtained in the step (1) into the same beaker, and manually stirring for several times.
3) Laying 10 layers of fiber prepregs with the thickness of 0.15mm, the length of 250mm and the width of 250mm into a stack with the thickness of 1.5mm along a single direction;
4) transferring the prepreg stack in the step 3 to a hot press, heating and pressurizing for curing treatment, wherein the curing temperature is 120 ℃, the pressure is 4Mpa, and the time is 1 h;
5) coating the resin glue solution with the microcapsules in the step 2 on the surface of the cured prepreg stack in the step 4 by using a brush;
6) bonding the two piled substances which are coated in the step 5, inserting a polyimide film with the thickness of 100nm and the length of 50mm into one end of a sample, transferring the sample to a hot press, heating and pressurizing the sample to carry out interlayer matrix curing treatment, wherein the curing temperature is 120 ℃, the pressure is 4Mpa, and the time is 1 h;
7) cutting the composite material plate prepared in the step 6 into a double-cantilever beam standard sample, and adhering a metal hinge;
8) the samples described in step 7 were subjected to a mode I interlaminar fracture test according to ASTM-D5528.
Table 1: interlaminar fracture toughness of T300/epoxy resin filled microcapsule
Table 1 the data illustrates:
the type I fracture toughness of the dual cantilever beam samples prepared by the example filling of the agglomerated microcapsules was improved by 116.58% over the original dual cantilever beam sample that was not toughened.
Claims (6)
1. A preparation method of an interlayer toughening composite material is characterized by comprising the following specific preparation steps:
the method comprises the following steps: the microcapsule with multiple capsule cores is selected as a composite material interlayer toughening material, and the capsule core comprises the following components: bisphenol A diglycidyl ether, (3-mercaptopropionic acid) pentaerythritol ester, (dimethylaminomethyl) phenol, wherein the capsule wall material is urea formaldehyde, the mass fraction of the core material is more than 95wt%, and the average particle size of the microcapsule is 9.4 mu m;
step two: impregnating continuous fibers in a resin matrix to prepare a prepreg of the resin matrix and the fibers;
step three: laying the prepreg obtained in the step two along a single direction, transferring the prepreg to a hot press, heating and pressurizing the prepreg and curing the prepreg at the curing temperature of 120 DEG CoC, the pressure is 4Mpa, and the time is 1 h;
step four: mixing the microcapsule, epoxy resin and curing agent, and manually stirring to prepare a resin glue solution with the microcapsule;
step five: coating the resin glue solution with the microcapsules on the surface of the cured prepreg stacking object by using a brush;
step six: bonding the prepreg stacks after the coating and curing in the two fifth steps, transferring to a hot press, heating and pressurizing to perform interlayer matrix curing treatment, wherein the curing temperature is 120 DEGoAnd C, the pressure is 4Mpa, the time is 1h, and finally the composite material laminated plate with improved interlayer toughness is obtained.
2. The method for preparing an interlayer toughened composite material as claimed in claim 1, wherein in said first step, the capsule core is selected from bisphenol a diglycidyl ether, (3-mercaptopropionic acid) pentaerythritol ester, (dimethylaminomethyl) phenol, and the capsule wall is selected from urea formaldehyde.
3. The method of claim 1, wherein in step two, the carbon fiber is selected from commercial T300.
4. The method for preparing an interlaminar toughened composite material as claimed in claim 1, wherein in the third step, the ply-bonding direction of the prepreg is a single direction.
5. The method of claim 1, wherein the interlayer toughening composite is prepared byCharacterized in that in the third step and the sixth step, the curing temperature is 120 DEGoC, the pressure is 4Mpa, and the time is 1 h.
6. The method for preparing an interlaminar toughened composite material according to claim 1, wherein in the sixth step, the two laminated prepreg stacks are coated with the resin glue solution of the capsules.
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JPH10176126A (en) * | 1996-12-18 | 1998-06-30 | Matsui Shikiso Kagaku Kogyosho:Kk | Water-based composition for coating building material and building material coated therewith |
JP2005205666A (en) * | 2004-01-21 | 2005-08-04 | Kubota Corp | Laminated cylindrical body excellent in heat insulating properties and thermal deformation resistance and plunger sleeve for die casting machine |
CN101215407A (en) * | 2008-01-18 | 2008-07-09 | 中山大学 | High temperature self-restoring fibre enhancement epoxy composite material and preparation method thereof |
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